MNL46 - Metallographic and Materialographic Specimen Preparation, Light Microscopy, Image Analysis and Hardness Testing 2007

Metallographic and
Materialographic Specimen
Preparation, Light Microscopy,
Image Analysis and Hardness
Testing
Kay Geels
In collaboration with Daniel B. Fowler,
Wolf-Ulrich Kopp, and Michael Rückert
ASTM International
100 Barr Harbor Drive
PO Box C700
West Conshohocken, PA 19428-2959
Printed in U.S.A.
ASTM Stock No. MNL46
Library of Congress Cataloging-in-Publication Data
Metallographic and materialographic specimen preparation, light microscopy,
image analysis and hardness testing
Kay Geels; in collaboration with Daniel B. Fowler, Wolf-Ulrich Kopp, and Michael
Rückert
p. cm.—共Manual; 46兲
ASTM stock number: MNL 46.
Includes bibliographical references.
ISBN 978-0-8031-4265-7
E-book ISBN 978-0-8031-5691-3
1. Metallography. 2. Metallographic specimens. I. Title.
TN690.G3785 2006
669⬘.95028—dc22 2006103391
Copyright © 2007 ASTM International, West Conshohocken, PA. All rights reserved.
This material may not be reproduced or copied, in whole or in part, in any printed,
mechanical, electronic, film, or other distribution and storage media, without the
written consent of the publisher.
Photocopy Rights
Authorization to photocopy item for internal, personal, or
educational classroom use, or the internal, personal, or educational classroom
use of specific clients, is granted by ASTM International „ASTM… provided that
the appropriate fee is paid to the Copyright Clearance Center, 222 Rosewood
Drive, Danvers, MA 01923; Tel: 978-750-8400; online: http://
www.copyright.com/.
The Society is not responsible, as a body, for the statements and opinions expressed
in this publication.
ASTM International does not endorse any products represented in this publication.
Printed in City, State

Month Year
iii
Preface
This book is written both for the experienced and unexperienced metallographer 共ma-
terialographer兲 who wants specific advice and information. It is also for persons seek-
ing a broader knowledge of metallographic/materialographic specimen preparation
and the examination methods, light microscopy, image analysis, and hardness testing.
Special emphasis has been made on relations between ASTM standards and
metallography/materialography.
The book will be useful for students in courses devoted to practical metallography
and materialography.
The scope of the book is to give relevant information, in an efficient and clear way,
covering the daily work in a metallographic/materialographic laboratory.
Metallographic/Materialographic Preparation
Kay Geels and Michael Rückert 共Sections 13.5/6兲
Part I is a description of sectioning, mounting, grinding, polishing, and etching of
specimens for examination in reflected light, enabling the reader to understand the
mechanisms of the entire preparation process. This is combined with practical advice
on specimen preparation and an introduction to existing equipment and consumables.
Part II is a “Hands-on” Manual guiding the metallographer/materialographer to
the correct preparation method, based on the material to be prepared and the purpose
of examination. More than 150 methods are indicated covering practically all types of
materials, describing the preparation process from sectioning to etching. This part
also includes a section on Trouble Shooting, covering all stages in the preparation pro-
cess and artifacts developed during the preparation.
Light Microscopy
Wolf-Ulrich Kopp
Part III is a description of the optical reflected-light microscope with photomicroscopy
giving the reader both an introduction to the subject and a manual for the daily work.
Also, a short introduction to electron microscopy and scanning probe microscopy can
be found in this part of the book.
Quantitative Metallography/Materialography—Automatic
Image Analysis
Daniel B. Fowler
Part IV gives an introduction to quantitative microstructural analysis and automatic
image analysis, both theoretically and practically, with emphasis on the examinations
based on ASTM standards and other types of commonly used analyses.
iv
Hardness Testing
Wolf-Ulrich Kopp
Part V gives a description of the hardness testing methods, Brinell, Vickers, Rockwell,
microhardness and instrumented 共nano兲 indentation testing based on ASTM stan-
dards, both theoretically and as a practical guide.
The Metallographic/Materialographic Laboratory

Kay Geels
Part VI gives directions on how to establish and maintain a modern metallographic/
materialographic laboratory. The important rules and regulations covering occupa-
tional safety are described and commented on.
The authors of this book, representing more than 100 years’ experience with prac-
tical metallography and materialography, have tried to make this book a practical tool
and helpful source of information to all who are involved in the noble art/science of
metallography/materialography—Kay Geels.
Acknowledgments
The authors wish to acknowledge the four reviewers, who brought forward valuable
insight for improvement. Special thanks to R. C. Nester, for his advice and suggestions
on extension and shortening of the chapters. Thanks to G. Petzow, F. Mücklich and L.
E. Samuels for permission to use a number of illustrations, and to B. Ottesen and W.
Taylor for reading the manuscript and giving good advice. A special acknowledgement
goes to fellow-metallographers/materialographers for support and advice through the
years and directly connected to the book. The list includes U. Täffner, S. Glancy, E.
Weidmann, A. Z. Jensen and A. Guesnier. A special thanks to L. Bjerregaard for her very
important advice on many of the preparation methods, and to H. Hellestad for her in-
valuable support in making the illustrations. Also, thanks go to W. Taylor and Struers
GmbH for providing important micrographs. The authors acknowledge the following
companies for supply of information and illustrations, Buehler Ltd., Carl Zeiss AG,
DoAll Company, Emco-Test GmbH, Leica Microsystems AG, Olympus Optical Co. Inc.,
and Struers A/S. Particular thanks to G. E. Totten and K. Dernoga at ASTM Interna-
tional for establishing and maintaining the project of making this book. Last but not
least, thanks to B. Freiberg and J. Hestehave for support and encouragement during
the years of making the book.
Abbreviations
AFM Atomic Force Microscope

BF Bright Field
CBN Cubic Boron Nitride
DF Dark Field
DIC Differential Interference Contrast
v
EBSD Electron Backscatter Diffraction

EDS Energy Dispersive Spectroscopy
EPMA Electron Probe Microanalyzer
FIB Focused Ion Beam
MFM Magnetic Force Microscope
PCB Printed Circuit Board
POL Polarized Light
SEM Scanning Electron Microscope
SPM Scanning Probe Microscope
STM Scanning Tunnel Microscope
STEM Scanning Transmission Electron Microscope
TEM Transmission Electron Microscope
Contents
Part I: The Metallographic/Materialographic Preparation Process
1 Introduction
1.1 Metallographic/Materialographic Preparation—The True
Microstucture. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
1.1.1 Henry Clifton Sorby 共1826–1908兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
1.2 The True Microstructure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
1.3 Selection of Preparation Method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
1.3.1 Artifacts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
1.3.2 Preparation Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
1.4 The Metallographic/Materialographic Specimen. . . . . . . . . . . . . . . . . . . 7
1.4.1 “Specimen” or “Sample”. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
1.5 The Preparation Process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
1.5.1 Sectioning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
1.5.2 Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
1.5.3 Preparation of the Surface. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
1.5.4 Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
2 Sectioning
2.1 Selection. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.1.1 General Studies or Routine Work. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.1.2 Study of Failures. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.1.3 Research Studies. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.1.4 Type of Section. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.1.5 Reporting of Locations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.2 Sectioning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.3 Wet Abrasive Cutting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.3.1 The Cut-off Grinding Process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.3.2 The Cut-off Wheel—Abrasives and Bond Materials. . . . . . . . . . . . . . . . 16
2.3.3 Grinding Mechanics. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
2.3.4 Mechanical Damage. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
2.3.5 Thermal Damage. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
2.3.6 Cut-off Wheel Wear. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
2.3.7 Cutting Fluids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
2.3.8 The Metallographic/Materialographic Cutting Operation. . . . . . . . . . . 29
2.4 Abrasive Cut-Off Wheels. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
2.4.1 Consumable Wheels. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
2.4.2 Slow Consumable Wheels. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
2.5 Abrasive Cut-off Machines. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
2.5.1 Design Principles of Wheel—Work Piece Contact. . . . . . . . . . . . . . . . . . 36
2.5.2 Machine Designs. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
2.6 Advice and Hints on Wet Abrasive Cutting. . . . . . . . . . . . . . . . . . . . . . . . 43
2.6.1 Cut-off Wheel Selection. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
2.7 Other Sectioning Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
2.7.1 Fracturing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
2.7.2 Sectioning by Melting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
2.7.3 Shearing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
2.7.4 Sawing—Table 2.1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
2.7.5 Wire Cutting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
3 Mounting
3.1 Purpose and Criteria. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
3.1.1 Purpose. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
3.1.2 Criteria for a Good Mount. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
vii
viii Metallographic and Materialographic Specimen Preparation
3.1.3 Surface Flatness—Edge Retention. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

3.2 Mounting Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
3.2.1 Clamping. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
3.2.2 Hot Compression Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
3.2.3 Cold 共Castable兲 Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
3.3 Hot Compression Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
3.3.1 Advantages of Hot Compression Mounting. . . . . . . . . . . . . . . . . . . . . . . 59
3.3.2 Disadvantages of Hot Compression Mounting. . . . . . . . . . . . . . . . . . . . . 59
3.3.3 MSDS 共Material Safety Data Sheets兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
3.4 Hot Mounting Resins. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
3.4.1 Thermoplastic Resins. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
3.4.2 Thermosetting Resins. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
3.5 Mounting Presses. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
3.5.1 The Heating/Cooling Unit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
3.5.2 The Hydraulic Press. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
3.5.3 The Air-operated Press. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
3.6 Advice and Hints on Hot Compression Mounting. . . . . . . . . . . . . . . . . . 65
3.6.1 Selection of Resins for Hot Compression Mounting. . . . . . . . . . . . . . . . 66
3.7 Cold 共Castable兲 Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
3.7.1 Advantages of Cold 共Castable兲 Mounting. . . . . . . . . . . . . . . . . . . . . . . . . 68
3.7.2 Disadvantages of Cold 共Castable兲 Mounting. . . . . . . . . . . . . . . . . . . . . . . 68
3.7.3 MSDS 共Material Safety Data Sheets兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
3.8 Cold Mounting Resins. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
3.8.1 Acrylics. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
3.8.2 Polyesters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
3.8.3 Epoxies. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
3.9 Accessories for Cold 共Castable兲 Mounting. . . . . . . . . . . . . . . . . . . . . . . . . 70
3.9.1 Mounting Molds. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
3.9.2 Clips. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71
3.10 Vacuum Impregnation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71
3.10.1 Dyes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
3.11 Special Mounting Techniques. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
3.11.1 Taper Sectioning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
3.11.2 Edge Protection. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
3.11.3 Mounting of Very Small Parts, Foils, and Wires. . . . . . . . . . . . . . . . . . . . 75
3.11.4 Mounting of Powders. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76
3.11.5 Mounting of PCB Coupons. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76
3.11.6 Conductive Mounts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
3.12 Recovery of Mounted Specimen. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
3.13 Advice and Hints on Cold Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78
3.13.1 Selection of Cold Mounting Materials. . . . . . . . . . . . . . . . . . . . . . . . . . . . 79
4 Marking—Storage—Preservation
4.1 Marking. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
4.1.1 Marking with Waterproof Ink. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
4.1.2 Identification Tag. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
4.1.3 Engraving. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
4.1.4 Stamping. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
4.2 Storage. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81
4.3 Preservation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81
ix
5 Cleaning and Cleanliness

5.1 Cleaning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82
5.1.1 Cleaning Before Start of Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82
5.1.2 Cleaning During and After Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . 82
5.2 Cleanliness. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 84
6 Mechanical Surface Preparation—Grinding
6.1 Grinding—A Basic Process. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
6.1.1 Plane Grinding 共PG兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
6.1.2 Fine Grinding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
6.2 Material Removal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
6.2.1 Rake Angle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87
6.2.2 Grain Shape—Contacting Points. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88
6.2.3 Grain Penetration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
6.2.4 Force on Specimens. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
6.2.5 Grinding/Polishing Fluids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
6.3 Deformation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
6.3.1 Metals. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
6.3.2 Brittle Materials—Ceramics. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
6.4 Grinding Abrasives. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
6.4.1 Aluminum Oxide. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
6.4.2 Silicon Carbide. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
6.4.3 Diamond—Diamond Products. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
6.4.4 Cubic Boron Nitride 共CBN兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.4.5 Boron Carbide. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.4.6 Hardness of Abrasives and Materials—Table 6.1. . . . . . . . . . . . . . . . . . . 97
6.5 Grinding/Polishing Fluids—Lubricants. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.5.1 Water-Based Lubricant. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.5.2 Alcohol-Based Lubricant. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
6.5.3 Water-oil Based Lubricant. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
6.5.4 Oil-Based Lubricant. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
6.6 Traditional Grinding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
6.6.1 Grinding Stones/Disks. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
6.6.2 SiC Wet Grinding Paper—Table 6.2. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100
6.6.3 Alumina—Zirconia Alumina Wet Grinding Paper. . . . . . . . . . . . . . . . . . 105
6.7 Contemporary Grinding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106
6.7.1 Magnetic Fixation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106
6.7.2 Resin-Bonded Diamond Grinding Disks. . . . . . . . . . . . . . . . . . . . . . . . . . . 107
6.7.3 Resin-Bonded SiC Grinding Disks. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 108
6.7.4 Metal-Bonded Diamond-Coated Disks. . . . . . . . . . . . . . . . . . . . . . . . . . . . 109
6.7.5 Diamond Pads. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109
6.7.6 Diamond/CBN/ Al2 O3 /SiC Film. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109
6.7.7 Rigid Composite Disks. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109
6.7.8 Fine Grinding Cloths. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 116
6.8 Grinding/Polishing Equipment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
6.8.1 Plane Grinding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
6.8.2 Fine Grinding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
7 Mechanical Surface Preparation—Polishing
7.1 Polishing: Producing the True Structure. . . . . . . . . . . . . . . . . . . . . . . . . . . 120
7.1.1 Rough Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120
7.1.2 Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120
x Metallographic and Materialographic Specimen Preparation
7.2 Material Removal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120

7.2.1 Influence of Polishing Abrasive on Removal Rate. . . . . . . . . . . . . . . . . . 121
7.3 Deformation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122
7.3.1 The Beilby Layer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122
7.3.2 Influence of Polishing Abrasive, Cloth, and Fluid on Deformation... 123
7.4 Polishing Cloths. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 124
7.4.1 Edge Retention—Relief. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 126
7.4.2 Cloths for Fine Grinding and Rough Polishing. . . . . . . . . . . . . . . . . . . . . 126
7.4.3 Cloths for Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 127
7.5 Polishing Abrasives. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 129
7.5.1 Diamond Suspensions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 129
7.5.2 Diamond Spray. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 129
7.5.3 Diamond Paste. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 130
7.5.4 Alumina. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 130
7.5.5 Silica. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131
7.5.6 Other Oxides. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 132
7.6 Polishing Lubricants. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 132
7.7 The Metallographic/Materialographic Preparation Methods—
Method Parameters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 132
7.7.1 RPM of Grinding/Polishing Disk. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 133
7.7.2 RPM of Specimen Holder. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 133
7.7.3 Direction of Specimen Holder. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 134
7.7.5 Process Time. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 134
7.7.6 Stock Removal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 134
7.8 Grinding/Polishing Equipment—Manual Preparation. . . . . . . . . . . . . . . 135
7.9 Grinding/Polishing Equipment—Automatic Preparation. . . . . . . . . . . . 135
7.9.1 Machine Design. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 135
7.9.2 Polishing Dynamics. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 139
7.9.3 Semiautomatic and Fully Automatic Systems. . . . . . . . . . . . . . . . . . . . . . 140
7.10 Special Preparation Techniques. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143
7.10.1 PCB Coupons. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143
7.10.2 Microelectronic Materials—Nonencapsulated Cross Sections. . . . . . . . 143
7.10.3 Microelectronic Packages—Table 7.2—Target Preparation. . . . . . . . . . 147
7.10.4 EBSD. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 149
7.11 Field Metallography/Materialography—Nondestructive Mechanical
Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 150
7.11.1 Portable Grinder/Polishers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 150
7.11.2 Replication. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 150
7.12 Chemical Mechanical Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151
7.12.1 Protection—Corrosion at CMP. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 152
7.13 Thin Sections. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 152
7.13.1 Thin Sections of Petrographic/Ceramic Materials. . . . . . . . . . . . . . . . . . . 152
7.13.2 Thin Sections of Plastics/Polymers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153
7.14 Microtomy—Ultramilling. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 155
8 Electrolytic Polishing/Etching
8.1 The Electrolytic Polishing/Etching Process. . . . . . . . . . . . . . . . . . . . . . . . . 156
8.1.1 The Polishing Cell. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 157
8.1.2 Smoothing and Brightening. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 157
xi
8.1.3 Electrolytic Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159

8.1.4 Advantages and Disadvantages. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160
8.2 Electrolytes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 163
8.3 Electropolishing in Practice. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 164
8.3.1 Factors Influencing Electrolytic Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . 164
8.3.2 Example of Electrolytic Polishing/Etching. . . . . . . . . . . . . . . . . . . . . . . . . . 165
8.4 Electrolytic Polishing Equipment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165
8.4.1 Electropolishers for Laboratory Use. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 165
8.5 Field Metallography—Nondestructive Electropolishing. . . . . . . . . . . . . 166
8.6 Electrolytic Thinning for TEM. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 167
8.7 Chemical Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 168
9 Etching
9.1 Microetching—Contrast. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
9.2 Contrast Without Surface Modifications—Microscope Techniques... 169
9.2.1 Dark-Field Illumination 共DF兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
9.2.2 Differential Interference Contrast 共DIC兲. . . . . . . . . . . . . . . . . . . . . . . . . . . 169
9.2.3 Polarized Light 共POL兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 169
9.2.4 Fluorescence. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170
9.3 Contrast with Surface Modification—Etching. . . . . . . . . . . . . . . . . . . . . . 170
9.3.1 Grain Contrast Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170
9.3.2 Grain Boundary Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 171
9.3.3 Reproducibility. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 171
9.3.4 Safety Precautions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.4 Classical Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.4.1 Chemical Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.4.2 Precipitation 共Color兲 Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.4.3 Heat Tinting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.5 Electrolytic Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.5.1 Anodic Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 172
9.5.2 Anodizing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
9.5.3 Potentiostatic Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
9.6 Physical Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
9.6.1 Relief Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
9.6.2 Ion Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 173
9.6.3 Thermal Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174
9.6.4 Vapor Deposition. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174
9.6.5 Sputtering. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174
9.7 Macroetching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174
Part II: Metallographic/Materialographic Specimen Preparation—A Hands-On

Manual
10 Introduction
10.1 Specimen Material. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 179
10.2 Purpose of Examination. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 179
10.3 Specimen Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 179
11 Specimen Material—Table 11.1
11.1 Classification of Materials. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181
11.2 How to Use Table 11.1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 181
11.3 Table 11.1—Materials/Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 182
xii Metallographic and Materialographic Specimen Preparation
12 Purpose of Examination
12.1 Purpose in General. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 188
12.2 Purpose: ASTM Standards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 188
12.3 Table 12.1: Purpose/ASTM Standards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 188
12.4 ASTM Standards—Metallography. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 188
12.4.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 188
12.4.2 ASTM Standards in this Book. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 190
12.4.3 ASTM Standards—Document Summaries. . . . . . . . . . . . . . . . . . . . . . . . . . 193
12.5 Chemical Microetching—Table 12.2—Table 12.3. . . . . . . . . . . . . . . . . . . 194
12.5.1 Etching Practice. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 194
12.5.2 Table 12.2—Numerical List of Etchants. . . . . . . . . . . . . . . . . . . . . . . . . . . . 195
12.5.3 Table 12.3—Etchant Names. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 217
13 Specimen Preparation
13.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 218
13.2 Mechanical Preparation—The “Traditional” and “Contemporary”
Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 218
13.2.1 Material/Preparation Tables. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 218
13.2.2 Method Tables—Generic Methods—Parameters/Consumables—
Table 13.1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 219
13.2.3 Material/Preparation Tables—Methods C-01/T-01 to C-68/T-68. . . . . . . 222
13.2.4 Manual Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 450
13.3 Electrolytic Polishing and Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 453
13.3.1 Electropolishers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 454
13.3.2 Electrolytes—Methods for Electropolishing—Table 13.2. . . . . . . . . . . . 454
13.3.3 Table 13.2—Electrolytes for Electropolishing/Etching. . . . . . . . . . . . . . . 454
13.3.4 Mechanical Preparation for Electropolishing. . . . . . . . . . . . . . . . . . . . . . 456
13.3.5 Electropolishing—Method Tables. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 456
13.3.6 Electropolishing—Methods El-01 To El-25. . . . . . . . . . . . . . . . . . . . . . . . . 456
13.4 Field Metallography/Materialography—Nondestructive
Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 475
13.4.1 Mechanical Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 475
13.4.2 Electrolytic Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 475
13.4.3 Replication. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 475
13.5 Trouble Shooting—How to Improve Preparation Results. . . . . . . . . . . 476
13.5.1 Sectioning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 477
13.5.2 Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 479
13.5.4 Electrolytic Polishing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 483
13.5.5 General Rules—“The Metallographer’s Rule of Thumb”. . . . . . . . . . . . 483
13.6 Trouble Shooting—How to Overcome Preparation Artifacts. . . . . . . . 484
13.6.1 Preparation Artifacts—Flow Charts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 484
13.6.2 Sectioning—General Problems—Flow Charts. . . . . . . . . . . . . . . . . . . . . . 485
13.6.3 Mounting—General Problems—Artifacts. . . . . . . . . . . . . . . . . . . . . . . . . . 495
13.6.4 Grinding and Mechanical Polishing—Flow Charts. . . . . . . . . . . . . . . . . . 498
13.6.5 Electropolishing—General Problems—Artifacts. . . . . . . . . . . . . . . . . . . . 521
Part III: Light Microscopy

14 Introduction
14.1 Visible Light–Table 14.1–Table 14.2. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 525
14.2 The Human Eye. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 526
xiii
14.3 Magnifying Lens and Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 527

14.4 Magnification. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 527
15 The Optical Reflected Light Microscope
15.1 The Path of Light Rays. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 528
15.2 The Objective. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 528
15.2.1 Numerical Aperture—Resolution-Magnification–Table 15.1–Table
15.2. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 528
15.2.2 Aberrations in Image-Formation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 532
15.2.3 Available Objectives. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 533
15.3 Eyepieces. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 535
15.4 Illumination. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 536
15.4.1 Koehler’s Illumination System. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 536
15.5 Microscope Options. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 537
15.6 The Reflected-Light Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 538
15.6.1 Upright Type of Reflected-Light Microscope. . . . . . . . . . . . . . . . . . . . . . . 538
15.6.2 Inverted Type of Reflected-Light Microscope. . . . . . . . . . . . . . . . . . . . . . 538
15.7 Optical Examination Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 540
15.7.1 Bright-Field 共BF兲 Illumination. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 541
15.7.2 Dark-Field 共DF兲 Illumination. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 541
15.7.3 Polarization Contrasting 共POL兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 542
15.7.4 Differential Interference Contrasting 共DIC兲. . . . . . . . . . . . . . . . . . . . . . . . 544
15.7.5 Fluorescence in Reflected Light. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 545
15.8 Practical Use of the Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 546
15.8.1 Setting up the Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 546
15.8.2 Working with the Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 547
15.8.3 Correct Adjustment of the Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . 548
15.8.4 Focusing and Practical Use. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548
15.8.5 Measurements of Length. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 549
15.8.6 Measurements of Height Differences. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 550
15.8.7 Maintenance of the Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 550
15.9 Documentation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 550
15.10 The Confocal Laser Scan Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 552
15.10.1 Function of Confocal Laser Scan Microscope. . . . . . . . . . . . . . . . . . . . . . 552
15.10.2 Applications of Confocal Laser Scan Microscope. . . . . . . . . . . . . . . . . . . 554
15.11 Stereo Microscopy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 555
16 Electron Microscopy—Scanning Probe Microscopy
16.1 The Transmission Electron Microscope 共TEM兲. . . . . . . . . . . . . . . . . . . . . . 558
16.1.1 The Scanning Transmission Electron Microscope 共STEM兲. . . . . . . . . . . . 558
16.2 The Scanning Electron Microscope 共SEM兲. . . . . . . . . . . . . . . . . . . . . . . . . . 558
16.2.1 Energy Dispersive Spectroscopy 共EDS兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 559
16.2.2 Electron Backscatter Diffraction 共EBSD兲. . . . . . . . . . . . . . . . . . . . . . . . . . . 559
16.2.3 The Electron Probe Microanalyzer 共EPMA兲. . . . . . . . . . . . . . . . . . . . . . . . 560
16.3 Focused Ion Beam 共FIB兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 560
16.4 Scanning Probe Microscopes 共SPM兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 560
Part IV: Quantitative Metallography/Materialography— Automatic Image Analysis

17 Quantitative Metallography/Materialography—An Introduction
17.1 Quantitative Metallography/Materialography. . . . . . . . . . . . . . . . . . . . . 565
17.1.1 Stereology–Table 17.1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 565
xiv Metallographic and Materialographic Specimen Preparation
17.1.2 Specimen Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 567

17.1.3 Calibration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 568
17.1.4 Field Selection—Bias. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 568
17.2 Volume Fraction—Point Count. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 569
17.2.1 ASTM Test Method for Determining Volume Fraction by
Systematic Manual Point Count 共E 562兲. . . . . . . . . . . . . . . . . . . . . . . . . . . 569
17.3 Inclusion Rating. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 570
17.3.1 ASTM Standard Test Method For Determining the Inclusion
Content of Steel 共E 45兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 570
17.3.2 ASTM Practice for Obtaining JK Inclusion Ratings Using Automatic
Image Analysis 共E 1122兲共withdrawn 2006, replaced by E 45兲. . . . . . . 570
17.3.3 ASTM Practice for Determining the Inclusion or Second-Phase
Constituent Content of Metals by Automatic Image Analysis
共E 1245兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 570
17.4 Grain Size. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 571
17.4.1 ASTM Test Methods for Determining Average Grain Size 共E 112兲. . . 571
17.4.2 ASTM Test Methods for Estimating the Largest Grain Observed in
a Metallographic Section 共ALA Grain Size兲共E 930兲. . . . . . . . . . . . . . . . . 573
17.4.3 ASTM Test Methods for Characterizing Duplex Grain Sizes 共E 1181兲.. 573
17.4.4 ASTM Test Methods for Determining Average Grain Size Using
Semiautomatic and Automatic Image Analysis 共E 1382兲. . . . . . . . . . . . 573
17.5 Banding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 574
17.5.1 ASTM Practice for Assessing the Degree of Banding or Orientation
of Microstructures 共E 1268兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 574
17.6 Porosity in Thermal Spray Coatings. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 574
17.6.1 ASTM Test Methods for Determining Area Percentage Porosity in
Thermal Sprayed Coatings 共E 2109兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 574
17.7 Decarburization—Case Depth—Coatings. . . . . . . . . . . . . . . . . . . . . . . . . . 575
17.7.2 ASTM Test Methods for Estimating the Depth of Decarburization
of Steel Specimens 共E 1077兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 575
17.7.3 Case Depth. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 575
17.7.4 ASTM Test Method for Measurement of Metal and Oxide Coating
Thickness by Microscopical Examination of a Cross Section 共B 487兲.. 576
17.7.5 ASTM Test Methods for Thickness of Diffusion Coating 共C 664兲. . . . . 576
17.8 Other ASTM Standards for Quantitative Materialography. . . . . . . . . . 576
18 Automatic Image Analysis
18.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 577
18.2 Qualitative and Quantitative Metallography/Materialography. . . . . . 577
18.2.1 The Transition to Quantitative Standards. . . . . . . . . . . . . . . . . . . . . . . . . 577
18.2.2 Structure, Stereology, and Statistics. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 578
18.3 Principles of Digital Imaging. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 579
18.3.1 What is Digital Image Analysis?. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 579
18.3.2 Image Acquisition. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 579
18.3.3 Image Digitization—Gray Scale. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 580
18.3.4 The Histogram. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 581
18.3.5 The Effects of Brightness and Contrast on Illumination
Distribution. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 581
18.3.6 Image Processing and True Microstructure. . . . . . . . . . . . . . . . . . . . . . . . 586
18.3.7 Image Calibration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 595
xv
18.4 Image Measurement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 598

18.4.1 Manual Measurements 共Operator Defines Points, Lines, or Areas兲... 599
18.4.2 Automatic Measurements 共Objects Defined by Image
Segmentation兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 600
18.5 Digital Imaging Applied to Quantitative Materialography. . . . . . . . . . 602
18.5.1 Percent Area 共Volume Fraction兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 602
18.5.2 Inclusion Rating. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 603
18.5.3 Grain Size. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 606
18.5.4 Degree of Banding. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 608
18.5.5 Depth or Thickness Measurements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 608
18.5.6 Graphite in Iron Castings. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 610
18.6 Digital Imaging Technology. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 613
18.6.1 Hardware. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 613
18.6.2 Software. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 616
18.7 Digital Imaging System Implementation. . . . . . . . . . . . . . . . . . . . . . . . . . 617
19 Digital Image Management „Archiving…
Part V: Hardness Testing

20 Introduction
20.1 Indentation Hardness. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 623
20.2 ASTM Standards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 625
21 Static Hardness Testing Procedures
21.1 Brinell Hardness Testing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 626
21.1.1 Calculations and Procedures. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 626
21.1.2 Brinell Hardness Testers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 628
21.2 Vickers Hardness Testers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 628
21.2.2 Vickers Hardness Tester. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 632
21.3 Knoop Hardness Testing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 633
21.4 Rockwell Hardness Testing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 634
21.4.2 Rockwell Hardness Testers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 636
21.5 Microindentation Hardness. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 636
21.5.1 Methods. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 636
21.5.3 Taking the Measurements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 638
21.5.4 Microindentation Hardness Testers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 639
21.5.5 Examples of Indentations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 639
21.6 Universal Hardness—Martens Hardness—Instrumented Indentation
Testing—Nano Indentation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 639
21.6.1 Instrumented Indentation Testing—Nano Indentation. . . . . . . . . . . . . 641
21.7 Precision of Hardness Values. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 642
21.8 Conversion of Hardness Values. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 642
22 Dynamic Hardness Testing Procedures
23 Special Methods for Hardness Testing
xvi Metallographic and Materialographic Specimen Preparation
Part VI: The Metallographic/Materialographic Laboratory

24 Introduction
24.1 Establishing a Metallographic/Materialographic Laboratory. . . . . . . . 649
24.2 Running a Metallographic/Materialographic Laboratory. . . . . . . . . . . . 649
24.3 Occupational Safety and Health. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 649
25 How to Build a Metallographic/Materialographic Laboratory
25.1 Purpose. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 650
25.1.1 Quality Control 共QC兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 650
25.1.2 Research and Education. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 651
25.1.3 Testing and Inspection Laboratories—Failure Analysis. . . . . . . . . . . . . . 651
25.2 Rationalization and Automation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 651
25.2.1 Reproducibility—Standards—Occupational Safety. . . . . . . . . . . . . . . . . . 652
25.2.2 Productivity—Cost Per Specimen. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 653
25.3 Planning the Metallographic/Materialographic Laboratory. . . . . . . . . 654
25.3.1 Basic Planning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 654
25.3.2 Detailed Planning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 655
25.4 Equipment and Laboratory Layout. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 656
25.4.1 Equipment—Table 25.1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 656
25.4.2 Layout—Furniture—Installations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 660
25.5 Maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 662
25.5.1 Organizing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 662
25.5.2 Cleaning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 662
25.5.3 Servicing. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 663
26 Occupational Safety and Health in the Metallographic/
Materialographic Laboratory
26.1 Dangers in the Metallographic/Materialographic Laboratory. . . . . . . 664
26.1.1 Sectioning. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 664
26.1.2 Mounting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 664
26.1.4 Electrolytic Polishing/Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 665
26.1.5 Etching—Etchants—Electrolytes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 665
26.1.6 Dust. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 667
26.1.7 Cold 共Castable兲 Mounting Resins. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 667
26.1.8 Standard Guide on Metallographic Laboratory Safety 共E 2014兲. . . . . 668
26.2 Safety Information. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 668
26.2.1 Identification. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 668
26.2.2 Material Safety Data Sheet 共MSDS兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 670
26.2.3 Standard Operating Procedure 共SOP兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 672
26.2.4 Job Safety Analysis 共JSA兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 672
26.3 Disposal of Chemicals. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 672
26.4 Occupational Safety in General. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 673
26.4.1 Standards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 673
26.4.2 Training. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 673
26.4.3 Maintenance and Service. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 673
26.5 Standards and Regulations—Organizations. . . . . . . . . . . . . . . . . . . . . . . 673
26.5.1 Designations and Abbreviations Used to Describe a Chemical
Substance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 673
26.5.2 ASTM Standard. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 674
26.5.3 OSHA—OSHA Standards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 674
xvii
26.5.4 National Institute for Occupational Safety and Health 共NIOSH兲. . . . . 681
26.5.5 International Chemical Safety Cards 共ICSCS兲. . . . . . . . . . . . . . . . . . . . . . . 682
26.5.6 Environmental Protection Agency 共EPA兲. . . . . . . . . . . . . . . . . . . . . . . . . . 683
26.5.7 National Technical Information Service 共NTIS兲. . . . . . . . . . . . . . . . . . . . . 683
26.5.8 American Conference of Government Industrial Hygienists
共ACGIH兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 683
26.5.9 National Toxicology Program 共NTP兲. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 683
26.5.10 Agency for Toxic Substance and Disease Registry 共ATSDR兲. . . . . . . . . . 683
26.5.11 National Fire Protection Association 共NFPA兲. . . . . . . . . . . . . . . . . . . . . . . 684
26.5.12 National Paint and Coatings Association 共NPCA兲—HMIS. . . . . . . . . . . . 684
26.5.13 BSI—ISO. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 684
26.5.14 EU. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 684
26.6 Literature on Laboratory Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 684
27 Literature
27.1 Books. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 685
27.2 Periodicals. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 686
Appendixes
Appendix I: Other Standards on Metallography/Materialography . . . . . . . . . . . . . 686
Appendix II: Other Standards on Hardness Testing . . . . . . . . . . . . . . . . . . . . . . . . . . 691
Appendix III: Hardness Conversion Tables for Metals 共E140兲 . . . . . . . . . . . . . . . . . . 694
Appendix IV: SI Quick Reference Guide: International System of Units 共SI兲 . . . . 694
Glossary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 695
Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 727
Part I:
The Metallographic/Materialographic
Preparation Process
1
Introduction
“METALLOGRAPHY” or “MATERIALOGRAPHY”? IN MODERN TECHNOL-
ogy and Materials Science we are examining the microstructure of all solid materials;
therefore, materialography seems to be the correct word instead of the traditional met-
allography. In 1968, Crowther and Spanholtz1 suggested this and it now seems appro-
priate to use the word “materialography” to cover the examination of the infinite num-
ber of existing and future materials. Also, the term “metallographer” should be
changed to “materialographer.” Changes of this kind, however, take time, and therefore
the terms “metallography” and “metallographer” are used in this book, except in con-
texts where materials other than metals are discussed.
G. Petzow2 defines Materialography 共metallography兲 as “an investigative method
of materials science. It encompasses the optical examination of microstructures, and
its goal is a qualitative and quantitative description of the microstructure.”
The term materialography includes ceramography 共ceramics兲, metallography
共metals兲, plastography 共polymers兲, and mineralogy 共minerals兲, in this way covering the
microstructural examination of most materials.
Metallography/materialography includes a wide field in material investigation; it
bridges the gap between science in new and existing materials and engineering using
the materials in modern technology. Figure 1.13 shows how materialography covers
the examination of parts from the centimetre and metre 共in and ft兲 range to atomic
dimensions in the nm and sub nm range.
The microstructure is characterized through size, shape, arrangement, amount,
type, and orientation of the phases and the defects of these phases, as schematically
Fig. 1.1—Metallography/materialography can be described as a bridge between engineering

and science, covering the examination of the part in cm and m to the examination of the
single atom in Å.
3
4 METALLOGRAPHIC AND MATERIALOGRAPHIC SPECIMEN
Fig. 1.2—The constituents of a microstructure and the factors affecting them.
shown in Fig. 1.23. Each material contains many millions of microstructural features
per cubic centimetre and these features strongly influence many of the properties of
the material. As seen in Fig. 1.1, the microstructural features can exist in sizes of at
least ten orders of magnitude. There are many instruments today that visualize nearly
all of the features across this range.
The image we see in the typical microscope is two-dimensional, but we should not
lose sight of the fact that the constituents in a material are three dimensionally ar-
ranged.
A photomontage shows the prepared surface of a silicon nitride alloy superim-
posed on a pile of silicon nitride crystals 共see Fig. 1.3兲.3 It shows that the true size of the
crystals cannot be deduced directly from the microstructure. A statistical extrapola-
tion of the two-dimensional surface shows that approximately 80 % of the crystals are
relatively short and have an equiaxial shape. Stereological calculations, however, show
a much higher variation in crystal length. The average crystal length is larger, corre-
sponding to the three-dimensional characteristics shown in Fig. 1.3.
It can be concluded that the analysis of the microstructure plays an important role
in modern materials science and engineering, and consequently, the metallographic/
materialographic preparation. It is important to secure the true microstructure be-
cause without this the best examinations and inspired interpretations will be of no
avail.
As stated in the Preface, this book concentrates on metallographic/
materialographic preparation and the most commonly used examination methods.
For a comprehensive, in-depth coverage of metallurgy and microstructures, including
interpretation of the microstructures, ASM Handbook, Volume 9, Metallography and
Microstructures,4 is recommended.
This part of the book concentrates on the preparation of the specimen surface for
examination in the reflected-light optical microscope. This preparation can also be
used frequently for the scanning electron microscope 共SEM兲. The mechanical removal
Chapter 1 Introduction 5
Fig. 1.3—Photomontage of a microsection of silicon nitride alloy superimposed upon a pile of

silicon nitride crystallites.
of material will be described and discussed rather intensively because it is the central
process in abrasive cutting, sawing, plane/fine grinding, and polishing, as will the prob-
lems involved in obtaining the true microstructure. The machines and consumables
available will also be described and discussed.
Etching, often performed after the specimen preparation process to obtain a con-
trast to highlight or clearly reveal certain features, will be described in theory and prac-
tice.
1.1 Metallographic/Materialographic Preparation—The True

Microstructure
The goal of the metallographic/materialographic preparation is to obtain the true mi-
crostructure or “The True Structure,” meaning an undisturbed material surface, which
can be analyzed in an optical 共light兲 microscope or an SEM.
The basic problem for a metallographer preparing a specimen is that the prepara-
tion process itself modifies the specimen surface and, theoretically, a “true structure”
completely without artifacts can never be obtained. Consequently, a preparation pro-
cess should be used that creates the smallest amount of artifacts, making it possible, in
practice, to analyze a microstructure in a satisfactory way.
1.1.1 Henry Clifton Sorby „1826–1908…

In the 1860s, because he understood that to obtain a “true structure” he had to remove
the irregularities of the material surface, H. C. Sorby was able to produce what is con-
Fig. 1.4—Original specimen prepared by H. C. Sorby, 1863, Bessemer steel 0.2 % carbon. BF,
450:1. Preparation Method—Rough grinding: Emery paper from coarse to fine. Fine grinding:
“Fine grained” water-of-Ayr stone. Rough polishing: “Finest grained” crocus 共Fe2O3 used for
industrial polishing兲. Polishing: “Very best and finest washed” rouge 共Fe2O3, jeweler’s rouge兲.
sidered the first true microstructure. In 1863 he prepared a specimen of Bessemer steel
by using a preparation method with several steps, a method similar to the mechanical
preparation used today. Figure 1.45 shows the microstructure, which was prepared in
several steps, a rough polishing step and a fine polishing step.
1.2 The True Microstructure

Based on studies by Vilella and Samuels,6–8 the true structure can be defined as:
No deformation—The plastically deformed layer created by the preparation should
be removed or be negligible.
No scratches—Scratches normally indicate a surface that is not yet sufficiently pre-
pared, but small scratches might be allowed if they do not disturb the examination.
No pull-outs—Especially in brittle materials, particles can be pulled out of the sur-
face leaving cavities that can be taken for porosity.
No introduction of foreign elements—During the preparation process, abrasive
grains can be embedded in the surface.
No smearing—With certain materials, the matrix or one of the phases might smear
共flow兲, resulting in a false structure or covering of structure details, or both.
No relief or rounding of edges—Relief can develop between different constituents of
the surface, caused by different hardness or other condition. Edge retention is impor-
tant if the edge has to be examined.
1.3 Selection of Preparation Method

The preparation process will always influence the prepared surface, creating artifacts.
Artifacts are defined as false structural details introduced during the preparation.
The choice of preparation is usually between using mechanical or electrolytic pol-

ishing, but chemical and chemical-mechanical polishing are also used.
1.3.1 Artifacts
A number of artifacts are already stated above under the true structure, but a few more
can be added. Microcracks, comet tails, pitting, contamination, and lapping tracks are
all caused by the preparation process. Artifacts can also be introduced during chemical
etching of the surface. Most of these artifacts can be readily observed under the micro-
scope. In some cases, artifacts can be accepted and the metallographer can decide
whether, for example, a scratch is acceptable as it does not disturb the structural analy-
sis, or whether the specimen surface should be reprepared.
In some cases it can be very difficult to establish the true structure, e.g., a smeared
layer can cover pores. It is important that the metallographer pay attention to this pos-
sibility when analyzing a structure 共see Section 13.5兲.
Artifacts of Mechanical Polishing

With mechanical polishing, it is possible to obtain an approximate true structure when
the correct procedures are followed, even with very heterogeneous materials. Figure
1.5 shows the following most common artifacts: relief between phases caused by differ-
ence in hardness; embedded abrasive grain; inclusion protruding 共it could also be
missing兲; pull-out looking like a pore; rounding of the edge; and deformation of the
matrix.
Artifacts of Electrolytic Polishing

With electrolytic polishing, the electrolysis might create problems if more than one
phase is present in the structure. Figure 1.6 shows the most common artifacts. Relief
between phases caused by a difference in electrochemical potential: in some cases one
phase will be removed much faster than another phase, in other cases a phase might
not be electrically conductive and, as such, will not take part in the polishing process.
Inclusions might react in the same way; they will often be dug out during the process.
Pitting might develop if the electrolytic process is not controlled correctly. Also, a pro-
nounced rounding of the edge will take place because the current density is always
stronger at the edge.
1.3.2 Preparation Methods

Because most materials are heterogeneous 共or even nonconductive兲, the conclusion
must be that mechanical polishing is by far the most commonly used method. For cer-
tain materials, however, electrolytic polishing gives very good results.
Alternatives to the above-mentioned methods are chemical polishing and
chemical-mechanical polishing. Chemical polishing is not used much, although reci-
pes for polishing of a number of materials are developed. Chemical mechanical polish-
ing or attack polishing can be seen as an extension of mechanical polishing and, when
relevant, recipes will be stated in connection with the specific material.
For recipes on chemical and chemical mechanical polishing, see Refs. 2, 4, and 9.
1.4 The Metallographic/Materialographic Specimen

In practice, the total work piece normally cannot be prepared and examined. For this
reason, a small part of the work piece, the sample 共specimen兲 must be extracted. For
Fig. 1.5—Mechanical polishing: the most common artifacts shown schematically.
both specimen preparation and examination, using an optical microscope or an SEM,

the ideal specimen size is 12– 40 mm 共0.5– 1.5 in兲 square or cylindrical, with a height of
12– 30 mm 共0.5– 1.2 in兲. There are, of course, exceptions like welds, where larger speci-
mens have to be prepared.
With the specimen being only a small part of the material to be examined, if the
interpretation is to be valuable, it is very important that the specimen be representative
of the material to be studied. This usually happens by cutting out the specimen from a
correct location and in the correct direction 共see Section 2.1兲. Most ASTM standards
covering examination of a metallographic/materialographic specimen offer guidance
in selection and sectioning of specimens 共see Section 12.4兲. The preparation can be per-
formed once the specimen is established.
1.4.1 “Specimen” or “Sample”

The two words are often used indiscriminately, describing the object prepared and ex-
amined. The “sample” can be defined as the piece of material in its “raw” state, as taken
Fig. 1.6—Electrolytic polishing: the most common artifacts shown schematically.
from the original material 共work piece兲. As soon as the “sample” is treated 共prepared兲
and described, it turns into a “specimen,” and for this reason only the word “specimen”
is used in this book, except in a few cases where “sample” is the correct description.
1.5 The Preparation Process

As mentioned above, several polishing methods are available, but in the diagram, Fig.
1.7, only the two methods used for almost all preparation, mechanical and electrolytic,
are shown. The diagram gives an overview of the total process, of which each step will
be discussed further in this part of the book.
Fig. 1.7—Diagram showing the total preparation process based on mechanical and electrolytic
preparation.
1.5.1 Sectioning
To obtain a specimen, some kind of sectioning from the basic material 共work piece兲 is
necessary. If this sectioning could take place without disturbing the specimen surface,
the specimen could be examined without further work, but unfortunately all the
known sectioning methods will leave some kind of irregularities on the surface. Abra-
sive wet cutting using a precision cut-off machine is considered as a sectioning method
giving a low deformation of the specimen surface. Figure 1.8 shows a surface from a
specimen cut on a precision cutter and measured with an atomic force microscope
共AFM兲, and the irregularities of the surface are evident.
Abrasive wet cutting is the most frequently used sectioning method, but other
Fig. 1.8—Surface cut with a precision cut-off machine in a very careful way to avoid
irregularities in the cut surface. Measurements with an atomic force microscope 共AFM兲 give the
peak-to-valley value of irregularities: higher than 1000 nm 共1 ␮m兲. This shows that even with
the most gentle sectioning technique, the cut surface will have deformations which have to be
removed in the following preparation steps.
methods, such as shearing, sawing, and punching are used as well 共see Section 2.7兲.
1.5.2 Mounting
In some cases, the sample taken from the base material can be handled and treated
directly as a specimen, but often a mount must be made to secure the handling and a
satisfactory preparation. The mounting can be made by clamping the specimen be-
tween two pieces of a material compatible to the specimen material. This way of
mounting has a number of drawbacks 共see Section 3.2.1兲; therefore mounting mainly
takes place as hot compression or cold 共castable兲 mounting in a mounting plastic
共resin兲. Figure 1.9共a兲 shows three mounts made with hot mounting, giving mounts with
very precise dimensions. Figure 1.9共b兲 shows three mounts made with cold mounting;
these mounts, made in molds, are less exact than the hot mounts.
1.5.3 Preparation of the Surface

The goal of the preparation is to obtain the true microstructure or at least a microstruc-
ture in a condition that makes a satisfactory examination possible. This means that the
number of irregularities 共artifacts兲 in the surface must be kept at a minimum.
The preparation is done through a number of steps, either mechanical or electro-
lytical 共see Fig. 1.7兲.
Fig. 1.9—Mounts made with hot compression mounting 共a兲 and cold 共castable兲 mounting 共b兲.
A mechanical preparation method will normally contain a plane grinding step, one
or more fine grinding steps, and one or more polishing steps.
Electrolytic polishing usually takes place as one electrolytic step, performed on a
mechanically ground or polished surface.
Fig. 1.10—Copper unetched 共a兲 showing a bright, reflecting surface and color etched with
Klemm III45 共b兲, revealing the microstructure.
1.5.4 Etching
The prepared surface often reacts as a mirror when examined in the microscope, not
showing all phases of the microstructure. For this purpose, the surface can be etched
chemically or electrolytically or treated in other ways to discriminate between phases,
grains, grain boundaries, and other details. Figure 1.10 shows a copper specimen 共a兲 in
an unetched condition, giving very little information; and 共b兲 one that is etched, show-
ing the microstructure.
2
Sectioning
2.1 Selection
IT IS VERY IMPORTANT THAT THE SPECIMEN IS SELECTED CORRECTLY SO
that the specimen material is representative of the material to be studied. The intent or
purpose of the examination will usually dictate the location of the specimen.
With respect to the purpose of the study, metallographic examination may be di-
vided into three classifications, as stated in ASTM Practice for Preparation of Metallo-
graphic Specimens 共E 3兲共see Section 12.4兲.
2.1.1 General Studies or Routine Work

Specimens should be chosen from locations that are most likely to show the maximum
varieties within the material being studied. For example, specimens should be taken
from a casting in the zones wherein maximum segregation should occur, as well as
specimens from sections where segregation should be at a minimum. In the examina-
tion of strip or wire, test specimens should be taken from each end of the coils.
2.1.2 Study of Failures

Specimens should be taken as closely as possible to the fracture or to the initiation of
the failure. Before taking the specimens, study of the fracture surface should be com-
plete, or, at the very least, the fracture surface should be documented. In many cases,
specimens should be taken from a sound area for a comparison of structures and
properties.
2.1.3 Research Studies

The nature of the study will dictate the specimen location, orientation, etc. Sampling
usually will be more extensive than in routine examinations.
2.1.4 Type of Section

After establishing the location of the specimen to be studied, the type of section to be
examined must be decided. For a casting, a section cut perpendicular to the surface
will show the variations in structure form the outside to the interior of the casting. In
hot-worked or cold-worked metals, both transverse and longitudinal sections should
be studied. Special investigations may at times require specimens with surfaces pre-
pared parallel to the original surface of the product. In the case of wire and small
rounds, a longitudinal section through the center of the specimen proves advantageous
when studied in conjunction with the transverse section.
Cross sections or transverse sections taken perpendicular to the main axis of the
material are more suitable for revealing the following information:
• Variations in structure from center to surface
• Distribution of nonmetallic impurities across the section.
• Decarburization at the surface of a ferrous material, see ASTM Test Methods for
14
Chapter 2 Sectioning 15
Estimating the Depth of Decarburization of Steel Specimens 共E 1077兲, Section

12.4.
• Depth of surface imperfections.
• Depth of corrosion.
• Thickness of protective coatings and structure of protective coating.
Longitudinal sections taken parallel to the main axis of the material are more suit-
able for revealing the following information:
• Inclusion content of steel, see ASTM Test Methods for Determining the Inclusion
Content of Steel 共E 45兲 and other ASTM standards, Sections 12.4 and 17.2.
• Degree of plastic deformation, as shown by grain distortion.
• Presence or absence of banding in the structure, see ASTM Practice for Assessing
the Degree of Banding or Orientation of Microstructures 共E 1268兲, Sections 12.4
and 17.5.
• The quality attained with any heat treatment.
2.1.5 Reporting of Locations

The locations of surfaces examined should always be given when reporting results and
in any illustrative micrographs. A suitable method of indicating surface locations is to
make a sketch of the work piece with an indication of the location.
2.2 Sectioning
The goal is to extract the specimen to be prepared from the material to be studied 共work
piece兲. This should be done so that the specimen is representative of the work piece
material and it should be done with a minimum amount of damage to the surface that
is to be prepared.
In principle, all methods, including sawing with a hacksaw, shearing, flame cut-
ting, fracturing, etc., can be used to separate a specimen from the work piece. It is,
however, important that the surface being prepared is only influenced mechanically or
by heat to a degree that is suitable for a rational preparation that follows. This limits
the sectioning methods to wet abrasive cutting and a few other methods that will be
described in the following sections.
2.3 Wet Abrasive Cutting

Abrasive cutting is a cut-off grinding process.
2.3.1 The Cut-off Grinding Process

The cut-off grinding 共abrasive cutting兲 is a special operation following the general prin-
ciples of the machining process, grinding.
Within the spectrum of machining processes, the uniqueness of grinding is found
in its cutting tool. Grinding wheels are generally composed of two materials: abrasive
particles called grains that do the cutting and a softer bonding agent to hold the count-
less abrasive grains together in a solid mass.
During most grinding processes the surface of the work piece is treated to obtain a
given accuracy or surface finish. In cut-off grinding, a very thin grinding wheel 共nor-
mally the thickness of the wheel is 1 / 100 of the wheel diameter, or less兲 grinds its way
through a work piece. In metallographic/materialographic cutting, this is to separate a
sample suited for further preparation from the work piece. Although there isn’t a de-
mand for high accuracy, the surface quality concerning mechanical damage, thermal
damage, and planeness is important.
Cut-off wheels are made by cementing together abrasive grains with a suitable
bonding material. Each grain is a potential microscopic cutting tool. The grinding pro-
cess uses thousands of abrasive points simultaneously and millions continually.
By choosing a cut-off wheel with the correct abrasive and bond and using it on a
suitable machine, both the mechanical and thermal damage and the planeness can be
kept inside narrow limits. This will shorten and facilitate the following preparation
process.
Figure 2.1 shows the surface roughness of mild steel after cutting, after grit P220
SiC grinding paper, and after P320 grinding paper. It can be seen that the irregular
scratches from the cut-off are removed by the grinding papers, and for most materials a
grinding with grit P220 after cutting will give a satisfactory surface for further prepara-
tion; this will be discussed further below. For certain materials P320 paper can be used
as the first step after cut-off, omitting plane grinding with grit P220.
2.3.2 The Cut-off Wheel—Abrasives and Bond Materials

The cut-off wheels belong to the category of “bonded abrasive tools.” Such tools consist
of hard abrasive grains held in a weaker bonding matrix. Depending on the particular
type of bond, the space between the abrasive particles may only be partially filled, leav-
ing voids and porosity, resulting in an open bond. A dense bond is the result of com-
pletely filled spaces between the grains. Aside from abrasive and bond material, fillers
and grinding-aid material may also be added. The correct combination of abrasive and
bond is important to ensure the right cut-off process.
Every abrasive particle has a number of cutting points with each removing a tiny
chip from the work piece. Eventually the cutting edge becomes blunt and it must bear a
larger force in order to remove the chip from the work piece. The force rises until it
causes the grain to fracture and present a new, sharp edge to the work piece. In this way
the grain reduces its size until finally the cutting force 共see Section 2.3.3兲 causes it to be
completely torn out of the wheel, exposing new grains. This “self-sharpening” process
is highly controlled by the combination of abrasive material and bond material 共see
Fig. 2.2兲 that schematically shows the abrasive grains in the bond with voids 共pores兲 in
between.
Depending on how the wheel is breaking down, the wheels are defined as either
“Consumable Wheels” or “Slow Consumable Wheels” 共see Section 2.4兲.
Cut-off Wheel Specifications

The basic specification of a consumable cut-off wheel defines the following param-
eters:
1. The type of abrasive, expressed with a number and a letter 共aluminum oxide: A,
silicon carbide: S兲.
2. The size of abrasive grains, expressed with grit number 共see Section 6.6.2兲.
3. The grade 共hard/soft兲 of wheel bond expressed with a letter.
4. The wheel’s structure expressed with numbers.
5. The bond material expressed with a letter.
6. A code in numbers to express the maker’s details of manufacture.
In the following sections parameters 1–5 will be described in detail.
Fig. 2.1—共a兲 Steel after wet abrasive cutting. An abrasive grain 共arrow兲, embedded in the
surface during the cutting, can be seen, 共b兲 after grinding with grit P220 SiC paper, and 共c兲
after grinding with P320 grinding paper.
Fig. 2.2—Schematic drawing of cut-off wheel showing abrasive grains and bond material with
voids 共pores兲.
Type of Abrasive
For cut-off wheels four types of synthetic abrasives, aluminum oxide 共Al2O3兲, silicon
carbide 共SiC兲, cubic boron nitride 共CBN兲, and diamond are used 共see Table 6.1 and also
Section 6.4兲.
Al2O3—Although this is the softest of the abrasive materials, it is the abrasive used
in most cut-off wheels. This is due to the fact that Al2O3 is best suited for ferrous mate-
rials, from mild steel to high-strength materials, i.e., alloy steels. Al2O3 is not suited for
cast iron 共see SiC below兲.
Al2O3 is made synthetically in different types with varying hardness and friability,
and is used for cutting of different materials. It is used in consumable cut-off wheels.
SiC—This synthetic material is harder and tougher than Al2O3, but dulls and
glazes rapidly when used with steels. It is well suited for cutting of softer materials like
nonferrous metals, and it is also suited for cast iron. SiC is made in two varieties, black
and green; normally the black type is used in cut-off wheels. It is used in consumable
wheels.
CBN—This very hard, synthetic abrasive 共superabrasive兲 is used for cutting of
hard materials that are not to be cut with Al2O3 and SiC. CBN is rather expensive; the
price is comparable to the price of diamond, but CBN has the advantage that it cuts
ferrous materials that cannot be cut with diamond. CBN has a very high thermal stabil-
ity and will work for a very long time before getting dull and needs little dressing 共see
Section 2.3.6兲. It is used in slow consumable wheels where the wheel consists of a metal
body, and CBN is only part of the rim in a very stable bond 共see Section 2.4兲. CBN grains
tend to be blocky shaped with sharp edges and smooth faces, which makes bonding
difficult. Therefore CBN, as diamond, normally is coated before being used in a resin
bonded cut-off wheel.
Diamond—Diamond is the hardest abrasive 共see Table 6.1兲 and is used for cutting
of the hardest materials. In spite of its extreme hardness, diamond has been found to be
unsuitable for cutting ferrous materials. This is due to graphitization and carbon diffu-
sion into the iron causing excessive diamond wear.10 Diamond is found as natural dia-
monds, but mostly synthetic diamonds are used in cut-off wheels. The diamond grains
Fig. 2.3—Schematic drawing of the cut-off process. The rotating cut-off wheel is cutting into
the fixed work piece.
are normally coated to improve the fixation of the grain in the bond. Diamond is only
used in slow consumable wheels as described under CBN above 共see Section 2.4兲.
Grain Size
The grain size is expressed as a grit number 共#兲. This number refers to the number of
openings per linear inch in a mesh screen through which the grain is just able to pass.
The grit sizes are standardized by ANSI 共American兲 and FEPA 共European兲共see Table
6.2 and Section 6.6兲. For cut-off wheels, grit sizes between 50 共336 ␮m兲 and 120
共125 ␮m兲 are normally used.
Generally speaking, large grains will have a higher material removal rate, but a
rougher finish.
Large grains also allow for a more open bond structure because the pores 共voids兲
between the grains can be relatively large 共see Fig. 2.2 and Structure below兲. An open
bond structure allows room for the chips created during the cutting process so that
they can be removed without disturbing the process. For this reason cut-off wheels
with large grains, which enable an open structure with large pores, are suited for cut-
ting of large work pieces. This creates a large contact area 共arc of contact兲 between cut-
off wheel and work piece 共see l in Fig. 2.3兲. In the long contact area, chips and bond
particles will be accumulated before they are removed from the wheel outside the work
piece, and this accumulation takes place in the large pores. If not accumulated in the
pores, the chips and particles will take room in the interface between wheel and work
piece, reducing the cutting action and creating heat.
Fine grains have a lower removal rate, but a better surface finish. Fine grains will
give a relatively dense bond structure 共small pores兲, and therefore a fine-grained cut-off
wheel is most suited for brittle materials 共very small chips兲 and smaller work pieces
with a short arc of contact.
Grade
The grade expresses the degree of retaining grip exerted on each grain by the bonding
material that corresponds to the cutting force needed to dislodge the grain Figure 2.2
shows the grains bonded together with voids 共pores兲 in between. When the cutting
force has increased to a certain point, the grain will be dislodged from the bond.
Wheel grades are expressed with letters from E 共very soft兲 to X 共very hard兲. Cut-off
wheels are mostly in the range K to R.
A soft grade of bond has a weak hold in the abrasive grain Blunt grains will be torn
away easily, thus the self-sharpening action will be pronounced. This is desirable when
cutting hard materials expressed in the rule: Hard Material—Soft Wheel.
A relatively soft wheel is used if the arc of contact is very large because the long arc
will normally reduce the force per grain 共see Sections 2.3.3 and 2.3.8兲.
If the wheel is too soft for a given material it will in most cases cut very well, but the
wheel wear will be excessive causing a bad economy. In principle, the hardest possible
wheel for a given material should be used to secure the most economical sectioning.
A hard grade has a stronger hold in the abrasive grain, making it suited for softer
materials expressed in the rule: Soft Material—Hard Wheel.
A hard wheel is also used with a short arc of contact 共see Section 2.3.6兲.
A hard bond gives a longer wheel life, but if it is too hard the blunt grains may be
retained for too long, leading to a condition called glazing of the edge of the wheel. In
this condition the wheel might stop cutting completely and will only generate heat.
A wheel may be made to act harder or softer by varying the forces acting on the
grains. Decreasing the wheel speed or raising the feed speed will increase the cutting
forces. This will cause the wheel to shed grains and wear quicker so it will appear to be
acting as a softer grade of wheel. Increasing the wheel speed or reducing the feed speed
will decrease the cutting forces and the wheel will act as a harder wheel.
This can be used in cut-off machines with variable speeds 共see Sections 2.3.3 and
2.3.8兲.
Structure
The structure is a measure of the relationship between the grain size and porosity of the
bond. Wheels can be manufactured to give specific structures ranging from very dense
to very open. Structure is expressed as a numerical value between 1 and 15, 1 being very
dense and 15 very open.
The porosity, the voids deliberately built into the wheel 共see Fig. 2.2兲, are designed
to take the chips away, to avoid clogging the wheel edge 共glazing兲, and to allow grains to
cut efficiently.
A dense structure has closely spaced, relatively small grains and small pores so
that only a small amount of material is removed. An open structure with larger grains
and larger pores can cope with higher rates of material removal as described in Grain
Size above.
Bond Material
The bond material keeps the abrasive grains together. In general, the bond must be
strong enough to withstand grinding forces, high temperatures, and centrifugal force.
Consumable 共abradable兲 cut-off wheels most often have a phenolic 共bakelite兲
bond. It is produced by mixing abrasive grains with phenolic thermosetting resin and
plasticizers, molding to shape and baking 共curing兲 at 150– 200° C 共300– 400° F兲. The
bond hardness and porosity are varied by controlling the amount of plasticizer and by
adding fillers.
Phenolics are also used for cut-off wheels of the slow consumable type, using CBN
and diamond. These wheels are soft compared to the metal bonded wheels 共see below兲
and will give a smooth cut on very hard materials, but the wheel wear will be relatively
high.
Bakelite wheels are sensitive to prolonged exposure to cutting fluids. The fluid low-
ers the strength of the wheel so that it wears quicker; therefore cut-off wheels must be
kept out of the fluid when not in use and stored in a dry place.
Rubber bonds consist of vulcanized natural or synthetic rubber. They are stronger
than phenolics and are often used for extra thin cut-off wheels. Bakelite rubber bond is
a mixture giving a stronger bond than pure bakelite that allows for a thinner wheel. The
disadvantage with rubber as part of the bond is a strong smell, even with an efficient
cooling during the cutting process.
Metal bonds are used for CBN and diamond wheels. The most common metal
bond is sintered bronze that is produced by powder metallurgy methods. Other metal
bonds that are generally stronger include iron and nickel. A low-cost diamond wheel is
made with the diamond grains fixed through an electroplating process. Metal bonds
and electroplating are used for slow consumable wheels 共see Section 2.4.2兲.
2.3.3 Grinding Mechanics

Abrasive cutting is a grinding process where the material removal takes place when the
abrasive grains interact with the work piece. The mechanics of the process highly influ-
ence the result and the economy of the cut-off process; the most important parameters
will be discussed below.
Grinding forces, power, and specific energy forces are developed between the
wheel and the work piece 共see Fig. 2.3兲. The total force against the wheel, F, can be sepa-
rated into a tangential component Ft and a normal 共radial兲 component Fn.10–12
The grinding power P associated with the force components in Fig. 2.3 can be writ-
ten as:
P = Ft · v 共1兲
where Ft is the tangential force and v is the wheel velocity.
An important parameter is the energy per unit volume of material removal 共spe-
cific energy兲, u.
u = P/d · l · b 共2兲
where d is down feed rate (feed speed), l is length of cut (arc of contact), and b is width of
cut (width of wheel).
The mean force per grain Ft⬘ is another important parameter since it determines
the tendency to cause grain fracture and therefore plays a major role in relation to
wheel wear 共self sharpening兲.
Ft⬘ = u · d · l · b/v · l · b · C = 共d/v兲u/C 共3兲
where C is the number of active cutting points per square mm/in of the wheel surface.
Fig. 2.4—Schematic drawing of an abrasive grain producing a chip from a metal work piece.
It can be seen from Eq 共3兲 that the ratio 共d/v兲, feed speed, and wheel velocity plays a
major role. At a higher force per grain, Ft⬘ a given wheel should wear faster. It can be
expected that Ft⬘ in a given cut-off operation will increase until the grain fracture
strength is reached, then the worn grain will either be sharpened 共fractured兲 or forced
from the wheel 共see Section 2.3.6兲.
Chips, Sliding, and Plowing

Some of the energy used in the grinding process is used for creating chips. These very
small chips are comparable to chips made by other cutting processes such as turning
and milling. The grinding chips are irregular, probably because of the variation in abra-
sive grains and the negative rake angles 共see below and Section 6.2.1兲.
Part of the energy is expended by mechanisms other than chip formation. One
such mechanism could be flattened parts of the abrasive grain sliding against the work
piece surface without removing any material, as shown in Fig. 2.4. Another part of the
energy will be used for plowing, only displacing the material without cutting 共see Fig.
6.3, Section 6.2兲.
The high energy used for grinding compared to other cutting processes can be ex-
plained with the energy used for sliding and plowing. The specific energy used for
grinding is virtually the same as the melting energy of the removed material.10
2.3.4 Mechanical Damage

Abrasive cutting generates a surface with scratches that are produced by interaction of
abrasive cutting points with the work piece, as shown in Figs. 2.4 and 2.5. Both figures
show chips being removed from the surface of the work piece. Both the making of chips
and the plowing will create deformation in the specimen surface 共see Section 6.3兲 and
the depth of the deformed layer will depend on the material, cut-off wheel, feed speed,
and other factors.
According to the literature7,13–17 the general deformation depth at wet abrasive
cutting will be so that it is easily removed by plane grinding with grit 220 SiC grinding
paper. For annealed polycrystalline 70:30, brass, the damage depth has been measured
to 700 ␮m 共maximum depth Dd, see Section 6.3兲 and significant deformation depth to
16 ␮m.7 For carbon steel the damage depth has been measured to 125 ␮m and for elec-
trolytic copper 250 ␮m.14 In case of precision cutting with very thin wheels, a low force
on the wheel and lower cutting speeds, the damage is lower, in the range of 50 ␮m.14
For annealed steel 共AISI/SAE 4130兲 deformation of below 10 ␮m has been measured at
conventional wet cutting and less than 2 ␮m at precision cutting.16
Very often the unplaneness of the cut surface will be in the range of 300– 500 ␮m
Fig. 2.5—Schematic drawing of fractures taking place in the abrasive grains and the bond of
the cut-off wheel during cutting.
共see below兲, which means that at least the same amount of material should be removed
to obtain a plane surface. The damaged layer will be removed during this process for
most materials.
Waviness—Unplane Surface
It is important to avoid waviness during the cut. Overloading the cut-off wheel so that it
does not cut straight can cause waviness. This is due to the flexibility of the wheel that
allows for cutting without breaking even if the wheel body is curved because of an ex-
cessive force 共Fn in Fig. 2.3兲. The wheel also might cut in a curve if the point of attack
between wheel and work piece is not straight 共perpendicular兲, forcing the wheel out of
the line of movement between wheel and work piece. The same effect can develop if the
cooling fluid is unevenly distributed to the wheel, causing a chisel-shaped edge of the
wheel 共see Sections 2.6 and 13.5.1兲. Correct clamping is also important 共see Section
2.3.5兲.
In a normal routine-cut specimen, the surface might be unplane with variations up
to several hundred ␮m.17 The variation is strongest at the entry and the exit of the cut-
off wheel; therefore, the feed speed should be regulated often at the start and the finish
of the cut 共see Section 2.6兲.
2.3.5 Thermal Damage

As described in Section 2.3.3 the total grinding energy input includes chip formation,
sliding, and plowing. Peak “flash” temperatures approach the melting point of the ma-
terial being ground. These very high temperatures, however, are of extremely short du-
ration and highly localized on the shear planes of the microscopic grinding chips. Just
beneath the surface the work piece feels nearly continuous heating. This heating, at
cut-off grinding, will mainly take place in the material under the wheel 共see below兲.
Specimen burn can take place if the cut-off conditions are not correct. Visible
burns with steels are characterized by bluish temper colors 共see Fig. 2.6兲 and might
Fig. 2.6—Macro photograph of a steel specimen cut with thermal damage. “Blue burn” can be
seen.
cause a metallurgical transformation in the heat-affected zone 共see Section 13.6.2兲.

The models developed for heat transfer at cut-off are for dry cutting used for indus-
trial purposes, but materialographic cutting with cooling should follow the same pat-
terns, but with lower temperatures. The heat is developed in the arc of contact and it
will move downwards in the material under the wheel. This means that the heated ma-
terial is continuously removed and only a relatively small part of the heat is transferred
to the cut surfaces of work piece and specimen. This process, however, will take place at
the end of the cut when the wheel is about to break through since no work piece mate-
rial remains to conduct the heat downwards. To avoid this it is recommended by
manual cutting to decrease the feed speed a moment before the wheel is through the
work piece. At automatic cutting a suitable low feed speed should be chosen for the
total cutting process.
Heat is also developed through friction between the sides of the wheel and the
work piece/specimen surfaces because of thermal expansion of the material under the
wheel not yet cut. The cutting parameters should be kept so that this expansion is re-
duced to a minimum 共see Section 2.3.8兲. Also, a correct clamping can reduce the fric-
tion between wheel and work piece 共see below兲.
Clamping
It is important that the forces developed by clamping do not influence the microstruc-
ture of the clamped work piece. This is mostly not the case when using a standard vice
for parts with a stiff cross section, but in the case of sensitive materials, bending and
deformation of the work piece should be avoided.
Clamping is often made by using two vices and clamping both the work piece and
the specimen, which-avoids a burr. When the wheel is completing the cut, and there is
little stock beneath the wheel, the temperature rises rapidly and the uncut material ex-
pands thermally. This forces the already cut surfaces against the sides of the wheel and
appreciable additional torque is involved. This, combined with internal stresses in the
work piece might cause the “disk brake effect” in which the two sides of material clamp
the wheel so hard that the rotation stops and most often the wheel breaks 共see Section
2.6兲.
Wet Cutting
During materialographic cutting it is important to keep the temperature low. For this
reason the process takes place with a strong supply of a grinding fluid, usually water
with an additive 共see Section 2.3.7兲.
2.3.6 Cut-off Wheel Wear

The cut-off wheel wear is decisive for the efficiency of the wheel. If the wear is too low
the cutting edge will grow dull causing glazing and the cutting will stop. If the wear is
too high, the economy of the process is not correct and the quality of the cut might be
good, but the number of cuts made with one wheel is too low.
The wheel wear involves three parameters: attritious wear, grain fracture, and
bond fracture 共see Fig. 2.5兲.10 Attritious wear involves dulling of abrasive grains and the
growth of wear flats by rubbing against the work piece 共see Fig. 2.4兲. Grain fracture
refers to the removal of abrasive fragments by fracture within the grain, and bond frac-
ture occurs by dislodging the abrasive from the binder 共see Fig. 2.2兲.
Both attritious wear and the two types of fracture depend on the tangential force,
Ft 共Fig. 2.3兲. If the force is too low, the process will stop and the grains will be blunt,
resulting in glazing and overheating of the cut. A Ft that is too high might cause an
increase in the temperature in the cut which leads to an excessive bond fracture.
Wheel wear is measured by the total weight of abrasive worn away during the pro-
cess. Experiments show that attritious wear is very little, grain fracture is only a small
part of the total wear, and bond fracture is the dominant part. Attritious wear, alto-
gether negligible, is probably the most important type of wear because it controls the
grinding forces and thus governs the probability of bond fracture and the overall rate of
wheel wear.
The grinding ratio 共G兲 is a convenient measure of wheel wear and is expressed as
follows:
G = Volume ground away 共Qw兲/Volume of wheel consumed 共Qs兲
The G-ratio needs to be as high as possible to secure a good economy of a cut.
The best G-ratio is obtained when the cut-off wheel and process parameters are
chosen correctly in relation to the material and shape of the work piece. Experiments12
have shown that the arc of contact 共l in Fig. 2.3兲 is important to obtain a high G-ratio. If l
is too high the longer cuts give chip interference, the space 共pores兲 between the grains
in the cut are not able to accommodate the chips that causes larger lumps to be broken
from the wheel edge, resulting in a lower G-ratio. It seems that the ideal length of l is
around 12– 20 mm 共0.5– 0.75 in兲. If l is smaller, the G-ratio also drops, probably due to
a very high load on the wheel edge due to the very short arc of contact. In practical
work, l can be up to around 15–20 % of the wheel diameter without problems, depend-
ing on the material11 共see Section 2.3.8兲.
Another important factor regarding the G-ratio is the down feed rate 共feed speed兲 d
in Fig. 2.3.12 It seems that at a too low d, excessive heat is generated, probably because
of the lack of sufficient chips to take the heat away that causes the wheel to wear too fast
because of the high temperature in the bond. At a certain optimum value of d the tem-
perature drops and the G-ratio increases. If the feed speed is further increased the
G-ratio drops because there no longer will be sufficient chip clearance to handle the
chips, the temperature increases, and the wheel edge breaks down, as described above.
In practical work the G-ratio is in the range 0.5 to 1.5 depending on the hardness of
the cut-off wheel and the material to be cut. For a material like medium-carbon steel
共40 mm 共1.50 in兲 diameter兲 cut with a medium hard wheel 共250 mm 共10 in兲 diameter兲,
this gives around 40 to 50 sectioned specimens.
Truing and Dressing

Truing and dressing are both connected to wheel wear. Truing is a process to be per-
formed when the grinding wheel is shaped incorrectly because wheel surface is worn.
Cut-off truing is done to an unround wheel, making it run concentrically. This is done
automatically with consumable wheels during the process, but truing might be neces-
sary at slow consumable wheels.
In metallographic/materialographic preparation using grinding disks having a
plane surface, truing is done to make the disk plane, and it implies that an amount of
the disk is removed to establish the original flatness of the disk surface.
Dressing is a process to reinstate the cutting ability of the grains. If the grains are
glazed or the edge/surface of the wheel/disk is clogged, the surface is opened by remov-
ing a small amount of bond material with a dressing stick, normally a piece of ceramic
bonded aluminum oxide or silicon carbide. Dressing should be limited because it
causes wheel/disk wear.
In cut-off, dressing is only done on CBN and diamond wheels 共see Section 2.4.2兲.
2.3.7 Cutting Fluids

Materialographic cutting is always performed as wet grinding, using a grinding fluid or
coolant. The fluid has the following simultaneous functions: cooling the work piece/
cut-off wheel interface; lubrication; flushing away the chips; protecting against corro-
sion of work piece and machine; and preventing development of bacteria and fungi.
Because water is a very good cooling medium, it is used as the main ingredient. How-
ever, an additive that contains a number of components is needed to obtain the men-
tioned functions.
Lubrication and Cooling

As described in Sections 2.3.3 and 2.3.5, heat is developed during the grinding opera-
tion due to chip formation and friction forces in the cut. For these reasons it is impor-
tant that a relatively high lubrication takes place, reducing the power required to re-
move a given volume of material and thereby keeping the heat generation as low as
possible, and at the same time cool the work piece to avoid a heat buildup.
Synthetic Grinding Fluids—Oil-Based Fluids

The so-called synthetic or chemical fluids used as additives to water are used for cut-off
grinding. These fluids, generally defined as grinding fluids contain no mineral oil and
are typically clear, but may be dyed.
The simplest fluid only contains some inorganic chemicals that protect against
corrosion and bacterial attack. This fluid can be described as “water that doesn’t make
rust,” producing a very good cooling, but no lubrication.
The most frequently used type of synthetic fluid has surface active components
共for better wetting of the surfaces兲 and other components that improve the lubrication,
cooling, and corrosion inhibition. The synthetic fluid is mixed as an additive in ratios of
1:30 to 1:50 with water.
Semisynthetic fluids have 3–30 % oil and give a stronger lubricating action than
the synthetic fluid. It can be used instead of emulsions for band sawing and other pro-
cesses with high friction.
Emulsions, emulsifiable oil in water and typically milky white are not normally
used for cut-off grinding, but are suited for other cutting processes, such as band saw-
ing, hacksawing, etc.
Oil-based fluids are, however, often used for cutting with precision cutters using
diamond cut-off wheels. This fluid can be used without mixing. Water-soluble 共emulsi-
fiable兲 oils, that mix with water in ratios of 1:5 to 1:20 are also available.
Grinding fluids normally have a high pH and can cause skin problems 共see Chapter
26兲 and skin contact should be kept to a minimum 共see below兲.
Application of Grinding Fluid

It is very important that the fluid is taken as close as possible to the area of contact
between work piece and wheel. Caused by the rotation of the wheel, a layer of air is
moving along with the sides of the wheel. It is important that the cooling fluid pene-
trates this layer and gets in contact with the sides of the wheel so that a laminar stream
of fluid is established along the sides of the wheel. In this way the centrifugal force of
the wheel takes the fluid into the wheel/work piece contact area. On most cut-off ma-
chines there are two nozzles positioned, one on each side of the wheel, that directs the
fluid under a certain pressure towards the wheel sides. In some cases other nozzles will
lead fluid to the work piece for extra cooling. Systems with the work piece totally sub-
merged in fluid have also been used. These systems should, however, only be used as a
supplement to the nozzles previously described because the coolant covering the work
piece will not be able to get in contact with the wheel sides due to lack of pressure.
The Cooling System

The most important parts of the cooling system are the pump and tank. The pump
should have a sufficient capacity to supply the fluid, normally from 10– 15 L / min
共2.6– 4 gal/ min兲 for tabletop machines with 200– 250 mm 共8 – 10 in兲 cut-off wheels and
20– 25 L / min 共5.3– 6.6 gal/ min兲 for larger machines with 300– 500 mm 共12– 20 in兲
cut-off wheels. The tank should have a sufficient size, containing 25– 30 L
共6.6– 7.9 gal兲, and 80– 150 L 共21.2–39.7 gal兲, respectively. If the tank is too small the
fluid might heat up during use, and the tank will fill up too fast with ground-off mate-
rial. The tank should have a number of weirs and baffles so that the swarf and grit settle
on the bottom of the tank and are not circulated in the system. Very long chips may be
floating on the surface of the fluid and may eventually clog the pump. Often a simple
filter positioned near the outlet of the machine will collect these chips. This filter
should be cleaned relatively often. Larger filters and filter conveyor swarf removal sys-
tems, originally developed for industrial machine tools, can be used.
Maintenance of Cooling System and Grinding Fluid

Considering the importance of a sufficient cooling, both the cooling system and the
fluid should be maintained regularly. The flow to the cut-off wheel should be checked
daily to assure that the flow is uniform on both sides of the wheel. Depending on the use
of the machine, the tank should be emptied and cleaned in regular intervals, at least
yearly. The tank should be emptied regularly for sludge to prolong the lifetime of the
grinding fluid. Often the content cannot be taken directly to the sewer because local
environmental restrictions will forbid this 共see below and Chapter 26兲. The machine,
cutting chamber, and piping should also be cleaned regularly with a detergent cleaner
to prevent development of bacterial attack 共see below兲.
Water Quality
The quality of the water is important to the performance of aqueous grinding fluids.
The hardness of the water 共content of carbonates兲 affects the fluid very often and the
amount of additive should be adjusted accordingly based on the advice of the additive
supplier. Water with a high calcium or magnesium content, or both, above 7.0 gpg
共120 ppm兲, is considered to be hard and precautions should be taken. Either a higher
percentage of additive can be used or the water can be softened. Hard water also in-
creases the bacteria/fungi growth 共see below兲. Very soft water might cause develop-
ment of foam that often can be suppressed by reducing the amount of additive in the
coolant. Other minerals, such as metal salts also may be present in the water, disturb-
ing the action of certain components in the additive.
Concentration of Grinding Fluid

During use, water evaporates and the concentration of additive and minerals will in-
crease 共see below兲. This can be checked by measuring the pH and using a refractometer
for exact measurements. According to the advice of the supplier, additive or water, or
both, should be added. Generally straight water should not be added, but always mixed
with additive in a higher or lower concentration so that the correct values are rein-
stated. A rule of thumb is to add water with half of the normal concentration to com-
pensate for evaporation. The concentration of the minerals originating from the water
also will rise to maybe three to four times that of the original water during use. There-
fore, the more pure the water used for mixing with the additive and added during use,
the longer the fluid can be used before problems might develop.
Bacteria and Fungi

Bacterial growth in the cooling system often develops if a machine has not been used
for a period of time or the cleaning has not been done for quite a while. Two types of
bacteria are found in the fluid: aerobic, which grow in the presence of oxygen, and
anaerobic, which grow in the absence of oxygen. The anaerobic bacteria that might
develop in the sludge in the bottom of the tank, produce hydrogen sulfide that can
cause dark staining of the work piece and machine and has a strong, unpleasant odor.
The growth of fungus 共mold兲 in the fluid can be a larger problem than bacteria,
depending upon the type of fluids used for cut-off. The presence of fungi can be seen in
the form of slimy, semisolid deposits that cling to the walls of the tank and the machine.
Development of fungi can be avoided by regular maintenance of the system as men-
tioned above. In case of serious attacks the supplier of the additive should be contacted.
In case of strong development of microorganisms, a biocide can be added to the
fluid, or in severe cases, the system must be emptied, completely cleaned, and treated
with a biocide 共germicide兲 before it is filled up with new grinding fluid. The choice of
biocide should be done according to information from the supplier of the original addi-
tive because the biocide added should not be antagonistic to the biocide already in the
formulation.
Disposal of Grinding Fluids

A number of components in a used grinding fluid might be dangerous to the environ-
ment and therefore should be treated with special care. These can be: components in
the original fluid 共additive兲, bactericides, and fungicides used for cleaning, sludge con-
sisting of metal particles, and particles from cut-off wheels. It is very important that all
these substances are listed and checked with the local authorities regarding their dis-
posal. Since disposal is often very troublesome and expensive, the advantage of good
maintenance is evident; by constantly removing sludge and keeping the fluid clean, the
disposal of the fluid can be done relatively seldom.
Health and Safety Aspects of Grinding Fluids

The operator working with wet abrasive cutting can be affected in one or more of the
following ways: skin contact, oral ingestion, inhalation, and eye contact. The fluids
used mostly for cutting are of the water-miscible synthetic 共chemical兲 type having a
high pH 共8.5–9.5兲 and a low surface tension. If skin is exposed to this fluid for a long
period of time it loses its protective oily layer and, in seldom but some cases, dermatitis
can develop. This can be avoided by careful prevention and the operator should not
come in contact with the fluid by using gloves, barrier creams, etc., and by maintaining
the fluid so that it is clean and the concentration is correct.
Inhalation of mist and fumes can be avoided by having the cutting chamber con-
nected to a ventilation system. The operator should use protective glasses to avoid eye
contact.
ASTM Standards
A number of ASTM standards are related to grinding fluids, the most important are:
• Standard Practice for Selecting Antimicrobial Pesticides for Use in Miscible Metal-
working Fluids 共E 2169兲
• Standard Method for Evaluation of Antimicrobial Agents in Aqueous Metal Work-
ing Fluids 共E 686兲
• Standard Test Method for Evaluating the Bacteria Resistance of Water-Dilutable
Metalworking Fluids 共D 3946兲
• Standard Practice for Safe Use of Water-Miscible Metal Removal Fluids 共E 1497兲
2.3.8 The Metallographic/Materialographic Cutting Operation

The metallographic/materialographic cutting operation has the following goals:
1. Produce a specimen surface with lowest possible deformations and scratches.
2. The surface should be without any thermal damage.
3. The surface should be flat without waviness and without a burr.
4. The cut-off should be done with lowest possible costs, meaning lowest possible
wheel wear 共high G-ratio兲 and in the shortest period of time.
Fig. 2.7—Schematic drawing of wet abrasive cutting process. The cut-off wheel is fed into the
work piece. The work piece being with a circular cross section, the arc of contact between
wheel and work piece, l, will vary from a “point” when the wheel touches the work piece to
the total diameter of the work piece, when the wheel is half way through.
The Parameters
The following parameters are available for the operator when cutting with a normal
cut-off machine 共see Section 2.5 and Figs. 2.3 and 2.7兲:
Cut-off Wheel rpm

This is normally in the range of 2000–3000, depending on the diameter of the wheel
共see below and Section 2.4.1兲.
Wheel Velocity
Based on the rpm, the velocity 共v兲 can be calculated. This should be in the range of
30 to 50 m / s 共6000– 10 000 fpm兲. On most cut-off machines the rpm, and conse-
quently, the velocity, is a fixed value that the operator will not be able to change. The
velocity will decrease with the decrease of the wheel diameter caused by wear.
On some newer models of cut-off machines the rpm is made variable, making a
variation in wheel velocity possible. This changes the forces on the wheel 共see Section
2.3.3兲 and therefore also strongly influences the wheel wear, meaning that a “hard”
wheel can be changed to a “soft” wheel by reducing the rpm and vice versa.
Force
The force 共F兲 is an important parameter relating to wheel grade 共hard/soft兲, work piece
material, and length of cut 共arc of contact兲. Normally the force is not used as a control-
ling parameter, but made available to accommodate the selected feed speed, even at
long arcs of contact 共see Section 2.3.6兲.
Feed Speed
The feed 共d兲 will vary according to material, length of cut, etc. It is usually in the range
of 0.005– 5 mm/ s 共0.0002 to 0.2 in/ s兲. This parameter can be controlled by the opera-
Fig. 2.8—The work piece should be placed correctly to obtain the shortest area of contact
between cut-off wheel and work piece. 共a兲 This position will give a short area of contact; 共b兲
this position will give a longer area of contact and should be avoided.
tor and is very important to obtain a correct cut 共see below兲.
Power
The electric motors available in the cut-off machines range from 15 W to 10 kW. The
power consumption expresses the tangential force, Ft in Fig. 2.3. The operator will of-
ten be able to observe the power consumption on an amp meter, and, if necessary, ad-
just the feed speed up for a higher power consumption and down for a lower
consumption.
Arc of Contact
The contact area 共l兲 between work piece and wheel plays an important role in the pro-
cess. Preferably the arc should be in the range of 12– 50 mm 共0.5– 2 in兲, but it is often
longer. As a general rule, the work piece should always be placed so that the arc is the
shortest possible 共see Fig. 2.8兲. When cutting large work pieces, it is helpful to use an
oscillating movement of the wheel or work piece, or to rotate the work piece 共see Sec-
tion 2.5.1兲.
Free Cutting
Based on the relations discussed earlier in this chapter, the expression “Free Cutting”
can be used as a “Rule of Thumb.” Free cutting is achieved when the correct balance is
obtained between force 共wheel against work piece兲, feed speed, and power consump-
tion, giving a correct cut with the highest G-ratio. The balance is reached at a feed
speed corresponding to the optimum chip removal. If the feed speed and force are too
low, the wheel edge gets blunt and heats up the work piece, stopping the process. On an
automatic machine, if the feed speed is set to a certain value, and a lower feed or no feed
is obtained, the same will happen because the wheel is too hard for the given material.
If the force is increased without a corresponding increase in feed speed, the cut be-
comes too hot, causing the bond to fracture, and the wheel will start to break down at a
rapid rate or bend.
Free Cutting by Hand

When cutting a work piece by hand, first a notch is made in the work piece with low
force to secure a straight cut. Then the force is increased until the feed speed is con-
stant, being the free cutting state. Free cutting is when an increase in force does not
increase the feed speed. If a reasonable feed speed is not obtained, even with a rela-
tively strong force, the wheel is too hard for the given material. If a relatively high feed
speed can be obtained without a reasonable force, the wheel is probably too soft.
Free Cutting—Automatic
Cut-off machines often have a hydropneumatic or electric 共electronic兲 feed system, en-
abling the operator to establish an automatic feed 共see Section 2.5兲. To obtain a “free
cutting,” feed speed and power consumption are compared, the consumption express-
ing the force in the cut. The feed speed is increased, and as long this increase has a
corresponding increase in power consumption, the situation is correct and free cutting
is made, provided that a sufficient force is available. When adjusting to a higher feed
speed, no increase can be observed but the power consumption goes up, the feed speed
should be reduced because the force in the cut is too high. The wheel will start to break
down at a too high rate or bend. The operation described is assuming that a sufficient
force between wheel and work piece is available. If the force is not adequate for a given
arc of contact, the feed will, of course, stop or be too low 共see Section 2.5.1兲.
2.4 Abrasive Cut-Off Wheels

Two types of wheels are used for metallographic/materialographic cutting: consum-
able wheels and slow consumable wheels. Consumable wheels are based on inexpen-
sive abrasives, whereas slow consumable wheels are made with diamond or CBN.
2.4.1 Consumable Wheels

With consumable cut-off wheels, the whole wheel is made from a resin 共bond兲, bakelite
or rubber, or a combination of these, with mixed-in abrasive grains, either aluminum
oxide 共Al2O3兲 or silicon carbide 共SiC兲共see Fig. 2.9 and Section 2.3.2兲.
The consumable wheel functions by wearing down during the cut-off process, the
wear being related to the wheel grade. The wheel grade goes from soft to hard, allowing
cutting of hard materials 共up to HV 700–800兲 with a soft wheel and soft materials with a
hard wheel. Al2O3 is used for cutting of most ferrous materials and SiC for nonferrous
and cast iron.
There are normally six to seven different grades available based on either Al2O3 or
SiC. Typically the grades are specified according to material type and hardness, span-
ning from soft nonferrous materials to very hard ferrous materials. When cutting
larger work pieces with a long arc of contact, a wheel with a relatively coarse abrasive
should be used and a soft grade might be needed 共see Section 2.3.2兲.
Wheel Velocity
The consumable wheels, being rather brittle, are not to be used with wheel velocities
higher than stated on the wheel, normally a maximum of 50 m / s 共9800 fpm兲 or 60 m / s
共11 800 fpm兲.
The wheel velocity depends on the rpm of the wheel and the wheel diameter. The
velocity can be calculated from:
Fig. 2.9—Consumable cut-off wheel. The entire wheel is made of a resin bond with an abrasive
共Al2O3 or SiC兲 and will be totally worn down during the process.
rpm · ␲ · Diameter of wheel 共mm兲

Velocity = m/s
60 · 1000
or
rpm · ␲ · Diameter of wheel 共in兲
Velocity = fpm
12
The velocity for consumable wheels is typically 35– 50 m / s 共6900– 9800 fpm兲.
Most cut-off machines for general use have a fixed rpm 共except precision cut-off
machines 共see Section 2.5兲, setting the wheel velocity. Because the wheel velocity, even
with consumable wheels for general use, has an important impact on the cut-off pro-
cess, newer machines can be made with variable rpm 共see Section 2.5兲.
Wheel Dimensions
The consumable wheels are normally available in diameters: 100 mm 共4 in兲, 125 mm
共5 in兲, 150 mm 共6 in兲, 175 mm 共7 in兲, 200 mm 共8 in兲, 235 mm 共9 in兲, 250 mm 共10 in兲,
300 mm 共12 in兲, 350 mm 共14 in兲, 400 mm 共16 in兲, 432 mm 共17 in兲, 450 mm 共18 in兲.
Thickness of the wheels varies from 0.5 mm 共0.02 in兲 at the smallest diameters to
3.0 mm 共0.12 in兲 at the largest.
Arbor 共shaft兲 diameter is normally 32 mm 共1.25 in兲. For small wheels for precision
cutting: 12.7 mm 共0.5 in兲.
Storing
Consumable wheels should be stored in a dry atmosphere and laid flat on a stiff flat
surface to prevent bending of the wheel. To safeguard the wheels it is useful to have a
Fig. 2.10—Slow consumable cut-off wheel, continuous rim. The body of the wheel is metal and
the rim is a bond 共metal or bakelite兲 with diamond or CBN. The wear is very low, caused by
cutting and dressing.
vertical shaft protruding from the holes in the wheels and a weight may be placed on
the top. Bakelite wheels especially will deteriorate when stored in a humid
environment.
2.4.2 Slow Consumable Wheels

As indicated in the designation, these cut-off wheels are worn during the process, but
not to the same degree as consumable wheels. The abrasives used in consumable
wheels are the super abrasives, diamond and CBN 共see Section 2.3.2兲. The single grain
is worn very slowly and therefore a very stable bond is used, either metal or resin
共bakelite兲. This secures that the abrasive stays in place and is not torn away from the
wheel, as is the case with consumable wheels.
The slow consumable wheels are usually made with a metal body and the abrasive
with the bond is placed around the periphery of the body 共see Fig. 2.10兲. The abrasive/
bond layer can be a continuous layer around the periphery 共continuous rim兲 or in seg-
ments. The metal body allows for very thin wheels, down to 0.15 mm 共0.006 in兲 suited
for precision cutting.
In cutting wheels with electroplated abrasives, the abrasives are placed in a band
along the periphery of a metal body and covered with a metal layer. These wheels only
have a thin layer of abrasive; they are less expensive than the wheels described above
and their lifetime is shorter.
Truing and Dressing

Because the slow consumable wheels have a very stable bond, the abrasive grain does
not readily break away even when very worn. Also, the edge of the wheel may clog up
with abraded material that stops the cutting action. Therefore, truing or dressing must
be done. With truing, the shape of the wheel is corrected 共see Section 2.3.6兲 and this is
normally not necessary for a slow consumable cut-off wheel. Dressing is important,
because it exposes new abrasive grains in the edge by removing bond material and to a
certain degree removes worn down grains. Dressing is done with a dressing stick made
from hard materials such as sintered Al2O3 and SiC that is held against the edge of the
wheel for 5 – 10 s.
Attention: Dressing should not be overdone because it wears down the relatively
expensive wheel.
Use
Slow consumable wheels are used frequently when consumable wheels are not suit-
able.
Cut-off in general: For cutting of ferrous metals with hardness higher than ap-
proximately HV 500–700 and up to HV 1400, CBN wheels are used. For sintered car-
bides, ceramics, and other very hard materials, diamond wheels are used. Tough 共duc-
tile兲 materials like sintered carbides are cut with a bakelite bond and most hard and
brittle materials with a metal bond.
Precision Cut-off
This operation, done on precision cut-off machines 共see Section 2.5兲 often calls for very
thin wheels below a thickness of 0.5 mm 共0.02 in兲; therefore, slow consumable wheels
are used. Normally, when cutting hard materials and composites, metal bond is used
with either high or low diamond concentration. High concentrations are used for the
softer materials and low concentrations for the hardest materials like ceramics. At low
concentrations the cutting action is high because of the fewer abrasive grains, creating
a higher force on each grain 共see Section 2.3.3兲. If possible, ductile materials, like most
metals, should not be cut with slow consumable wheels. The ductile metal will con-
stantly clog up the edge of the wheel, the cutting action will be very low, and the wheel
will “wear” its way through the work piece. When cutting most metals on a precision
cut-off machine, a thin resin bonded consumable wheel should be used if a thickness of
0.5 mm 共0.02 in兲 can be allowed.
Wheel Velocity
The wheel speed should be approximately 25 m / s 共4900 fpm兲. This can be established
with most precision machines 共see Section 2.5兲, but often the heavier machines for gen-
eral cutting will not be able to accommodate this relatively low wheel velocity. At low-
speed cutting with small precision cutters, very low wheel speeds in the range of 2 m / s
共395 fpm兲 are used 共see Section 2.5.2兲.
Wheel Dimensions
Slow consumable wheels for general use are available in diameters from 200– 400 mm
共8 – 16 in兲. Thickness from 1 – 2.2 mm 共0.04– 0.09 in兲. Shaft diameter 共arbor兲 is nor-
mally 32 mm 共1.25 in兲.
Wheels for precision cutting 共wafering兲 are available in diameters from
75– 200 mm 共3 – 8 in兲. Thickness varies from 0.15– 0.9 mm 共0.006– 0.035 in兲. Shaft 共ar-
bor兲 is normally 12.7 or 22 mm 共0.5 or 0.87 in兲.
Storing
Slow consumable wheels should be stored laid flat on a stiff, flat surface. Especially
thin wheels should be treated with utmost care because of the risk of bending the
wheel. The boxes in which the wheels were supplied should be used for storage.
2.5 Abrasive Cut-off Machines

Metallographic/materialographic cut-off machines are made for wet abrasive cutting
of a work piece to obtain a sample 共specimen兲. The machine is normally built for a cer-
tain size of the cut-off wheel, deciding the power of the electric motor driving the
wheel.
It is important that the cut-off wheel and work piece are sealed off from the opera-
tor during the cutting to avoid damage to persons in case of wheel breakage.
The machine has a system for moving either work piece or wheel to establish a feed
movement 共see below兲. It also has a system for adding cooling/lubricating fluid to the
cutting area. The work piece is normally placed on a table to allow for fixing the work
piece before cutting. The spindle carrying the wheel should be without play and the
machine design should be stable to avoid vibration.
During the cutting, mist and fumes are developed, and the machine should have an
outlet for an exhaust system.
2.5.1 Design Principles of Wheel—Work Piece Contact

As described in Sections 2.3.3 and 2.3.8, the arc of contact 共or contact area兲 between
work piece and cut-off wheel should be kept around ideally 12– 50 mm 共0.5– 2.00 in兲,
and preferably kept constant during the whole operation. This is often not possible at
“direct” or “chop” cutting where the contact area will vary strongly with the shape and
the size of the work piece 共see below兲. To avoid this, a number of designs have been
developed to keep the contact area constant.
Direct Cutting
The wheel and work piece contact is dependent on the shape of the work piece as
shown in Fig. 2.7 and 2.12共a兲. If a 50 mm 共2 in兲 shaft is cut, the length of the contact
area will vary from a “point” when the wheel first touches the work piece to more than
50 mm when the diameter of the work piece is reached. This means that the force be-
tween cut-off wheel and work piece can be very low at the beginning but has to increase
to ensure a sufficient force on the abrasive grains at the long arc of contact 共see Section
2.3.6兲. This is normally solved by operating with a sufficiently high force and control-
ling the feed speed, keeping it constant through the whole cut. With the correct cut-off
wheels and machine data, a direct cut can be made on almost all materials, even up to
large sections. A rule of thumb would be that a dimension up to 15–20 % of the wheel
diameter can be cut directly, depending on the material and the type of wheel.
Oscillating Cutting
During oscillating cutting, the feed movement between the work piece and the wheel is
combined with a relative movement between the two. This means that the arc of con-
tact is kept low and dependent of the length of the total cut only to a certain degree so
the cutting force can be kept at an optimum value. For metallographic/material-
Fig. 2.11—Principle of oscillating cutting; the cut-off wheel moves relative to the work piece.
ographic cutting the oscillating movement also has the advantage of making room for
the cooling fluid, improving the cooling in the cut.
Oscillating cutting can be made with an oscillating wheel or an oscillating work
piece as shown in Figs. 2.11 and 2.12共b兲. In most cases, the arbor 共spindle兲 carrying the
wheel is moved in a circle 共ellipse兲 or a horizontal 共lateral兲 movement in the same plane
as the wheel, in this way creating a movement relative to the work piece, as shown in
Fig. 2.12共b兲. Only a small amplitude, 1 – 2 mm 共0.04– 0.08 in兲, a in Fig. 2.11, is neces-
sary to limit the arc of contact.
When oscillating the work piece, the table with work piece is moved in a tilting or
reciprocating movement. Figure 2.12共b兲, shows an oscillating wheel but it can easily be
imagined that the work piece has a movement giving the same effect.
Oscillating cutting makes it possible to cut very large work pieces even from diffi-
cult to cut materials. The short arc also makes it possible to work with harder wheels,
thus reducing the costs.
Fig. 2.12—Comparison between direct cutting 共a兲 and oscillating cutting 共b兲. At oscillating
cutting the cut-off wheel can be moved relative to the work piece, as shown, or the table with
the work piece can have a tilting or reciprocating movement, not shown.
Step Cutting
Another way of avoiding the long arc of contact is step cutting 共Fig. 2.13兲. In this prin-
ciple the wheel is moved in increments into the work piece, or vice versa, while moving
the wheel back and forth, performing the process in steps. The depth of each step 共in-
crement兲 dictates the contact arc and this depth can be selected according to the hard-
ness of the work piece material and the hardness of the wheel. The advantage of step
cutting is that very long work pieces can be cut independently of the size of the wheel
and very hard and tough materials can be cut.
Fig. 2.13—Schematic drawing of step cutting. The cut-off wheel is fed into the work piece in a
step of 1 – 5 mm 共0.04– 0.2 in兲 and moved along the work piece to the end where a new step is
made.
Fig. 2.14—Schematic drawing of a rotating work piece showing complementary 共⬎⬎兲 and
contra 共⬎⬍兲 rotation. With a rotating work piece, the cut-off wheel and work piece only touch
in a “point,” and the specimen will be cut off when the wheel reaches the center of the work
piece; this will double the cutting capacity of the machine.
Rotating Work Piece

In the case of a rotating work piece, the arc of contact is only a point where work piece
and cut-off wheel are touching each other 共see Fig. 2.14兲. In some cases this is the only
way to cut very hard materials like sapphire, and by cutting of coatings, the coating is
supported all the way around, avoiding peel-off. This way of cutting also will give
double cutting depth because the cut-off wheel will only reach halfway through the
work piece. Complementary rotation should be preferred 共see Fig. 2.14兲. The figure
shows a work piece with a circular cross section, but other shapes can be rotated and
cut. However, this usually causes some cutting in air because the wheel will first touch
the corners of the work piece.
A rotating work piece is mostly used at precision cutting but special rotating
chucks are also available for general use machines.
2.5.2 Machine Designs

Cut-off machines can be designed according to different principles regarding move-
ment of work piece/wheel 共see Fig. 2.15兲.18 The wheel is either moved towards the work
Fig. 2.15—Design principles for the metallographic/materialographic cut-off machines. At a, b,

and c, the cut-off wheel is fed into the work piece. At d, e, and f, the work piece is fed into the
cut-off wheel.
Fig. 2.16—Standard manual laboratory cut-off machine for chop cutting with dual vices to
clamp samples on both sides of the cut-off wheel. A 3 kW motor and 254 mm 共10 in兲 cut-off
wheels with cut capacity 76 mm 共3 in兲 in diameter.19
piece, a, b, c, or the work piece is moved towards the wheel d, e, f. In the case of the
radial in-feed shown in a, c, d, and f, the depth of the cut is limited to the part of the
wheel outside the flange. At b and e, the work piece is attacked tangentially, and a larger
work piece can be cut if the movement of the cut-off wheel b or the work piece e allows
for it.
Most modern machines are built according to c, where the cut-off wheel is moved
into the work piece that is fixed on a stationary table, or e, where the work piece, fixed to
a movable table, is moved into the stationary cut-off wheel which in most cases is
placed on the motor shaft. In some machines the two principles are combined, giving
more flexibility.
Cut-off Machines for General Use

Smaller machines for wheels of 200– 250- mm 共8 – 10- in兲 diameter are mostly table top
models with an external recirculation system for the cooling fluid. Most of these
smaller machines are hand-operated, and the cut is a direct cut 共see Section 2.5.1兲. The
motor power for these machines is in the range of 1 – 4 kW. An example of a hand-
operated table-top machine is shown in Fig. 2.16.
Machines for wheels of 300 mm 共12 in兲 and larger are mostly floor models with
recirculation systems included in the machine, with motor power ranging from
4 – 10 kW. These machines are usually automatic, meaning that the feed speed is con-
trolled by hydropneumatics or by electric means. In the case of electrically driven feed,
this can be controlled by a microprocessor, allowing for adaptive control so that the
optimum feed speed in relation to motor power is found 共see Section 2.3.8兲. An ex-
ample of an automatic, floor-based machine is shown in Fig. 2.17.
Fig. 2.17—Automatic cut-off machine with oscillating cutting and step cutting for obtaining
the minimum contact area. A 10.5 kW motor and 432 mm 共17 in兲 cut-off wheels with cut
capacity 160 mm 共6.3 in兲 diameter, cutting length 450 mm.20
Most machines have tables with T-slots for flexible positioning of the work piece,
often with quick clamping devices. The cutting compartment should be closed accord-
ing to the rules of safety. It shall not be possible for the operator to open into the com-
partment before the wheel has stopped. The compartment should be easy to clean,
without too many components and corners. It is also an advantage if electrical parts,
such as the motor, are not placed in the cutting compartment.
An efficient cooling system is important, taking the grinding fluid effectively into
the cut, with easy access to cleaning.
Large machines should have a system for reducing the arc of contact between
wheel and work piece 共see Section 2.5.1兲.
Precision Cut-off Machines

Precision cut-off machines are defined as machines being able to cut with relatively
high precision, the work piece being placed in a fixture, moved with a micrometre
screw or automatically. Where machines for general use are mostly used for metals, the
precision machines are often used for other 共hard兲 materials such as ceramics and elec-
tronic parts to be cut with diamond cut-off wheels. Most of these cutters have variable
speed, from very low 共50 rpm兲 to 5000 rpm. The wheels are from 75 to 200 mm
Fig. 2.18—Low speed precision saw for low volume applications. A 15 W motor, 0 – 300 rpm
and up to 125 mm 共5 in兲 diamond wheels, 32 mm 共1.25 in兲 cutting capacity.19
共3 to 8 in兲 in diameter and often very thin, securing a very low loss of material 共kerf
loss兲 which can be important when cutting materials of high value. On most modern
machines both consumable and slow consumable wheels can be used. The work
pieces, electronic parts, optical parts, and other parts where a precision cut is needed,
are normally of a size up to 50– 75 mm 共2 – 3 in兲.
Fig. 2.19—Precison cut-off machine for automatic precision cutting of larger specimens.
Adjustable vertical position of the cut-off wheel makes use of small wheels, 75 mm 共3 in兲, and
large wheels, 200 mm 共8 in兲, easier to work with. Automatic feed speed adjustment and 5 ␮m
specimen positioning. An 800 W motor, up to 5000 rpm. Cutting capacity 60 mm 共2.3 in兲,
cutting length 190 mm 共7.5 in兲.20
Precision machines are built according to the same principles as the general pur-
pose machines 共see Fig. 2.15兲. The smallest machines are built according to f in Fig.
2.15, with the work piece being fed into the wheel by a weight 共constant force兲. These
machines are made for use with slow consumable wheels 共diamond兲 because consum-
able wheels cannot be used with the very simple feed system without getting unround.
The speed is low, in the range corresponding to 300 to 600 rpm, and the motor power is
very low, 15– 100 W. An example of a low-speed cutting machine is shown in Fig. 2.18.
The larger machines typically have a table with the fixed work piece moving linear
into the rotating cut-off wheel, Fig. 2.15, d and e. The motor power is in the range of
500– 1000 W.
The feed, “y-movement,” can be hand-operated or automatically controlled by a
microprocessor. The fixture, placed on a table carrying the work piece, can be with a
micrometre or with automatic control of the “x-movement,” positioning the work
piece. An example of an automatic precision cutter is shown in Fig. 2.19. All machines
have a system for cooling fluid to be taken into the cut. With machines running more
than approximately 300 r / min, the cutting compartment is protected by a hood and it
should be secured that the wheel is stopped if the hood is opened.
2.6 Advice and Hints on Wet Abrasive Cutting

When working with cut-off, it is possible to routinely make a number of precautions to
secure a good cut and, therefore, a good specimen.
• Fix the work piece securely before cutting. Take care that the cut-off piece 共the
specimen兲 is not squeezed against the wheel during the cutting. Preferably the
specimen should be lightly clamped to avoid a burr.
• When clamping sensitive work pieces, place some soft material, such as plastic,
between the work piece and the clamp to avoid damage.
• When introducing the wheel into the work piece at manual cutting, do it slowly and
stop the feed for 2-–3 s to allow a notch 共kerf兲 to be formed. This secures a straight
cut. This is especially important at tapered or rounded work pieces. If the wheel is
not cutting straight from the beginning it will cut sideways and ultimately break.
• Pay attention at manual cutting when the cut-off wheel is almost through the work
piece. Lower the feed speed to avoid overheating of the edge of the specimen or
pinching of the wheel.
• Check the edge of the cut-off wheel. It should be flat 共square兲 when cutting medium
thick sections, flat with rounded corners 共large sections兲, or concave 共thin sec-
tions兲, indicating that the proper cut-off wheel is used and normally giving a burr-
free cut. If the edge is strongly rounded 共convex兲 or pointed, the wheel is probably
too hard for the material and a softer wheel should be used. A glazed edge indicates
a wheel that is too hard, which requires a too high force and therefore develops
excessive heat. If the edge is chisel shaped, the flow of cooling fluid to the wheel is
uneven, giving a crooked cut possibly causing wheel breakage 共see Section 13.6.2兲.
• Disk brake effect: In some materials having internal stresses the work piece will
tend to pinch the wheel, very often when the cut is almost finished. This can cause a
breakage of the wheel because the pressure between the two parts of the work piece
is so high that the rotation stops. This effect might be avoided when working with a
very low feed speed, 0.5 mm/ s 共0.02 in/ s兲 or lower, and preferably oscillating/step
movement, minimizing the development of heat.
• When cutting a material for the first time, check that the feed speed and power con-
sumption 共force in the cut兲 are in reasonable balance. If yes, the wheel is “free-
cutting” 共see Section 2.3.8兲. If the force on the wheel increases, shown by an in-
crease in power consumption, without a visible increase in feed speed, the setting
of the feed speed is probably too high and it should be reduced. If the force is al-
lowed to mount, the wheel might bend and a straight cut 共plane surface兲 is not ob-
tained, or the wheel might break.
• Cutting of a work piece with a coating: Take care that the cut-off wheel is moving
through the section of the coating to be examined and into the base material. In
this way the coating is preserved, because it is in compression and not torn away
from the base material.
• Mounting before cutting: In some cases it is an advantage to mount the specimen
before sectioning to be able to establish a correct cutting plane or avoid breakage.
This can be failure analysis with cracks/corrosion, electronic parts, small speci-
mens of plastic, or very brittle specimens. The mounting is done mostly with a cold
mounting resin, preferable epoxy 共see Section 3.8兲. To avoid clogging of the edge
see electronic parts below.
• Cutting of electronic parts: Often these parts contain soft 共copper兲 and very hard
共brittle兲 materials 共ceramics兲. Use an electroplated diamond wheel 共precision cut-
ting兲; this wheel has diamonds on both the edge and the sides, and it will cut
through ductile and brittle materials without clogging 共see Dressing below兲.
• When the wheel is too hard 共glazing兲, and a softer wheel is not available, try a worn-
down wheel which causes a lower cutting speed and thereby a softer acting wheel,
or use a thinner wheel. In the case of hand cutting, “pulse cutting,” by beating the
wheel into the work piece will create a wheel wear and the wheel will start cutting;
only the lifetime of the wheel is reduced. Another possibility is to make incisions in
the periphery of the wheel, using a pair of pliers to break out small pieces with
50– 75 mm 共2 – 3 in兲 in distance. This also increases wheel wear.
• Cutting may cause harmful gases derived from the phenolic bond and a rubber
bond will normally develop a strong smell. Therefore, the cut-off machine should
be connected to an exhaust system.
• The hood of the cutting machine should be left open after use so that the machine
and cut-off wheel can dry out, reducing corrosion of the machine and prolonging
the lifetime of the wheel.
• Dressing: Diamond and CBN wheels can have a material build-up on the edge of
the wheel 共clogging兲, reducing the cutting ability. The edge is dressed, “cleaned,”
using a dressing stick of Al2O3, for about 5 – 10 s.
For Trouble Shooting, see Section 13.5.
2.6.1 Cut-off Wheel Selection

Rule of thumb: Use a soft wheel for a hard material or a large work piece and a hard
wheel for a soft material or a small work piece.
Both hardness and ductility of the material must be evaluated. A soft material will
not wear out the abrasive very fast, therefore a hard wheel can be used. A ductile mate-
rial might clog the wheel rim so that a softer wheel must be used. On the other hand, a
ductile material might pull out the grains, causing excessive wear. A hard material will
wear out the grains fast, therefore the wheel should break down, releasing new grains.
General Use
Nonferrous metals—These are relatively soft 共up to HV 350兲. Use a hard bakelite
共phenolic resin兲 wheel with SiC.
Soft ferrous metals—共Up to HV 350兲. Use a hard bakelite or rubber-resin wheel
with Al2O3.
Medium hard ferrous metals—共Up to HV 550兲. Use a medium hard bakelite or
rubber-resin wheel with Al2O3.
Hard ferrous metals—共Up to HV 950兲. Use a soft bakelite or rubber-resin wheel
with Al2O3.
Very hard ferrous metals—共Harder than HV 950兲. Use a slow consumable CBN
wheel with bakelite bond.
Sintered carbides/hard ceramics „relatively ductile…—Use a slow consumable
diamond wheel with bakelite bond.
Ceramics/minerals „relatively brittle…—Use a slow consumable diamond wheel
with metal bond.
Precision Cutting
Soft and medium hard materials—Use a medium hard bakelite wheel with
Al2O3.
Medium hard and hard materials, hard, ferrous metals—Use a medium soft
bakelite wheel with Al2O3.
Very hard ferrous metals—Use a slow consumable CBN wheel with high concen-
tration, metal bond.
Extremely hard ferrous metals—Use a slow consumable CBN wheel with high
concentration, bakelite bond.
Ceramics, minerals, very hard materials, general use—Use a slow consumable
diamond wheel with high concentration, metal bond.
Brittle materials „ceramics, minerals兲—Use a slow consumable diamond wheel
with low concentration, soft metal bond.
Electronic parts, hard tough materials, medium to soft ceramics, structural
ceramics—Use a slow consumable diamond wheel with low concentration, metal
bond.
Polymers and other soft materials—Use a slow consumable diamond wheel
with high concentration and metal bond, or a toothed saw blade.
Soft and ductile nonferrous metals—Use a medium hard bakelite wheel with
SiC.
2.7 Other Sectioning Methods

As described earlier, wet abrasive cutting is the dominating cut-off method for
materialographic specimens. Other methods, however, are used either because they
are simple and effective like fracturing, shearing, punching, and sawing, or because
they give a gentler treatment of the cut surface, like wire cutting, than can be obtained
with wet abrasive cutting.
2.7.1 Fracturing
Fracturing can be done on brittle materials like hardened tool steels, ceramics, etc. Of-
ten a notch is made to control the fracture. Less brittle steels and cast iron can be
cooled in liquid nitrogen before fracturing.
2.7.2 Sectioning by Melting

Cutting using methods based on melting the material to be cut is not recommended for
metallographic specimens. The melting process always develops zones affected by heat
and changes the material, often far from the cut surface.16,21 As some of these methods
are used in spite of the drawbacks, the most important methods should be mentioned.
Oxyacetylene Torching
This method should only be used when no other method is available and it should only
be used for obtaining a relatively large work piece for further cutting in the laboratory
with other means. When cutting-off steel specimens it should be considered that a zone
of at least 25 mm 共1 in兲 has been affected by heat during the torch cutting,21 but often
the affected zone is wider 共see Fig. 13.1兲.
Plasma Torching
This method also creates a heat-affected zone with material changes and
microcracks,16 and should only be used for cutting a work piece for further cutting.
Laser Cutting
During laser cutting the heat-affected zone is the range of 0.5 mm 共0.02 in兲 for an an-
nealed steel 共AISI/SAE 4130兲,16 and care should be taken to remove enough material at
the grinding stage if laser cutting is used for the specimen.
Electric Discharge Machining

Electric discharge machining 共EDM兲, or spark machining, is a process that uses sparks
in a controlled manner to remove material from a conducting work piece in a liquid
dielectric.22 The sparks melt the specimen material creating craters in the surface and a
heat-affected zone below the surface. With certain materials that have been melted and
then solidified, the molten material may absorb extraneous alloying elements from the
surroundings.7 A layer containing cracks also may develop immediately beneath the
surface. Both the craters and the heat-affected zone can be several hundred ␮m deep,
and care should be taken, especially in heat-sensitive materials, so that the damaged
layer is removed during the grinding process.
2.7.3 Shearing
A shear can be used for cutting of sheets and other flat products of not very hard materi-
als. The edge of the produced specimen will be heavily damaged by cold work and a
burr often develops. The cold work will alter the microstructure in a layer of the speci-
men in most cases, and it is important that this material is removed during the plane
grinding and fine grinding process. For this reason, shearing is not recommended for
materials that are sensitive to mechanical twin deformation.9
A hand shear can be used for cutting work pieces up to 4 – 6 mm 共0.15– 0.25 in兲,
depending on the type of material. For shearing of stock up to 13 mm 共0.5 in兲 a power
shear is needed. The power shear is built with a table for placing the work piece and a
lower blade integrated in the table and an upper blade moved mechanically or by hy-
draulics. The work piece is fixed during the shearing process by a hold down foot very
close to the lower blade. The upper blade is not attacking the work piece in its full
length, but the blade has a slope called the rake. The rake is given by the design of the
shear. The load required to shear the work piece material depends on the thickness and
type of material and the rake. In normal shearing a portion of the material is sheared
and the rest is broken through due to the shearing action. As an example, in mild steel
up to 6 mm 共0.25 in兲, one-half will be sheared and the rest will break. The shearing load
increases strongly with the thickness of the work piece, although mild steel of 9.5 mm
共0.38 in兲 is only approximately 50 % thicker than 6 mm 共0.25 in兲; the load needed is
225 % higher. For this reason, a shear should not be used for cutting of metallographic
material thicker than the rated capacity, even in narrow pieces. On most power shears
the upper blade will move in a plane 0.5–1° away from vertical, allowing the upper
blade to contact the work piece immediately above the edge of the lower blade. When
the upper blade moves downwards and edge contact is obtained, the correct clearance
is developed and this clearance will increase when the blades overlap. In principle, the
blades should be adjusted according to the thickness of the work piece, but at most
modern shears the blades can be set for a wide range of thicknesses. If shearing of both
thin and thick products are made, the shear should be adjusted to minimum clearance
to avoid thin stock wedging between the blades. It is very important that the clearance
setting is correct and accurate grinding of the blades is maintained. If the edges of the
blades are rounded by wear, or the clearance is too high, the burr mentioned above will
increase.
The shear is a safe tool to use as long the operator follows the given rules.
The shear is a precision machine tool and should be kept in good working order
according to the instructions of the supplier.
Punching
Punching is shearing using a die and a punch and it is used for foils and thin plates to
make circular or rectangular specimens. An example of a circular specimen is the
punching of samples for electrolytic thinning 共see Section 8.6兲. Rectangular specimens
are used for printed circuit boards 共PCBs兲共see Section 7.10.1兲. Rectangular specimens
also are used for steel sheet because the long edge of the specimen can be aligned to the
rolling direction of the sheet.
As with shearing 共see above兲, cold work and a burr will be developed in the process
and this should be removed during the grinding stage of the preparation.
2.7.4 Sawing—Table 2.1

Sawing is a machining process using a circular blade or a straight band having a series
of small teeth for cutting of most materials. By sawing, material is removed from the
work piece in chips as described in Section 6.2 and shown in Figs. 6.1 and 6.2. When
sawing, the rake angle 共see Fig. 6.2兲 is always neutral 共0°兲 or positive, up to 10° for
power hacksawing and bandsawing and 18° for circular sawing. The distance between
adjacent teeth on the saw blade is called the pitch, normally expressed in number of
TABLE 2.1—Recommended Band Pitches for Sawing of Work Pieces of Different Thickness.
Work Piece Thickness Band Pitch
Less than 25 mm 共1 in兲 10 or 14
25– 75 mm 共1 – 3 in兲 6–8
75– 150 mm 共3 – 6 in兲 4–6
150– 300 mm 共6 – 12 in兲 2 or 3
Over 300 mm 共12 in兲 1
1 to 3
2
teeth per inch, and it depends primarily on the cross section area of the work piece to be
cut and to a lesser degree on the type of material. As a rule, two or three teeth should be
engaged with the work piece at all times during sawing. Under Bandsawing, below, the
tooth geometry, pitch, etc., are further discussed. Sawing should be performed with a
cutting fluid 共see Section 2.3.7兲.
The surfaces created by sawing normally are rather rough, but if correctly treated
in the following specimen preparation, sawing can be used for sectioning of
metallographic/materialographic specimens.
Hacksawing
The hand-held hacksaw often can be used for cutting of a work piece from a large part,
maybe placed outside the materialographic laboratory, the work piece later to be sec-
tioned by wet abrasive cutting to produce a specimen. If the hacksaw is used for cutting
a specimen from a work piece, the surface should be carefully prepared, often with an
extended plane-grinding step to remove cold work and deformation 共see Fig. 13.2兲.
Power Hacksawing
Power hacksawing is characterized by the reciprocating action of a relatively short,
straight-toothed blade that is drawn back and forth over the work piece in much the
same manner as a hand hacksaw.
Hacksawing machines consist of a supported reciprocating frame and saw blade
mounted to a base for supporting the work piece. The machines are made as both hori-
zontal and vertical designs, horizontal machines being the most popular. The blade is
fed into the work piece with a feed mechanism and a flow of cutting fluid is led to the
cutting area. Because of the limited possibilities for clamping the work piece, power
hacksawing is well suited for cutting of stock material, tubing, etc., but less suited for
cutting of more complicated parts. The surfaces produced with power hacksawing are
very rough and the problems mentioned above with cold work and deep deformation
are evident. Therefore, this cutting method should only be used for cutting of a work
piece from a larger part, the specimen to be cut later from the work piece by wet abra-
sive cutting.
Circular Sawing
Circular sawing is a process using a rotating, continuous cutting blade with teeth on its
periphery to cut most materials under a flow of cutting fluid. A circular saw produces
better surfaces than power hacksawing, but the limitations regarding cutting of other
work pieces than stock material and tubes, etc., are the same.
Bandsawing
Bandsawing uses a long, endless band traveling over two or more wheels in one direc-
tion. The band, with only a portion exposed, produces a continuous and uniform cut-
ting action using a cutting fluid to improve the cutting, cool the work piece, and in-
crease band life.
In bandsawing the cutting takes place as a continuous, single-direction cutting,
and this, combined with blade guiding and tensioning, gives the possibility of follow-
ing a free cutting path, making contour cutting possible. In this way a specimen can be
cut out from a work piece of odd form, a great advantage compared to other types of
sawing mentioned above.
A number of saw blade types are available for bandsawing, but only two of them
are suited for cutting of metallographic/materialographic specimens. These types are
“conventional sawing” with a bandsaw blade with teeth, used primarily for cut-off and
contour cutting of most materials, and “saw-grinding” with a blade with continuous/
segmented edge for the cutting of very hard materials and composites 共see below兲.
The quality of the cut is generally better than hacksawing, but still a relatively
strong deformation caused by cold work is developed.16,21 At conventional properly
performed bandsawing, the heat developed will not create an altered microstructure
but this could happen if the cooling has not been efficient or the feeding pressure has
been too high. Care should be taken so that cold work and heat-affected zones are to-
tally removed during the grinding steps of the preparation process.
Safety at Bandsawing
The dangerous area when bandsawing is the point of operation where the saw band
traverses to process the work piece. It is very important that the operator is careful to
keep his hands out of the immediate sawing area whenever the band is moving. The
work piece should always be guided into the band with some kind of distance piece so
that the hands will not be close to the band, even when the band has cut totally through
the work piece.
Bandsaw Blades
It is important to select the correct saw band 共blade兲 for the given work piece to be
cut.23 Important factors are:
• Type and hardness of the work piece material that determine the tooth form and
composition of the band.
• The size and variation in cross section of the work piece that determine the pitch of
the teeth of the band.
• Type of cut, is it straight, contoured or both? If cutting in small radii, the width of
the band should be limited.
• Type and condition of the machine to be used.
• Whether a cutting fluid will be used.
Different bandsaw blades with different width, thickness, and tooth geometries
are available for cutting of different materials, ranging from relatively soft carbon steel
bands for cutting of mild steel, cast iron, copper, and other relatively soft materials, to
bi-metal and tungsten carbide-tipped blades for hard, very hard, and tough materials
like work-hardening alloys, high temperature alloys, hastalloy, and titanium. Bandsaw
blades with a grit edge are available with a tungsten grit for cutting hardened tool steel,
titanium, nickel- and iron-based superalloys, glass fiber optics, low density ceramics,
and composites. The more expensive diamond edge blades are used for very hard,
brittle materials, such as minerals and ceramics.
Figure 2.20 shows the terminology commonly used for saw bands. The cutting ac-
tion of the band depends on the tooth geometry. There are three main types of tooth
forms: precision, claw, and buttress, as shown in Fig. 2.21. The precision form nor-
mally has a 0° rake angle, but a positive rake angle is also available. It has a full-rounded
gullet with a smooth radius; the gullet is taking up the chip as long as the tooth is in
contact with the work piece. Bands with precision-form teeth are the most versatile,
have a smooth finish, and are recommended for cutting of most metallographic/
materialographic specimens. The claw form has the same form as the precision except
Fig. 2.20—The terminology commonly used for bandsaw blades.
the gullet is more shallow with less chip capacity but greater backing strength and a 10°
rake angle that requires less feed force. The claw form is recommended for the toughest
materials that demand heavy feed and yield small chips. The buttress form also has a
more shallow gullet and neutral rake angle and is a stronger, less aggressive variant of
the claw form for cutting of wood and plastics.
The band width should be as high as possible for the given cutting operation 共see
Fig. 2.20兲. The wider the band, the greater its beam strength and the more accurate the
cut. For straight cuts the widest band that the machine can accommodate should be
used. Narrower bands should be used only for contour cutting.
The band thickness is important for the strength of the band, especially if the band
width is small.
The tooth set is the distance between the outer corners of oppositely set teeth, de-
termining the kerf 共width of the cut兲. The teeth are set by bending the single tooth to
one side of the band. At straight set the bending alternates all teeth left and right. Raker
set includes one unset tooth 共raker兲 in each sequence of 3, 5, or 7 teeth. The raker set is
recommended for materialographic cutting of ferrous materials.
Fig. 2.21—The three main types of bandsaw blades.

The band pitch, the number of teeth per inch of length 共see Fig. 2.21兲 is primarily
determined by the thickness of the work piece to be cut. A thin work piece requires
bands with a finer pitch 共more teeth per inch兲, thick stock a coarser pitch 共see Table
2.1兲. The work piece material and the surface finish required also must be considered
when selecting the optimum pitch. It should, however, be assured that at least two teeth
are in contact with the work piece at all times during sawing.
Definitions, tooth form and set, pitch sizes, etc., regarding bandsaw blades are dis-
cussed in ASME Standard B94.51M, “Specifications for Band and Saw Blades 共Metal
Cutting兲.”
Bandsawing Machines
Bandsawing machines are built as vertical machines and horizontal machines. The
vertical type23 having a vertical band and a horizontal table on which the work piece is
moved into the band is the most versatile and typically used for cutting of
metallographic/materialographic specimens 共see Fig. 2.22兲. The table often can be
tilted to allow for cutting under an angle to the work piece, and the maximum work
height is in the range of 300– 400 mm 共12– 16 in兲. Most machines have variable band
speed in the range from 0.2– 28 m / s 共39– 5500 fpm兲, but most cutting takes place at
speeds in the range of 0.6– 5 m / s 共118– 985 fpm兲, the speed varying with the hardness/
ductility of the work piece material and the cross section to be cut 共see below兲. Most
metals are cut with speeds in the range of 0.4– 2 m / s 共847– 394 fpm兲 for a cross section
of 25 mm 共1 in兲 reducing the speed to half or less at sections above 150 mm 共6 in兲. For
soft materials like copper the speed can go up to 5 m / s 共985 fpm兲.
Cutting Fluids
For cutting fluids, semisynthetic or emulsion type fluids are used because a relatively
high mechanical lubricity is needed to prevent the chips from bonding to the tooth
faces. A good cooling is also important to keep the teeth cool when they are in the cut,
and the viscosity may also be important depending on the application 共see Section
2.3.7兲.
Advice and Hints on Bandsawing

• For a higher cutting rate, increase the blade velocity or use a band with a coarser
pitch. A higher feeding pressure also will give a higher cutting rate.
• To increase the life of the blade, the blade velocity should be reduced or a band with
a finer pitch should be used. Be careful that the feeding rate 共feeding pressure兲 is
not too high.
• To improve the finish of the cut, precision bands 共0° rake angle兲 should be used
共preferably with a fine pitch兲. The band velocity may be increased and the feeding
rate 共feeding pressure兲 may be reduced.
• To improve accuracy of the cut, the band velocity may be increased and the feeding
rate may be reduced.
• A bandsaw is a relatively dangerous machine, and all precautions should be taken
to avoid accidents when the work piece is guided towards the moving band, see
above.
For Trouble Shooting, see Section 13.6.2.
Fig. 2.22—General purpose contour bandsaw machines, Model 2013-V3 and Model 3613-1.
Model 2013-V3 is designed for contour sawing, band filing and band polishing; it cuts metal,
wood, plastics and other materials. It has a 660⫻ 660 mm 共26⫻ 26 in兲 table that tilts 45° right,
and 10° left and a 330 mm 共13 in兲 work height. The band speed can be varied through a two-
speed transmission from 17–97 or 292– 1585 m / min 共55–300 or 960– 5200 fpm兲. The band
width capacity is 1.5– 27 mm 共1 / 16– 1 in兲 and the motor capacity is 2.25 hp.23
2.7.5 Wire Cutting

When sectioning very sensitive materials with relatively small dimensions, wet abra-
sive cutting might be too rough; therefore, other methods have been developed.
Among these, electro-erosive, chemical, and mechanical principles have been
used, but only the mechanical sectioning, based on a wire with embedded diamond
grains, has gained ground and is commercially available.
Wire cutting uses a metal wire with diamond particles pressed into the metal, in
this way anchored so that they can remove material from a work piece when the wire is
drawn against the work piece under a certain force. The wire, the length up to 10– 20 m
共30– 60 ft兲, is rolled on two drums moving in two directions, the wire being rolled from
one drum to the other. This gives a strong wire 共no welding兲 which can be highly tight-
ened, securing a good precision of the cut. The force in the cut, creating the feed move-
ment, is achieved using a weight. The wire is 0.2– 0.5 mm 共0.008– 0.02 in兲 thick and
moves with up to 2.5 m / s 共493 fpm兲. The process runs without cooling because the re-
moval rate is very low. A fluid is used only for cleaning the wire, keeping the diamonds
free from swarf.
Work pieces up to 50 mm 共2 in兲 can be cut.
The advantages are a very low deformation of the cut surface and a low material
loss 共kerf loss兲. The disadvantage is the long cutting time.
3
Mounting
MOUNTING IS A PROCESS IN WHICH THE SPECIMEN, IN ONE WAY OR AN-
other, is encapsulated to facilitate and often improve the following preparation. The
mounting normally takes place after sectioning 共for mounting before sectioning, see
Section 2.6兲 and several methods are available.
3.1 Purpose and Criteria

3.1.1 Purpose
Mounting is needed for a number of reasons:
• The specimen is small and is difficult to handle.
• The specimen has an awkward shape and mounting is necessary to secure the
preparation of the correct surface.
• Edge retention and flatness of the specimen is important for a correct examination.
• The specimen is brittle or has cracks or pores, and the mounting 共impregnation兲
will stabilize the surface. Also the specimen could be a powder material or in a
shape not fit for preparation.
• A standard specimen size is required when using semiautomatic or automatic
preparation equipment.
3.1.2 Criteria for a Good Mount

If mounting is done only for handling a small, awkwardly shaped specimen, and the
demands for the quality of the prepared surface are relatively low, a simple mounting,
such as clamping, can be used 共see Fig. 3.4兲. In most cases, however, a mounting in
plastic is performed 共see Fig. 1.9兲. This is to ensure a certain quality of the mount to
avoid problems when cleaning the specimen 共see Fig. 3.1兲. The problem shown in Fig.
3.1 is due to a gap between the specimen and the mounting material, letting fluids
共etchants兲 or abrasives, or both, from the preparation leak onto the prepared surface
after drying of the specimen. In case of an etchant, the objective of the microscope
might be damaged. The gap develops because the shrinkage of the mounting material
is too high or with a clamped specimen, a gap exists between the specimen and the
clamp material. This gap also spoils the edge retention of the specimen which is one of
the common advantages at mounting.
To obtain a good mount the following criteria should be fulfilled:
• No gap between specimen and mount material.
• Rate of removal 共wear resistance兲 of mounting material should correspond to that
of the specimen material.
• No air bubbles in the mounting material or along the edge of the specimen.
• The mounting material should be resistant to common etchants.
• The mounting material should not pick up abrasive grains during the preparation.
3.1.3 Surface Flatness—Edge Retention

To obtain a satisfactory examination in a light microscope the specimen surface has to
be relatively flat. This is due to the depth of field of the microscope, the distance along
54
Chapter 3 Mounting 55
Fig. 3.1—Fluid leaking from a gap between mounting material and specimen onto the
prepared surface.
the optical axis over which details of the specimen surface can be observed with ad-
equate sharpness. The depth of field decreases with increasing magnification, at 100,
250, and 500⫻ the distance is 20, 3, and 1 ␮m, respectively. This means that if a speci-
men should be examined at 250⫻ or higher, special care should be taken to obtain a
plane specimen surface. This can be obtained by mounting as described below for edge
retention, but another important factor is the use of the correct preparation process
共see Sections 6.6 and 6.7兲.
When examining surface layers, a very good edge retention is definitely needed,
even for low magnifications. However, also in other cases, a flat specimen surface with-
out edge rounding is wanted. Figure 3.2 shows a specimen with 共a兲 a rounded edge due
to a gap between mounting material and specimen. In 共b兲 there is contact between
mounting material and specimen, which provides a good edge retention.
To support the edge of the specimen, the mounting material must be in contact
with the specimen, and ideally, the surface of the mounting material should be in the
same level as the specimen 共no relief兲. To obtain this the mounting material should
have the lowest possible shrinkage, good adhesion, and a removal rate 共wear resis-
tance兲 corresponding to the specimen material.
Plating the edges of the specimen, mostly with electroless nickel, is used also, but
with modern preparation methods this relatively laborious process can be avoided.
Attention: Although the edge retention to a high degree depends on a good support
of the edge, the correct preparation process is even more important, using the right
grinding/polishing surfaces 共see Chapters 6 and 7兲.
Shrinkage and Adhesion

All mounting materials typically have a higher shrinkage than the specimen material.
In case of hot mounting materials, using powder of polymers 共see Section 3.4兲, the
shrinkage is due to the thermal expansion of the polymer during heating and the con-
traction during cooling. This means that hot mounting resins that usually have a
higher thermal expansion than the specimen material will have a stronger contraction
than the specimen. Therefore, they will “squeeze” the specimen, making a good con-
tact. This means, however, that a gap will develop in a hole or cavity in the specimen.
Fig. 3.2—Edge retention: 共a兲 In case of a gap between mounting material and specimen, a
rounding of the specimen edge is developed; 共b兲 with contact between specimen and
mounting material, edge retention is obtained.
To ensure a good contact, hot compression mounting materials should always be

cooled under pressure 共see Section 3.3兲.
In cold 共castable兲 mounting resins, the shrinkage takes place during the polymer-
ization of the components 共see Section 3.7兲 and a gap will develop if the shrinkage is
high. The shrinkage of cold mounting resins can be reduced by mixing a mineral pow-
der in the resin If the polymerization process is accelerated by heating, then the shrink-
age is usually increased. High adhesion between the resin and the specimen material
ensures the contact, but only epoxy has a strong adhesion.
Material Removal Rate—Wear Resistance

During the preparation process, the specimen material and the mounting material are
removed from the surface, expressed in the material removal rate 共see Sections 6.2 and
7.2兲. Ideally the removal rate should be equal for both materials. In most cases, how-
Fig. 3.3—Relief at mounting: 共a兲 In case of a mounting material that is too soft, a positive relief
is developed, and the edge of the specimen is rounded. 共b兲 With a mounting material that is
too hard, a negative relief is developed.
ever, the mounting material 共resin兲, being relatively soft, has a much higher removal
rate than the specimen. This could be critical because a positive relief is developed 共Fig.
3.3共a兲兲, and the edge of the specimen is not protected. In some cases, if the specimen
material has a higher removal rate than the resin, a negative relief develops, with the
specimen material being in a lower level than the resin 共Fig. 3.3共b兲兲.
The removal rate of the resin, as it pertains to “wear resistance,” depends to a high
degree on the hardness of the resin Tests have shown that when grinding on a P240 SiC
grinding paper, the removal 共abrasion兲 rate of an acrylic or phenolic mounting material
is 10 to 15 times as high as for soft metals like copper and brass. At rough polishing on a
cloth with 4 – 6 ␮m diamond, however, the removal 共polishing兲 rate is only 2–3 times
higher.7 It seems that not only the hardness of the mounting material plays a role, but
also the machinability, meaning that at rough polishing the mounting material to a cer-
tain degree will be removed with the same speed as the sample material.
Wear resistance can be regulated by adding hard fillers to the resin, and this type of
resin should be used if a good edge retention is wanted 共see Sections 3.4 and 3.7兲.
See also Sections 3.6.1 and 3.13.1 with indications of the material removal rate for
the single mounting material.
If the wear resistance of a resin is very high, as known from hot mounting epoxy
with filler, it will influence the preparation process and probably a negative relief will
develop, as mentioned above. The resin will behave like a hard material and if SiC
grinding papers are used, these will wear out the same way as by hard materials. This
also means that if a standard preparation time for a given specimen, mounted in nor-
mal phenolic resin, is 2 to 3 min, it might be doubled if the specimen is mounted in the
epoxy resin with filler.
3.2 Mounting Methods

3.2.1 Clamping
By clamping, the specimen is fixed mechanically without using a mounting material.
For automatic preparation, the specimens can be clamped in a holder 共see Fig. 3.4共a兲
and Fig. 3.5共a兲 for flat specimens and Fig. 3.5共b兲 for circular specimens兲.
In Fig. 3.4共b兲 a clamp, normally used for hand preparation, is shown. It has two flat
pieces of soft steel or stainless steel which are kept together with two screws and the
Fig. 3.4—Clamping of specimens. 共a兲 Specimen holder for clamping of flat specimens for
automatic preparation; 共b兲 six pieces of sheet metal clamped between two flat pieces of steel
for manual preparation.
specimen 共often pieces of sheet metal兲 placed between the two pieces that should have
rounded outer edges to avoid excessive wear of the polishing cloth. If possible, the
clamp material and the specimen material should be compatible.
Common for all clamping: it is difficult to avoid rounding, and often, when clamp-
ing several sheets, gaps will retain abrasives or fluids, creating problems during the
examination.
3.2.2 Hot Compression Mounting

Hot compression mounting or hot mounting indicates that the specimen is placed with
an amount of resin in a cylinder in a mounting press and heated under pressure for a
specified period of time. The resin polymerizes around the specimen, and after cooling,
a mount can be ejected from the press 共see Section 3.3兲.
3.2.3 Cold „Castable… Mounting

Cold mounting typically takes place at room temperature but often the temperature
during the curing will reach 30– 130° C 共82– 265° F兲共peak temperature兲.
During cold mounting, the specimen is normally placed in a mold 共mounting cup兲
and a mixture of a resin and a hardener is poured into the mold. After 5 min to 20 h the
plastic will cure, and a mount can be taken from the mold 共see Section 3.7兲.
3.3 Hot Compression Mounting

Hot compression mounting is based on the fact that certain plastics, such as powder, in
the following called resins, can be formed to a given shape, usually cylindrical, when
heated and cooled under pressure in a metallographic/materialographic mounting
press.
Fig. 3.5—Clamping in specimen holders without mounting: 共a兲 specimens of a flat shape; 共b兲
specimens of cylindrical shape.
3.3.1 Advantages of Hot Compression Mounting

• The quality and wear resistance 共hardness兲 is generally superior to cold mounting.
• Fast method for making one single mount.
• A choice of diameters from 25 mm 共1 in兲 – 50 mm 共2 in兲.
• The diameter of the mount is very exact.
3.3.2 Disadvantages of Hot Compression Mounting

• High initial cost for mounting press.
• Fragile and brittle specimens can be damaged by the pressure in the cylinder that is
from 20– 30 MPa 共2.900– 4.350 psi兲.
• Heat sensitive materials can be damaged. The temperature is normally 120– 200° C
共250– 400° F兲 in the mounting cylinder.
• If mounting large series of specimens, hot mounting is slow because usually only a
limited number of mounting presses will be available.
3.3.3 MSDS „Material Safety Data Sheets…

Hot mounting resins are generally not hazardous, but the MSDS should always be ob-
tained from the supplier and studied before use. Vapors from the heated material
might be irritating; especially vapors from phenolics that might contain formaldehyde
should be avoided. Prolonged skin contact with phenolic and epoxy materials may irri-
tate the skin and cause a skin rash 共dermatitis兲, and, of course, all skin contact to very
hot mounts should be avoided.
Fig. 3.6—Schematic drawing of thermoplastic polymer, not cross-linked.
3.4 Hot Mounting Resins

The resins for metallographic/materialographic mounting are used as powders and
can be classified into two groups: thermoplastic and thermosetting.
A thermoplastic resin is a polymeric material that can be formed on application of
heat and pressure and is solidified by cooling.
A thermosetting resin is a polymeric material that can be formed and cured by the
application of heat and pressure but cannot be reformed on further heat and pressure.
For selection of the correct hot mounting resin for a given purpose, see Section
3.6.1.
3.4.1 Thermoplastic Resins

Thermoplastic materials undergo no permanent change on heating. They flow and
may be molded into a shape which they retain on cooling. The material will flow again
when reheated and can be remolded. Thermoplastic polymers contain linear mol-
ecules that are not cross linked; these are shown schematically in Fig. 3.6.
Acrylics
A number of well-known plastics are thermoplastics. For metallography/material-
ography, acrylics 共polymethylmethacrylate 共PMMA兲兲 are used. Acrylics are known as
sheets used instead of glass for many purposes. This transparency often is an advan-
tage for mounting. Acrylics have to be heated to 150– 180° C 共300– 360° F兲 to flow 共melt兲
and cooled to obtain its shape. The pressure is in the range of 30 MPa 共4350 psi兲 like
most other hot mounting resins. The pressure can be omitted or kept very low during a
preheating period, and this can be of advantage when mounting porous specimens
when the resin penetrates into the pores. Cooling under pressure should be performed
down to 40° C 共104° F兲, preferably room temperature, before the mount is removed
from the press. The total time for heating and cooling is 14– 24 min depending upon
the diameter of the mount.
Acrylics are resistant to water, alcohol 共when properly cured兲, solutions of most
salts, diluted alkalies, hydrochloric acid, and sulfuric acid, but soluble in nitric and
acetic acids, some ketones, and esters. Acrylics are notch-sensitive and cracks may de-
velop if stress is too high 共see Section 13.6.3兲.
The shrinkage is relatively high, hardness is medium, compared to other mount-
ing resins, and wear resistance is low 共see Section 3.1.3兲.
Acrylics with Fillers

Acrylics can be made electrically conductive by adding a metal powder, usually Fe or
Cu, and the mount loses its transparency. This is done to create a conductive mount for
electrolytic polishing. This type of conductive mounting material cannot be recom-
mended for use with SEM because the metal powder 共Fe or Cu兲 can contaminate the
Fig. 3.7—Schematic drawing of thermosetting polymer with a high degree of cross-linking.
specimen surface leading to false results. For SEM, a resin with graphite should be
used 共see Section 3.4.2兲.
3.4.2 Thermosetting Resins

Thermosetting resins for hot mounting are capable of a high degree of cross-linking
shown schematically in Fig. 3.7. They are generally molded in a practically polymer-
ized state so that they can flow by the application of heat and pressure. During the
molding process further polymerization occurs, and the plastic becomes highly cross-
linked and can no longer flow or be changed on further application of heat and pres-
sure.
The following three types of thermosetting resins are available for hot mounting:
phenolics 共bakelite兲, diallyl phthalate, and epoxy.
Phenolics
The phenolic resin is made from phenol and formaldehyde and a filler. Formaldehyde,
being a critical solvent, should only be present in very low amounts 共below 1 %兲 in the
finished resin The filler is important to obtain the right properties of the mount. Gener-
ally wood flour is used as a filler giving brown mounts. Added colors provide phenolic
resins with a number of colors. The temperature for a correct polymerization is
150– 180° C 共300– 360° F兲, and although the thermosetting resin need not be cooled for
curing, the mount should be cooled under pressure to approximately 60° C 共140° F兲 to
reduce shrinkage. The pressure in the cylinder should be approximately 30 MPa
共4350 psi兲 and the total time for heating and cooling is in the range of 8 – 13 min. Phe-
nolics have a number of drawbacks, but being the most inexpensive of the mounting
resins, they are used for routine examinations.
Phenolics are resistant to weak acids, organic solvents, hydrocarbons, detergents,
and cleaning fluids, but attacked by strong alkalis, oxidizing acids, and hot 共boiling兲
etchants.
Phenolics have good mechanical properties. The shrinkage is relatively high, the
hardness is low, and the wear resistance is low 共see Section 3.1.3兲.
Phenolics with Conductive Filler

Graphite can be added as a filler, making the resin electrically conductive. This resin is
used for mounts to be examined in an SEM.
Phenolics in Tablet Form

Tablets or premounts are made by pressing phenolic powder to form a “mount,” with
dimensions slightly smaller than the diameter wanted. It is used for mounting of solid
specimens, which are not influenced by the pressure, when the tablet is pressed on the
specimen. The advantage is that working with a powder resin is avoided.
Diallyl Phthalate
The diallyl phthalate 共DAP兲 resin is a polyester with a filler. The filler strongly influences
the strength of the resin, and for materialographic mounting, mineral and glass fiber
共short兲 are used with glass fiber-filled resin, the most all-round material. The tempera-
ture for a correct polymerization is 150– 180° C 共300– 360° F兲 and the pressure in the
cylinder 25– 30 MPa 共3650– 4350 psi兲. The total time for heating and cooling is
8 – 13 min.
Compared to phenolics, DAP has a number of advantages but it is more expensive
than phenolics.
DAP is resistant to most chemicals and the mechanical properties are excellent.
The shrinkage is much lower than in phenolics, and the filler causes a relatively high
hardness and a high wear resistance, securing a good edge retention 共see Section 3.1.3兲.
Epoxy
Epoxy resin for hot mounting is made as a powder with a filler. Epoxy has a number of
properties very suitable for mounting. The filler is a mineral like calcium carbonate
ground to a very fine powder which to a high degree reduces the removal rate and con-
sequently improves the wear resistance of the resin 共see Section 3.1.3兲. The tempera-
ture for a correct polymerization is 150– 180° C 共300– 360° F兲, and the pressure in the
cylinder is approximately 10 MPa 共1450 psi兲, considerably less than for other resins.
The total time for heating and cooling is 9 – 15 min.
The resistance to all chemicals, even to hot etchants, is very high. The mechanical
properties are excellent and the strong adhesion to the specimen and an extremely low
shrinkage make epoxy resin the best resin for retention of edges. The strong adhesion
can cause problems with adhesion to rams and cylinder walls in the mounting cylinder.
These parts need to be treated with a release agent 共see Section 3.6兲.
3.5 Mounting Presses

Heating, pressure, and cooling are needed when making a mount from a hot mounting
resin
The temperature should be in the range of 100– 200° C 共210– 400° F兲 and cooling
should take place from the maximum temperature to approximately 60° C 共140° F兲 in a
reasonable time. Cooling is necessary for thermoplastics, but even thermosetting res-
ins should be cooled to around 60° C 共140° F兲 under pressure to secure the lowest pos-
sible shrinkage. The force between the lower and upper ram during the process should
be in the range of 1 – 50 kN 共225– 11.235 lbf兲 making it possible to establish a pressure
of 10– 30 MPa 共1450– 4350 psi兲 in the mounting cylinder at diameters from 25– 50 mm
共1 – 2 in兲.
3.5.1 The Heating/Cooling Unit

The heart of the press is the heating/cooling unit consisting of mounting cylinder
共mold兲, lower ram, upper ram, top closure, heating coil, controlled by a thermostat,
and cooling coil 共water cooling兲共see a schematic drawing in Fig. 3.8兲. The cylinder can
be typically supplied in diameters of 25 mm 共1 in兲, 30 mm 共1.18 in兲, 31.75 mm
共1.25 in兲, 38.1 mm 共1.5 in兲, 40 mm 共1.57 in兲, and 50 mm 共1.97 in兲.
The lower ram is moved up and down in the mounting cylinder by hydraulics 共or
by air兲. Before the sample is placed in the cylinder, the lower ram is normally placed in
Fig. 3.8—Schematic drawing of heating/cooling unit. The heating and cooling coils can be seen
around the mounting cylinder with upper and lower ram.
the top to secure the right position of the sample. After moving down the lower ram, an
amount of resin is put into the cylinder. This amount should cover the sample so that
the upper ram should not be damaged when the resin is put under pressure, and there-
fore has a volume reduction. The upper ram with top closure is placed and secured, and
the lower ram is moved upwards, building up pressure. Heating is switched on for a
few minutes, followed by cooling, usually water cooling as shown in Fig. 3.8, but also
air cooling with cooling blocks is used. After about 9 – 24 min, depending on the resin
and the diameter, the mount can be pushed out of the top after removing the upper
ram.
Considering that both pressure and heating should be continuously adjusted dur-
ing the process, an automatization is a great advantage for the operator 共see below兲.
The heating/cooling unit is typically exchangeable so that one press can be used for
a number of different mount diameters, or the cylinder can be exchanged in the
heating/cooling unit.
If the cylinder has enough space, two mounts can be made at the same time, using
an intermediate ram 共piston兲 separating the two mounts.
On modern units, the heating and water-cooling coils are totally integrated with
the mounting cylinder, Fig. 3.8. This secures the best heat transfer, saving energy, water,
and time.
3.5.2 The Hydraulic Press

Hydraulic presses are the most frequently used way of obtaining the relatively high
pressure needed. The first presses were car jacks operating inside a frame, the jack put-
ting a pressure on the lower ram and the frame holding the cylinder and upper ram in
place. Heating was done with a jacket containing a heating element with a thermostat
placed around the cylinder and exchanged with a cooling block 共air cooling兲 or a jacket
with water.
From this simple setup, the hand-operated presses were developed, the pressure
established through a hand pump, and the heating/cooling unit as part of the press 共see
Fig. 3.9—Hand-operated mounting press for mold sizes from 25– 38 mm 共1 – 1.5 in兲. The
standard model is with air cooling, and water cooling is optional.19
Fig. 3.9 which shows a hand-operated mounting press for mold sizes from 25– 38 mm
共1 – 1.5 in兲兲.
Heating is switched on and off manually and the temperature is controlled by a
built-in thermostat. Water cooling is controlled by a water tap, and the operator has to
be careful that the pressure in the mounting cylinder is maintained during the process.
To avoid the requirement for an operator to be present during the whole process, auto-
matic presses are available.
The simplest automatic press uses a motorized hydraulic pump which automati-
cally keeps the pressure controlled by an adjustable pressostat. The operator switches
the heating and cooling on and off.
With more advanced presses, all parameters, pressure, temperature, cooling 共cool-
ing rate兲, and time, are microprocessor-controlled. In some cases, a number of meth-
ods for different mounting materials and mount sizes can be programmed and stored.
Figure 3.10 shows an electrohydraulic, automatic, programmable press with two
heating/cooling units with mold diameters from 25– 50 mm 共1 – 2 in兲.
Fig. 3.10—Electrohydraulic, automatic, programmable press with two heating/cooling units

with mold diameters from 25– 50 mm 共1 – 2 in兲.20
3.5.3 The Air-operated Press

Compressed air has been used for establishing the pressure during hot mounting. An
air-operated press could be made at a lower cost than a hydraulic press. The drawback
is the compressibility of the air which makes the ejection of the finished mount difficult
to control. The air presses seem to have vanished from the market.
3.6 Advice and Hints on Hot Compression Mounting

• Check that the specimen to be mounted is not too brittle, has brittle layers 共spray
coatings might change the porosity under pressure兲, or is not suited for compres-
sion mounting or in other ways. If in doubt, use cold mounting.
• Check that the specimen material can be treated at minimum 150° C 共300° F兲.
• Take care that the specimen is clean and dry, without grease or other residues.
• Keep the mounting cylinder and rams 共upper/lower兲 clean.
• Mold release agent: Treat the upper and lower ram with a thin layer of agent. This is
especially important for resins, like epoxy, sticking to metal surfaces.
• Process time depends upon the amount of resin; therefore, keep the amount low.
On the other hand, the distance from the specimen to the cylinder wall should be
not less than 3 mm 共0.12 in兲, and the resin should effectively cover the top of the
specimen so that the upper ram will not touch the specimen.
• Save expensive resin: Only use the expensive resin in a thin layer around the speci-
men and fill up with a less expensive “back-up” resin
• Pressure: At phenolics and other thermosetting resins, apply the pressure at the
same time as the heating. At acrylics and other thermoplastic resins, the pressure
may be applied after a preheating period 共see below兲. Never use excessive pressure.
• Phenolic mounts: Cool the mount under pressure down to approximately 60° C
共140° F兲. Do not take out a very hot mount and cool it directly in water; the mount-
ing material might crack or a gap along the specimen will develop, or both.
• Specimens with layers requiring a superior edge retention: Use an epoxy resin
• Porous specimens: Use a thermoplastic resin 共acrylics兲; if possible preheat the
resin or use cold mounting.
• Small specimens: These can be supported during the process by using a clip 共see
below兲.
• Electrolytic polishing: Use a conductive resin but apply a thin layer of nonconduc-
tive resin around the specimen to avoid an electrolytic reaction in the resin
For Trouble Shooting see Sections 13.5/6.
3.6.1 Selection of Resins for Hot Compression Mounting

Temp., Heat./
°C 共°F兲 Cool.
Specific Mounting Force Time Price
Purpose Property Resin KN 共lbf兲共min兲 Range
Glass clear mounts Thermoplastic Acrylics, 150–180 6 / 8 at Medium
Porous specimens Transparent transparent 共300–360兲 25 mm
共low pressure兲 Low initial without 15–50 共1 in兲
Nonconductive pressure, fillers 共3375– to 12/ 12
surface for slow cure 11250兲 at 50
electropolishing Medium mm
shrinkage 共2 in兲
Low hardness
High removal rate
at grinding,
medium at
polishing
Low chemical
resistance
Tendency to
defects
Routine Thermosetting Phenolics 150–180 6 / 3 at Low
examination Fast cycle 共Bakelite兲共300–360兲 25 mm
Back-up resin Medium shrinkage as powder 15–50 共1 in兲
Color marking Medium hardness with wood 共3375– to 11/ 4
Serial mounting High removal rate flour filler, 11 250兲 at 50 Low
of uncomplicated at grinding, with or mm 共2
shapes Resin in medium at without in兲
tablet form polishing color
Medium Phenolics
chemical 共Bakelite兲
resistance in tablet
form
Good edge retention Thermosetting Diallyl 150–180 5 / 3 at High
共Thermal spray Low shrinkage phthatalate 共300–360兲 25 mm
coatings兲 High hardness with glass 15–50 共1 in兲
High planeness Low removal rate fiber 共3375– to 9 / 4 at
Chemical resistance Medium/high or mineral 11 250兲 50 mm
chemical filler 共2 in兲
resistance
Temp., Heat./
°C 共°F兲 Cool.
Specific Mounting Force Time Price
Purpose Property Resin KN 共lbf兲共min兲 Range
Very good edge Thermosetting Epoxy with 150–180 6 / 3 at Medium
retention Very low mineral 共300–360兲 25 mm
共Thermal spray shrinkage filler 5–50 共1 in兲
coatings, Good adhesion 共1125– to 11/ 4
plated layers兲 High hardness 11 250兲 at
Very high planeness Very low 50 mm
removal rate 共2 in兲
Medium/high
chemical
resistance
Electroytic Thermoplastics or Acrylics or 150–180 6 / 3 at High
polishing, thermosetting phenolics 共300–360兲 25 mm
to be used with a Electrically with metal 15–50 共1 in兲
nonconductive conductive or carbon 共3375– to 11/ 4
resin as surface Low shrinkage filler 11 250兲 at 50
against electrolyte Phenolics mm High
Examination in with 共2 in兲
SEM carbon
filler
3.7 Cold „Castable… Mounting

Cold mounting, or castable mounting, is used parallel to hot compression mounting.
Normally cold mounting is not “cold” 共room temperature兲; often temperatures will
reach 30– 150° C 共82– 265° F兲.
In most cases with cold mounting, two components, either two liquids or a powder
and liquid, are mixed. The components, resin and hardener, are measured either by
weight or by volume with a relatively high precision. In the case of very small quanti-
ties, measurement by weight is recommended. The mixing of the components should
be very careful to secure a total distribution of the hardener. The time after mixing until
the curing starts, the pot life varies for the different resins, but as a rule the mixed resin
should be used immediately, securing the lowest possible viscosity of the mixture. The
mixture is preferably done in disposable paper cups which can be discarded after use.
Normally the clean, grease-free specimen is placed in a mounting mold 共see be-
low兲, and the mixture is poured carefully into the mold, avoiding entrapment of air,
when the mold is filled. The low viscosity ensures that the resin flows into all irregulari-
ties of the specimen and air bubbles, if any, will be able to move to the top of the mount.
To improve the penetration of the resin into the specimen, vacuum impregnation can
be used 共see Section 3.10兲. A pressure chamber that creates a pressure with a small
compressor, 0.2– 0.28 MPa 共30 to 40 psi兲, will help to avoid bubbles and improve the
infiltration of the resin into the specimen.
During the curing, the temperature increases to the peak temperature, depending
on the type of resin Up to 130° C 共265° F兲 is measured. The temperature can be kept
down if good heat conduction is established. The different resins have different peak
temperatures 共see Section 3.13.1兲.
3.7.1 Advantages of Cold „Castable… Mounting

• Low initial cost.
• Brittle and fragile specimens are not damaged.
• Specimens with cracks and pores, or both, can be impregnated.
• Large series can be made simultaneously, using inexpensive mounting molds.
3.7.2 Disadvantages of Cold „Castable… Mounting

• Some of the resins have a relatively high shrinkage.
• Some of the resins are relatively soft with a low wear resistance 共high removal rate兲.
• The shape 共diameter兲 is not very exact.
• Risk of bubbles and cracks around the specimen.
• Hazardous vapors and risk if skin is in contact with chemicals.
3.7.3 MSDS „Material Safety Data Sheets…

Some cold mounting resins can be hazardous and special care should be taken during
use. MSDS should be obtained from the supplier and studied carefully. Special precau-
tions to be taken for the different resins are mentioned below.
3.8 Cold Mounting Resins

Similar to hot mounting resins, cold mounting materials can be both thermoplastic
and thermosetting 共see Section 3.4兲.
3.8.1 Acrylics
Acrylics are thermoplastic and are supplied as a resin, a powder 共polyamized methyl
methacrylate 共MMA兲兲 with an initiator, and a fluid, the hardener 共MMA monomer兲,
with a promoter.
The size of the single particles 共beads兲 of the resin has a specific importance. They
vary from 5 – 50 ␮m. Figure 3.11 shows the beads and the grains of a filler. With small
beads, the flow of the mixed resin is more viscous, and better able to penetrate into
microcracks and pores. The peak temperature is 90– 110° C 共194– 240° F兲 and curing
time 5 – 15 min 共see also Section 3.13.1兲.
The acrylics 共without filler兲 are translucent and will cure in down to 5 – 10 min
which makes it the fastest curing resin If the system is expanded with a filler, the shrink-
age can be reduced considerably 共see below兲.
Acrylics being thermoplastic have a tendency to melt during grinding, clogging up
the cut-off wheel and grinding paper if not efficiently cooled.
Acrylic cold mounting materials are not as chemical resistant as the hot mounting
materials 共see Section 3.4.1兲.
The shrinkage is relatively high and this material should not be used if a very good
edge retention is wanted. The wear resistance is relatively low but both this and the
shrinkage can be modified with fillers 共see below兲.
Attention: Fumes from methyl methacrylates are considered hazardous and skin
contact should be avoided so work should be done with gloves and under a fume hood.
Fig. 3.11—Acrylic-mounting material with filler. The small gray particles between the beads of
the polymer are the filler.
Acrylics with Fillers

With hot mounting materials, the fillers usually are established during the manufactur-
ing process, the filler being integrated into the polymer. With acrylics used for cold
mounting, fillers like fine ground calcium carbonate are mixed into the powder and the
grains of the filler will be integrated in the finished mount 共as shown in Fig. 3.11兲. Acryl-
ics with fillers are opaque.
Combinations of acrylics 共MMA兲 with styrene 共see below兲 have been developed
having two liquid components and a powder component consisting mainly of filler ma-
terial. This resin has a very low shrinkage and good edge retention.
Attention: Grains from the filler can be released from the surface during prepara-
tion and cause scratches in the finished specimen.
3.8.2 Polyesters
Polyester is a thermosetting resin that is supplied as two liquids: an unsaturated poly-
ester resin and styrene acting as an accelerator with peroxide as the initiator. A polyes-
ter mount is transparent.
The amount of accelerator is very small compared to the amount of resin, making
the measurement of the two components relatively difficult, when small amounts
should be used. The peak temperature is 50– 110° C 共122– 240° F兲 and curing time is
from 45 min to 6 – 8 h 共see also Section 3.13.1兲.
The shrinkage is high, and polyester should only be used for mounting of speci-
mens with no need for edge retention. The price is relatively low, however, and the resin
is often used for routine mounts.
Attention: Styrene is considered a dangerous material and all work with measure-
ment and mixing should take place under a fume hood using gloves. Polyester has a
limited shelf life 共6 to 12 months兲; therefore, the container should be marked with the
date of receipt to secure that the oldest material is used first.
3.8.3 Epoxies
Epoxy is a thermosetting resin supplied as two liquids, a “resin” and a hardener. Epoxy
is the cold mounting resin with the lowest shrinkage and the best grinding and polish-
ing properties. Epoxy adheres strongly to the specimen, and if the curing time is rea-
sonably long, more than 6 – 8 h, the shrinkage is extremely low. If curing time is short-
ened, either by adding accelerator to the hardener 共30– 45 min兲 or by introduction of
heat 共2 – 4 h兲, the shrinkage will be higher. By introduction of heat, the negative effect
can be reduced by letting the epoxy cure in 1 h after mixing at room temperature and
then complete the curing at 60– 70° C 共140– 158° F兲.
Epoxies are supplied with a very low viscosity and a high boiling point, securing an
efficient impregnation of porous specimens 共see below兲.
Epoxies are transparent and cure through an exothermic reaction. The peak tem-
perature varies with the curing time. Curing for periods from 6 to 20 h gives a peak
temperature 40– 60° C 共104– 140° F兲, while curing for 45 min results in peak tempera-
tures from 85– 100° C 共185– 220° F兲. The peak temperature can be kept low by placing
the mold in a fridge. To avoid very high temperatures at mounts larger than the normal
size, cooling with air using a fan is recommended. Epoxies for cold mounting are nor-
mally not supplied with fillers for metallographic/materialographic purposes, but fill-
ers can be mixed in by the user 共see Section 3.11.2兲.
The two parts, resin and hardener, should be measured in a precise manner be-
cause even a small variation can cause problems after curing 共see Section 3.13兲.
The good adhesion properties of epoxy can result in problems with removal of the
finished mount from the mounting mold. The mold should be made of a plastic mate-
rial with low adhesion and certain flexibility, like POM 共see Section 3.9兲.
Epoxies are not attacked by weak acids, weak alcohols, and organic solvents.
Strong acids and strong alcohols give a slight attack. Resistance to heat: 90– 250° C
共200– 500° F兲.
Epoxy has good mechanical properties and it is the strongest, most durable of the
cold mounting resins. The shrinkage, as mentioned previously, is very low if the curing
process is not shortened down. The hardness is relatively high and the wear resistance
is relatively high 共see Section 3.1.3兲.
Attention: Epoxies can cause allergies and all work should be done with correct
gloves under a fume hood.
3.9 Accessories for Cold „Castable… Mounting

In most cases it is important to have a relatively exact shape of the finished mount and
therefore a mounting mold 共cup兲 is normally used. Clips are other accessories that sup-
port the specimen during the curing.
3.9.1 Mounting Molds

In most cases these are cylindrical molds, made of a flexible plastic like POM or of sili-
cone rubber 共see Fig. 3.12兲. The specimen is placed on the bottom of the mold and the
liquid mounting resin is poured into the mold. Some molds have a removable bottom
to allow the mount to be pushed out after curing. Molds made of silicone rubber are
normally in one piece, the high flexibility of the silicone rubber allowing the mount to
be removed from the mold. To secure the removal of the mount, the mold can be
smeared with a silicone compound before the resin 共epoxy兲 is introduced. Reusable
molds of a square or rectangular shape are also available.
Disposable ring forms often made of phenolics remain as an integrated part of the
mount after curing. The ring is placed on an adhesive film so that the resin will not leak
Fig. 3.12—Mounting molds consisting of two parts, a bottom and a cylinder. The specimens are
supported by clips.
during the curing. The specimen is placed inside the ring and, after curing, the ring
with resin and specimen is taken for preparation.
Another type of disposable mounting mold is an aluminum cup used for packaging
of foods, etc. This is especially useful for large specimens of odd shapes.
3.9.2 Clips
If specimens are small and flat, it helps to support the specimen during the curing. Plas-
tic and metal clips that squeeze the specimen are available, being an integrated part of
the mount 共see Fig. 3.12兲. The clips can be used for both hot and cold mounting.
3.10 Vacuum Impregnation

Specimens like sintered materials and ceramics having pores, cracks, etc., are difficult
to prepare without an impregnation 共infiltration兲 of the surface. If not impregnated the
pores will increase in size and cause pullouts, resulting in a microstructure that is not
showing the correct conditions of the material. Also, electronic parts or other parts of a
complicated structure that should be kept in place during the preparation may be en-
capsulated using vacuum impregnation.
Impregnation in depth can only take place in a material with open pores. In the
case of closed pores, only the pores on the surface will be infiltrated. Normally the im-
pregnation takes place after cutting, but to certain, very brittle materials, impregnation
should be done before cutting. In the case of closed or very narrow pores, the impreg-
nation should take place both after cutting and after plain grinding or even fine grind-
ing.
Impregnation is done in vacuum 共80– 120 mbar兲 using an epoxy resin with a low
viscosity and a boiling point high enough to avoid boiling in the vacuum chamber.
The impregnation takes place in a vacuum chamber which can be a normal labora-
Fig. 3.13—Apparatus for impregnation; the mounting molds are placed in a vacuum chamber
and the epoxy is sucked into the chamber through a tube.
tory bell jar or an apparatus made for the purpose 共see Fig. 3.13兲. The specimen, care-
fully cleaned and degreased, is placed in a mold in the vacuum chamber and a vacuum
is established for an appropriate time from a couple of minutes for not very porous
specimens up to half an hour for very porous specimens. The impregnation is done by
sucking the mixed epoxy into the mold through a tube until the specimen is covered.
共For best results, only a small amount of resin is taken into the mold, just covering the
area of interest and then slowly returning the chamber to atmospheric pressure. The
back pressure will further the penetration of the resin into the specimen. Repeat the
evacuation of the chamber and let in epoxy to completely cover the specimen.兲 Now the
mold can be removed for curing, or curing can take place in the vacuum chamber with-
out vacuum.
A simpler method, which can be used for materials with less pores, is to place the
specimen in a mold with epoxy and immediately after pouring in the epoxy, the mold is
placed in the vacuum chamber and vacuum is established. To obtain the best result, the
first method should be preferred.
Cold mounting can also be done under a low pressure 共see Section 3.7兲.
3.10.1 Dyes
Dyes can be used in connection with vacuum impregnation of porous materials, the
dye being mixed into a low viscous cold mounting epoxy resin By using a dye it is pos-
sible to contrast the voids into which the resin has penetrated against the surrounding
structure. The contrast is created through fluorescence. Figure 3.14共a兲 shows a micro-
structure in bright field where the pores cannot be identified. In Fig. 3.14共b兲, the same
structure in fluorescent light is shown and the pores filled with epoxy can be clearly
identified. To obtain the fluorescence, a so-called short-pass filter in the microscope is
needed to excite the areas with dye, and a long pass filter is needed to see the fluorescent
light 共see Section 15.7.5兲. Dyes are commercially available.
3.11 Special Mounting Techniques

For some materials special mounting techniques are necessary, i.e., examination of
very thin layers, powders, wires, etc.
Fig. 3.14—Use of impregnation with epoxy and dye. 共a兲 Microstructure in bright field; 共b兲 and
the same structure in fluorescent light revealing the pores filled with epoxy.
3.11.1 Taper Sectioning

This technique allows the examination of very thin layers and was highly developed by
L. E. Samuels in his work with surface deformation at metallographic/material-
ographic preparation 共see Section 6.3兲.7
TABLE 3.1—Taper Sectioning: Enlargement Factor, f, with the Corresponding Taper Angle, ␣.
f ␣ f ␣
100:1 0° 30⬘ 10:1 5°40⬘
50:1 1° 20⬘ 5:1 11°30⬘
25:1 2° 20⬘ 3:1 19°30⬘
20:1 2° 50⬘ 2:1 30°
15:1 3° 50⬘ 1.5:1 41°50⬘
1:1 90°
Fig. 3.15—Taper section with taper angle, ␣. The thin layer with thickness A can be analyzed
and measured, B.
The specimen is placed under an angle to the plane of examination, in this way
enlarging the width of the layer, when examined in an optical microscope 共see Fig.
3.15兲.
If measured as a normal cross section in an optical microscope, the lower limit of a
layer thickness is approximately 2 ␮m because below this the measurement uncer-
tainty is too big, the limit of the optical microscope being 0.5 ␮m. Very thin layers can
be examined or measured using taper sectioning because, depending on the taper
angle, an enlargement of 1.5⫻ to 100⫻ can be obtained. Table 3.1 shows the enlarge-
ment factor, f, and the corresponding taper angle, ␣.
If only the layer or the diffusion zone, or both, should be analyzed without mea-
surement of layer thickness, a suitable angle can be established with a spacer, the angle
not being exact.
In case of measurement of the layer thickness, the taper angle should be known
and exact, or the dimension of the specimen should be known. The angle can be estab-
lished with a wedge. If the angle is known, the layer thickness A = B sin ␣, as shown in
Fig. 3.15.
If the dimensions X and Y are known, A = X B / Y, as shown in Fig. 3.16.
3.11.2 Edge Protection

When examining layers, it is absolutely necessary to have a good edge retention. The
edge retention depends very much on the type of preparation performed; it can to a
very high degree be obtained by using the modern grinding and polishing methods and
automatic polishing 共see Section 6.7兲.
In some cases, especially if preparation has to take place with SiC grinding paper,
some precautions can be taken to preserve the edge.
Section 3.1.3 describes the use of the correct mounting resin to protect the edge
and often this will be sufficient.
Fig. 3.16—Taper section with known dimensions X and Y.

If further edge protection is needed there a number of methods available.
Plating
During plating a thin layer of metal is deposited on the surface to be analyzed. The idea
is that the edge rounding takes place on the plated layer, leaving the original layer
plane.
Plating can be done electrolytically, placing the specimen as cathode in a bath con-
taining a Cu, Ni, or Fe salt. Electrolytic plating is laborious and the result is not often
satisfactory for metallographic/materialographic examination.
Electroless plating gives better results and is easier to perform. Electroless nickel
is the most commonly used metal for metallographic/materialographic specimens.
Most metals can be plated. Only bismuth, cadmium, tin, lead, and zinc cannot be
plated.9
Other materials such as plastics, wood, glass, carbide, silicon, and porcelain can
be plated.
An example of a formula for electroless nickel:
45 g nickel chloride
11 g sodium hypophosphite
100 g sodium citrate
50 g ammonia chloride
1000 mL distilled water
pH 8.5–9
Use the mixture at 90– 100° C 共194– 212° F兲. The plating rate will be in the range of
0.015 mm/ h.
Instead of mixing the solutions yourself, different solutions for electroless plating
are commercially available.
Fillers
Many mounting resins are supplied with integrated fillers, in this way improving the
edge protection 共see Sections 3.4 and 3.8兲. Fillers can be mounted together with the
specimen, placed in the surface of the mount close to the edge to be protected, and
preferably adjusted to correspond to the hardness of the specimen.
The preferred filler is alumina used together with epoxy cold mounting resin to
avoid shrinkage and increase hardness. The alumina should be made preferably as hol-
low nodules to secure the stability of the alumina grain in the resin If grains fall out
during the final steps of the preparation this might create scratches in the specimen
surface.
Fillers are commercially available.
Back-up Materials
A relatively simple way of securing the edge is to mount a piece of material similar to
the specimen material close to the edge of the specimen.
A metal foil can be wrapped around a cylindrical specimen, which, in the case of
hot mounting, is pressed close to the specimen because of the high pressure in the
mounting cylinder.
3.11.3 Mounting of Very Small Parts, Foils, and Wires

Very small parts and foils can be difficult to place correctly for mounting. A solution
would be to mount several at a time placed in a piece of tube.
It can be advantageous to use a fast curing glue 共cyano acrylate兲 to fix the parts to
the bottom of a mounting mold before the resin is poured into the mold. Clips for stabi-
lizing the parts are commercially available 共see Section 3.9兲.
Wires can be examined as cross sections or longitudinal sections. Longitudinal
sections can be done, as mentioned above, but cross sections, especially at thin wires,
can be difficult. If hot mounting is possible, Nelson24 recommends drilling holes in a
mount made of thermoplastic resin without a specimen. The wires are put into the
holes, the holes are filled with resin and some resin is placed over the top of the mount
to avoid damage of the upper ram. Then the mount is reprocessed. Transparent mounts
are to be preferred when working with small parts and wires, making it possible to ob-
serve the position of the specimen.
3.11.4 Mounting of Powders

The most common method for mounting of powder is mixing the powder with epoxy
resin The problem can be the settling of the particles because they either settle around
the periphery of the mounting cup or, if the powder has a lower gravity, the setting is
not efficient, the powder being suspended in the liquid epoxy.
Metal powder will settle, but often irregularly, and Glancy25 suggests a method of
filling a small plastic vial or plastic tube with powder. The vial is placed in a vacuum
impregnation apparatus 共see Section 3.10兲 under vacuum and epoxy is added, the same
as at a normal impregnation. Once the epoxy has cured, the plastic vial is cut length-
wise using a razor knife. Now the slug is mounted by hot or cold mounting. Care should
be taken at cold mounting that the slug does not float.
For powder with particles sizes under 2 ␮m, Petzow2 suggests the following: The
powder is placed in a test tube in a low vacuum 共like at impregnation, see Section 3.10兲.
It is then impregnated with a mixture of methacrylic acid methyl ester and 1 % 共wt %兲
of benzole peroxide. This mixture cures in 12 h at 50° C 共122° F兲 with the test tube
closed. The test tube is then broken and the content is mounted as usual.
3.11.5 Mounting of PCB Coupons

A test coupon, normally around 10 by 20 mm 共0.4 by 0.75 in兲 with two reference holes
of 2 mm 共0.079 in兲 is needed if a PCB board should be inspected metallographically/
materialographically with an automatic system. In some cases the coupon is produced
together with the board and it can be removed from the board and taken directly for
mounting.
Very often, the coupon has to be made from the finished board, in this way destroy-
ing the board. For hand preparation, the reference holes are not needed.
Test Coupon
According to the American standard IPC-TM-650, the plated-through holes 共inspection
holes兲 of a PCB board should be inspected metallographically. For this purpose a test
coupon is produced and prepared so that the exact center of the plated holes can be
inspected in a microscope. To obtain the exact position of the coupon during automatic
preparation, two positioning 共reference兲 holes must be made in an exact distance from
the inspection holes 共see Fig. 3.17兲.
Often the coupon is produced through punching the board, risking deformations
in the areas of the coupon later to be examined. If a router is used, this deformation is
avoided and the two reference holes are made in the same operation.
Fig. 3.17—PCB test coupon. It can be seen that the distance from the upper edge of the
precision pins, placed in the positioning holes, to the center of the plated 共inspection兲 holes is
5 mm.
Mounting for Automatic Preparation

A preparation system, made according to IPC-TM-650, Method 2.1.1.2, is typically
used. As mentioned earlier, this means that two reference holes are drilled in the cou-
pon. Two or more coupons are placed on two precision pins so that the pins are in a
given distance from the holes to be measured. Now the coupons with pins are
mounted, allowing the ends of the pins to be used as contact surface in a special speci-
men holder. Generally acrylics are used for mounting of PCB coupons but polyester
and epoxy can be used also. It is important that the mounting resin is able to flow into
the holes to be measured. When using acrylics, the coupon can be dipped in the mono-
mere component ensuring a good penetration into the very small inspection holes, of-
ten down to 50 ␮m 共for preparation, see Section 7.10兲.
3.11.6 Conductive Mounts

Conductive mounts can be necessary for electropolishing and for observation in an
SEM. The simplest way of mounting is using a conductive resin, either thermoplastic
or thermosetting 共see Section 3.13.1兲.
The conductive resin should only be used to establish conductivity to the top of the
mount. Around the specimen surface contacting the electrolyte, a nonconductive resin
should be used.
If the specimen should be cold mounted, the simplest way is letting the specimen
protrude at the top of the mount. This is only possible if the specimen has a certain
height.
Another effective way is to drill a hole in the cold mount and insert a piece of metal
or a screw to make contact to the specimen. Also, a wire can be soldered to the speci-
men before mounting and the wire taken outside the top of the mount.
3.12 Recovery of Mounted Specimen

In some cases, the specimen cannot be etched or examined, or both, when mounted in
a mounting resin The resin can be removed mechanically, chemically, or by heating. It
is important that the prepared surface is not damaged. First, as much resin as possible
is removed mechanically by sawing, grinding, and breaking the resin away from the
specimen. When only a small amount of resin is left on the surface of the specimen,
possibly impregnated in the surface, this can be removed chemically or by heating.
M-Pyrol 共N-Methyl-2-Pyrrolidone兲 is a resin solvent, classified as a combustible liquid,
which is less hazardous than other solvents used for removal of resin The stripped
down specimen is placed in M-Pyrol at room temperature for 24 h and in most cases
the remaining resin is dissolved or can be removed.
An alternative is boiling N,N-Dimethyl-formamide 共approximately 150° C
共300° F兲兲 or in a laboratory furnace at 500– 600° C 共900– 1100° F兲. Epoxy can be dis-
solved by submerging the mount in methylene chloride. Methylene chloride is a strong,
hazardous solvent and is carcinogenic. The mount can also be dipped in boiling glycer-
ine for 1 or 2 h, which will soften the epoxy so that the specimen can be removed.
All work should be done under a fume hood and with suitable protection. The rele-
vant MSDSs should be studied carefully before commencing the work.
3.13 Advice and Hints on Cold Mounting

Check that the specimen material is not being influenced by the mounting material, if
the material is at all sensitive to heat, use epoxy curing in 6 – 20 h.
• Ensure that the specimen is clean and dry without grease.
• If using a mounting mold, take care that the material of the mold is suited for the
mounting material. Relatively flexible molds should be used when using epoxy.
• Be careful when mixing that the exact amount of each component 共by volume or by
weight兲 is measured out. Stir for the time stated in the directions for use. It is very
important that the components are totally mixed.
• Specimens with layers requiring a perfect edge retention: Use an epoxy resin
• In case of epoxy mounts larger than 50 mm 共2 in兲, the heat developed can acceler-
ate the process causing shrinking. To avoid this the amount of hardener can be re-
duced or the mount can be cooled in a refrigerator for the first period of time, or
both.
• If using a filler mixed into the mounting material, this mixture need only be in a
thin layer around the specimen. When this layer is partly cured, fill up with normal
resin
• Always use special gloves when handling epoxy.
• Always use a fume hood for all cold mounting resins.
• Cold mounting materials, especially polyester have a limited shelf life; take care to
mark the containers upon receipt to ensure that the oldest material is used first.
For long-term storage, use a refrigerator.
For Trouble Shooting see Sections 13.5/6.
3.13.1 Selection of Cold Mounting Materials

Approxi-
mate Peak
Curing Temp.
Specific Mounting Time at 20 °C Price
Purpose Properties Material °C 共68° F兲共°F兲 Range
Serial mounting Thermoplastic Acrylics, resin 6 – 15 min 90–110 Medium
Routing Translucent 共powder兲共194–
examination Medium with one 220兲
Fast curing shrinkage hardener
Translucent Low hardness Without filler
共Printed circuitHigh removal rate
boards兲 Medium chemical
resistance
Good edge Thermoplastic Acrylics, resin 8 – 15 min 90 Medium/
retention Low shrinkage 共powder兲 with 共194兲 high
Serial mounting High/medium one hardener
Fast curing hardness and with
Low removal rate mineral filler
Medium chemical
resistance
Routine Thermosetting Polyester, resin 45 min to 50–110 Low
examination Transparent and hardener, 6– 8 h 共122–
Serial mounting High shrinkage both liquids 240兲
Medium hardness
High removal rate
Low chemical
resistance
Very good edge Thermosetting Epoxy, resin 6 – 20 h 30–60 Medium
retention Transparent and hardener, 共86–
Transparent Low shrinkage both liquids 140兲
mounts Medium
Porous hardness
specimens Medium removal
Impregnation rate
共Plated layers, Low viscosity
thermal
spray coatings兲
Mineralogy
Serial mounting Thermosetting Epoxy, resin 30– 45 min 85–100 High
Routine Transparent and 共185–
examination Medium shrinkage hardener, both 220兲
Transparent Low hardness liquids
mounts Medium removal
rate
4
Marking—Storage—Preservation
4.1 Marking
MARKING OF METALLOGRAPHIC/MATERIALOGRAPHIC SPECIMENS IS
very important because a proper identification of the specimen is the only thing that
ensures that the result of the analysis is correctly used. This is true for both quality
control and research, and it can be said that the specimen must be marked in all cases
where a metallographic/materialographic analysis should be reported.
The marking should not in any way influence the microstructure of the surface to
be examined; therefore, this risk should be considered before marking is done. It
should also be considered that the marking is placed where it is not disturbed or re-
moved during the preparation process.
The backside of the specimen/mount is usually used for marking. Considering the
limited space, a code expressing job number, material treatment, etc., is used most of-
ten.
If the final marking is done on the mount, special care should be taken that the
specimen is identified at the stage after sectioning, before mounting, so that correct
marking of the mount is assured.
A number of methods for marking are available.
4.1.1 Marking with Waterproof Ink

This cannot be recommended because the treatment of the specimen/mount will in
most cases remove the ink. Marking ink or pencil can be used as an intermediate.
4.1.2 Identification Tag

This works well if the tag 共carton or metal兲 is placed on the backside of the specimen
and mounted in a reasonably transparent resin, the resin protecting the tag. A tag
placed on the outside of the specimen/mount, however, might be removed during
cleaning in water and alcohol.
4.1.3 Engraving
One of the most widely used methods of marking is vibration engraving. A very hard
vibrating needle induces a visible deformation of the surface of the mount/specimen.
This method will stress the material layer below the surface and it should not be used
for thin specimens like foils.
Electro engraving gives less damage to the surface, but can only be used on electri-
cally conducting materials. The engraving, on a clean and smooth surface, is done
through the melting/evaporation of metal, caused by a high temperature spark.
Hand engraving, using a hard needle, is also possible in most, not too hard,
materials.
4.1.4 Stamping
Stamping a number or code in the specimen is possible but because of the very strong
deformation below the stamped surface this method should only be used in cases
where it will not disturb the material to be examined.
80
Chapter 4 Marking—Storage 81
4.2 Storage
It is important that the prepared surface of a specimen is not disturbed by attack from
the atmosphere. Therefore, the prepared specimen is placed very often in a dessicator
with moisture-absorbing material. Airtight cabinets are also commercially available.
For long-term storage, often the specimen should be stored for several years, a direct
preservation of the surface is recommended 共see below兲.
4.3 Preservation
To absolutely protect the prepared surface a lacquer usually from a spray can is used.
The microstructure can be examined through the lacquer, or the lacquer can be re-
moved easily with acetone and the specimen resprayed after examination.
5
Cleaning and Cleanliness
TO AVOID ARTIFACTS IT IS VERY IMPORTANT, ESPECIALLY IN THE POLISH-
ing stage, that the specimen/specimen holder is carefully cleaned between each step. It
is also important that the room in which the process takes place and the operator’s
hands are clean to avoid contamination of the polishing cloths.
Cross contamination: Considering that the preparation process often includes
abrasives with grain sizes spanning from grit 180 共82 ␮m兲 grinding paper to 1 ␮m dia-
mond suspension, it is evident that cross contamination, larger grains from an earlier
step, cannot be tolerated. Cross contamination can be caused by an inadequate clean-
ing of the specimen, specimen holder, or by the operator’s hands.
The polishing disk may become contaminated from airborne particles or excessive
debris in the machine.
5.1 Cleaning
5.1.1 Cleaning Before Start of Preparation
All greases, oils, and other residues on the specimen should be removed by water with a
detergent or a suitable organic solvent. Failure to clean thoroughly can prevent cold
共castable兲 and hot compression mounting resins from adhering to the specimen sur-
face. Also oxidation, etc., should be removed 共unless these products are to be exam-
ined兲. As some of the more rough cleaning methods, like shot blasting and wire brush-
ing might damage the surface, it should be considered whether this might influence the
final result of the preparation. In special cases, where normal procedures are unsuc-
cessful, electrolytic or chemical cleaning can be used 共see ASTM Standard Practice for
Preparation of Metallographic Specimens 共E 3兲, Section 12.4兲.
5.1.2 Cleaning During and After Preparation

In principle, the specimen and the specimen holder 共fixed specimens兲 should be
cleaned between every step in the grinding and polishing process, but at wet grinding
on SiC paper, using a constant flow of water, a careful cleaning can be limited to after
the last grinding step. When grinding on other media, like rigid composite disks and at
polishing, a cleaning between each step is absolutely necessary.
There are, however, some materials or some constituents in materials that will be
preferentially attacked by water 共zinc coatings on steel, lead inclusions in machining
steels, etc.兲, therefore, water must be avoided completely in the latter preparation
steps.
Cleaning by Hand
For cleaning of most metals and other materials without pores, cracks, etc., manual
cleaning is the most effective method.
The specimen or specimen holder is held under running lukewarm water and
rinsed with a soft brush or cotton ball dipped in water with a detergent. In cases of soft
materials and after the last polishing step, a cotton ball is used to clean the prepared
82
Chapter 5 Cleaning and Cleanliness 83
surface. The cleaning is finished with the spraying of ethylene alcohol from a spray
bottle on the prepared surface and possibly wiping the surface before it is taken for
drying. Ethanol containing a denaturation additive can be used as long as the additive
does not leave a film on the specimen. In case of specimens with pores, cracks, etc., and
mounts with a gap between mounting material and specimen, ultrasonic cleaning is
recommended, except for fragile materials.
In case the standard cleaning methods are inadequate, the cleaning solutions
stated in ASTM Standard Practice for Preparation of Metallographic Specimens 共E 3兲,
TABLE X1.1, can be used.
Ethanol
Although ethanol 共ethyl alcohol兲 is taken by many persons in different forms, the etha-
nol used in a laboratory has the following Hazards Identification, Human Health: “Or-
ganic solvents may be absorbed into the body by inhalation and ingestion and cause
permanent damage to the nervous system, including the brain. The liquid may irritate
the skin, the eyes and the respiratory tract.”
Ultrasonic Cleaning
Ultrasonic cleaning is efficient and relatively fast, removing dirt from pores, gaps,
cracks, etc.
The specimen or specimen holder is placed in a tank with a liquid, water with a
detergent, alcohol, or an organic solvent like acetone. In cases of dirt difficult to re-
move, weak acids and basic solutions can be used.
A transducer vibrates under the bottom of the tank, with 20– 40 kHz creating gas
bubbles 共cavitation兲 in the liquid. These bubbles implode and a rubbing effect occurs
which removes the dirt. The dirt contaminates the liquid and therefore a specimen
must be rinsed, as mentioned above, before drying. Ultrasound penetrates glass so it is
possible to place one or more beakers in the tank with water with a detergent around
the beakers. When the specimens are only placed in the beakers, in a suitable liquid,
this liquid can easily be exchanged when contaminated. Cleaning usually takes
0.5– 1 min. Some soft, very porous and brittle materials should not be cleaned ultra-
sonically or only for 10– 30 s. Using specimen holders, the whole holder can be placed
in the tank.
Ultrasonic Apparatus
Ultrasonic apparatuses are supplied with tanks of different size from 1.5– 10 L
共0.4– 2.6 gal 共U.S.兲兲 and with capacities from 80 W to 470 W. The ultrasound is pro-
duced mostly from a piezoelectric transducer but magnetostrictive transducers can
also be used with large units. The frequency is 20– 50 kHz.
Drying
Drying should take place in a stream of mild air. It is important that the layer of alcohol
is not dried on the prepared surface but is blown away and evaporates from the sides of
the specimen/mount. Air can be supplied from a fixed hair dryer type apparatus allow-
ing both hands to be free to clean the specimen with soft cotton wool and alcohol. Com-
pressed air can be used as well, in which case a clean, dry, oil free air must be secured. A
hair dryer is recommended for the finished specimen to avoid possible oil drops from
the compressed air.
Cleaning of Grinding Disks and Polishing Cloths

Grinding disks based on diamond usually are used with water as a lubricant and clean-
ing shouldn’t be necessary. Rigid composite disks 共RCD兲, lubricated by a special lubri-
cant, will be covered with swarf after use. This typically will not disturb the function,
but if the swarf has dried and therefore filled up the openings between the segments of
the disk, the disk should be cleaned. This is done with a brush, detergent, and luke-
warm water. A cloth that has been contaminated can be cleaned in the same way but
different brushes should be used for the grinding disks and the cloths because of the
different grain sizes.
5.2 Cleanliness
It has already been mentioned above that a high level of cleanliness is needed when
preparing metallographic/materialographic specimens. The operator should be aware
that no contamination takes place through transfer of debris from the hands of the op-
erator. The room in which polishing takes place should be clean and should not contain
dust in the air. The room for preparation, when possible, should not be part of a pro-
duction environment.
It is advisable that cutting does not take place in the same room as grinding and
polishing, as the cutting produces large amounts of debris.
The grinding/polishing machines should be kept clean according to a weekly
schedule, securing that no contamination can take place from the sides of the machine,
splash ring, etc. This also prolongs the lifetime of the equipment.
6
Mechanical Surface
Preparation—Grinding
6.1 Grinding—A Basic Process
AFTER SECTIONING AND POSSIBLY MOUNTING, THE METALLOGRAPHIC/
materialographic specimen is now to be prepared to obtain the true microstructure or
a structure, which, in spite of certain defects 共artifacts兲, will give a true examination
result. For a thorough description of artifacts and how to avoid them, see Sections
13.5/6.
The true structure has been defined in Section 1.2, indicating a surface with no or
few artifacts. In practice only two ways are open to obtain this, either mechanical
preparation, grinding and polishing, or grinding, followed by electrolytic polishing
共see Fig. 1.7 to get an overview兲. In some cases a chemical attack can be included in the
mechanical polishing, creating chemical mechanical polishing, and, more seldom,
chemical polishing is used 共see Sections 7.12 and 8.7兲, but in all cases one or several
grinding steps are performed before the polishing takes place.
In this book, grinding is defined as an abrasive machining process with a fixed
abrasive. The abrasive grain might be fixed from the start of the process, either by a
bond 共ceramic, metal, resinoid兲 or placed on a flexible backing covered by a coating,
like at SiC grinding paper, or covered by a thin layer of metal on a backing of metal
plate. Also the abrasive grain, normally suspended in a liquid, can be added to the abra-
sive machining process taking place on a plane, prepared disk. In this case some of the
grains will be forced into the disk surface, be fixed in the moment of cutting, and grind-
ing takes place. In case the abrasive grain is not fixed but staying loose and rolling be-
tween the work piece and the disk surface a lapping process takes place. Consequently
in this book, a disk to be used with loose abrasive grains is called a “grinding disk,” if
the majority of the grains are fixed when the material removal takes place, producing a
“ground surface,” and a disk where the majority of the grains are loose, producing a
“lapped surface,” is called a “lapping disk” 共see also Section 6.7.7兲.
6.1.1 Plane Grinding „PG…

Plane grinding, also called planar grinding, may be necessary for three reasons:
共1兲 To plane the surface after sectioning, depending on the sectioning method, the sec-
tioned surface might not be plane.
共2兲 To remove the deformation caused by the sectioning and establish a known “start
surface” of the specimen to secure a reproducible further preparation.
共3兲 When a number of specimens are fixed in a specimen holder, the specimen sur-
faces are not in the same plane, and material has to be removed to obtain this.
Plane grinding is usually performed with relatively coarse abrasive grains and will
be described further under the different grinding methods mentioned below 共see also
Fig. 13.14兲.
85
6.1.2 Fine Grinding

Fine grinding is the process used for establishing a specimen surface suited for the first
polishing step. This means that the relatively rough surface from sectioning or plane
grinding, through one or several steps with finer and finer grain sizes, is changed into a
surface that can be treated by polishing. The fine grinding step共s兲 are needed because
the material removal is relatively high, opposite to the polishing steps with a low mate-
rial removal 共see below兲.
Fine grinding is further described under the different grinding methods men-
tioned below 共see also Fig. 13.15兲.
Grinding plays a major role in the preparation process and, therefore, it will be
discussed in depth in the following. The mechanics of the grinding process, being a
“cutting” process producing chips are the same as in wet abrasive cutting 共see Chapter
2兲, and they are basically the same in mechanical polishing.
In mechanical grinding/polishing, the following two features should be
considered.
Material Removal
Material is removed from the specimen surface during the process. The amount of ma-
terial removed can be expressed by the removal rate, often measured as ␮m per minute
or ␮m per a certain travel in m 共metres兲 of the specimen on the preparation surface.
The preparation process is controlled mostly by time, assuming that a certain
amount of material is removed from the specimen per time unit. This assumption is
often not correct because a number of parameters that are not totally controlled, such
as preparation surface, abrasive, and lubrication, influence the removal rate. By the
device, “stock removal,” sometimes used on grinding machines, the process is not con-
trolled by time but through a constant measurement of the actual removed amount of
material. In this way the process can be stopped when the amount of material planned
for is removed 共see Section 7.7.6兲.
Deformation
Deformation can be defined as the nature and depth of the plastically deformed layer
that is produced in the specimen surface during material removal.
In general, the removal rate should be as high as possible and the deformation as
low as possible. This depends on the interaction between the abrasive grain and the
specimen surface as described in the following.
6.2 Material Removal

Grinding is defined as a process with fixed abrasive grains, acting like machine tools.
Figure 6.1 shows a schematic drawing of a tool removing a chip from a work piece. The
abrasive grains will remove chips from the specimen surface in the same way.
Using a normal machine tool like a lathe for the cutting process, macroscopic
chips in the form of ribbons or particles having a thickness of from about
0.025 to 2.5 mm 共0.001– 0.1 in兲 are produced. In grinding, the chips produced are
much smaller, ranging in thickness from 0.0025 to 0.25 mm 共0.0001– 0.01 in兲. The
reason for this is the shape and size of the abrasive grains, acting very differently as
“tools.”
During the cutting process the tool and work piece are forced against each other
Chapter 6 Mechanical Surface 87
Fig. 6.1—Basic model of cutting process indicating shear zone.
and a compressive force is set up which causes the metal to deform in front of the tool
point.
The deformation will take place in a zone along the shear plane 共see Fig. 6.1兲 and
the metal is forced to slide over the tool surface. In doing this, the stress will cause the
material to separate as a chip, if the rake angle is correct 共see below兲. The cutting pro-
cess is very complex, influenced by cutting speed, tool geometry, and feed rate.
A mathematical model has been developed for abrasive machining of a work piece
moving in a linear path across a planar abrasive device like grinding paper under a
constant normal load 共L兲.7 In this model the material removal rate can be expressed as:
m = f␳DL/共H␾m兲共1兲
where m is the mass of material removed, f is the fraction of the contacting points that cut a
chip, ␳ is the density of the work piece material, D is the distance traveled, L is the load, H is
the indentation value of the surface layers of the work piece material and ␾m is a form
factor expressing the shape of the contacting points. The most interesting aspect from a
metallographic/materialographic viewpoint is that the material removal increases with in-
creasing load and decreases with increasing hardness of the work piece material. This lat-
ter assumption, however, only covers hard metals where the removal rate can be expected
to be relatively small, but the relative removal rates for metals of low and intermediate
hardnesses are virtually unpredictable.7
6.2.1 Rake Angle
The rake angle ␣ is the angle between the top face of the tool and a plane perpendicular
to the work piece, as schematically shown in Fig. 6.2.
Rake angles may be classed as positive, negative, or neutral 共tool face perpendicu-
lar to the work piece兲, as shown in Fig. 6.3.
To create a chip, the rake angle has to be positive, neutral, or to a certain degree
negative. With a positive rake angle, the area under shear decreases, leaving less defor-
mation in the surface of the work piece, and the friction 共heating兲 is lower than with a
neutral or negative angle.
At a certain negative angle, the critical rake angle, the chip is not produced any-
more and a “plowing” takes place as shown in Fig. 6.3.7
When plowing, the rake angle is so negative that only a groove is made in the work
piece surface. A standing wave bulge forms in front of the tool, and material is dis-
Fig. 6.2—Basic model of cutting process indicating rake angle.
placed into a ridge on each side of the groove. The material removal approaches zero
and the deformation of the surface increases.
6.2.2 Grain Shape—Contacting Points

In cutting, using a machine tool like a lathe, the shape of the cutting tool is given with a
fixed geometry. In grinding, using the abrasive grains as cutting tools, the shape of the
grain and the number of edges and points vary extremely. Figure 6.13 shows the grains
of a grit 220 SiC grinding paper. The most effective shape of the grain is a V-form creat-
ing an efficient chip provided that the rake angle is correct. If the grain is flat, the cross
section of the chip is reduced and in the case of flat grains of a certain size the specific
pressure between grain and surface will decrease and no cutting will take place, result-
ing in plowing or no action at all.
It is very important that a high number of contacting points are available to obtain
an efficient grinding. Only a small number of the visible contacting points make con-
tact with the specimen surface. At coarser SiC papers like grit 220 only approximately 1
in 10 points make contact and at finer papers like grit 600 only 1 in 20.7
Fig. 6.3—Schematic drawing of possible rake angles with abrasive grains in different positions.
Cutting is shown with a chip being removed from the work piece and plowing is indicated as a
groove with ridges.7
6.2.3 Grain Penetration

The depth of penetration at the contacting points of an abrasive grain into the work
piece is only a small percentage of its size. At grinding, the maximum value is in the
range of 5 %, meaning that a grit 220 grain with an average size of 68 ␮m using a pres-
sure of 40 kPa 共6 psi兲 will penetrate less than 3 – 4 ␮m into the specimen surface. In
practice, at grit 220 SiC grinding paper the penetration 共scratch depth兲 at an annealed
30 % Zn brass will be up to 5 ␮m in the first seconds and drop to 2 – 2.5 ␮m.7
6.2.4 Force on Specimens

In principle, the material removal increases linearly with the increase in specific pres-
sure between specimen surface and grinding surface. This means that a certain force is
needed to obtain a satisfactory high removal rate. It is, however, a problem with SiC
paper that a too high specific pressure might cause stronger deformation in the speci-
men. This is especially important during the first few seconds when the paper has a few
large grains causing a very aggressive attack 共see Section 6.6兲.
At grinding, the force should correspond to a specific pressure from 30– 100 kPa
共4.35– 14.5 psi兲 depending on the material to be ground. In theory the specific pressure
should be kept regardless of specimen size, but experience has shown that the force on
the single specimen should not exceed 50 N 共11 lbf兲, and as compensation, to obtain
the necessary material removal the preparation time is extended. A too high pressure
might cause the grinding paper, in most cases held only by a water layer 共see Section
13.2.4兲 to be dragged off the support disk and the more expensive paper with adhesive
backing or a double adhesive foil must be used. If a polishing cloth is used for “grind-
ing” the cloth may overheat.
6.2.5 Grinding/Polishing Fluids

The fluids used for metallographic/materialographic grinding/polishing has no lubri-
cating effect regarding the actual cutting process taking place between the abrasive
grain and the work piece 共specimen兲 material, creating chips.7 The fluid has a strong
cooling effect and especially in case of grinding, the fluid, usually water, will remove the
swarf. If the debris is not removed the grinding surface becomes clogged and it will
create deformation in the specimen surface.
At polishing the fluid, also called lubricant, is lubricating the surface of the polish-
ing cloth, reducing the friction and heat developed between cloth and specimen, at the
same time removing swarf from the cloth surface. For more details on fluids and lubri-
cants see Sections 2.3.7 and 6.5.
6.3 Deformation
6.3.1 Metals
In metals, being ductile materials, the separation of a chip during machining opera-
tions induces complex systems of plastic deformation in both the separating chip and
the specimen material. An inevitable consequence is that a layer, plastically deformed
during machining, is left in the new surface that is produced. In general terms, the
strains in this layer are very large at the surface and decrease more or less exponentially
with depth. See also Figs. 13.3–13.6 and Figs. 13.19–13.22.
This deformed layer becomes important in metallography when the plastic defor-
mation changes the microstructure of the specimen in a way that can be detected in the
microscopic examination that is to be performed. The layer is then an important poten-
Fig. 6.4—Section of a chip cut in 70:30 brass by an orthogonal tool with a highly negative rake
angle.7
tial source of false structures, or preparation artifacts, the avoidance of which is one of
the primary objectives of a metallographic preparation sequence.
As mentioned above, the abrasive grains act as machine tools set at different rake
angles. When a chip is separated from the surface, the shear strains are concentrated in
the so-called shear zone in front of the tool. A region adjacent to this shear zone, and
extending into the specimen in advance of the tool is also plastically deformed though
to a lesser degree, as shown in Fig. 6.4.
Samuels7 has done an exhaustive study of the deformation created in the specimen
surface of metals, by using taper sections 共see Section 3.11兲.
A taper section of annealed polycrystalline 30 % Zn brass ground on a 220 grit SiC
paper, etched with different etchants shows the surface of the specimen with scratches
and the deformation in Fig. 6.5.
Samuels7 splits up the layers into two levels of deformation, the shear-band layer
at the surface that has been subjected to large strains, and the deformed layer beneath
the shear-band layer. The shear-band layer typically extends preferentially beneath in-
dividual polishing scratches for approximately twice the depth of the scratch with
which it associates. In the deformed layer the material has been strained by simple
compression, and the magnitude of the strains decreases with depth until a level is
reached where the material is only elastically strained. This elastic-plastic boundary
defines the lower limit of the deformed layer. An important difference between the
shear-band layer and the deformed layer is that the presence of shear-band layer mate-
rial is always apparent after etching with any etchant suited for the material, whereas
the presence of the less deformed material becomes apparent in light microscopy only
Fig. 6.5—Taper section of the surface of annealed polycrystalline 30 % Zn brass that has been
ground on grit P220 SiC paper. The section has been etched by several methods that have
different threshold strains for revealing deformation as follows. 共a兲 Ferric chloride reagent
共threshold strain: 5 % compression兲. 共b兲 Cupric ammonium chloride reagent 共threshold strain:
0.1 % compression兲. 共c兲 Low sensitivity thiosulfate etch 共threshold strain: 0.1 % compression兲.
共d兲 High-sensitivity thiosulfate etch 共threshold strain: elastic limit兲. In each case, the base of the
layer, in which the manifestations of deformation have been developed, is indicated by an
arrow. Taper ratio 8.2, 250:1.7
in a rather limited number of materials, and then, perhaps, only after etching by spe-
cific methods.
Samuels splits the deformed layer into two depths, the total deformed layer Dd and
the significant deformation Ds. This gives the following three levels of deformation in
an abraded materialographic specimen:
Depth of shear-band layer 共Dsb兲: The maximum depth beneath the root of the sur-
face scratches of the shear-band layer.
Depth of deformation 共Dd兲: The maximum depth beneath the root of the surface
scratches to the elastic-plastic boundary.
Depth of significant deformation 共Ds兲: The maximum depth beneath the root of the
surface scratches of the deformation that would noticeably affect the observations to
be made on the finished surface.
The value of Ds is the most important one regarding metallographic preparation. It
varies with materials and the etchant used and the level of the finished specimen sur-
face should always be beyond Ds.
Example: Annealed Polycrystalline 30 % Zn Brass7
SiC grinding paper, 220 grit, with water, hand abrasion
Dsb 共scratches兲: 2 ␮m
Dd: 77 ␮m
Ds: 7.5 ␮m
Fig. 6.6—Schematic drawing of surface damage to ceramic material. Because of the brittleness
of the material, micro cracks and pull-outs 共surface fractures兲 are developed in the surface
during the grinding. When a sharp point 共a兲 is pressed into the surface, a pseudo-plastic zone
共1兲 of irreversible deformation is produced beneath the indentation. A median vent crack 共2兲 in
vertical direction may develop. By increasing force 共b兲 lateral vent cracks 共3兲 may develop. If an
indentation is made with a spherical point, 共c兲 first a pseudo-plastic zone 共1兲 develops, at
increasing force followed by a cone 共ring兲 crack 共2兲 and by further increase of the force also a
median vent crack 共3兲 may develop. Pull-outs of whole grains or parts of grains, 共d兲 and smaller
pull-outs 共e兲. Crack following grain boundary 共f兲.
6.3.2 Brittle Materials—Ceramics

The above description covers ductile materials like metals, which when stressed, will
plastically deform a significant amount before fracture occurs. This is not the case with
brittle materials like most ceramics, which deform only elastically prior to fracture by
propagation of a crack. To understand the effect often taking place at grinding of brittle
materials, it can be seen how the indentation of a sharp point and a spherical point
affects the surface of a specimen. When a sharp point, 共a兲 in Fig. 6.6, is pressed into the
surface, a pseudo-plastic zone 共1兲 of irreversible deformation is produced beneath the
indentation. This impression stays in the surface, and by increasing force a so-called
median vent crack in vertical direction 共2兲 develops, and by further increase of the force
lateral vent cracks develop 共b兲共3兲. When this lateral vent crack develops to the surface,
a relatively large volume of material is removed which can be called a fracture chip,
considerably larger than the chips earlier described under metals.7 If an indentation is
made with a spherical point, 共c兲 in Fig. 6.6, first a pseudo-plastic zone 共1兲 develops, at
increasing force followed by a cone 共ring兲 crack 共2兲 and by further increase of the force
also a median vent crack develops 共3兲. The circular symmetry of the ring crack will be
lost if the indenter is drawn across the surface as by grinding/polishing, and the crack
might follow grain boundaries and cause pull-outs of whole grains or parts of grains,
共d兲 in Fig. 6.6. The same might happen with the crack formation shown in 共a兲, Fig. 6.6.
As mentioned above the material removal in brittle materials to a high degree takes
place with fracture chips, leaving cavities in the surface 共e兲 in Fig. 6.6, but according to
Samuels7 this is mainly the case at the larger abrasive grain sizes, whereas below grit
P1200 共approximately 15 ␮m兲 it seems that chip cutting without fracturing takes over.
It can be seen in Fig. 6.6 that beneath the fracture cavities and pull-outs, a crack-
containing layer develops, 共f兲, which extends to considerable depth. This layer must be
removed during the preparation.
A normal preparation procedure for ceramics and other hard and brittle materials
is grinding with a bonded diamond grinding disk followed by grinding on rigid com-
posite disks or very hard polishing cloths with diamond and a final polishing on a me-
dium hard cloth with silica. The most serious problem is the development of pull-outs
and cavities developed during the first grinding step共s兲 with bonded diamond disks.
These artifacts, which as a mistake can be considered to be pores belonging to the true
structure, must be effectively removed during the grinding on the rigid composite disks
共see Sections 3.10, 6.6.1, 6.7.7, and 13.5/6兲.
Preparation of ceramics is stated in Material/Preparation Tables 02–06 in Section
13.2.3. For in-depth information on ceramics and preparation of ceramics, see Refs. 26
and 27.
6.4 Grinding Abrasives

The abrasives already described in Section 2.3 for abrasive cutting are also used for
grinding, but below a further description related to grinding/polishing is given.
6.4.1 Aluminum Oxide

Hardness: 2500 HV
Although Al2O3, alumina, has certain advantages, especially for grinding of steel, it
is not used much for metallographic/materialographic grinding except in ceramic
grinding stones and in connection with zirconia in wet grinding paper for plane grind-
ing.
Very fine alumina is used for polishing 共see Section 7.5兲.
Aluminum oxide was the first grinding medium found in nature, typically emery
共about 50 % Al2O3 with other oxides, principally iron oxide兲 and corundum. Around
1900 a process was found to turn bauxite into Al2O3 and today it is the most used abra-
sive. Al2O3 is available in different crystals with the ␣ particles mostly used for grind-
ing. Al2O3 easily forms substitutional solid solutions like the combination Al2O3 and
ZrO2 mentioned above.
Being made in many different types, Al2O3 also has very different surface struc-
ture. The types with relatively smooth surfaces are used for rough grinding operations.
Types with a surface with sharp facets are used for finer grinding.
6.4.2 Silicon Carbide

Hardness: 2700 HV
SiC plays an important role in metallographic/materialographic grinding with SiC
grinding paper being used for both plane grinding and fine grinding 共see Section 6.6.2兲.
SiC is the first synthetic abrasive, made in the 1890s. There are two grades of SiC.
The green type is relatively friable and has fewer impurities; the black type has the
same hardness as the green type but is less friable. Most of the SiC used for grinding is
of the black type. Silicon carbide is the second most widely used type of abrasive.
The surface structure of an SiC grain is rather irregular, resembling fractured
glass. This is an advantage when coated on an SiC grinding paper because the grain will
be fixed firmly in the coating cement but the irregular surface combined with an irregu-
lar shape will give an increased deformation of the specimen surface 共see Section
6.6.2兲.
6.4.3 Diamond—Diamond Products

Hardness: 8000 HV
Diamond plays an increasing role in metallographic/materialographic prepara-
tion. A number of products based on diamond are developed using diamond grains as
fixed or loose abrasive for both grinding and polishing 共see below兲.
Diamond, together with cubic boron nitride 共CBN兲, belongs to the superabrasives.
Since the 1940s, natural diamonds have been used for grinding purposes. After many
years of research, methods to make synthetic diamonds were developed in the 1950s–
60s and today almost all diamonds used for grinding and polishing are synthetic. Dia-
monds are made with two crystal structures: polycrystalline and monocrystalline.
The polycrystalline grain, having many sharp edges, is relatively friable and will
break down during use, giving a self-sharpening effect, as shown in Fig. 6.7. Polycrys-
talline diamonds are considered the most effective for materialographic preparation
because of a higher removal rate than monocrystalline diamonds in most materials.7
Monocrystalline grains are stronger, having a blocky form with relatively few cut-
ting edges and will not easily break down. If they break down, it takes place along
straight lines, as shown in Fig. 6.8, not creating many new cutting edges.
Fig. 6.7—Schematic drawing of polycrystalline diamond grain before and after grain fracture
creating many new cutting edges.
Fig. 6.8—Schematic drawing of monocrystalline diamond grain before and after grain fracture
creating only a few new cutting edges.
Fig. 6.9—Diamond grains 共2兲, uniform size 共a兲 and nonuniform size 共b兲, between grinding/
polishing disk 共3兲 and specimen 共1兲. The smallest grains 共b兲 are not active.
Diamond Products with Fixed Grains

Diamond is used in a number of products, all having the diamond grains fixed in some
kind of bond. These materials are used for grinding of metallographic/material-
ographic specimens, ranging from plane grinding with relatively coarse grits to ex-
tremely fine grits used in the diamond 共lapping兲 films 共see below兲.
Diamond Grinding Disks—The diamond grains are placed in a metal or bakelite
bond. Primarily used for “traditional” grinding of very hard materials 共see Section
6.6.1兲.
Resin-Bonded Diamond Grinding Disks—The diamonds are placed in a thin layer
in a resin bond 共not bakelite兲. This type of disk is used for “contemporary” grinding of
all materials harder than 150 HV 共see Section 6.7兲.
Metal-Bonded Diamond Disks—The diamonds are placed in a thin layer fixed by a
nickel coating 共see Section 6.7.4兲.
Diamond Pads—The diamonds are placed in a bond of metal or resin in a dot ma-
trix on a self-adhesive backing. Used for plane and fine grinding of hard materials 共see
Section 6.7.5兲.
Diamond Film—The diamonds are coated to a very thin film 共lapping film兲. This
product is used for grinding/polishing of electronic devices, wafers, etc. 共see Section
6.7.6兲.
Diamond Products with Loose „Free… Grains

A number of products are available with the diamond grains mixed with a carrier, en-
abling grinding or polishing with free grains on the surface of the grinding/polishing
disk 共see below兲.
Grain Size
It is very important that the grains for a given grain size are selected with a narrow
tolerance. If the grains are relatively uniform, as shown in Fig. 6.9 共a兲 a very high part of
the grains are active, securing a high removal rate; Fig. 6.9 共b兲 shows diamond grains
with a large difference in grain size and it can be seen that a high number of grains are
present only as “filler” and with only a few acting grains. This causes the specific pres-
sure on each grain to be high, possibly causing deeper scratches in the specimen
surface.
Diamond Suspensions
The use of diamond suspensions 共slurries兲 is increasing because applying the abrasive
in small quantities during the process is an advantage, giving a more constant removal
rate than other types of diamond products.28
Suspensions are suited for being applied from a dosing unit, in this way making
the charging of the grinding disk/polishing cloth, automatic. The automatic dosing can
be performed as spray, creating aerosols, which are considered dangerous to health, or
by pumps, supplying the suspensions in drops. Also the suspension can be conve-
niently applied by hand from a pump 共spray兲 bottle.
Diamond suspensions can be based on water, alcohol, oil, or other hydrocarbons.
Water-based suspensions are to be preferred, because of the nontoxic nature of water.
To the suspension should be added an ingredient that stabilizes the diamond grains so
that they do not sediment or only sediment very slowly. In case sedimentation takes
place, the bottle with suspension can be placed on a stirring apparatus or in other ways
be stirred during the process.
In certain cases, when the material to be prepared is sensitive to water, a water-free
suspension based on oil or preferably on alcohol, should be used. Diamond suspen-
sions are available with both polycrystalline and monocrystalline diamonds in the
range 45 ␮m to 0.05 ␮m. The grain sizes most used are 9 and 6 ␮m for fine grinding/
rough polishing and 3, 1, 0.25, 0.1, and 0.05 ␮m for polishing and final polishing.
The polycrystalline suspension is preferred if the highest removal rate and best
finish is wanted. This is due to the fact that the polycrystalline grains break down dur-
ing the process and in this way creates new cutting edges. Monocrystalline suspensions
are normally less expensive than polycrystalline, and the removal rate is considered to
be lower.
Normally the suspension is used in combination with a lubricant 共see Section 6.5兲.
In this way the adding of new grains and the establishment of a lubricating film are
separated, making it possible for a more exact dosing of both. Diamond suspensions,
also acting as lubricants, however, are available. Using these, only one product is added
to the grinding/polishing disk, establishing both a sufficient number of active grains
and a lubricating film.
Diamond Sprays
Both polycrystalline and monocrystalline diamonds are available in spray cans. The
advantage of using spray is the very small amount of “other material” introduced to the
process that are opposite of suspensions and pastes which contain a high amount of
carrier. Diamond sprays are available in the grain sizes 45, 25, 15, 9, and 6 ␮m for fine
grinding/rough polishing and 3, 1, and 0.25 ␮m for polishing.
Diamond Pastes
This is the original way of distributing the diamond, by rubbing a small amount of dia-
mond paste into the polishing cloth. For this reason diamond cannot be added during
the process and in certain cases, like working with a rigid composite disk 共RCD兲, the
paste will disturb the process.
A variation of paste is the stick, where the diamonds are placed in a harder wax;
this is easier to apply than paste. Pastes are available with both polycrystalline and
monocrystalline diamonds. The grain sizes available are 15, 9, and 6 ␮m for fine
grinding/rough polishing and 3, 1, and 0.25 ␮m for polishing
6.4.4 Cubic Boron Nitride „CBN…

Hardness: 4500 HV
CBN is made along the same lines as diamond, with high pressures and high tem-
peratures. The main reason why CBN is of interest as an abrasive is that it is much
more chemically stable than diamond in the presence of hot iron 共see Section 2.3兲.
CBN crystals are relatively smooth which makes bonding difficult. Therefore, the
grains are often coated with metal, suck as nickel.
CBN can be used in grinding disks in a metal or bakelite bond for very hard ferrous
metals.
6.4.5 Boron Carbide

Hardness: 2800 HV
Boron carbide 共B4C兲 was developed for grinding purposes, but for different rea-
sons the use is limited. It is used as a suspension for lapping purposes, the grain having
a porous structure with many sharp edges. B4C is seldom used in metallographic/
materialographic grinding and polishing.
6.4.6 Hardness of Abrasives and Materials—Table 6.1

Table 6.1 gives a comparison between the Vickers hardness of a number of materials to
be prepared and the abrasive materials used in the preparation process.
6.5 Grinding/Polishing Fluids—Lubricants

The most commonly used fluid for “traditional grinding” 共see Section 6.6兲, with grind-
ing stones and SiC wet grinding paper, is water with or without an additive. If the water
is recirculated, an additive should be used to prevent corrosion and reduce bacterial
growth in the water 共see Section 2.3.7兲.
For “contemporary grinding” 共see Section 6.7兲, using grinding disks with fixed
grains, water is also used, but in the case of fine grinding on rigid composite disks
共RCDs兲, lubricants, also called extenders 共normally used for polishing兲, are used. They
are described below.
6.5.1 Water-Based Lubricant

This lubricant is to be used if possible because it has no environmental effects. It is
suited for polishing of most materials using polishing cloths. In case of fine grinding on
rigid composite disks, the water-based lubricant should be dosed in small amounts to
avoid “aqua planing” where the specimen is planing on the fluid layer, not getting into
contact with the surface of the disk. For polishing of certain soft, ductile materials, a
water-oil based lubricant should be used 共see below兲.
6.5.2 Alcohol-Based Lubricant

This type of lubricant gives a high removal rate and a good cooling due to the fast
evaporation of the alcohol. For this reason this lubricant can be used as an alternative
for a water-based lubricant for work on rigid composite disks, which shall work “dry”
to secure that the specimen is in direct contact with the disk surface. An alcohol-based
lubricant should be used for materials that are sensitive to water.
Alcohol 共ethanol兲 is considered dangerous to health by inhalation and ingestion
and for this reason this lubricant should be avoided if possible.
TABLE 6.1—Hardness of Abrasives and Materials.
6.5.3 Water-oil Based Lubricant

This type of lubricant, water with an in-mixed oil forming an emulsion, will give a less
aggressive action between cloth/abrasive and specimen surface than the water- and
alcohol-based types. An oil film will act as a membrane between the polishing cloth and
specimen. The lubricant is used for polishing of soft, ductile materials. Because of the
oil, which might cause skin problems, the use should be as limited as possible.
6.5.4 Oil-Based Lubricant

This lubricant is a “lapping oil” based on mineral oil 共heavy petroleum distillate兲. Like
with the water-oil based lubricant mentioned above, it is used for soft, ductile materials
Fig. 6.10—Grinding stone for plane grinding, the grinding takes place on the top surface of
the stone.
to reduce the formation of deformations. Mineral oil may cause irritation by repeated
skin contact and by inhalation of vapors or aerosols, or both. For these reasons the use
should be limited or avoided, if possible.
6.6 Traditional Grinding

The expression “traditional grinding” covers the grinding methods used for a very long
time in metallographic/materialographic preparation: Grinding stones/disks with ce-
ramic or bakelite bonds and silicon carbide 共SiC兲, alumina 共Al2O3兲, and zirconium-
alumina wet grinding paper.
6.6.1 Grinding Stones/Disks
Grinding Stones for Plane Grinding of Metals

Grinding stones with aluminum oxide as abrasive and a ceramic bond are used mainly
for plane grinding when a relatively large amount of material shall be removed. The
wheel normally is of the recessed type 共see Fig. 6.10兲, the specimen holder being
pressed against the top surface of the stone.
The grinding stones change during the process, the main problems being uneven
wear and clogging of the surface. The stone has to be trued regularly to keep the surface
plane and dressed to remove material clogging the surface 共see Section 2.3.6兲. This is
usually done with a diamond truing device placed on the grinding machine.
Diamond Disks for Grinding of Very Hard Materials

Ceramics and other very hard materials have to be ground with diamond. This can be
grinding disks with a metal bond or a bakelite bond. The metal bond gives a relatively
rough surface of the specimen and the wear is relatively low. Bakelite bond produces a
specimen surface with less deformation but the wear is higher than by the metal bond.
Both types of diamond grinding disks are very expensive and only used for grinding of
sintered carbides, ceramics, and other very hard materials. In the past few years, a new
type of diamond disk with resin bonded fixed grains has been developed. These disks
are considerably less expensive and suited for a wide scale of materials 共see Section
6.7兲.
TABLE 6.2—Comparison between Grit Numbers according to

ANSI Standard B74.18 and FEPA “P” Standard 43-GB.
FEPA
Approx. Average Grain
“P”
Diameter
Standard
43-GB- ANSI
1984 R FEPA P ANSI B74.18-
1993 µm µm 2006
P60 269 268 60
P80 201 192 80
P100 162 141 100
P120 125 116 120
P150 100 93 150
P180 82 80 180
P220 68 67 220
P240 59
P280 52 52 240
P320 46
P360 41 42 280
P400 35 34 320
P500 30
P600 26 27 360
P800 22 22 400
P1000 18 16 500
P1200 15 13 600
P1500 13
P2000 10
P2500 (P2400) 8.4 6.5 (800)
(P4000) 5 5 (1200)
6.6.2 SiC Wet Grinding Paper—Table 6.2

SiC paper is the traditional grinding medium, used since the 1950s, both for plane
grinding and fine grinding. SiC grinding paper is made of a waterproof paper backing
with a layer of SiC abrasive grains. As shown in Fig. 6.11, an adhesive layer called the
make coat is first applied to the backing before the abrasive grains are applied. As the
backing material passes through a strong electrostatic field the particles are oriented
with their longest dimension in the vertical direction. This provides good grain reten-
tion and also orients the particles with their sharpest edges upwards. A second layer of
adhesive, called the size coat, is then applied over the entire assembly.
Fig. 6.11—Schematic drawing of cross section of SiC grinding paper.

The paper backing can be of A-type, relatively thin, and C-type, which is somewhat
thicker. Type C is normally used for metallographic/materialographic grinding. The pa-
per is supplied as disks in the diameters 200 mm 共8 in兲, 230 mm 共9 in兲, 250 mm
共10 in兲, and 300 mm 共12 in兲.
The SiC abrasive is classified according to standards established by ANSI 共Ameri-
can National Standard Institute兲 and FEPA 共Federation of European Abrasive Produc-
ers兲. The grit sizes are split into two categories: macrogrits and microgrits.
Macrogrits ranging from grit 12 to grit 220 are determined by sieving, the grit
number indicating the number of openings per square inch. Macrogrits are the same in
the ANSI standard and the FEPA standard, the FEPA designation having a P before the
number.
Microgrits ranging from grit 240 to grit 4000 are determined by sedimentation,
and the grit numbers covering a specific grain size are not the same in the two stan-
dards 共see Table 6.2兲.
Comparison Between Standard Grits—Table 6.2

In practical preparation a selection of grits is used. The suppliers of consumables for
metallographic/materialographic preparation supply both according to the American
and European Standards. In Table 6.2, the most commonly used grits are shown for
comparison 共P2400 and P4000 are not FEPA designations, 800 and 1200 are not ANSI
designations兲.
Plane Grinding
For plane grinding the grits 120 共P120兲, 180 共P180兲, 220 共P220兲, or 240 共P280兲 normally
are used. As mentioned above, the finest possible grit should be chosen to limit the de-
formation of specimen surface 共see below兲. When using SiC paper, the last plane-
grinding step should be grit 220 or 240 共P220 or P280兲 to be sure of the correct result
共reproducibility兲 of the following preparation method. Considering that each sheet of
paper is only grinding efficiently in 20– 60 s, depending on the material to be ground,
often several sheets must be used to secure a totally plane specimen surface co-planar
to the grinding surface.
Fine Grinding
For fine grinding, three to four steps based on the following grits are used typically: 280
共P320兲, 320 共P360兲, 360 共P500兲, 400 共P600兲, 500 共P1000兲, 600 共P1200兲, 800 共P2400/
P2500兲, 1200 共P4000兲. A normal fine grinding sequence could be 320–400–600 using
ANSI-designated paper or P320, P500, P1200 using FEPA designated paper.
In the case of soft ductile materials, one or two fine steps can be added, 800, 1200
共ANSI兲 or P2400/P2500, P4000 共FEPA兲.
Material Removal
The material removal rate for SiC paper is relatively high as long as the paper is not
worn down. This is due to the abrasive grains being rather exposed and having a good
space in between, allowing for the chips to be produced and taken away by the water
flow. This is opposite to dry grinding on emery paper, which will very soon have a
clogged surface causing deformations and material flow in the specimen surface.
Because of the brittleness of the SiC and the relatively high load on the grains, they
break down caused by fractioning and wear. In Fig. 6.12 this is shown schematically,
the SiC grains with different rake angles are broken and worn, creating new, negative
Fig. 6.12—Schematic drawing of grains on a SiC paper with different rake angles, as new and
after 30–60 s use, the gray parts are worn away or fractured.
rake angles resulting in a loss of cutting action.29 This develops in 20– 60 s or longer,
depending on the material to be ground, hard materials strongly reducing the time.
According to tests made by Samuels7 the removal rate when grinding some metals like
copper and copper alloys, aluminum and aluminum alloys, silver and titanium stays
constant over a long period of time, and for some metals like nickel-chromium austen-
itic steels, nickel and nickel alloys, titanium alloys, chromium and gold, a deterioration
in removal rate occurs in the first minutes and is followed by a period of relatively high
material removal. These tests were based on a single specimen at a time, whereas in
modern preparation three to six specimens often are ground at the same time, conse-
quently reducing the lifetime of the paper.
In Fig. 6.13, an SEM micrograph shows the single grains of a 220 grit SiC paper
with the different shapes and sizes. Also the large variation in contacting points and
rake angles can be seen. At 220 grit, the median grain size is 63 ␮m and the largest
allowed grain size is 74 ␮m. Because of this large variation in shape and size, only
around 5–10 % of the many visible contacting points of the grinding paper actually get
in contact with the specimen surface. Only a fraction of these points are able to remove
material from the surface. Samuels7 estimates that less than 1 in 1000 of the grains
visible can be expected to actually remove material. During the process when the SiC
grains break down, the cutting effect will change into plowing, shown in Figs. 6.3 and
6.14. At certain soft, ductile materials, grains or parts of fractured grains can be embed-
ded in the specimen surface 共see Fig. 2.1 and Section 13.6.4兲.
Deformation
As shown in Section 6.3, a 220 grit SiC paper will induce a relatively strong deforma-
tion of the specimen surface. This is mostly because of the single large SiC grains being
very aggressive in the first seconds of the grinding process. Figure 6.14 shows a com-
parison between an SiC grinding paper and a grinding disk with diamond abrasive
grains in a resin bond. The situation after 2 – 5 s, 共a兲 Fig. 6.14 shows the introduction of
Fig. 6.13—SEM micrograph of a P220 SiC paper. The irregular shapes of the grains and the
variety in grain size can be seen.
the deep deformations by the paper, whereas the grinding disk with grains embedded
in a bond gives more moderate deformation.
Edge Retention—Relief
In Section 3.1.3 edge retention is discussed, concentrating on mounting. Another im-
portant aspect is the resilience of the substrate, the surface, used for the grinding/
polishing. To totally avoid a rounding of edges, a hard substrate without resilience
must be used. SiC paper has some resilience because the paper backing has a certain
flexibility, but in most cases a sufficient planeness can be obtained for most materials.
In more extreme cases, however, where edge rounding or relief, or both, must be abso-
lutely avoided, SiC paper might have too much resilience. In Figs. 6.15 and 6.16 grit 220
SiC paper is compared to a diamond grinding disk with the same grain size, having
almost no resilience. In Fig. 6.15, two unmounted, similar specimens are compared.
The specimen on the SiC paper was rounded due to resilience of the paper backing; the
specimen on the diamond disk is not rounded due to the very low resilience of the disk.
Even with mounted specimens, SiC paper in certain extreme cases will create a round-
Fig. 6.14—Comparison of surface deformation using SiC paper and a resin bonded diamond
disk. After 2 – 5 s 共a兲 single large grains of the SiC paper give deep deformations, after 30 s 共b兲
the SiC grains are wearing down, and after 60 s 共c兲 the SiC grains are worn down creating
plowing, causing deformation, see Section 6.2.1. The diamond grinding disk gives less
deformation and remains almost constant during the process.
ing of the specimen or a relief of the specimen surface. In Fig. 6.16 a drawing of a me-
dium hard, nitrided steel, mounted in epoxy resin, is shown. When prepared on SiC
paper, the SiC particles grind away the surface irregularly due to the high differences in
hardness between the nitrided layer and the core steel. Because of the limited differ-
ence in hardness between the nitrided layer and the SiC particles and the resilience of
Fig. 6.15—Comparison between SiC grinding paper and a resin bonded diamond disk. The SiC
paper has a relatively high resilience, and an edge rounding is introduced on an unmounted
specimen. The diamond disk has no resilience and gives no rounding.
the paper backing, the layer protrudes above the surface of the specimen due to the
relatively low rate of material removal. The diamond disk cuts all parts of the surface
uniformly due to the extreme hardness of the diamond particles and the lack of
resilience.
Environment—Economy
As mentioned above the efficient grinding time to a high degree depends on the speci-
men material and the number of specimens prepared at the same time. At soft and me-
dium hard materials the total plane and fine grinding might be performed with only
four sheets of paper, but at hard materials, especially with several specimens in a
holder, several sheets of each grain size must be used. In case of a high production of
specimens this is relatively costly and it will cause a relatively high amount of waste. As
a waste substance, the SiC paper is neutral.
6.6.3 Alumina—Zirconia Alumina Wet Grinding Paper

Using alumina or zirconia alumina instead of SiC as the abrasive, a longer efficient
grinding time is obtained. The alumina grinding paper is available in grit 120 and the
zirconia alumina papers are available in the grits 60 共P60兲, 80 共P80兲, 120 共P120兲, and
180 共P180兲, and consequently they are only for plane grinding. Due to the longer effi-
cient grinding time they are especially suited for automatic preparation using speci-
men holders with many specimens.
The influence on the specimen surface is as described under SiC paper.
Fig. 6.16—Comparison of edge rounding and relief with a mounted specimen with a hard
surface layer prepared on SiC paper and a resin bonded diamond disk. At the SiC paper a relief
develops between the hard layer and the mounting material/basic material.
6.7 Contemporary Grinding

“Traditional” grinding described in the previous section has a number of drawbacks,
especially when used for semiautomatic and fully automatic preparation. For this rea-
son “contemporary” grinding has been developed, in this way eliminating or reducing
the drawbacks:
• Quality of specimen surface: Better edge retention, less deformation.
• Constant removal rate: Fewer steps and higher reproducibility.
• Less handling: By using fewer steps, and using automatic preparation systems,
handling is reduced to a minimum and operation time is saved.
• Less waste: By using longer lasting consumables, the amount of waste is reduced.
In short it can be said that with contemporary grinding it is possible to prepare
specimens with extreme hardness differences as a routine process. These specimens
could only be prepared with great difficulty using the traditional methods. The grind-
ing media used for contemporary grinding are almost all based on diamond as the
abrasive, either as fixed 共bonded兲 in the surface of a rigid grinding disk, or added during
the process on a rigid composite grinding disk 共rigid composite disk 共RCD兲兲. The prod-
ucts are supplied as disks in the diameters 200 mm 共8 in兲, 250 mm 共10 in兲, 300 mm
共12 in兲, and 350 mm 共14 in兲.
6.7.1 Magnetic Fixation

As part of the development of the products for advanced preparation, it was important
also to avoid the relatively troublesome handling of grinding papers and polishing
cloths with adhesive back. For this purpose magnetic systems were developed using a
Fig. 6.17—Resin bonded diamond disk for magnetic fixation on a support disk with a
permanent magnet.
supporting disk with a permanent magnet foil on which the substrate, a grinding disk
or polishing cloth, made with a ferromagnetic backing, is fixed 共see Fig. 6.17兲. The hold-
ing power is very high in the direction parallel to the supporting disk, in this way keep-
ing the substrate on the disk, but vertically the holding power is low enabling the opera-
tor to easily remove the substrate. A further advantage is the use of only one supporting
disk for all grinding/polishing steps instead of changing the supporting disk for each
step. Normally the magnetic supporting disk is made especially for that purpose, but it
is possible to convert a normal metal grinding/polishing disk by placing a magnetic foil
with adhesive back on the disk. The drawbacks are an increase in the disk thickness,
and after some time, the foil might loosen due to attack from liquids during the prepa-
ration process.
6.7.2 Resin-Bonded Diamond Grinding Disks

Section 6.6.1 describes conventional diamond disks. These have either a metal or
bakelite bond and because of the high price and careful maintenance 共truing is impor-
tant to keep the surface plane兲, they are only used for very hard materials, harder than
600 HV 共55 HRC兲, where SiC and Al2O3 are not hard enough. Diamond as an abrasive,
however, would be ideal for grinding of softer materials.
In the past five to ten years, a new type of diamond grinding disk has been devel-
oped, taking advantage of the hard diamond, but supplied at a reasonable price, which
matches the SiC grinding paper. The disk is suitable for materials harder than HV 150.
The cost is kept low because the diamonds are fixed only in a thin layer in a resin bond
and placed in segments on the surface of the disk as shown in Fig. 6.17
The figure shows how the disk is fixed to the supporting disk by a permanent mag-
net, as described above, but the disk can also be fixed by a double adhesive foil placed
on a normal grinding/polishing disk.
The bond keeping the diamond grains, Fig. 6.18, is made so that it allows the grains
to leave the surface when the grain is worn. The disk is used with water like SiC paper.
Using only a thin layer of bond with diamonds, the disk needs not to be trued, when the
layer is worn away at the center of the disk the disk is discarded, see Section 6.7.7 for a
more extensive description of this wear. Only a dressing of the surface with a dressing
stick is needed if the surface is clogged.
Plane Grinding
The disks are used for plane grinding, using the same grain sizes as for SiC paper, grit
80 共P80兲 to 220 共P220兲. Because of the constant removal rate 共see below兲 the whole
grinding sequence can take place in one operation, even when much material shall be
removed and the material has a high hardness.
Fig. 6.18—Resin bonded diamond disk. Diamond grains placed in a bond.
Fine Grinding
The disks can also be used for fine grinding in the grit sizes 360 共P600兲 and 600 共P1200兲.
Material Removal
The disks have a relatively high, constant removal rate securing that the grinding pro-
cess can be finished without interruptions. This is due to the high hardness of the dia-
monds and the ability of the bond to break down, releasing fresh abrasive grains.
Deformation
The diamond grains, being of a more regular shape and with a closer tolerance of the
grain size than SiC grains, will produce less deformation than SiC paper, as shown in
Fig. 6.14. Also the position of the grains, placed in a bond 共see Fig. 6.18兲 gives less im-
pact when touching the specimen surface, creating less deformation. The segmented
surface, with grooves to lead away the swarf, is important to avoid smearing of the
specimen surface.
Edge retention, to a high degree depending on the resilience of the disk, is very good.
The resin bond is relatively hard and unflexible 共see Figs. 6.15 and 6.16兲 and the very
hard diamonds are able to remove material even from very hard phases in the speci-
men surface, avoiding relief
The diamond disk as described above has very little environmental impact when dis-
carded. It only consists of a thin, tinned steel plate 共as used for canned food兲 and a very
thin layer of synthetic resin
Depending on the material to be prepared, one disk is equivalent to 100 sheets of
SiC paper or more, making the cost comparable to the cost of SiC paper.
6.7.3 Resin-Bonded SiC Grinding Disks

The diamond disks described above are only suited for materials harder than HV 150.
Therefore, disks have been developed with SiC as an abrasive suited for softer materi-
als. In general, the above description of the diamond grinding disks also covers the SiC
grinding disks.
6.7.4 Metal-Bonded Diamond-Coated Disks

These types of disks are different from the conventional metal-bonded disks. The dia-
mond abrasive is placed in a very thin layer on a metal surface and bonded 共coated兲
with a layer of nickel.
These disks can be used for the softest to the hardest materials, but they are not
used much because the cost per prepared specimen is high.
6.7.5 Diamond Pads

This product, originally developed for grinding/polishing of glass, uses the diamond in
a metal or bakelite bond in a dot matrix covering the surface of the pad.
The metal bond is only suited for plane grinding of ceramics, sintered carbides,
and other very hard materials. The grain size varies from 250 ␮m in steps down to
20 ␮m. The bakelite bond can be used for fine grinding of hard materials, being avail-
able in grain sizes 30, 10, and 2 ␮m.
Dressing: It is important that the diamond pads are dressed regularly with a dress-
ing stick, normally Al2O3 or SiC in a ceramic bond. This is to open the surface of the
disk when clogging has taken place 共see Section 2.3.6兲.
6.7.6 Diamond/CBN/Al2O3 / SiC Film

In the case of preparation of microelectronic devices, wafers, optical fibers, and certain
ceramics where extreme flatness and very low deformation is needed, films 共lapping
films兲 coated with diamond, CBN, Al2O3, or SiC can be used.
The very accurately graded abrasive is coated on a thin polyester film either for
gluing 共PSA兲 or for adhering only using water 共plain back兲. The films are used wet or dry
and they are available both with a continuous layer of abrasive and with the abrasive as
dots allowing the swarf to flow away. The film with dots 共ceramic beads兲 gives a higher
material removal, a longer life, and a coarser finish, compared to films with a continu-
ous layer.
The films are available in steps from 30 ␮m down to 0.05 ␮m.
6.7.7 Rigid Composite Disks

Since the 1970s, the rigid composite disk 共RCD兲 has been available for materialo-
graphic preparation. The RCD has the advantage of making very flat specimens with a
constant removal rate and relatively little deformation, and this makes the RCD very
well suited for fine grinding of most materials. During the process on an RCD, a dia-
mond suspension is continuously added. This is known from lapping, a very common
abrasive machining process used in the industry to produce flat surfaces. Normal lap-
ping takes place on cast iron disks and the surface obtained is not suited for
metallography/materialography 共see below兲. The surface of an RCD consists of a resin
with mixed-in metal powder in different grain sizes, and it seems to be the effect of this
surface which changes the process taking place on an RCD, from lapping to grinding.
To explain the mechanisms of an RCD, a comparison was made between lapping 共loose
grains兲 on a glass disk, grinding on a diamond film 共fixed grains兲, and grinding on two
RCDs of different hardness.30
Experiment: Lapping Versus Grinding

The scratch pattern of the specimen surface created with an RCD is similar to a surface
made with grinding paper, apparently ground, with grinding defined as a process with
Fig. 6.19—Pattern of scratches and deformations after grinding on a diamond film. SEM.
fixed abrasive grains, each grain acting as a machine tool producing a chip. This seems
strange because when using an RCD, the abrasive, mostly diamond with a grain size of
6 – 9 ␮m, is added during the process. Normally these loose grains should create a lap-
ping, defined as a process with loose abrasive grains, rolling and flowing in nearly a
single layer between specimen surface and disk, and not a grinding. At lapping, the
corner of the rolling grain digs into the specimen surface, the grain tumbles onto an
edge, and then another corner contacts the specimen, and so on. Lapping is considered
less appropriate for metallographic/materialographic preparation because the re-
moval rate is low, and the specimen surface is rather strongly deformed.
A steel specimen with a high finish was used for all parts of the experiment. Grind-
ing took place on a diamond film, 9 ␮m, to secure a perfect grinding. For the lapping a
floated glass disk with an alcohol/water diamond suspension was used with 9 ␮m of
the same type of diamonds used on the film, added during the process. The RCD pro-
cess was performed on two RCDs, RCD 1 and 2, both of the disposable type 共see below兲
with the composite placed in segments on the disk surface 共see Fig. 6.27 below兲. RCD 1
was with metal powder composite 共relatively hard and aggressive兲, and RCD 2 was with
a composite without metal powder, which is relatively soft and with less aggressive ma-
terial removal. For both RCDs the diamond suspension mentioned above was used.
All the resulting surfaces were analyzed in an SEM.
The results showed that the specimen ground on the film showed a typical grind-
ing pattern with scratches in all directions 共Fig. 6.19兲. To the naked eye the surface was
relatively bright.
The specimen lapped on the glass plate showed a typical lapping pattern with two
distinct features 共Fig. 6.20兲. The freely moving 共rolling兲 diamond grains have made a
relief with cavities in the surface, and a few very large scratches have been produced,
probably due to single grains fixed in the surface of the glass disk. It can be seen that the
lapped surface is considerably rougher than the ground surface 共Fig. 6.19兲. To the na-
ked eye the surface was dull.
The specimen prepared on RCD 1 共Fig. 6.21兲 has scratches very similar to the
Fig. 6.20—Pattern of scratches and deformations after lapping on a glass plate. SEM.
scratches initiated by grinding 共Fig. 6.19兲, only a little larger. The surface is reasonably
plane between the scratches. To the naked eye the surface was relatively bright.
The specimen prepared on RCD 2 共Fig. 6.22兲 has almost the same scratch pattern
as at grinding 共Fig. 6.19兲. It is finer than the RCD 1 pattern due to the fact that RCD 1 is a
more aggressive RCD. This also can be seen from the removal rates 共see below and Fig.
6.23兲. To the naked eye the surface was relatively bright.
The conclusion of the SEM analysis is that according to the scratch pattern, the
same process takes place when grinding on a film with fixed diamond grains and on an
RCD surface with loose grains added during the process.
The removal rate was also measured, defined as material removal in ␮m per 300 m
共movement of specimen on the grinding/lapping surface兲共see Fig. 6.23兲. It can be seen
that the diamond film is very active during the first approximately 50 m and wears out
after approximately 250 m. The glass disk has a relatively constant removal rate during
the whole distance and the same is the case with the two RCDs. This is because the
abrasive is added during the whole process. The aggressive RCD 1 shows a higher re-
moval rate than the other three surfaces.
Based on the above experiment, a suggestion for the mechanisms taking place dur-
ing the processes was made and a model proposed.
Lapping on a hard, homogenous disk: It is beyond doubt that the process with roll-
ing grains makes indentations in the specimen material, in this way breaking particles
out of the surface 共Figs. 6.20 and 6.24兲. A fractured, indented, dull surface can be seen
only with a few scratches. A few grains will penetrate into the surface of the disk and
produce a scratch like grain 共b兲 in Fig. 6.24.
Process on an RCD: On an RCD the surface is very much softer than the sample
material. This means that the abrasive grain is pressed into the disk surface so that a
rolling is prevented and a process, creating chips like at grinding, takes place. Only a
very small number of grains are rolling 共see Fig. 6.25兲. According to Samuels7 it seems
that the abrasive grains embed in the upper regions of the edge faces of the segments
where they can contact the specimen surface.
Fig. 6.21—Pattern of scratches and deformations after grinding on a hard rigid composite disk
共RCD兲. SEM.
At RCD 1, the surface consists to a high degree of metal powder 共Fig. 6.25兲. This
gives a variation in surface hardness, and the abrasive will penetrate differently into
the surface, less in the metal particles. This means that the grain is able to make a larger
chip, counting for the higher removal rate of RCD 1. In the case of RCD 2 with a consid-
erably softer surface, the abrasive grains penetrate deeper into the disk resulting in a
smaller effective diamond size, and the abrasive is held more firmly, which is important
when grinding ductile materials.
Rigid Composite Disks „RCD… for Longtime Use

The original RCDs were made as solid disks with a thick layer of composite material,
consisting of a synthetic resin with mixed-in metal powder 共iron, copper兲, or a mineral
powder like Al2O3. The surface can be with segments of different composites and with
grooves of different types to remove the swarf during the process.
The disks can be used for plane grinding with 30– 45 ␮m, but they are mostly used
for fine grinding with 6 to 9 ␮m diamond suspension added during the process. The
process has to run relatively dry, with a minimum of lubricant added during the pro-
cess. As the disk surface texture turns smooth during use, a dressing is necessary with
intervals to regain a rough surface and thereby secure the removal rate.
The disks are difficult to use for hand preparation and are normally used with a
semiautomatic specimen mover 共see Section 6.8兲. Most specimen movers work with
the specimen holder placed eccentrically on the grinding disk 共see Polishing Dynamics
共Section 7.9.2兲. This eccentricity causes a wear concentrated around the center of the
disk, making it concave 共Fig. 6.26兲. This unevenness will, when exceeding
100– 200 ␮m, cause an unevenness of the specimens and the effect of the disk will be
reduced. The concave surface must be trued to regain the planeness and this is mostly
done with a truing tool using diamond. Due to this rather laborious truing, many RCDs
were not used and the use of SiC paper was preferred.
The development of the thin, disposable RCD changed this situation.
Fig. 6.22—Pattern of scratches and deformations after grinding on a soft rigid composite disk
共RCD兲. SEM.
Rigid Composite Disk, Disposable

Taking into consideration the advantages of the RCD, it was evident that an RCD with-
out the drawbacks mentioned above, and even compatible with SiC paper, should be
developed.
This was done with the disposable RCD, consisting of a tinned steel foil or a steel
plate with segments of composite material. This is fixed magnetically to a supporting
disk with a permanent magnet 共Fig. 6.27兲. The disposable RCD is made in two versions,
one relatively aggressive for materials harder than 150– 200 HV and a softer one for
softer materials in the 40– 250 HV range and for composite materials.
Plane Grinding
The disposable RCD is normally not suited for plane grinding because it should not be
used with diamond grain sizes larger than 15 ␮m. In some cases, however, when work-
Fig. 6.23—Comparison of removal rates of specimens after grinding on a diamond film,

lapping on a glass plate and grinding on a hard and a soft RCD.
Fig. 6.24—Schematic drawing of a lapping process. The abrasive grains are loose and rolls
between the specimen and the lapping disk. A corner of the grain digs into the specimen
surface, and the grain tumbles onto an edge. A track of angular indentations 共cavities兲 is
produced in the specimen surface.
ing with “single-specimen preparation,” 共see Section 7.9.1兲 the amount of material to
remove at this stage is so low that grinding with a hard RCD using 9-␮m diamond sus-
pension can be considered a “plane grinding.”
Fine Grinding
The disposable RCD is made for fine grinding with diamond suspension 9, 6, or 3 ␮m.
The total fine grinding stage can be performed usually in only one step in 2 – 4 min and
the specimen is ready for the first polishing step.
Material Removal
The removal rate is considerably higher than at a conventional RCD. This is mostly
because the disposable RCD works at a higher specific pressure and the removed mate-
rial 共swarf兲 is efficiently removed through the channels between the segments. Also, it
Fig. 6.25—Schematic drawing of a material removal process on a rigid composite disk 共RCD兲.
The majority of the abrasive grains are fixed in the surface of the disk 共grinding兲; only a small
amount is moving 共lapping兲.
Fig. 6.26—Wear pattern of grinding/polishing disk. Due to the geometry of disk and specimen
holder, the wear around the center of the disk is stronger than at the periphery, causing a
concave disk surface, after a certain preparation time.
shall not be dressed during use, but keeps its surface texture during the whole lifetime,
securing a constant removal rate. The material removal varies with material type and
type of RCD. The hard, more aggressive type has the highest removal rate 共see Fig.
6.23兲.
Deformation
Using diamonds 共9 – 6 ␮m兲 with a narrow tolerance on the relatively flexible RCD sur-
face, the grain, momentarily fixed in the surface, will not have the same damaging im-
pact on the specimen surface as with fixed grains 共SiC paper兲. Also, by varying the
amount of metal in the composite, the aggressiveness of the surface can be minimized
which is very important with soft materials.
The composite material, although “microflexible,” will be rigid and plane as a total sur-
face. This, together with the high cutting capacity of the diamond grains, will give a
very good edge retention and practically no relief.
Wear
As described earlier, an RCD turns concave during use 共see Fig. 6.26兲. To avoid the
troublesome truing of the surface, the disposable RCD is discarded when the segments
around the center of the disk are worn away, showing the user that the difference in
planeness between periphery and center is so high that uneven specimens will be
produced.
Fig. 6.27—Disposable rigid composite grinding disc 共RCD兲 magnetically fixed to a support disc
with a permanent magnet.
The disposable RCD can be compared with a piece of tin plate or a thin stainless steel
plate with a layer of paint, and it can be disposed of like a normal tin can or metal piece.
The price per specimen using the RCD depends on the material to be prepared, but
at normal use more than 100 specimen holders can be prepared on one RCD.
6.7.8 Fine Grinding Cloths

When using very hard cloths, absolutely without nap, like nonwoven chemo textiles
and nylon, with diamond suspension or spray/paste of a grain size of 9 ␮m or larger,
the process can be defined as “fine grinding” if the pressure on the specimen is high.
Polishing can be defined as grinding producing very small chips and is explained
further in Chapter 7. In the above-mentioned case, however, a material removal similar
to grinding can be obtained.
The materials used for the fine grinding cloths are stainless steel mesh, woven
polyester, woven silk, woven nylon, and nonwoven synthetics. These are all without
nap and used with 15, 9, 6, or 3 ␮m diamond suspension or spray 共see Section 7.4兲.
With the introduction of rigid composite disks 共RCDs兲 for soft materials 共see Sec-
tion 6.7.7兲, the use of these cloths has been reduced.
Material Removal
The removal rate is not as high as with an RCD, but higher than at a normal polishing
step.
Deformation
The deformation is much lower than at grinding on a disk with fixed abrasives. It is
comparable to the deformation created by an RCD 共see Section 6.7.7兲.
Due to the relatively high resilience of the cloths, except the steel mesh, a certain edge
rounding and relief might develop.
All materials mentioned above can be discarded as normal waste; the cost per speci-
men is comparable to SiC paper.
6.8 Grinding/Polishing Equipment

Mechanical grinding and polishing are normally performed on the same type of ma-
chines.
Fig. 6.28—Polisher/grinder with two disks 共200/ 250 mm 共4 / 6 in兲 diameter兲 and 300 rpm for
manual preparation.20
Only in a few cases machines only for grinding 共mostly plane grinding兲 are sup-
plied. For this reason only equipment that can be described as “grinders” are included
in this section. The grinders/polishers are described in Sections 7.8 and 7.9.
6.8.1 Plane Grinding
Manual Grinding
Plane grinding using grit 220 共240兲 or coarser can be done by hand on a rotating disk of
a 200- 250- 300 mm 共8 - 10- 12 in兲 diameter disk with a grinding paper. The paper can
be placed with a plain back in a water-filled disk, and the paper is sucked to the disk
when rotating due to the centrifugal force, which moves the water to the outside of the
paper. The paper may also have a self-adhesive backing or a double-adhesive foil can be
used.
For the technique of manual 共hand兲 grinding see Section 13.2.4.
Fig. 6.29—Belt grinder with two workstations for coarse grinding. Adjustable water flow and
sink.19
Fig. 6.30—Semiautomatic grinding machine 共grinding stone兲 for plane grinding with specimen
holders. Diameter of grinding stone 356 mm 共14 in兲, 1450 rpm.20
Machines with one or two disks are available and used for both grinding and pol-
ishing; two disks can be of advantage when using four steps for grinding with SiC pa-
per. Figure 6.28 shows a two-disk grinder/polisher 共250 mm 共10 in兲 disk diameter兲 with
a single speed, 300 rpm, for hand grinding on SiC grinding paper.
For a more effective grinding by hand, a belt grinder can be used, built with one or
two work stations. The belt grinder works with a belt moving on two rolls and with a
flow of water; it can be used for both plane and fine grinding. Figure 6.29 shows a belt
grinder with two work stations, water flow system and sink.
Automatic Grinding
Plane grinding of specimen holders with six or more specimens can be done on most
automatic systems, which are described in Section 7.9.
At very large holders with large specimens, it can be an advantage to plane grind on
Fig. 6.31—Four stage hand-grinder for wet grinding on four strips of grinding paper in rolls.19
a grinding stone with a relatively high speed 共1450 rpm兲 and a diameter of 356 mm
共14 in兲. The machine, shown in Fig. 6.30, is only for plane grinding and fine grinding/
polishing must take place on another automatic grinder/polisher.
6.8.2 Fine Grinding
Manual Grinding
Fine grinding by hand takes place on equipment spanning from simple apparatus with
four strips of grinding paper 共Fig. 6.31兲, to rotating grinder/polisher as mentioned un-
der plane grinding 共Fig. 6.28兲. Figure 6.31 shows a four stage hand-grinding apparatus
with four strips of SiC grinding paper supplied from rolls for plane and fine grinding.
Automatic Grinding
Fine grinding of specimen holders either with a number of fixed specimens 共central
force兲 or individually loaded 共single force兲 takes place on semi- or full-automatic
grinders/polishers described in Section 7.9
Automatic grinding/polishing systems have gained ground because they reduce
the work load on the metallographer and produce an overall better specimen quality.
Also, the reproducibility is improved, securing that if a certain method is followed, the
result always is consistent.
7
Mechanical Surface
Preparation—Polishing
7.1 Polishing: Producing the True Structure
AFTER PLANE GRINDING AND FINE GRINDING THE SPECIMEN SURFACE
must be polished to obtain the true microstructure or a structure, which is satisfactory
for a given analysis. In principle, the surface always will have a certain deformation
共artifacts兲, but if not too deep this can often be removed through the etching of the sur-
face 共see Chapter 9兲. For a thorough description of artifacts and how to avoid them, see
Section 13.5/6.
This chapter covers mechanical polishing and chemical mechanical polishing
共CMP兲. Electrolytical and chemical polishing are described in Chapter 8.
Mechanical polishing is defined as a material removing process with loose abra-
sive grains placed on a substrate like a polishing cloth. The abrasive can be added be-
fore or during the process and normally lubricant is applied during the process for lu-
brication and cooling.
CMP can be defined as a material removal process where the material removal
takes place chemically and mechanically at the same time 共see Section 7.12兲.
Mechanical polishing is by far the most used process, and depending on the type of
material and the nature of the preceding fine grinding step, one or several polishing
steps are needed 共see Fig. 1.7兲.
7.1.1 Rough Polishing

This step immediately follows the last fine grinding step and is usually done on a hard,
napless cloth with 9 or 6 ␮m diamond. This step can be compared to the last step of fine
grinding done on a hard, napless cloth 共see Section 6.7.8兲. The rough polishing step is
very important because most of the material, damaged by the grinding, is removed in
this step 共see Table 7.1兲.
7.1.2 Polishing
The polishing is done in one to three steps with hard, medium hard, or soft cloths with
diamond 3 – 0.25 ␮m or finer polishing media, such as silica and alumina, 0.1– 0.05 ␮m
共see Section 7.5兲, depending on the material to be polished.
7.2 Material Removal

The process of material removal during polishing, micromachining, is considered to
be the same as it is during grinding 共see Section 6.2兲. According to Samuels7 it seems
that another mechanism, delamination, takes place when polishing with diamond
abrasives below 3 ␮m. Delamination does not produce the elongated chips that result
from micromachining, but small, plate-shaped equiaxed particles are produced. No ex-
120
Chapter 7 Mechanical Surface Preparation 121
Fig. 7.1—Schematic drawing of an abrasive grain fixed in a fiber of a polishing cloth.
planations have been advanced for the mechanism by which delamination occurs dur-
ing the polishing with the smallest grain sizes.
At micromachining, the abrasive grain is able to produce a chip, implying that the
grain is, at least momentarily, fixed in the polishing cloth, as shown schematically in
Fig. 7.1. The diamond grain wedges between the cloth fibers with a rake angle sufficient
to be able to cut a chip from the specimen surface. To obtain a high removal rate at
rough polishing, hard cloths are used, creating a higher load on the grain, giving a
larger chip. Using softer, more resilient cloths for the final steps, the load on the grain is
reduced, causing smaller scratches and less deformation of the specimen surface.
7.2.1 Influence of Polishing Abrasive on Removal Rate

For grinding, the hardness of the abrasive is important. Therefore, diamond is used for
both rough polishing and polishing. For final polishing, alumina 共Al2O3兲, colloidal
silica 共SiO2兲, and magnesia 共MgO兲 are also used.
Likewise, the shape of the grain plays a role. Polycrystalline diamonds give a
higher removal rate than monocrystalline diamonds,7 probably because the individual
polycrystalline grain contains more angular points of the size needed to provide cut-
ting points than those of monocrystalline.

In principle, the removal rate increases linearly with the increase in specific pressure
between specimen surface and the polishing surface once a certain low threshold value
has been exceeded. Using a high force causing a high specific pressure might create a
rounding of the specimen, and often the lubrication will not be satisfactory and heat
might develop. Also, an increased wear of the polishing cloth will take place. For nap-
less, hard cloths the specific pressure should be in the range of 30 to 100 kPa
共4.35 to 14.5 psi兲; for softer cloths the pressure should be 15 to 50 kPa 共2.2 to 7.25
psi兲. Experience has shown that in specimens from 40 mm 共1.5 in兲 diameter and up,
the force per specimen should not exceed 50 N 共11.5 lbf兲 to avoid overheating of the
cloth and excessive wear. To compensate, the polishing time may be extended
1 to 4 min.
7.3 Deformation
Polishing, as mentioned earlier, in principle being the same process as grinding, will
produce shallower deformed layers. With hard cloths with a low resilience, a stronger
deformation will develop than with softer cloths. The depth of the deformed layers is
an order of magnitude smaller than that on surfaces ground with SiC paper, as shown
by Samuels7 共see Table 7.1兲. This shows the importance of the rough polishing step
共6 ␮m diamond兲.
For explanations of Dsb, Ds, and Dd see Section 6.3.1.
In theory, even the finest abrasive will create a deformed layer. It is, however, pos-
sible to obtain a surface very close to the true structure with the use of very fine abra-
sives like alumina 共Al2O3兲 and silica 共SiO2兲 for the final polishing step. Silica, having a
carrier liquid with a pH in the range of 8.5 to 11 共see Section 7.5.5兲 and a grain size of a
fraction of a micron, will create a combined mechanical and chemical material re-
moval 共see Section 7.12兲.
Deformation in the form of smearing can take place with soft metals, the material
being smeared across the surface. For this and other types of deformation, see Section
13.6.
In the literature, the very thin deformed layer left by the last polishing step is often
called the Beilby Layer. The existence of such a layer is not supported by recent re-
search and the use of this term should be avoided; however, to give an impression of the
mechanisms taking place, a short description of the theories by Beilby31 and Samuels7
will be given in the following section.
7.3.1 The Beilby Layer

At the beginning of the 20th century, Sir George Beilby established the theory of the
so-called Beilby layer. This layer was proposed to be of an amorphous nature created by
a smeared layer that had passed through the liquid state 共Fig. 7.2兲.31
The layer would fill out the existing scratches and give the surface its mirror-like
character. The layer was thought to have developed due to the very high temperatures
TABLE 7.1—Depth of the Plastically Deformed Layer. Annealed Polycrystalline 30 % Zn Brass by Manual
Grinding/Polishing.
Scratches/
Abrasive Grade µm / Grit Dsb, µm Ds, µm Dd, µm
SiC paper 220 2.0/- 7.5 77
SiC paper 400 1.5/- 6.5 43
SiC paper 600 0.8/- 5.0 22
Diamond 6 0.08/ 0.17 ¯ 1.0
Diamond 1 0.05/ 0.1 0.7
Alumina, ␣-type 0–1 ¯ ¯ 2.5
Alumina, ␥-type 0–0.1 0.03/- ¯ 0.7
Fig. 7.2—Beilby layer, diagrammatic section of a calcite plate across the line of flow. The
flowed material has completely filled up even the deepest scratches.31
attained at the points where an abrasive grain touches the specimen surface. This high
temperature, being close to the melting point, would cause the material to melt or be-
come very plastic.
According to Samuels7 the layer, which Beilby considered amorphous and could
be removed by etching, a phenomenon known to most metallographers, is simply de-
formed material still remaining on the surface 共see Fig. 7.3兲. When the original scratch
and most of the deformation below the scratch is removed, the polished surface looks
perfect. After etching, the deformed material is etched preferentially and the original
scratch seems to reappear. This was supposed by Beilby, but what reappears is not the
scratch, but an artifact created by the scratch. It could be called a scratch trace.
7.3.2 Influence of Polishing Abrasive, Cloth, and Fluid on Deformation

Deformation will decrease with a lower abrasive grain size as shown in Table 7.1. The
type of abrasive will play a role, diamond grains, especially on soft materials, will give
more scratches than ␥-type alumina and silica; therefore, the small grain sizes of dia-
mond 共1, 0, 25 ␮m兲 are not used for the final polishing of softer materials.
Hard polishing cloths, without nap, will normally create more deformation than
napped cloths; however, napped cloths might create other artifacts like relief and
rounding of phases and edges.
The polishing fluid is very important for lubrication, cooling, and removal of
swarf. The lubrication is necessary to obtain a reduced friction between the cloth and
Fig. 7.3—Schematic drawing of Beilby Theory and Local Deformation Theory.7

the specimen surface. The type of lubricant gives different lubricating effects, the oil-
based lubricants giving the strongest effect, recommended for softer materials. The
water-based type gives a medium effect suited for general purpose use, and the alcohol
type gives a low effect suited for brittle materials. The oil-based lubricants also give a
thin surface film on the cloth that minimizes the damaging effect from the cloth, im-
portant for soft materials. The cooling effect of the lubricant is important when many
specimens at a time under a relatively high pressure are polished. The alcohol- and
water-based lubricants cool most efficiently; the water-based type is preferred. In ex-
treme cases, with many specimens with high pressure and a large disk diameter, a spe-
cial disk cooling, usually with water, might be necessary to keep the temperature low
enough. When using rigid composite disks 共RCD兲 it is important to have an efficient
removal of swarf to prevent it from damaging the specimen surface. To a lesser degree,
this is the case with hard cloths and even less on soft cloths.
7.4 Polishing Cloths

Polishing cloths can be defined as substrates upon which a polishing medium is ap-
plied to perform a polishing process. The polishing cloth is supported by a rigid polish-
ing disk made of metal or a polymer. As described in Section 7.2, the abrasive grain
should, at least momentarily, be fixed by the cloth, making material removal possible.
The fixing of the abrasive can be done in several ways, depending on the structure of the
cloth. For hard cloths, the abrasive grains will be placed on the surface of the cloth,
placed in hard fibers, securing a more aggressive attack, whereas on a soft cloth, the
grains will penetrate into the nap of the cloth, and a less aggressive material removal
will take place. Consequently, the cloth is a very important factor regarding material
removal, but also the deformation developed during the process and the edge retention
and relief are strongly influenced by the cloth.
The term pad is often used for certain polishing cloths made of nonwoven material
共see below兲, but in the following cloth is used as the general term.
A polishing cloth can be characterized through the following:
• Material: All kinds of flexible materials can be used. The most used are: Chemotex-
tiles, nonwoven materials, woven nylon, woven acrylates 共satin兲, woven silk, woven
wool, a backing 共often cotton兲 with synthetic flocked nap.
• Surface Structure: The material can be smooth, porous, perforated, woven, or
flocked 共nap兲. The flocked cloths always have a nap, but other types also might have
a napped surface. The nap normally will give the cloth a high resilience 共see below兲,
but with certain cloths a high nap will lay down during use and create a compact,
smooth surface with a relatively low resilience. The surface structure might
strongly influence the polished surface 共see below兲.
• Resilience: The resilience, the elasticity of the cloth in the vertical direction, dic-
tates whether a cloth is hard or soft. All cloths can be compressed when subject to
pressure from the specimen. A cloth having a low resilience is hard and a cloth with
a high resilience is soft. A hard cloth, which can only be slightly compressed, will
usually give a high material removal and create deep scratches and more damage
to the specimen than a soft cloth. Two cloths, however, with the same low resilience
can perform differently caused by the surface structure of the cloth. Figure 7.4
shows an aluminum/silicon specimen polished on a very hard cloth with an un-
smooth, woven surface, shown in Fig. 7.6; the deformations in the Al/ Si surface are
Fig. 7.4—AlSi material after polishing with 3 ␮m diamond suspension on a very hard cloth with
a very irregular surface structure. The surface has deep scratches and strong deformation. The
cloth is shown in Fig. 7.6. BF.
strong. Figure 7.5 shows the same specimen polished on a cloth with the same re-
silience, but with a relatively smooth, woven surface, shown in Fig. 7.8, the defor-
mations are considerably reduced. A soft cloth with nap will normally have a rela-
tively low material removal and create little deformation and small scratches. The
nap will make an edge rounding. Also, because of the brushing effect 共the fibers of
the nap brushing the specimen surface兲, a relief might develop if the specimen sur-
face has phases of different hardness; the softer phase being preferably removed.
Polishing cloths are fixed to the supporting grinding/polishing disk with a self-
adhesive backing 共PSA兲 or through magnetism established by a steel foil integrated in
the cloth 共see Section 6.7.1兲. Cloths can also be fixed by using a retaining ring that
stretches the cloth over the disk. This often causes wrinkles of the cloth and should be
avoided.
Polishing cloths are supplied in the following diameters: 73 mm 共2.9 in兲, 102 mm
共4 in兲, 200 mm 共8 in兲, 250 mm 共10 in兲, 300 mm 共12 in兲, 350 mm 共14 in兲, and 400 mm
共16 in兲. For a table of available polishing cloths, see Section 13.2.2, Table 13.1.
Fig. 7.5—The same material as in Fig. 7.4 after polishing with 3 ␮m diamond suspension on a
hard cloth with a smooth surface structure. The surface has considerably less scratches and
deformation although the abrasive is the same. The cloth is shown in Fig. 7.8. BF.
Fig. 7.6—Napless, very hard, woven, coated polyester cloth for fine grinding/rough polishing.
SEM.
7.4.1 Edge Retention—Relief

As described in Section 3.1.3 and Sections 6.6.2/6.7.7, edge retention is often very im-
portant and development of a relief should be avoided. The sections mentioned earlier
and Figs. 6.15 and 6.16 describe how the resilience, the vertical flexibility of the prepa-
ration substrate, is decisive for the development of edge rounding and relief. It is evi-
dent that when using a cloth with a relatively high resilience as substrate, the risk of
edge rounding and relief will increase strongly. This means that a good fine grinding,
either on SiC grinding paper or on rigid composite disks, might be spoiled if the polish-
ing cloths used for the following steps have a too high resilience or the polishing times
are too long, or both. It is important that cloths with the lowest possible resilience to
obtain a satisfactory result are used and the times are kept at a minimum. The charac-
teristics regarding edge retention and relief will be discussed further for the single
cloths below.
7.4.2 Cloths for Fine Grinding and Rough Polishing

These cloths are all hard with very low to medium resilience. Although primarily used
for fine grinding and rough polishing, some of the cloths can also be used for final pol-
ishing of medium hard and hard materials. They are typically used with diamonds
from 15– 1 ␮m.
Fig. 7.7—Napless, hard, non woven, synthetic cloth for fine grinding/rough polishing. SEM.
Fig. 7.8—Napless, hard, woven nylon, silk or acetate cloth for fine grinding/polishing. SEM.
All cloths for fine grinding and rough polishing, except the woven steel cloth, will have a
low, often very low, resilience, which theoretically will cause an edge rounding of the
specimen. In practice, however, if the preparation time is kept inside reasonable limits,
the edge retention is high with these hard cloths, which, used with diamond as an abra-
sive, give a good flatness without relief.
Cloths
Woven Steel: This is a cloth made of stainless steel wire mesh. The resilience is close to
zero and consequently the edge rounding is very low. The cloth is used for fine grinding
with 15– 6 ␮m diamond for hard metals, ceramics, and composites.
Woven Coated Polyester 共Fig. 7.6兲: A napless, very hard, coated polyester cloth for
use with 15– 3 ␮m diamond for fine grinding/rough polishing of metals, composites,
ceramics, and hard metals. The resilience is very low giving very little edge rounding.
Nonwoven Textile 共Fig. 7.7兲: A napless perforated/not perforated nonwoven cloth
for use with 15– 3 ␮m diamond for fine grinding/rough polishing of harder materials
and softer materials depending on the resilience of the cloth. On cloths with a certain
resilience, an edge rounding may take place after prolonged polishing.
Woven Nylon 共Fig. 7.8兲: A napless cloth for use with 9 – 1 ␮m diamond. Medium
hard and suited for rough polishing and polishing of ferrous materials and cast irons to
retain inclusions/graphite and maximize flatness. The very low resilience gives very
little edge rounding.
Woven Silk 共Fig. 7.8兲: A napless cloth for use with 9 – 1 ␮m diamond. Hard and
suited for fine grinding/rough polishing and polishing of most metals, coatings, and
plastics. The low resilience gives good flatness and very little edge rounding.
Woven Synthetic Silk 共Acetate兲共Fig. 7.8兲: A napless cloth for use with 3 – 1 ␮m dia-
mond. Hard and suited for rough polishing of most metals to maximize flatness with
very little edge rounding and retention of hard phases.
7.4.3 Cloths for Polishing

These cloths have medium to high resilience and are used for one or more polishing
steps, an intermediate step or a final step. They are used with diamond in the
6 – 0.25 ␮m, mostly from 3 – 1 ␮m. Also, some can be used for oxide polishing 共see Sec-
tion 7.5兲 for the final step. Some of these cloths are napless; some have naps of different
height and structure.
Fig. 7.9—Napless, medium hard, woven wool cloth for polishing. SEM.
The polishing cloths, having medium to high resilience and often a nap, will cause an
edge rounding of the specimen, depending on the preparation time and force on the
specimen. As a rule the polishing time should be kept as short as possible, with most
time used on a napless cloth, which gives less rounding, and less time used on a napped
cloth, often only for a short final polishing. The force on the specimen should be kept as
low as possible, especially on napped cloths. In general, the napless polishing cloths
will not develop a relief, but the napped cloth might develop relief if phases of different
hardness are present in the specimen surface.
Cloths
Woven Wool 共Fig. 7.9兲: A napless, soft cloth with medium resilience for use with
6 – 1 ␮m diamond. It is suited for polishing and fine polishing of minerals, glass, met-
als, composites, coatings, and polymers. An edge rounding might develop, but it will
usually be acceptable. No relief will develop except in extreme cases.
Synthetic Nap on Woven Backing 共Fig. 7.10兲: A cloth with a medium nap of flocked
fibers on a 共cotton兲 backing for use with 6 – 0.25 ␮m diamond, alumina, and silica 共see
Section 7.5兲. This cloth is for general usage for final polishing. The nap and backing
give a very high resilience that will cause rounding of the edges of the specimen surface
and often create a relief because of the brushing effect 共see Section 7.4兲. For these rea-
Fig. 7.10—Medium napped, soft, with synthetic fibers flocked on a backing, cloth for polishing.
SEM.
Fig. 7.11—Napless, soft, porous synthetic cloth for polishing with silica and alumina and for
chemical mechanical polishing. SEM.
sons the cloth should only be used for a short time to establish the final specimen sur-
face.
Synthetic Nap on Nonwoven Backing: A soft cloth with a dense nap with high resil-
ience to be used with 3 – 1 ␮m diamond. It is suited for one-step or final polishing of soft
to hard ferrous and nonferrous metals. The dense nap gives relatively good edge reten-
tion in spite of the high resilience and no relief.
Synthetic Porous Material 共Fig. 7.11兲: A soft, napless cloth with high resilience.
The synthetic material 共neoprene兲 is chemically resistant and will take up the very fine
alumina and silica suspension in the pores, and it is used with oxide suspensions
0.02– 0.05 ␮m 共see Section 7.5兲. The cloth is suited for the final step for most materials.
The time should be short to avoid edge rounding. The risk for a relief is very little, but a
certain relief might develop because of a chemical mechanical attack from the polish-
ing medium.
Woven Felt: A soft, napless cloth with very high resilience used for 9 – 1 ␮m dia-
mond, alumina, and silica 共see Section 7.5兲. It is suited for rough and final polishing of
hard metals, cast iron, and mild steels, preserving inclusions. The high resilience will
cause edge rounding and possibly relief.
7.5 Polishing Abrasives

The polishing abrasives are used in connection with a polishing cloth for the steps from
rough polishing 共fine grinding兲 to the final polishing step. In general, diamond is used
for all steps except the last step 共final polishing step兲. In case of harder materials, dia-
monds, down to 0.1 ␮m also cover the final step, but often, especially with softer mate-
rials and composites, a final cleaning step is made with an oxide, normally silica 共SiO2兲
or alumina 共Al2O3兲.
7.5.1 Diamond Suspensions

Diamond suspensions are described in Section 6.4.
7.5.2 Diamond Spray

Diamond spray is described in Section 6.4.
Fig. 7.12—Alumina, agglomerated, the large agglomerates can be seen.
7.5.3 Diamond Paste

Diamond paste is described in Section 6.4.
7.5.4 Alumina
Alumina 共Al2O3兲 has been the classic polishing medium in metallographic/material-
ographic preparation. Earlier it was used for all polishing steps, often causing bad re-
sults, because the removal rate is very low. In modern preparation, alumina should
only be used for the final polishing steps in grain sizes 1 – 0.05 ␮m.
Alumina is available as suspensions and powders with two crystal types, alpha and
gamma. The alpha crystal has relatively sharp edges giving the highest removal rates,
whereas gamma is more rounded, causing a very small removal rate suited for the last
polishing step.
Both powder and suspension can be supplied in agglomerated and deagglomer-
ated condition. In agglomerated alumina the particles will form agglomerates 共Fig.
7.12兲 because of the electric forces between the particles. These agglomerates will give
a higher removal rate and might cause scratches in the specimen surface, although
they are normally broken down during the polishing. In the deagglomerated alumina
the material is treated to avoid the agglomerates so that only the single particles will be
active 共Fig. 7.13兲, ensuring an ultrafine specimen surface.
Alumina is available in grain sizes from 5 – 0.05 ␮m.
Fig. 7.13—Alumina, deagglomerated.

Fig. 7.14—AlSi surface after polish with 3 ␮m diamond suspension, strong deformations in
both matrix and silicon phase. BF.
Suspensions
These are ready for use either in diluted or undiluted condition. In some cases the sus-
pension is stabilized so that the alumina does not come out of suspension when not
used. This is an advantage if used in automatic dispensing systems 共see Section 7.9.3兲.
Alumina can be mixed with silica 共see below兲 to form special polishing
suspensions.
Powders
Powders have to be mixed with distilled or demineralized water to form a suitable sus-
pension. In special cases, if water is not allowed for the preparation, the powder can be
mixed with other fluids like glycerine or alcohol.
7.5.5 Silica
Originally developed for the preparation of silicon wafers, colloidal silica 共SiO2 in a
suspension兲 has gained ground in metallographic/materialographic preparation. The
grain size is very small, 0.1– 0.02 ␮m, and the grains are almost spherical and softer
than alumina, causing a very low mechanical material removal making SiO2 very well
suited for the final polishing step. By comparing the microstructures of an aluminum-
silicon alloy 共Figs. 7.14 and 7.15兲, the effect of silica can be recognized. The strong de-
formations from the 3 ␮m diamond polishing as shown in Fig. 7.14 are removed and
both matrix and silicon are perfectly polished, see Fig. 7.15.
For wafers and many other materials, the colloidal silica suspension works ac-
cording to a chemical mechanical polishing 共CMP兲 process. The suspension, having a
pH between 8.5 and 11, plays an important role in the material removal mechanism in
CMP.32
The CMP gives SiO2 suspensions and suspensions based on SiO2 and other oxides,
like iron oxide, an increased removal rate on ceramic materials and metal/ceramic
composites and a number of metals 共see Section 7.12兲.
A CMP can be established also when mild chemicals like hydrogen peroxide
共H2O2兲 and an ammonia 共NH3兲 solution are mixed into the suspension; this will be de-
scribed under each material in the Material/Preparation Tables, Section 13.2.3. In this
way, very soft and ductile materials can be mechanically polished to a deformation-free
Fig. 7.15—The same material as in Fig. 7.14 but polished with colloidal silica after 3 ␮m
diamond. The deformations are removed and the true structure can be seen. BF.
finish, avoiding electropolishing. Colloidal silica is available only as suspensions with a

pH 8.5–11 and grain sizes from 1 – 0.02 ␮m.
Attention: A colloidal silica suspension should not be allowed to dry on the polish-
ing cloth, because it will then be unusable. The polishing cloth shall be carefully
cleaned after use to avoid dried-in crystals which will cause scratching of the specimen
surface. It can be of advantage to finish the polishing process by running up to 10 s only
with water to clean the cloth and the specimen; otherwise the chemical attack might
continue, resulting in etching of the specimen surface.
7.5.6 Other Oxides

Magnesium oxide 共MgO兲, iron oxide 共Fe2O3兲共jeweler’s rouge兲, chromium oxide 共CrO兲,
and cerium oxide 共CeO兲 are all polishing media which now are used very seldom. Al2O3
and SiO2 will in most cases do the same job and are much easier to work with.
7.6 Polishing Lubricants

Polishing lubricants are described in Section 6.5.
7.7 The Metallographic/Materialographic Preparation

Methods—Method Parameters
As described above under sectioning, grinding, and polishing, a deformed or otherwise
damaged layer inevitably is formed during the machining processes. The depth of this
layer decreases with decreasing grain size of the used abrasive, and for this reason the
specimen, in the preparation process, goes through a number of steps with each step
removing the deformations from the previous step. The diagram in Fig. 1.7 shows the
processes of both mechanical preparation and electropolishing. Figure 13.18 shows a
typical process consisting of three stages, sectioning 共cutting兲, grinding, and polishing.
The grinding stage and polishing stage both have two steps, plane grinding/fine grind-
ing and rough polishing 共Polishing 1兲 and fine polishing 共Polishing 2兲. It can be seen
that the deformations from the previous step are removed and the last step ends with
very little or no deformation. The most critical steps are between cutting and plane
grinding and between the last grinding step and rough polishing; this is especially the
case when using SiC grinding paper for the last fine grinding step.
It is important that the method is adapted to the specific material being prepared.
For an overview of available methods refer to the 67 Traditional and Contemporary
Methods covering most materials that is stated in Section 13.2.3.
The following contains a brief description of the basic methods for most metals
共methods used for ceramics and other very hard materials are described in Section
6.3.2兲.
The grinding stage: As described in Sections 6.6 and 6.7 this book discriminates
between “Traditional” grinding based on SiC grinding paper and “Contemporary”
grinding based on rigid composite disks 共RCDs兲. This gives two types of preparation
procedures: The Traditional Methods 共T-Methods兲 based on grit P220 SiC paper for
plane grinding and grits P320, P500, 共P1000兲 for fine grinding, and the Contemporary
Methods 共C-Methods兲 based on SiC paper grit P220 for plane grinding, and one or two
RCDs with 9 or 6 ␮m diamond abrasive for fine grinding.
The polishing stage: At the T-Method the rough polishing step normally is on a
hard, napless cloth with 6 ␮m diamond, a very important step for removal of the
scratches and deformations from the grinding. In the C-Method the rough polishing
step is often on a hard, napless cloth with 3 ␮m diamond for removal of the scratches
and deformations from the RCD. For the T-Method, the rough polishing step is fol-
lowed by a 3 ␮m diamond step on a hard, napless cloth followed by a final step on a
soft, napped cloth with 1 ␮m diamond or on a soft, napless, porous cloth with alumina
or silica. In the C-Method, the rough polishing step is followed by a final polishing as
mentioned for the T-Method.
The end result is to a high degree influenced by the consumables used in the prepa-
ration, as described earlier in this chapter, but also the parameters of the process play
an important role.
In the case of automatic polishing with the use of a specimen mover on a grinding/
polishing machine, all parameters, not associated with consumables, are controlled by
the machine 共see Section 7.9兲. For manual 共hand兲 polishing, only the rpm of the polish-
ing disk is a machine parameter.
7.7.1 RPM of Grinding/Polishing Disk

This is typically in the range of 50– 600 rpm, but for certain machines with continu-
ously variable speed, the rpm can be varied from close to 0 up to 1200 rpm.
The rpm of the disk will, to a high degree, influence the relative velocity between
specimen and grinding/polishing substrate. In principle this should be high to secure a
high removal rate, but experiments have shown 共see Section 7.9.2兲 that at polishing,
certain limits shall be observed, and for automatic polishing, 150 rpm is recom-
mended. At grinding, however, higher velocities can be allowed corresponding to
300 rpm or more.
7.7.2 RPM of Specimen Holder

To obtain the best results, the rpm of the specimen holder should be approximately the
same as the rpm of the disk 共see Section 7.9.2兲. The direction, whether it rotates
complementary to or contra to the direction of the disk is important 共see below兲. Most
machines have rpm in the range from 3 – 300 rpm.
7.7.3 Direction of Specimen Holder

Most modern grinder/polishers work with the specimen mover rotating in the same
direction as the grinding/polishing disk, complementary 共comp兲. This makes synchro-
nous polishing possible 共see Section 7.9.2兲 securing the best polishing action, avoiding
certain artifacts. If contra rotation 共counter rotation兲 is used, the removal rate is higher,
the specimen mover and the disk rotating in opposite directions, but this can only be
recommended for grinding, not polishing. Contra rotation is also used to keep the ox-
ide suspension on the polishing cloth because then the specimen mover pulls the sus-
pension towards the center of the polishing cloth, but according to polishing dynamics,
as described in Section 7.9.2, the contra rotation has certain drawbacks, as mentioned
above.

The force 共load兲 on the specimens is important to obtain a satisfactory removal rate. At
grinding the specific pressure shall be relatively high, in the range of 3 to 10 N / cm2
共4.35 to 14.5 psi兲共30 to 100 kPa兲, corresponding to a force of 20 to 70 N 共4.5 to 15.8
lbf兲 for a 30-mm 共1.25-in兲 specimen.
The pressure will in certain cases influence the degree of deformation, especially
for soft, ductile materials. Therefore, the pressure on the specimens shall be lower at
polishing than at grinding, in the range of 14 to 40 kPa, corresponding to a force of
10 to 30 N 共2.3 to 7 lbf兲 for a 30-mm 共1.25-in兲 specimen. In principle, the specific pres-
sure shall be the same for large specimens, but experience has shown that a maximum
force of 50 N should be established on specimens of 40 mm 共1.5 in兲 in diameter and
larger. This is to avoid an overheating and excessive wear of the polishing cloth. To
compensate for the loss of material removal, the time can be extended from 1 to 4 min.
7.7.5 Process Time

The duration of each step basically depends on the amount of material removed from
the specimen surface 共stock removal兲. This, however, cannot normally be measured on
most machines, and therefore the process time is used as an indicator. When grinding,
the amount of material removed is so high that measurement is possible 共see below兲,
but the removal rate at polishing is so low that measurement on a polisher is not pos-
sible. Only by measuring the time can a reproducible process be established. It should,
however, be recognized that a specific preparation time does not guarantee that the
necessary material is removed from the surface; this is only the case if the consumables
used react like the consumables when the process was established. Also, parameters
such as force should be correct to ensure reproducibility.
7.7.6 Stock Removal

The whole preparation process is based on removal of material from step to step. The
ideal way of working would be to measure the material 共stock兲 removed and stop the
process when the preselected amount, corresponding to the deformations from the
previous step, is removed. This is possible at the grinding steps, removing stock from
40 to 50 ␮m to several hundred micrometres per step. Grinder/polishers with mea-
surement of stock removal are available in the market. At polishing, the stock removal
is so low 共for example, 3 to 6 ␮m per 5 min兲 that it cannot be measured without high
precision instruments, which are not usually available on grinder/polishers.
7.8 Grinding/Polishing Equipment—Manual Preparation

The basic polishing machine has a rotating turntable on which an interchangeable
disk, covered with a polishing cloth, is placed. Normally the polishing process will con-
sist of two to four steps, including rough polishing, polishing, and final polishing. In
some cases, when the fine grinding has been done with the contemporary method 共see
Section 6.7兲 only one polishing step might be sufficient.
As described in Section 6.8, plane grinding, fine grinding, and polishing can take
place on the same grinder/polisher only by changing the disk/disk surface used for each
step. See Section 13.2.4 for the technique of manual 共hand兲 polishing.
The grinder/polisher is a standard piece of equipment that is available in many
models and sizes. Most models have one turntable for 200 mm 共8 in兲, 230 mm 共9 in兲
共for SiC paper兲, 250 mm 共10 in兲, or 300 mm 共12 in兲 disks, one/two speeds or continu-
ously variable speed, a water supply and a drain Figure 7.16 shows a grinder/polisher
with mineral casting base. It will work with 200 and 254 mm 共8 and 10 in兲 disks 共plat-
ens兲 and is available in different models with one or two wheels 共turntables兲. One
model has 150 and 300 rpm; another model has 30 to 600 rpm. A grinder/polisher with
two turntables is also shown in Fig. 6.28.
Very often the grinder/polisher is prepared for retrofitting of a semiautomatic
specimen mover.
7.9 Grinding/Polishing Equipment—Automatic Preparation

If we look at the typical specimen mover system for “automatic polishing,” the correct
term would be “automatic preparation” because polishing is only part of the process.
Also the word “automatic” needs explanation, taking into consideration that in most
cases it expresses semi- or part-automation, meaning that only the basic process in
each step is mechanized, all handling of specimen holders, change of disk, cleaning,
etc., is done by hand. In some cases, however, the whole process is automated 共“fully
automatic”兲 as described below. In the following the word “automatic” refers only to
the basic process involving manual work. If the system is “fully automatic,” this will be
described.
The reason for using automatic equipment is that hand grinding/polishing is hard
and, in the long run, overloads the hand and arm of the metallographer. Automatic
preparation also ensures a better quality of the specimen through a uniform process
that is reproducible. The dependence on the skill of the operator is reduced as well.
7.9.1 Machine Design

The Englishman I. E. Stead, who continued the work done by H. C. Sorby, already in-
vented a rotating specimen holder in 1900 for four specimens mounted on a movable
arm so that the holder would sweep the rotating polishing disk.
Many other principles have been suggested over the years, but the “specimen
mover” with a number of specimens placed eccentrically on the grinding/polishing
disk is dominating today. A supplement is vibratory polishing 共see below兲.
The standard specimen mover system is a grinding/polishing machine with a ro-
tating disk and a rotating specimen holder placed eccentrically on the disk 共see Fig.
7.17兲. The specimen holder or the individual specimens are pressed against the disk
surface to obtain a grinding/polishing action.
Fig. 7.16—Grinder/polisher, with mineral casting base for manual preparation and, as shown,
with a specimen mover for semiautomatic preparation, 200/ 250 mm 共8 / 10 in兲 disks,
150– 300 rpm or 30– 600 rpm.19
Fig. 7.17—Specimen holder placed eccentrically on the grinding/polishing disk.
For a specimen holder with several fixed specimens, these are fixed in suitable
holes 共see Fig. 7.18兲 and during the operation, a central force is established pressing all
the fixed specimens against the disk surface. The advantage of this system is a good
flatness of the specimens, with the whole holder acting as a large “specimen” that
avoids the angling of the holder in comparison to the disk surface 共see below兲. The dis-
advantage is the work 共fixing兲 involved, and the need for at least three specimens in the
holder to keep the balance. In the event that only one specimen is to be prepared, “blind
specimens” must be used. Also, the plane grinding may be prolonged to obtain that all
specimens are in the same plane. The microscopic inspection of the specimens during
the preparation process is rather tedious, having to put the whole holder on the micro-
scope.
The alternative is that specimens are placed in a holder plate and individually
loaded and called “single specimen preparation” 共Fig. 7.19兲. The advantage is easy han-
dling and being able to take out a specimen after every step of the preparation for in-
spection. The disadvantage is a tendency to “angling,” the specimen being only at-
tacked in one direction, or “penciling,” the specimen being attacked along the
periphery, especially when grinding on SiC paper 共see Fig. 7.20兲. In the first moments of
the grinding the SiC grains will create a very strong pull in the specimen surface caused
by the grains removing very much material in the first seconds 共see Section 6.6兲. The
tendency will be to remove most material at the edge where the grains move into the
specimen. As soon as an unevenness has been made, the specimen might start rotating
Fig. 7.18—Specimen holder with fixed specimens and central load.

Fig. 7.19—Specimen holder plate with specimens placed in holes without fixation and
individually loaded 共single specimens兲.
around its own axis and penciling will take place, or it might stay without rotation cre-
ating angling. Penciling and angling can be suppressed by working with as low speci-
mens as possible and establish the smallest possible distance, d in Fig. 7.20, between
holder plate and disk surface. Also, an exact guidance of the specimen in the holder
plate will suppress the angling.
The force on the specimens can be established through compressed air or by me-
chanical means. With central pressure the force is transferred through the center of the
specimen holder. By individual load, a pressure foot will be lowered against each speci-
men 共see Section 7.7.4兲.
A number of parameters should be controlled during the process 共see Section 7.7兲.
On simpler systems, the operator sets the rpm of the disk and the force. The rpm of the
holder is mostly fixed, and in some cases the direction, complementary or contra, can
be set. The operator will stop the machine after a certain period of time.
On more advanced systems all parameters are controlled through a microproces-
sor and programmed before the start of the process. This makes storing of programs
共methods兲 possible so that a method, once developed, can be reused whenever neces-
sary. The microprocessor also may control other parameters such as dosing of abrasive
suspension and lubricant 共see Section 7.9.3兲.
The fully automatic systems are based on the above; only several preparation steps
including cleaning and drying are programmed as a process. This means either the
disks are changed automatically during the process or a certain number of disks are
available in the machine 共see Section 7.9.3兲.
Fig. 7.20—Schematic drawing of a single specimen placed in the holder plate on a grinding/
polishing disk. If the distance d is too long, angling or penciling will take place at grinding on
surfaces with fixed abrasives.
Fig. 7.21—Polishing dynamics for a specimen holder eccentrically placed on a grinding/

polishing disk. Velocity vectors for two specimen holders, 30 rpm and 149 rpm are shown.
7.9.2 Polishing Dynamics

As described above, the most common way of automatic polishing is placing the speci-
mens in a specimen holder which rotates eccentrically on a polishing disk 共Fig. 7.21兲.
As the dynamics between grinding/polishing disk and specimen holder have a certain
influence on the preparation result, these dynamics shall be briefly described. It is evi-
dent that the relative velocity between the surface of the polishing disk and the surface
of the specimen will depend on three factors: rpm of the disk, rpm of the holder and
direction of rotation.
Two systems that are quite common can be compared.
共1兲 Polishing disk: 150 rpm

Specimen holder: 30 rpm
Complementary 共comp兲 rotation
共2兲 Polishing disk: 150 rpm
Specimen holder: 149 rpm
Complementary 共comp兲 rotation
Comparing the velocity vectors in Fig. 7.21, we see that for system 共1兲 the velocity
vectors are one-sided, causing a nonuniform material removal. This phenomenon is
even more pronounced during contrarotation.
In system 共2兲 the vectors cover all directions causing a uniform removal.
This means that certain conditions, the optimum dynamic conditions 共ODC兲 can
be defined.33 ODC will be when the relative velocity is constant during a full revolution
of the specimen holder 共synchronous polishing兲, as can be seen in 共2兲共Fig. 7.21兲. If the
rpm of the grinding/polishing disk is higher than the specimen holder, ODC is not ful-
filled and the preparation might result in having artifacts like comet tails 共see Section
13.6兲.
Fig. 7.22—Automatic grinding/polishing system for one specimen at a time.19
7.9.3 Semiautomatic and Fully Automatic Systems

Considering that automatic preparation is useful, even with an output of very few
specimens, semiautomatic and fully automatic systems can be considered very impor-
tant. They are supplied in different sizes, catering from one to six specimens or more at
a time.
The tendency is to include as many parameters as possible in the automatic pro-
cess, still maintaining the manual change of the disk and handling 共cleaning兲 of the
specimen holder with the semiautomatic systems.
With the microprocessor a programming of all parameters is possible.
Small Semiautomatic Systems

The small systems will handle one to three specimens at a time on a 200 or 150 mm 共8
or 10 in兲 disk. The load is mostly supplied by a spring or a weight. In some cases a timer
controlling the process is available.
Figure 7.22 shows a grinder/polisher for low volume semiautomatic preparation,
preparing one specimen at a time. Figure 7.23 shows a specimen mover for low volume
Fig. 7.23—Specimen mover for one to three specimens, 8 rpm and force 2 – 20 N.20
semiautomatic preparation mounted on a grinder/polisher, preparing up to three

specimens at a time. Specimens with very low deformations especially suited for EBDS
共see Section 7.10兲 can be produced.
Medium to Large Semiautomatic Systems

These systems carry the work load in most laboratories. They work with 250, 300, 350,
400 mm 共10, 12, 14, 16 in兲 disks and specimen holders for six specimens or more, and
mostly rpm, force, and process time can be controlled and preset 共see Section 7.7兲.
A dispensing system 共see below兲 may also be included in the controls so that the
total preparation sequence including dosing of abrasive and lubricant can be pro-
grammed. The possibility of a permanent storage of programs for different materials
might be included as well, and newer systems allow for connection to a local net 共LAN兲
and for establishment of databases with preparation methods. It is even possible to
download preparation methods from the Internet and use them directly.
Figure 7.24 shows a semiautomatic system consisting of a number of grinder/
polishers, specimen movers and a dosing unit. The system is microprocessor con-
trolled allowing for connection to a local network 共LAN兲, sharing preparation methods
with other users.
Dispensing Apparatus
Dispensing 共dosing兲 of abrasive and lubricant is part of the preparation process. Basi-
cally, the operator can perform this before and during the process, but especially add-
ing lubricant during the process that ties the metallographer to the machine is against
the idea of automatic preparation. Therefore, most semiautomatic systems have a
lubricant-dispensing 共dosing兲 unit connected to the system, in this way adding small
amounts 共adjustable兲 in regular intervals 共adjustable兲 to the disk surface during the
process.
To obtain a constant removal rate it is an advantage to apply the abrasive, prefer-
ably as a diamond suspension, during the process. This can be done with dispensing
Fig. 7.24—Modular preparation system with single and central pressure, available in three
different disk sizes, 200-, 250-, and 300- mm diameter. Equipped with an automatic dosing unit
and programmable with preparation methods.20
共dosing兲 units available for one or several bottles of suspension/lubricants. An oxide

polishing suspension can also be part of the suspensions to be applied, but this needs a
water cleaning system as part of the dispensing unit.
The more advanced semiautomatic preparation systems include the control of a
dispensing unit.
Stock Removal
Stock removal 共controlled material removal兲 is sometimes included in the control sys-
tems covering the grinding steps 共see Section 7.7兲.
Fully Automatic Systems

These systems include all tasks of the preparation process. All parameters for the pro-
cess are programmed and stored permanently before the start, and the automatic pro-
cess includes: grinding, dispensing of abrasive and lubricant, cleaning and drying of
specimen holder after every step, change of grinding/polishing surface, and polishing
in several steps. In some cases stock removal can also be programmed. The goal is to
supply a specimen ready for the microscope.
In some cases the specimen holder with specimens is plane ground on another ma-
chine before going into the automatic system. In other systems, the plane grinding is
part of the automated process.
Figure 7.25 shows a fully automatic system that combines the function of a semi-
automatic grinder/polisher, a dispensing system, an ultrasonic cleaner, and specimen

dryer in one compact unit to be placed on a tabletop. It has single and central pressure,
and it is programmable with permanent storage of methods.
Vibratory Polishing Systems

Vibratory polishing is an alternative to the specimen mover described previously. It
was originally developed for use in the hot cells preparing radioactive materials. The
reason was the very simple design without rotating parts, cutting maintenance down to
a minimum.
Vibratory polishing is based on the principle of a vibrating plate in the shape of a
bowl. A number of specimens, typically up to twelve, are mounted in weights and
placed face down on the polishing cloth, covering the plate. The bowl shape takes care
that a suspension, mostly Al2O3 or SiO2, stays on the cloth. The vibration has both a
vertical and horizontal movement, normally established with an electromagnet. This
means that the single specimen, caused by the inertia, moves slowly along the periph-
ery of the bowl, in this way being polished through the movement between cloth and
specimen. By adjusting the amplitude of the vibratory movement, the speed around the
bowl can be controlled and set according to sample size and weight. The polishing ac-
tion is very low, suited for sensitive materials making a scratch-free surface possible
with very low deformation. Due to the low removal rate, a normal final polishing step
will take several hours in which the apparatus can be left unattended.
Figure 7.26 shows a heavy duty vibratory polisher with variable settings.
7.10 Special Preparation Techniques

7.10.1 PCB Coupons
Printed circuit boards 共PCB兲 are often metallographically/materialographically in-
spected to ensure the quality of the metal layer in the holes of the board. For this pur-
pose a so-called coupon is made 共see Fig. 3.17兲.
PCB coupons to be tested according to the American standard IPC-TM-650 should
be prepared so that the prepared surface is exactly through the middle 共diameter兲 of the
holes to be inspected. This is usually done by mounting several coupons on two preci-
sion pins using two reference holes 共see Section 3.11.5 and Fig. 3.17兲. The two precision
pins can be used as contact surface in a special specimen holder so that the coupons are
placed exactly in relation to the holder. In this way the target 共the middle of the inspec-
tion holes兲 can be reached by using a number of adjustable stops on the holder. The
stops are calibrated according to the surface on which the pins are resting, in this way
securing that the process stops before the target is reached. Normally a rough SiC
grinding paper is used for the first step, the grinding being stopped 100 to 200 ␮m
from the target. By readjusting the holder the next step with a finer SiC paper will stop
very close to the target. According to the type of PCB, the grinding steps shall be fol-
lowed by one or more polishing steps. These steps are made without stops because the
material removal at polishing is very low, minimizing the risk of removing too much
material from the PCB. For a preparation process, see Method T-27 in Section 13.2.3.
7.10.2 Microelectronic Materials—Nonencapsulated Cross Sections

Microelectronic materials are cross-sectioned to a specific point 共target兲 for both light
microscopy and scanning electron microscope 共SEM兲 examination.
Fig. 7.25—Fully-automatic, microprocessor controlled grinding/polishing system, with built-in

dispenser, ultrasonic cleaner, and specimen dryer. Programmable, with permanent storage of
methods.19
Cross sections serve two main functions:34

• Cuts through representative structures within an IC show relationships of layers
and features, such as step coverage, interfaces between layers, and possibly em-
bedded defects or voids.
• Precision cross sections through specific defects often lead to the process step or
mechanism that produced the defect.
When applicable, nonencapsulated cross-sectioning is simpler and faster than the classi-
cal encapsulated method. Results of nonencapsulated cross-sectioning are more suitable
for viewing in a scanning electron microscope.
The passivation layer of the IC provides sufficient encapsulation of malleable met-
allization to prevent smearing. Rounding of the front edge is avoided by using hard, flat
grinding and polishing surfaces.
Tripod Fixture—The Process

Cross sections can be prepared with the relatively simple tripod fixture where the speci-
men is the third leg on a fixture 共see Fig. 7.27兲. Cross sections can also be prepared on
Fig. 7.26—Heavy duty vibratory polisher, horizontal vibratory movement, with variable
settings.19
semiautomatic systems and fully automatic systems; both are commercially available.
In the following only the use of the tripod fixture will be described 共see also
Material/Preparation Tables 22, Section 13.2.3兲.
SiC paper 共600 grit兲 was used originally to grind to within 20 to 30 ␮m of the tar-
get. Polishing from that point was accomplished solely and slowly on a glass disk.34,35
However, the need for faster throughput and the introduction of hard tungsten plugs
necessitated new polishing media and techniques.
The procedure described below using a hand-held tripod fixture is basic, simple,
and fast. It produces excellent results that can be imaged on either standard or field
emission SEMs.
The grinding procedure described involves several short steps with Al2O3 and dia-
mond lapping film starting with relatively coarse grits. Satisfactory results can be ob-
tained by grinding longer with fewer steps, but the procedure will be tedious if the over-
all grinding time is increased by using fine grain sizes to remove material slowly.
Additionally, if the grinding time is excessive, the material removal rate may decrease
as grinding/polishing media wear and it is difficult to judge whether enough material
has been removed.
Cross sections wider than the 5 by 5 mm 共0.20 by 0.20 in兲 in width will require
significantly longer grinding and polishing times. The use of worn out grinding media
should be avoided; fresh, finer grain size grinding/polishing media may have a faster
removal rate than coarser, worn media.
Even if a cleaved edge is close to the desired final line such that no grinding is re-
quired, a brief grinding on grit P4000 共US grit 1200兲 is recommended to make a flat
surface. Grind only as necessary to create a flat surface, even if a part of the surface
remains untouched. Jagged edges on a cleaved sample, if not removed, will scratch
away the Al2O3 or diamond from the film.
Equipment and Consumables

A tripod fixture with the specimen mounted on a sample mount 共paddle兲共see Fig. 7.27兲
is used by hand on the rotating grinding/polishing disk of a grinder/polisher with a
200 mm 共8 in兲 disk and variable speed, preferably 10 to 150 rpm 共see Section 7.9兲.
Fig. 7.27—Tripod fixture, the specimen is placed as one of three “legs” of the hand
held-holder.
A stereomicroscope and a metallurgical microscope with measuring abilities are

required to check the progress of the preparation process.
Sample mounts are used for carrying the sample 共specimen兲 during the prepara-
tion steps and for the analysis in SEM. The process involves grinding paper and lapping
films, Al2O3 and diamond, and for polishing diamond suspension and a polishing
cloth. Dry nitrogen 共or a supply of aerosol cans兲 is required to blow the specimens dry.
Preparation, See also Method C-22, Section 13.2.3

Sectioning can be done on a precision cut-off machine with a diamond wheel 共see Sec-
tion 2.5兲. The desired cross section target should be within 50 ␮m of one edge. The sili-
con piece is then attached to a sample mount such that the edge containing the target is
parallel to and extending over the edge of the sample mount 共cantilever fashion兲, plac-
ing the specimen on a hot sample mount 共125° C 共250° F兲兲 using wax, as shown in Fig.
7.28.
Grinding takes place in three to four steps. The purpose of grinding is to rapidly
achieve a surface, 1 ␮m away from and parallel to the desired cross section line 共tar-
get兲.
The surface left by grinding, later to be polished, should be flat and scratches
should be no greater than those caused by 1 ␮m Al2O3 or diamond particles on
Al2O3/diamond films. The grinding procedure typically requires less than 15 min in-
cluding inspection time.
In Method C-22 the total preparation process is described. It is important that the
specimen is adjusted so that the ground surface is parallel to the cross section line 共tar-
get兲. The time in minutes is not stated at the grinding steps, but the distance remaining
to the target. This is to ensure that all deformation from the previous step is removed
and to ensure that the target is not reached in a too early step.
Polishing is used when a very fine finish is wanted. Microelectronics with metal
systems of Al 共no tungsten兲 or gold 共no tungsten兲 are polished using a 0.05 ␮m Al2O3
lapping film or a soft, napped or napless, porous cloth using colloidal silica as the abra-
sive. In case of metal systems with Al/ W and Au/ W, polishing is done with a napless,
hard, woven synthetic cloth and 0.1 ␮m diamond suspension or a napless, soft, porous
cloth with 0.1 ␮m diamond suspension mixed in a 50:50 solution with colloidal silica.
Fig. 7.28—Microelectronic specimen mounted on a sample mount for a tripod fixture.
7.10.3 Microelectronic Packages—Table 7.2—Target Preparation

Electronic and microelectronic assemblies are complex material composites. The ma-
terials used are dissimilar in their chemical composition, their crystal structure, and
their microstructure. Of technical importance for the qualification of the components
are interfaces, grain boundaries and phase boundaries as well as heterogeneous pre-
cipitations. Imaging and analysis of the microstructure is a prerequisite for estimating
the quality of a component. Further criteria for qualification, from the materialo-
graphic point of view, are inclusions, contaminations, pores, cracks, holes, as well as
the evaluation of contours, e.g., the wetting angle of a soft solder connection.36
Due to the close packaging of electronic and microelectronic devices with many
various materials within a small volume, microstructural examination is faced with
the problem of simultaneously imaging different materials that have very different
properties. Specimen preparation therefore involves the simultaneous processing of
hard, often brittle materials and soft materials exhibiting plastic deformation. The ma-
terials most used in advanced integrated circuit packaging and interconnection tech-
nology, their use and hardness 共HU, see Section 21.5兲 are listed in Table 7.2.37
Each of the materials stated in Table 7.2 has its specific properties and, as can be
seen, the hardness is very different and often the materials are brittle. This must be
taken into consideration during the materialographic preparation; each individual
step from cutting through grinding to the final polishing step is of significance. Mis-
takes made in the first stages of preparation can only be corrected during the subse-
quent steps with considerable difficulty or not at all. For each step the rate of material
removal and the deformation layer which remains are important factors. The prepara-
tion parameters used 共grinding surface, type of abrasive, grain size, lubricant兲 must be
carefully selected on the basis of the physical properties. The general rules for the
preparation of solid materials are that soft and medium-hard materials should be
plane ground using SiC grinding papers, whereas hard materials require resin-bonded
TABLE 7.2—Materials Used in Electronic and Microelectronic Devices and Interconnections.

Common Applications in
Mounting and Connection
Material Technology Universal Hardness (HU)
Al2O3 ceramic Carriers (hybrid technology), 17000
body of components
Silicon Semiconductors, transistors, ICs 9300
Nickel-phosphorus (NiP) Resist layer, metallization 4000
Kovar (FeNiCo) Lead frames, circuit board core 1900
Invar (FeNi) Lead frames, lead wires 1800
Aluminum (Al) Housing, heat sinks, capacitor 1300
foils
Copper-silver (CuAg) Solder (brazing) 1100
solder
Gold (Au) Surface finishing layers, 500
(connectors, solder, adhesive and
wire bond contacts)
Tin-silver (SnAg) solder Soft solder 300
Copper (Cu) Metallization on circuit boards, 300
lead frames
Epoxy-fiberglass sheet Circuit board material 280
Tin-lead (SnPb) solder Soft solder 230
disks with fixed diamond grains or rigid composite disks 共RCDs兲 with added diamonds.
Very often for the devices described herein, both extremely hard and very soft materials
must be prepared at the same time, and in such cases the preparation must be based on
a compromise. The goal of the preparation is to obtain a flat specimen without relief
between the different constituents and good edge retention, while at the same time
avoiding deformation and other artifacts of the soft and brittle constituents. If only SiC
grinding papers are used for grinding of hard materials, then edge rounding and relief
will set in at an early stage. Plane grinding and the first steps of fine grinding should be
done with the hardest possible abrasive suited for the hardest materials in the speci-
men and always using the finest grain size possible. Often SiC paper should not be used
with a grit coarser than P500 to avoid damage to the brittle materials in the specimen,
and during both grinding and polishing the pressure should be kept low to avoid
damage.36
In the Material/Preparation Tables 19–26, Section 13.2.3, eight methods are indi-
cated covering the preparation of different electronic components. To be able to select
the method best suited for a given component, it shall be analyzed before the prepara-
tion starts to be able to decide on the best method and how the preparation shall be
performed.
Inspection and Location of Fail Site—Target Preparation

Before the preparation starts, the structure of the assembly should be studied by visual
macroscopic methods to decide on the materials involved and to locate critical sites
and the locations of both obvious and possible defects to be marked. Typical fail sites
共targets兲 include: poor solder joints, cracks in components, or defects in the circuit
board material. These faults are then investigated more closely using other techniques
like radiography, ultrasonic imaging, fine and gross leak testing, and die penetration.
The orientation of the plane of preparation will depend upon the orientation or the
features to be imaged and is often marked on the assembly plan. If the fail site 共target兲
has been located then this will determine the plane of preparation, often starting with
the sectioning close to this plane. Special apparatus for target preparation is available
in the market.
Sectioning and Mounting „Encapsulation…

Sectioning must be done so that the site of interest is not damaged by deformation or
input of heat. Therefore, very often the device is mounted 共encapsulated兲 before the
sectioning takes place. Encapsulation shall be accomplished with only a low develop-
ment of heat and the resin shall be able to fill out all cavities without shrinkage. This
means that an epoxy with a low viscosity should be used, preferably under vacuum so
that an impregnation takes place 共see Section 3.10兲. It is very important that the speci-
men is cleaned very effectively in acetone, preferably using ultrasonics before the en-
capsulation. After cleaning, the specimen should only be handled with a pair of twee-
zers and dried with N2 or absolutely clean air, not normal compressed air.
Sectioning and mounting are described in detail in the Material/Preparation
Tables 19 to 26.
7.10.4 EBSD
Electron backscatter diffraction 共EBSD兲 has gained ground in recent years as an acces-
sory to a scanning electron microscope 共SEM兲. The main advantage of EBSD is the
possibility to link morphology 共grain size and shape兲 with crystallographic features
共phase, orientation, disorientation兲 on the microscopic scale, but still in a representa-
tive specimen area.38 The preparation is much simpler than for thin foils for TEM 共see
Section 8.6兲, but more demanding than that for normal SEM.
The information depth of EBSD is very low, in the range of 20– 370 nm depending
on material, SEM, etc. This means that the surface of the specimen shall be without the
thin distorted layer that normally exists after a mechanical polishing 共see Section 7.3兲.
This can be obtained by etching, but etching should often be avoided for EBSD. For
certain materials electrolytic polishing can give a deformation-free surface, but for
many materials like ceramics, heterogeneous materials, etc., mechanical preparation
is the only possibility to obtain a flat and distortion-free surface.
For this reason the standard grinding/polishing process shall be adjusted, espe-
cially with regard to the last polishing step. In principle, the normal method used for a
specific material can be used with special attention to the last polishing step using
silica, which often is prolonged. A long preparation time using silica as an abrasive
might give an unwanted relief, and therefore polishing cloths must be chosen very
carefully.
Specimen Mover Systems

The most used specimen mover 共standard system兲 for normal metallographic/mate-
rialographic preparation has a specimen holder rotating eccentrically on the grinding/
polishing disk 共see Section 7.9兲.
The preparation methods described in Section 13.2.3 are based on the use of this
standard specimen mover, normally operating with 150 rpm 共grinding/polishing disk
and specimen holder兲 and a force per specimen not lower than 5 N 共1.1 lbf兲. This sys-
tem will give acceptable results for EBSD for very hard materials like ceramics, possi-
bly using chemical mechanical polishing 共CMP兲共see Section 7.12兲.

For most materials, however, it is not possible to obtain a distortion-free surface
after the last step, and this step either has to be prepared on a special slow moving
specimen mover or by vibratory polishing.
Specimen movers with very low rotation and force per specimen are commercially
available. The rpm of both the disk and specimen holder can be adjusted to a relative
velocity close to zero 共see Section 7.9.2兲 and the force on the specimen down to close to
zero. This means that all metals can be prepared for EBSD in a reasonable time, often
using CMP, see under the specific materials in Section 13.2.3. CMP is also needed for
hard materials like certain ceramics. For specific preparation data for a high number of
materials see Ref. 38.
Vibratory Systems
Vibratory polishing normally gives good results for EBSD; the main drawback being
the very long preparation times, although the vibratory polisher can work unattended.
If vibratory polishing is used for all steps including grinding, a high surface wavi-
ness can be observed and due to the long polishing times a relief can develop. There-
fore, vibratory polishing should be limited to the last step, having done the previous
steps on the standard specimen mover or the slow specimen mover described above.38

Mechanical Preparation
Field metallography is, as the term indicates, used in the field, often called in situ or on
the spot. It is based on the grinding and polishing processes described above; portable
apparatus is available that is able to prepare a small area nondestructively. Field metal-
lography is used on large parts, steam pipes, etc., to be able to check the microstructure
without destructing the work piece. Very often it is not possible to analyze the prepared
spot and a replica is taken 共see below兲. The preparation methods and etching proce-
dures to be used can be seen from Table 11.1 and Section 13.2.3.
Many materials like steel, aluminum, and titanium are very well suited for electro-
lytic polishing using a portable electropolisher 共see Section 8.5兲.
7.11.1 Portable Grinder/Polishers

These are available with a hand piece with a flexible rotating disk upon which a small
piece of grinding paper or polishing cloth is placed. This apparatus can be supplied
from the mains or battery operated. The normal preparation process in a number of
steps is employed and normally, after etching, the prepared spot is analyzed with a por-
table microscope to ensure that the microstructure is acceptable for further examina-
tion. Following this, a replica is made. This replica is taken to the laboratory for exami-
nation.
Often the grinder/polisher is used for the preparation of a spot that is finally
electropolished/etched to obtain the microstructure 共see Section 8.5兲.
7.11.2 Replication
Replication is a very important part of nondestructive preparation. Replication is a
nondestructive procedure that records and preserves the topography of a materialo-
graphically prepared surface as a negative relief on a plastic film or other medium 共rep-
lica兲. See also the ASTM Standard Practice for Production and Evaluation of Field Met-
allographic Replicas 共E 1351兲共Section 12.4兲.
The replica material shall have a number of characteristics:
• All features present on the surface that was replicated shall be accurately repro-
duced.
• Simple and reproducible handling.
• High stability and strength.
• Flexibility so that replica can be made on curved surfaces.
Replicas should be made either using a piece of plastic 共acetate兲 film or a fast cur-
ing silicone rubber-based material.
Plastic Film
The film or foil is 12 by 18 mm 共0.5 by 0.75 in兲 in size. Two methods can be followed
which are described in Section 13.4.3.
Silicone Rubber
The silicone rubber-based material used is a two-component silicone rubber that is
available in different types according to the specific purpose.
The compound is supplied in cartridges that are mixed and dispensed on the pre-
pared surface using a special hand-operated gun. The silicone rubber is very flexible,
suited for curved surfaces, inside tubes, etc. The material is also very suitable for engi-
neering inspection applications like microcracks, wear marks, corrosion marks, etc.
For use of silicon rubber, see Section 13.4.3.
7.12 Chemical Mechanical Polishing

Chemical mechanical polishing 共CMP兲 has been highly developed for the preparation
of silicon wafers, but CMP is also used with advantage for other materials.
In CMP, also called etch polishing or attack polishing, the specimen surface is at-
tacked both mechanically 共by an abrasive兲 and chemically at the same time.32 Nor-
mally an abrasive suspension with an in-mixed chemical substance is used. Material
removal occurs as a consequence of a combination of the chemical reaction of the
chemical with the specimen surface material and the continuous removal of the reac-
tion materials by the abrasive. Because of the removal of the reaction products, even
chemical solutions that typically would not attack a given material will have an effect
because the passivating layer is constantly removed. CMP is established either by using
suspensions of silica 共SiO2兲 often with a pH between 8.5 and 11 or alumina 共Al2O3兲,
with a pH between 3 and 7, or by mixing a chemical solution, often an etchant, with the
oxide suspension.
CMP, using a very fine abrasive like silica with a grain size of 0.02/ 0.05 ␮m, and a
relatively weak chemical attack, will create surfaces almost without deformation and
scratches. This means that CMP is very well suited for the final polishing step for most
materials, creating a clean surface. Especially in soft and ductile materials this is an
advantage. The polishing will take place on a relatively soft, porous polishing cloth, and
therefore the time shall be limited to 0.5 to 1.5 min.
Aluminum, refractory metals, Ti, and other metals can be polished with silica with
or without an added chemical. Also, ceramics and other materials with high abrasion
resistance are suited for CMP; both acidic alumina suspensions and basic silica can be
used.
For some materials like Ti and most Cu alloys, the final polishing step can be made
using a silica suspension with the addition of hydrogen peroxide and ammonia solu-
tion. Ferrous metals and Ni-based alloys can be polished with acidic alumina. If the pH
should be lowered, oxalic acid can be added, and if the pH shall be raised a chemical
like potassium hydroxide can be added.
For solutions used for the specific materials, see the Material/Preparation Tables,
Section 13.2.3.
With the modern advanced methods of preparation, CMP is mostly limited to the
suspensions and solutions mentioned earlier. CMP, however, can be performed with a
very high number of chemical solutions, mostly etchants.2,9
7.12.1 Protection—Corrosion at CMP

When using the chemical solutions recommended in this book 共see Section 13.2.3兲 the
corrosive attack on equipment and accessories is minimal. In the case of suspensions
mixed with stronger chemicals 共acids兲, care should be taken to protect equipment and
persons working with the mixture. Also, only synthetic polishing cloths made for CMP
should be used.
7.13 Thin Sections

For certain materials such as minerals, ores, ceramics, and plastics, the use of reflected
light for microscopic examination is not always satisfactory. By using thin sections
with a thickness of 20– 35 ␮m 共down to 7 – 10 ␮m at plastics and polymers兲 it is pos-
sible to examine the specimen in transmitted light, and if the thin section is polished,
also in reflected light.
To make a thin section a high amount of material must be removed by cutting,
lapping/grinding, and polishing. The process is time consuming and extreme care
should be taken not to make changes in the material of the thin section.
Below follows a short description of thin section preparation for petrographic/
ceramic materials and for plastics/polymers.
7.13.1 Thin Sections of Petrographic/Ceramic Materials

The preparation of thin sections can be done on machines and consumables available
in the market. In the following a method as shown in Fig. 7.29 is described. Often im-
pregnation of the material is needed before the cutting or the preparation, or both, can
take place. For this and for a further description of the cutting, lapping, and polishing
see Material/Preparation Tables 共M/P T兲 39 and 40 for petrographic/mineralogical ma-
terials and M/P T 02–06 for ceramics.
1. The specimen to be sectioned is selected often from a larger piece.
2. The specimen is sectioned normally with wet abrasive cutting using a diamond
metal bond cut-off wheel. The size of the specimen depends on the size of the glass
slide used 共see below兲.
3. For minerals, one side of the specimen is lapped in two steps with SiC powder, grit
P220 and P1000, on a cast iron disk to obtain a plane surface; normally this is done
in a special specimen holder plate on a semiautomatic grinder/polisher. For ce-
ramics, grinding and polishing of one side are made as described in M/P T 02–06.
4/5. A glass slide 27 by 46 mm, 28 by 48 mm or 30 by 45 mm is ground to a given

thickness, e.g., 1.164 mm on a special machine with a diamond grinding wheel
or lapped in a holder as described in No. 9 below.
6. The specimen, with the prepared side towards the glass, is glued to the glass slide
under vacuum using epoxy.
7. The surplus material of the specimen is removed by cutting with a diamond cut-off
wheel to a thickness of about 0.5 mm 共0.02 in兲.
8. The mineralogical thin section is ground down to 80– 100 ␮m on a special ma-
chine with a diamond grinding wheel, or only lapped as described under No. 9.
Ceramics are ground according to M/P T 02–06 to a thickness of approximately
80 ␮m.
9. Mineralogical materials are lapped with SiC powder on a cast iron disk in a special
holder on a semiautomatic grinder/polisher so that the finished section has a
thickness, including the resin layer, of e.g., 30 ␮m. The holder has built-in sticks of
boron carbide or diamond so that the process stops when the section has the thick-
ness that is wanted. If the thin section has been ground down to 80– 100 ␮m on a
special machine, lapping only with grit P1000 SiC powder is needed. If all material
shall be removed by lapping, two steps are used, grit P220 and grit P1000. Ceram-
ics are fine ground and polished down to 5 – 30 ␮m depending on the ceramic. The
preparation procedure follows M/P T 02–06.
10. If the thin section is to be polished, this is done in a special holder so that the final
thickness is in the range of 20– 25 ␮m.
The finished thin section can now be examined in reflected light. For examination
in transmitted light, a cover glass shall be placed on the polished surface.
7.13.2 Thin Sections of Plastics/Polymers

Thin sections are made when plastics and polymers are required to be examined by
transmitted light or contain hard inclusions. Most often unfilled plastics and polymers
can be examined in the form of thin microtome slices 共see below兲. If carefully prepared,
the thin sections made by grounding/polishing will be less damaged than a thin micro-
tome section so it is to a high degree the purpose of the examination that decides which
method to use. In the following a method for preparing thin sections39–41 is described
that is based on the methods stated in Material/Preparation Tables 64 and 65, Section
13.2.3.
1. A specimen with good edge retention is made.
2. A thin slice is cut from the prepared side of the specimen. See Material/
Preparation Tables 64 and 65.
3. The prepared side of the slice is glued to a glass slide with an adhesive while not
disturbing the specimen material and without air bubbles.
4. Grind down manually or in a holder to about 20 ␮m from the required thickness.
5. Fine grind to about 5 ␮m from the required thickness.
6. Polish with 3 ␮m diamond and finish with alumina, step P 3 in Method C-64 to a
thickness of 10– 15 ␮m.
For examination in transmitted light, a cover glass is placed on the polished sur-
face; this is not needed for reflected light.
As mentioned above, thin sliced specimens of plastic and polymers can be made
with a microtome, where the slice is cut in a thickness of 3 – 30 ␮m, generally around
10 ␮m. For further information, see Refs. 40, 41 and Section 7.14.
Fig. 7.29—Method for preparation of petrographic/ceramic thin sections. 1. Sampling. 2.

Cutting of a specimen. 3. Lapping of the specimen. 4./5. Grinding/lapping of glass slide. 6.
Cementing of specimen to glass slide using epoxy under vacuum. 7. Cutting of surplus material.
8. Grinding on a special machine of thin section, or lapping as shown in 9 down to 80 ␮m 9.
Lapping of thin section in a special holder down to e.g., 30 ␮m 共section and resin layer兲. 10.
Polishing in a special holder down to approximately 25 ␮m. 11. The finished thin section.
7.14 Microtomy—Ultramilling
Both microtomy and ultramilling are mechanical preparation processes comparable
to grinding and polishing, and made on relatively sophisticated equipment. In most
cases the specimen, soft metal, or other soft materials can be examined without further
preparation.
Microtomy is developed for preparation of biological specimens for transmitted
light. In this case the thin section is made by moving the specimen with a controlled
feed into a fixed tool 共knife兲. In this way a section of a thickness of 0.5 to 60 ␮m can be
made, suited for examination in transmitted light. This method can be used for prepa-
ration of plastics as described in Section 7.13.2 and for preparation of bone, teeth, and
other organic materials.
When used for metals the microtome produces a surface comparable to a plane
grinding or polishing for examination in reflected light. To justify the use of a micro-
tome and ultramilling 共see below兲 the finished surface should be of a high quality, ready
for the microscope. Soft, nonferrous metals up to a hardness of 150 HV can be pre-
pared on very stable microtomes using special knives with hard metal or diamond
edge.
Microtomes are commercially available.
In ultramilling the specimen surface is prepared not with a knife but with a rotat-
ing milling tool.
The specimen is placed on a sledge traveling underneath the milling head consist-
ing of a vertical, rotating spindle equipped with a diamond cutting tool. The rotational
speed of the spindle is adjustable between 500 and 3000 rpm. The feed between speci-
men and milling tool can be adjusted in steps from 1 ␮m, securing a very fine surface.
Also the speed of the sledge can be adjusted according to the properties of the specimen
material. The process is done in two steps, pre-milling with a special cutter, where the
deformations from sectioning, etc., are removed, and the finishing step using a milling
tool which leaves a very smooth surface ready for investigation.
Ultramilling equipment is commercially available.
8
Electrolytic Polishing/Etching
ELECTROLYTIC POLISHING OR ELECTROPOLISHING „ANODIC POLISHING…
is a polishing method whereby the specimen is placed as an anode in an electrolytic cell
and the electrolysis establishes a surface suitable for metallographic analysis.
In principle, electropolishing is the ideal polishing method because no deforma-
tions are added to the surface during the process, and most or all deformations intro-
duced before the polishing are removed. Also, the process is done in a very short time,
usually in 5 to 20 s.
The electrolysis has some effects that unfortunately limit the use. Most pure met-
als and a vast number of alloys can be electropolished, with special advantage to metals
that are relatively difficult to polish mechanically, such as aluminum/aluminum alloys
and copper/copper alloys. But as soon as the material has several phases with a certain
difference in potential, the results are not satisfying. To limit the negative influence of
the electrolysis by shortening the process time, the specimen is usually mechanically
ground and sometimes polished before the electropolishing.
An advantage with electropolishing is the possibility of electrolytic etching of the
specimen as part of the process.
8.1 The Electrolytic Polishing/Etching Process

Electrolytic polishing is the anodic dissolution of the specimen surface in an electro-
lytic cell 共see Fig. 8.1兲.42 An electrolytic cell is used very often for depositing a coating
on a work piece, the cathode, removing the material from the anode; in this case a pol-
ishing of the anode barely takes place. It is, however, possible to control the conditions
in the cell so that a “smoothing”, removal of all large-scale irregularities 共above 1 ␮m兲,
takes place. This is followed by a “brightening” which is a removal of all submicro-
scopic irregularities down to approximately 0.01 ␮m, establishing a surface of the an-
ode without irregularities that is suited for microscopical examination. The amount of
Fig. 8.1—Schematic drawing of an electrolytic cell, showing the anode, cathode and
electrolyte.
156
Chapter 8 Electrolytic Polishing 157
material removed is so small that the metal ions stay in the electrolyte without being
deposited on the cathode.
A number of factors play a role for obtaining the right conditions for polishing:
• Shape of polishing chamber, position of anode and cathode.
• Voltage.
• Anode current density.
• Electrolyte composition and temperature.
• Flow of electrolyte.
• Condition and area of the specimen surface.
• Polishing time.
The process, especially the brightening, is not fully understood, but the supposed
process is described in the following.
8.1.1 The Polishing Cell

The specimen surface normally has been ground on SiC grinding paper or on a dia-
mond disk, 共grit P500 or finer兲, before electropolishing 共see Chapter 6兲. In some cases,
however, it is possible to go straight to electropolishing from the cut-off, but in most
cases a fine grinding, as mentioned, and even a rough polishing is needed. The surface
before electropolishing will in all cases have “hills” and “valleys” as shown in Fig. 8.2.
This figure shows the development of the process from the rough ground surface to the
finished surface 共see further explanation below兲.
The specimen is placed in an electrolytic cell 共Fig. 8.3兲 shown schematically with
the specimen as anode, a thermometer for temperature control, a stirrer to obtain an
electrolyte flow, and a cooling vessel around the cell to keep the temperature constant.
The dc voltage is controlled by a potentiometer, the voltage and amperage can be mea-
sured on meters, and a timer will control the process time.
8.1.2 Smoothing and Brightening

To explain the theory behind the process, an ideal polishing sequence based on an elec-
trolytic cell using a potentiostat is used. The resulting current-density curve is shown in
Fig. 8.4 with the developments on the specimen surface as shown in Fig. 8.2.
When starting the process in the cell shown in Fig. 8.3, by increasing the voltage
from 0 V towards Point B 共Fig. 8.4兲, at first a direct anodic dissolution takes place. At
Point B, a viscous film is developed and an electroetching of the specimen surface takes
place, removing very little material 共see Section 9.5兲. When the voltage/current density
reaches the level of Point B an unstable condition develops until Point C, where a stable
plateau is established with increasing voltage. At this plateau the previously developed
viscous film, having a passivating effect, reaches equilibrium, enabling a smoothing of
the specimen surface 共see Fig. 8.2兲. The material removal by diffusion through the vis-
cous layer will be higher at the tops of the hills, the current being higher, because the
diffusion path is shorter than at the valleys. This creates a smoothing of the surface.
The best polishing takes place between C and D on the curve. With increasing current
density, D towards E, oxygen bubbles develop and make openings in the viscous layer,
creating pitting in the specimen surface. Close to D the gas development is still rela-
tively low and polishing may take place, but at E the amount of bubbles will totally
destroy the film and polishing is not possible.
The presence of the viscous layer, however, cannot explain the brightening of the
submicroscopic irregularities. On many examinations it has been proven that a thin
solid film will arise on the surface of the anode, which will play an important part dur-
Fig. 8.2—Schematic drawing showing the surface of the specimen during the different steps
developed during the electrolytic polishing and etching. The letters A to E refer to the curve in
Fig. 8.4.
ing the polishing. This film is considered to have a thickness of a few atom layers and is
very difficult to identify with regard to its composition. Some scientists think the film
consists of metal oxide, but a final proof of that has not been obtained. The presence of
the film, however, must be taken for granted. The very thin film follows very exactly the
surface of the anode 共specimen兲 and the decrease of metal ions will be the same every-
where. This will cause a removal of the quite small irregularities.43
The voltage/current density curve at a cell without potentiostat will not show the
same distinct plateau. Figure 8.5 shows a curve taken from polishing of mild steel on a
commercial electropolisher.
Fig. 8.3—Schematic drawing of an apparatus for electrolytic polishing/etching.
8.1.3 Electrolytic Etching

For many materials, the etching process can take place as a continuation of the polish-
ing but at a lower voltage. The low voltage, usually around one-tenth of the polishing
voltage between A and B on the curve 共Fig. 8.4兲 creates a weak attack on the specimen
Fig. 8.4—Theoretical curve showing current density versus voltage during the process of
electrolytic polishing/etching.
Fig. 8.5—Current density/voltage curve at electropolishing of mild steel.
surface, preferably attacking the grain boundaries 共see Fig. 8.2兲. In some cases, like
with stainless steel, the polishing electrolyte cannot be used for etching, and etching
must be performed with another electrolyte outside the polishing chamber 共see Sec-
tion 9.5兲.
8.1.4 Advantages and Disadvantages

At the time when specimen preparation to a high degree was based on manual polish-
ing with alumina, with long polishing times, the quality of the achieved preparation
result was relatively low. Therefore, when electrolytic polishing was commercially de-
veloped around 1950, it gained ground for many years because the quality was higher
than with alumina polishing. A number of artifacts developed during electropolishing,
problems with edge retention, etc., were accepted as “necessary evils.” With the devel-
opment of diamond polishing, rigid composite grinding disks and better polishing
cloths, the quality of mechanical polishing has increased considerably, and the weak
points of electropolishing can hardly be accepted for a number of materials, even when
mechanical polishing normally takes more time than electrolytic polishing. With softer
materials, relatively difficult to polish mechanically, the electropolishing still has an
advantage.
Electropolishing should be performed on commercially available polishers, spe-
cifically developed for that purpose. In principle, electropolishing can be performed in
any electrolytic cell, but because of the risk of fire, explosion, spill, etc., the commer-
cially developed apparatus provides better safety and good, reproducible results 共see
Section 8.4兲. The following descriptions relate to the use of a commercial
electropolisher.
Advantages
• Etching included: For most materials it is possible to include the etching as the last
step in the process.
• No deformation: The process leaves a clean, undistorted surface, not adding defor-
mation to the specimen surface. This is an important feature when doing research
work which is surface-related, or for preparing surfaces for micro hardness test-
ing, X-ray studies and electron microscopy.
• Fast: The method is very fast. The polishing, which takes place after mechanical
grinding and in some cases rough polishing, only takes 5 to 15 s for the polishing
and 2 to 10 s for etching 共if possible兲. This can be very important in quality control.
• Reproducible: When all parameters of a procedure are established, the process can
be exactly repeated giving reproducible results.
Fig. 8.6—Mild steel mechanically polished with the inclusions clearly visible 共a兲, and elec-
trolytically polished with the inclusions partly removed by the polishing process 共b兲.
• Automatic: The modern electropolishers are totally automated so that all param-
eters are programmed before the process starts. This secures that the operation is
totally independent of the operator. Also, a number of different methods can be
saved in the database of the apparatus.
Disadvantages
• Nonuniform material removal: The different phases in the specimen surface will
have a different electrochemical potential. This means that the material removal
will be different from phase to phase 共preferential attack兲, the more anodic phase
having the biggest removal rate. An example is gray cast iron, where the graphite
will stand in relief relative to the matrix. Also, at inclusions a problem exists. See
Fig. 8.6 showing mild steel polished mechanically 共a兲 with visible inclusions, and
electropolished 共b兲 with inclusions partly removed. This takes place because the
Fig. 8.7—Surface with deformations from grinding still visible after electrolytic polishing.
current density will increase around the inclusion so that material from the matrix
is preferably removed which causes a relief or even a dropout of the inclusion 共see
also Fig. 1.6兲.
• Low removal rate: The removal rate is relatively low, so in case of deep deformation
in the specimen surface, the polishing time must be long, causing different arti-
facts to develop 共see below兲. Caused by the low removal rate, the deformations
from the grinding scratches are not removed and they are visible in the surface, as
shown in Fig. 8.7. This can be avoided if the grinding is done with a finer grit up to
P4000, or even a rough polishing with 9 or 6 ␮m is performed.
• Bad edge retention: Even when the edge of the specimen is protected with a lacquer
or mounted, the edge will be preferentially attacked and rounded 共see Fig. 8.8兲.
• Limited polished area: Depending on the available amperage restricting the cur-
rent density, the polished area is limited. Short time polishing performed on com-
Fig. 8.8—Edge rounding after electrolytic polishing.

mercial electropolishers takes place at 1 to 2 A / cm2 共0.16 A / in2兲. In most cases a

polisher is made for a maximum amperage of 10 A 共see below兲.
• Artifacts—Unplane Surface: Due to the different potentials mentioned above, all
variations in the specimen material tend to cause artifacts like increasing the size
of pores, preferential attack of differently oriented grains and pitting 共see Fig. 1.6兲.
The surface is often not plane but wavy, which causes problems at high magnifica-
tions. See also Sections 13.5.4 and 13.6.5.
8.2 Electrolytes
The electrolyte is an important factor in the electropolishing process. A good electro-
lyte should have a number of characteristics to support a good polishing and etching.
When choosing an electrolyte for polishing a metal, certain basic principles must be
taken into consideration. The electrolyte must have a low viscosity since the viscosity
determines the quality of the viscous layer that forms on the specimen surface. It must
be a good solvent for the anodic material under the prevailing electrolytic conditions.
The formation of any insoluble reaction products that deposits on the specimen sur-
face interferes with the polishing operation. The electrolyte should, preferably, not at-
tack the metal in the absence of the current, but it is not always possible. Similarly,
preference will be given to an electrolyte that can be used at room temperature, and is
little affected by changes in temperature, because in practice it is difficult to control
and maintain an exact electrolyte temperature during the polishing operation. Lastly,
the electrolyte must be stable and safe to handle.
The most used electrolytes are based on perchloric, phosphoric, hydrochloric, or
sulfuric acids mixed with ionizing solutions like acetic acid, alcohol, or water. Perchlo-
ric acid 共HClO4兲 is by far the most universal acid suited for polishing of a great number
of metals. Unfortunately HClO4 is a very dangerous substance that can cause explo-
sions, especially when mixed with acetic anhydride 共共CH3CO兲2O兲. It is safe, however, to
use perchloric acid if the correct recommended recipes are used and the necessary pre-
cautions are taken 共see Section 13.3.2, Table 13.2兲. Nevertheless, use of perchloric acid
is not permitted in some laboratories. If possible, an electrolyte that is mixed with per-
chloric acid and acetic acid 共glacial兲 should be avoided. The temperature of a perchlo-
ric acid electrolyte should not exceed 30 to 35° C 共90 to 100° F兲.
It is practical to limit the number of electrolytes used in a laboratory from one to
three, covering most materials. With a general purpose electrolyte based on perchloric
acid covering aluminum/Al alloys, steel, stainless steel, zinc, lead, magnesium, tita-
nium, and other metals, supplemented with an electrolyte based on phosphoric acid
covering copper and copper alloys, most needs should be covered.
These two electrolytes are:
No. 1-1 共Table 13.2兲 78 mL perchloric acid 共60 %兲, 90 mL distilled water, 730 mL
ethanol 共96 %兲, 100 mL butylcellosolve 共ethylene glycol monobutyl ether兲.
The perchoric acid which must be shipped and stored separately, should be added
to the mixture of ethanol, butylcellosolve, and water immediately before use.
This electrolyte has a lifetime of around two months according to use.
Attention: With this and other perchloric acid electrolytes, they should never be
allowed to become more concentrated by evaporation of one or more of the compo-
nents 共water/ethanol兲 during storage or use.
No. 3-2 共Table 13.2兲 250 mL phosphoric acid, 500 mL distilled water, 250 mL etha-
nol 共96 %兲, 50 mL propanol 共n-propanol, 100 %兲, 5 g urea 共carbamide兲.

Water, ethanol, and propanol are mixed and the acid is added under constant stir-
ring.
For more electrolytes see Table 13.2, ASTM Standard Guide for Electrolytic Pol-
ishing of Metallographic Specimens 共E 1558兲 and Refs. 2,4, and 9.
For Safety Precautions, see Section 26.2.
8.3 Electropolishing in Practice

As already mentioned above electrolytic polishing has some limitations, but also has a
number of advantages. Before deciding on the use of electropolishing for a given mate-
rial a number of factors should be evaluated that are given below. See also Section
13.5.4 and 13.6.5.
8.3.1 Factors Influencing Electrolytic Polishing
Material
The material must be electrically conductive and, if mounted, a good electrical connec-
tion should be secured. At the same time, the mounting material around the specimen
should not be conductive 共see Section 3.2.2兲.
Electrolyte
The right electrolyte composition for a given material should be selected.
The Area to be Polished

When using a commercially available electropolisher 共see below兲, the specimen is
placed on a mask, defining the area to be polished. The area should be in relation to the
voltage/amperage 共current兲 available. The smaller the area, the better, giving the best
polishing conditions and the lowest development of heat. Typically an area of
1 to 2 cm2 共0.16 to 0.32 in2兲 is polished.
Voltage/Current
The voltage depends on the type of material and electrolyte. Usually the voltage creat-
ing the necessary amperage 共current兲 to establish the correct current density is set.
The Flow of the Electrolyte

It is important that the reaction products established on the specimen surface during
the process are removed continuously and the temperature in the polishing chamber is
kept low. This is done by circulating the electrolyte through the chamber. At the same
time it is important not to create any air bubbles that are caused by a flow rate that is
too high.
The Temperature of the Electrolyte

The temperature should be kept as close to room temperature as possible. This gives
the best polish with high reproducibility. If the electrolyte is heated to temperatures
above 30 to 35° C 共90 to 100° F兲, the process deteriorates and with electrolytes with
perchloric acid and ethanol, the risk of fire and explosion will increase. Therefore, if
Fig. 8.9—Schematic drawing of a polishing table for electrolytic polishing.
more than a few polishings are done in a short period of time, the electrolyte must be
cooled.
Time
The polishing time should be as short as possible to avoid the negative effects of the
electrolysis. For this reason it is important to prepare the specimen before the
electropolishing.
8.3.2 Example of Electrolytic Polishing/Etching

See Method E 1-01, Section 13.3.6 stating a much used method for steel.
8.4 Electrolytic Polishing Equipment

Electropolishers have been commercially available for many years, both for normal
polishing in the laboratory and as portable polishers for polishing on the spot. Also,
apparatus for electrolytic thinning of specimens for TEM is available 共see Section 8.6兲.
Only electropolishers for normal polishing for laboratory use will be described below.
8.4.1 Electropolishers for Laboratory Use

These are usually built in two parts: a polishing table, the cell where the actual polish-
ing is done, and an operating unit containing electronics and software.
The Polishing Table

The main components 共see Fig. 8.9兲 are: the polishing chamber with cathode and mask
upon which the specimen is placed, the electrolyte container with a pump circulating
the electrolyte, driven from outside the electrolyte container with a magnet, cooling
coil, and a contact beam making anodic contact to the specimen.
The specimen is placed with the surface to be polished against the exchangeable
mask. The mask has a hole of 0.5 to 5.0 cm2 共0.08 to 0.8 in2兲, allowing contact between
the electrolyte and the specimen. The cathode of stainless steel is placed in the bottom
of the polishing chamber and during the polishing/etching the pump circulates the
Fig. 8.10—Electrolytic polisher/etcher with electrolyte temperature control and a load

simulation mode for pre-selection of polishing/etching voltages. Input to power source is
1 kVA.19
electrolyte through the chamber in a laminar flow. This flow can be adjusted. Often the
pump is driven magnetically as shown to avoid corrosion of metal parts. A cooling coil
of stainless, acid resistant steel is placed around the pump, through which cooling wa-
ter can be circulated to keep the electrolyte temperature constant, normally between
20 to 30° C 共70 to 90° F兲. In certain cases a cooled liquid is circulated making polishing
at sub 0 ° C 共32° F兲 temperatures possible. The container is exchangeable, and in this
way the electrolyte can be stored covered with a lid when not in use. This allows for the
least possible handling of the electrolytes.
The Operating Unit

The operating unit has controls for all process parameters and a power supply. Using a
microprocessor, storing of polishing methods is possible that saves time when different
materials are to be polished.
Electropolishers
Electropolishers are only made by a few suppliers; an example is shown in Fig. 8.10. It
has electrolyte temperature control and a load simulation mode for preselection of
polishing/etching voltages. Input to power source is 1 kVA.
8.5 Field Metallography—Nondestructive Electropolishing

One of the very first commercially available electropolishers in the 1940s was made for
nondestructive polishing. Only a spot of 1 mm 共0.04 in兲 in diameter was made, allow-
ing the tested product to be sold as “new.” This was done in the laboratory or at the
manufacturer, but today nondestructive polishing is mostly “in the field,” “on the spot”
共in situ兲, used for inspection of work pieces such as steam pipes still in function.
For the right type of materials 共see earlier in this chapter兲 electropolishing is well
suited for nondestructive on the spot polishing because the polishing time is short.
Normally the same electrolytes and data are used as for normal electrolytic polishing
depending on the type of polisher used 共see Section 13.3.6兲. In most cases the spot to be
examined is first treated mechanically 共see Section 7.11兲 to secure a deformation-free
Fig. 8.11—Specimen of bronze for TEM. Electropolished with jets from two sides, 87 mA, 7.4 V,
5 min and 50 sec, electrolyte No. 3-2 共Table 13.2兲, electrolyte temperature 5 ° C 共41° F兲.
surface after electropolishing/etching. Often a replica is taken after polishing and etch-
ing 共see Sections 7.11.2 and 13.4兲.
Portable polishers consisting of a “pencil” with a polishing chamber to be pressed
against the work piece and a unit supplying electrolyte and an electric current are com-
mercially available.
8.6 Electrolytic Thinning for TEM

In a transmission electron microscope 共TEM兲, normally a 3-mm 共0.118 in兲 diameter
specimen is used. This specimen must be very thin to allow for the TEM analysis, and
electropolishing is suited for thinning of conductive metal specimens. By electrolytic
thinning a hole is made in the specimen, and the edge of this normally is very thin, as
shown in Fig. 8.11.
The specimen is normally thinned first by grinding so that a 3-mm 共0.118-in兲 diam-
eter disk with a thickness of 0.5 to 0.1 mm 共0.02 to 0.004 in兲 can be thinned. The thin-
ning is a normal electrolytic polishing as described above, except the thinning, in most
cases, takes place on both sides at the same time. This can actually be done in a glass
beaker, positioning the specimen as anode, with a lacquer to cover the edges so that
only the center is polished. This “window” technique is stopped when a hole is estab-
lished in the specimen, and it is quickly taken under water to avoid further attack. This
method is relatively laborious, giving less reproducible results; therefore, the commer-
cial jet thinners have been developed. See Fig. 8.12 which shows a cross section of the
polishing chamber. The specimen is placed in the middle in a movable holder. On each
side of the specimen holder a nozzle holder is placed with a nozzle leading the electro-
lyte flow toward the sides of the specimen. A cathode is placed at each nozzle. The pro-
cess is observed from one side either by watching or with a photocell reacting to the
light which breaks through the hole in the specimen created by the polishing process.
The light comes from a light source placed behind the specimen, and when the photo-
cell is “hit” the process stops automatically, ensuring a very small hole in the specimen.
Electrolytes and data from normal electrolytic polishing can often be used, but in
Fig. 8.12—Schematic drawing of a polishing cell for electrolytic jet polishing for TEM. The
specimen placed in a holder for quick removal, is attacked from both sides simultaneously,
having two cathodes and the electrolyte in two jets conducted towards the specimen. Using a
photocell instead of an eye, the process can be switched-off immediately when the light
breaks through the specimen, assuring a very small hole in the specimen.
certain cases special electrolytes and temperatures, considerably below room tem-
perature, are needed to be able to effectively control the process. See the literature on
electrolytic thinning.44
8.7 Chemical Polishing

Chemical polishing is a relatively simple method, comparable to electrolytic polishing,
only without an electric current. It is a process based on the electrolytic action that
takes place when a chemical solution gets into contact with the metal surface 共see also
Section 9.4.1兲. The chemical polishing solutions are developed so that material is re-
moved from the surface of the specimen in much the same way as in electrolytic polish-
ing. This means that chemical polishing has the same disadvantages as mentioned
above under electropolishing. The polishing is made by immersing the specimen into
the polishing solution often combined with a rubbing to remove reaction products.
Due to the disadvantages of the method and the trouble/danger with handling of
chemicals, chemical polishing is not used much. With certain sensitive materials, how-
ever, like cadmium, lead, zinc, tin, and zirconium, chemical polishing might be useful
when mechanical polishing or electropolishing are unsuccessful. See the literature,
Refs. 2 and 9 for further information and for chemical polishing solutions.
9
Etching
9.1 Microetching—Contrast
MICROETCHING IS ETCHING OF MICROSTRUCTURES TO BE OBSERVED BY
magnification higher than 25⫻ 共50⫻ in Europe兲. For macroetching, see Section 9.7.
In the bright field illumination 共BF兲 of the light microscope, a prepared
metallographic/materialographic specimen will only show certain features like inclu-
sions, nonmetallic phases 共graphite兲, pores, cracks, etc. It is usually not possible to see
the microstructure because the light is reflected equally from the bright surface.
Figure 9.1 shows a steel specimen, unetched 共a兲, and chemically etched 共b兲, the
etched surface revealing the grains of the microstructure 共see also Fig. 1.10兲. To obtain
an image with the structure details, a contrast between the elements in the microstruc-
ture has to be established. The contrast can be caused by a number of methods 共see the
diagram Fig. 9.2兲. The most important of these methods will be further discussed in the
following sections. Chemical microetching of metals is covered by ASTM Standard
Practice for Microetching Metals and Alloys 共E 407兲, see also Section 12.5. For further
study see the literature, Refs. 2, 4, 9, 21, 26, 27, 45–49.
9.2 Contrast Without Surface Modifications—Microscope

Techniques
In the bright field illumination 共BF兲 of the light microscope only structure details that
differ in reflectivity from one another can be distinguished from each other. For this
reason special microscope techniques have been developed, making it possible to ob-
serve certain details that cannot be observed in BF. See also Part III of this book.
9.2.1 Dark-Field Illumination „DF…

In dark-field illumination, the light beam is angled to the specimen surface, making it
possible to observe details like inclusions and scratches that stand in relief to the sur-
rounding structure. This can be of advantage when observing some features, such as
lightly etched grain boundaries and light scratches 共see Fig. 15.10兲.
9.2.2 Differential Interference Contrast „DIC…

This illumination technique uses a beam splitter to direct two beams towards the speci-
men surface. This makes even very small differences in height 共relief兲 visible, and DIC
can be used with great advantage using relief polishing 共see below兲, in this way avoid-
ing an additional “etching” process 共see Fig. 15.14兲.
9.2.3 Polarized Light „POL…

Using polarized light the microstructure of anisotropic metals such as zirconium and
titanium can be observed without any treatment of the prepared surface. For isotropic
共cubic兲 metals, polarized light can be used when an anisotropic surface film is estab-
169
Fig. 9.1—Unetched steel specimen. 共a兲 Only the inclusions can be seen. 共b兲 Etched in 3 % Nital
共100 mL ethanol 96 %, 3 mL nitric acid 65 %兲 revealing the grains.
lished on the specimen surface. In some cases a chemically etched surface can also be
observed on an anisotropic material 共see Fig. 15.12兲.
9.2.4 Fluorescence
Some materials emit radiation when illuminated by certain types of light. Fluores-
cence can be used to distinguish pores and other surface details 共see Section 3.10 and
Fig. 3.14兲.
9.3 Contrast with Surface Modification—Etching

To obtain the necessary contrast so that a surface can be observed in bright field in a
reflected light microscope, a treatment, often called “etching” must take place. The
most used method is “chemical etching” based on an electrochemical attack of the sur-
face, but “electrolytic etching” and other methods such as “physical etching” are also
used 共see Fig. 9.2兲.
9.3.1 Grain Contrast Etching

To obtain grain contrast etching, certain grains in the specimen surface are influenced.
Figure 9.318 shows 共1兲 a grain in relief caused by relief polishing 共which could also be
established by ion etching 共see below兲; 共2兲 grains which are differently attacked by the
Chapter 9 Etching 171
Fig. 9.2—Diagram showing the methods to create surface contrast.
etchant; 共3兲 a grain covered by an interference layer 共film兲 that is selectively deposited;
共4兲 a layer deposited independently of the grains; and 共5兲 the film deposited according
to the orientation of the grains.
9.3.2 Grain Boundary Etching

In this type of etching the grain boundaries only are attacked 共see Fig. 9.3兲. Figure 9.3
shows: 共6兲 a grain boundary attacked by chemical etching; and 共7兲 a grain boundary
after treatment under heat and vacuum.
9.3.3 Reproducibility
During the preparation of the specimen, the process of making a contrast shall be re-
producible. It is important that the “etching process” does not introduce artifacts, but
Fig. 9.3—Schematic drawing of grain contrast “etching.” 共1兲 Relief polishing, 共2兲 grains
differently attacked, 共3兲 grain covered with interference layer, 共4兲 layer deposited
independently of the grains, 共5兲 film deposited according to the orientation of the grains, 共6兲
grain boundary etch, 共7兲 grain boundary treated under vacuum and heat.
ensures that the true structure is revealed. This is particularly important when image
analysis is to be performed on the specimen in question 共see Part IV兲.
Typical artifacts developed during etching are stains if the specimen surface was
not properly cleaned after the last polishing step. Also pitting and other artifacts can be
developed at over-etching.
9.3.4 Safety Precautions

Especially in chemical etching it is important to take necessary safety precations. Be-
fore using or mixing any chemical, all product labels and pertinent Material Safety
Data Sheets 共MSDS兲 should be read and undertood concerning all of the hazards and
safey precautions to be observed 共see Section 26.2兲.
9.4 Classical Etching

9.4.1 Chemical Etching
The most commonly used method for creating the necessary contrast in the specimen
surface is chemical etching, also called dissolution etching.2,4,9,21,26,45–47
Chemical etching is a process based on the electrolytic action that takes place
when a chemical solution 共etchant兲 is in contact with a metal surface. The etchant, nor-
mally having a “reduction” component that is usually an acid, an “oxidizer” compo-
nent, and a “modifier” component, causes an electric potential between differently ori-
ented grains, different phases, grains and boundaries, inclusions, and matrix, etc. The
difference in attack, which is the amount of material removed from the single details,
reveals the structure. For electrolytic etching, where the specimen is placed as an an-
ode in an electrolytic cell, the applied current acts as the oxide component.
A number of etchants for chemical etching are stated in Table 12.2.
9.4.2 Precipitation „Color… Etching

This etching method, also called color etching or tint etching, uses a chemical etchant
that reacts with the specimen surface and deposits a very thin insoluble film. The film
acts as an interference layer producing colors in bright field illumination and polarized
light. Variations in the grains influence the observed colors. Precipitation etching re-
quires a high quality of the prepared specimen; even small scratches or deformations
will be visible when the film is established.46,47
9.4.3 Heat Tinting

Oxidizing will take place on the surface of metal specimens that are heated to tempera-
tures in the range 250 to 700° C 共500 to 1300° F兲 in air. The oxidized film will vary in
thickness according to the variations in the specimen material. If the layer is thicker
than 30 nm, interference colors can be seen in the bright field of the microscope. Heat
tinting is not suited for carbon steels and low-alloy steels, but works well with high-
alloy steels, tool steels, stainless steels, titanium, and other metals.
9.5 Electrolytic Etching

9.5.1 Anodic Etching
Anodic etching, also known as electrolytic etching, is in principle the same as chemical
etching, except in this case the specimen is placed as an anode in a galvanic cell. This
means that material is removed from the specimen surface, causing an etching and not
a polishing as with electrolytic polishing 共see Fig. 8.1兲. The etching takes place because
the voltage and current density are low 共see Fig. 8.4兲.
Frequently, electrolytic etching can be performed as the second step of the
polishing-etching process, using a voltage of approximately 1 / 10 that used as the pol-
ishing voltage. In many cases, however, the electrolyte suited for polishing cannot be
used for etching. In this case, electrolytic etching often takes place using a stainless
steel vessel connected as a cathode containing the etchant. The specimen is handled
with a pair of tongs, connected as an anode, and a suitable low direct current is estab-
lished between the cathode and anode. An example is etching of stainless steel that can
be electrolytically etched in an electrolyte 共etchant兲 of 10 g oxalic acid in 100 mL water,
using a voltage of 6 V in 10 to 15 s. A number of etchants for electrolytic etching are
stated in Table 12.2.
9.5.2 Anodizing
During this process that is closely related to electrolytic etching/polishing, a layer, often
an oxide film, is established on the surface of the specimen 共see Fig. 9.3共3–5兲兲. This in-
terference layer will produce a colored image in bright field illumination and with po-
larized light. The layers can be related to the layers created at precipitation etching,
heat tinting, and vapor deposition.
9.5.3 Potentiostatic Etching

A reproducible, selectively working electrolytic etching is made with an electronic po-
tentiostat and a reference electrode. With the potentionstat it is possible to establish a
constant potential at the specimen surface 共anode兲.
Because of the controlled etching process, potentiostatic etching is very well
suited for selective etching of desired microstructural constituents with high repro-
ducibility.
9.6 Physical Etching

9.6.1 Relief Polishing
In some cases it is possible to establish a contrast by relief polishing that creates a small
relief between the grains or the grain boundaries, or both 共see 1兲 in Fig. 9.3兲.
Relief polishing is often done with a relatively resilient cloth 共see Section 7.4兲 and a
very fine polishing medium like colloidal silica or alumina 共see Section 7.5兲. Relief can
also be established through chemical mechanical polishing 共see Section 7.12兲.
Relief polishing should only establish a very small relief between the single grains
or other constituents, not to disturb the microstructure; therefore, often DIC is used
when examining relief polished surfaces 共see Section 9.2.2兲.
9.6.2 Ion Etching

This method, also called ion beam etching, uses an ion bombardment of the specimen
to remove material from the single grains, depending on orientation and phase compo-
sition. Ion beam etching can be used for thinning of specimens for transmission elec-
tron microscopy 共TEM兲 as an alternative to electropolishing 共see Section 8.6兲. It is,
however, also suited for etching microstructures, especially of nonconductive materi-
als for materialographic examination.48 The ions, often argon, are supplied in a strong
vacuum 共10– 4 mbar兲 by an ion gun towards the specimen which is often placed so that
the surface is bombarded under an angle.
9.6.3 Thermal Etching

Thermal etching takes place at high temperatures in an oven with an inert atmosphere
or vacuum. Both metals and ceramics can be thermally etched. During the process
grooves are formed in the grain boundaries/phase boundaries and grain surfaces are
curved. The method can be used at high-temperature microscopy for metals, but ther-
mal etching is mostly used for etching of ceramics taking place at temperatures be-
tween 1000 and 1400° C 共1800 and 2500° F兲.26
9.6.4 Vapor Deposition

Interference films can be established on the specimen surface by vacuum deposition of
a suitable material. This method 共Pepperhof兲 will enhance the irregularities in the pol-
ished surface and the structure will be visible through the interference between the
light reflected from the top of the film and the specimen surface. The film materials
shall have a high refractive index; ZnS, ZnTe, ZnSe, and TiO2 are often used. The pro-
cess takes place in a chamber with a vacuum of about 10– 5 mbar.49
9.6.5 Sputtering
Sputtering—Cathodic Discharge
Interference layers 共films兲 can be produced by sputtering. In sputtering, materials like
carbon, gold, or gold-palladium alloys are atomized by bombarding a surface 共target兲
with high energy particles. Positively charged gas ions produced by electrical discharge
共1 to 5kV dc兲 are accelerated by a potential difference between the anode 共specimen兲
and cathode 共target兲 so that they bombard the cathode, thereby dislodging atoms that
leave the surface in all directions. These atoms settle on the specimen surface where
they form the desired layer. If undesirable reactions with the target material shall be
avoided, the process shall take place at 0.03 to 0.05 mbar in an inert gas like argon.49
Reactive Sputtering
At reactive sputtering, not an inert gas, but an atmosphere of oxygen is used. This
means that the atomized target material is oxidized, forming oxidic layers on the
specimen.49
9.7 Macroetching
Macroetching can be defined as revealing the macrostructure for examination with the
naked eye or at a magnifications up to 10⫻, either direct or by using sulfur prints 共Bau-
mann prints兲.
Macroetching is considered outside the scope of this book.
Macroetching is described in great detail in the three following ASTM standards
共see also Section 12.4兲.
Standard Test Method for Macroetching Metals and Alloys 共E 340兲. This standard
is very comprehensive covering a wide range of materials.
Standard Methods for Macrotech Testing Steel Bars, Billets, Blooms, and Forging
共E 381兲
Standard Practice for Preparing Sulfur Prints for Macrostructural Examination

共E 1180兲
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phy’,” Metal Progress, September 1968, p. 21.
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hagen, Denmark, 2000.
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Park, Ohio, USA, 1999.
关10兴 Malkin, S., Grinding Technology, Ellis Horwood Ltd., Chichester, UK, 1989.
关11兴 Shaw, M. C., Principles of Abrasive Processing, Clarendon Press, UK, 1996.
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关14兴 Wellner, P., “Investigations on the Effect of the Cutting Operation on the Surface Deformation
of Different Materials,” Practical Metallography, Vol. 17, 1980, p. 525.
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Cutting in Materialographic Cut-Off Machines,” Proceedings, MC95 International Metal-
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关16兴 Cloeren, H. H., “Thermische und mechanische Probenentnahme und deren Einfluss auf das
wahre Gefüge,” Fortschritte in der Metallographie, Vol. 33, Werkstoff-
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Informationsgesellschaft mbH, Frankfurt, Germany, 2003, p. 93.
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关19兴 Courtesy of Buehler, Ltd.
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关21兴 Bramfitt, B. L. and Benscoter, A. O., Metallographer’s Guide, Practices and Procedures for Iron
and Steels, ASM International, Materials Park, Ohio, USA, 2002.
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关24兴 Nelson, J. A. and Slepian, R. M., Practical Metallography, Vol. 7, 1970, p. 510.
关25兴 Glancy, S., Structure, Vol. 22, 1990, p. 14.
关26兴 Carle, V., Schäfer, U., Täffner, U., Predel, F., Telle, R., and Petzow, G., “Ceramography of High
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Description of the Microstructure,” Practical Metallography, Part I, Ceramographic Etch-
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542–552; Part V, Silicon Nitride, Vol. 28, 1991, pp. 592–610; Part VI, High-Temperature Su-
perconductor YBa2Cu3O7, Vol. 28, 1991, pp. 633–648; Part VII, Boron Carbide, Vol. 31, 1994,
pp. 218–233; Part VIII, Aluminum Oxide, Vol. 32, 1995, pp. 54–76.
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rialographic Preparation, Elsevier Science Inc., New York, USA, 1999.
关28兴 Exner, E. and Kuhn, K., Practical Metallography, Vol. 8, 1972, pp. 453–469.
关29兴 Bousfield, B., Surface Preparation and Microscopy of Materials, John Wiley & Sons, Chi-
chester, UK, 1992.
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466–476.
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关32兴 Luo, J. and Dornfeld, D. A., “Material Removal Mechanism in Chemical Mechanical Polish-
ing: Theory and Modeling,” IEEE Transactions on Semiconductor Manufacturing,
2000.
关33兴 Geels, K. and Gillesberg, B., Practical Metallography, Vol. 37, 2000, pp. 150–159.
关34兴 Burgess, D. and Blanchard, R. A., Wafer Failure Analysis for Yield Enhancement, Accelerated
Analysis, Half Moon Bay, California, USA, 2001.
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关36兴 Wulff, F. W. and Arens, T., Structure, Vol. 32, 1998, p. 9.
关37兴 Reiter, K., Reiter, M., and Arens, T., Structure, Vol. 34, 1999, p. 12.
关38兴 Katrakova, D., Damgaard, M., and Mücklich, F., Structure, Vol. 38, 2002, p. 19.
关39兴 Kopp, W.-U. and Linke, U., Practical Metallography, Vol. 17, 1980.
关40兴 Trempler, J., Practical Metallography, Vol. 5, 2001, pp. 231–269.
关41兴 Trempler, J., Practical Metallography, Vol. 10, 2003, pp. 481–531.
关42兴 McG. Tegart, W. J., The Electrolytic and Chemical Polishing of Metals in Research and Industry,
Pergamon Press Ltd., London, 1956.
关43兴 Knuth-Winterfeld, E., Korttidsmetoder til metallografisk elektropolering ved stuetemperatur,
C. A. Reitzel, Copenhagen, Denmark, 1952.
关44兴 Thompson-Russell, K. C., and Edington, J. W., Monograph Five, Electron Microscope Speci-
men Preparation Techniques in Materials Science, N. V. Philip’s Gloeilampenfabrieken, Eind-
hoven, Holland, 1977.
关45兴 Beckert, M. and Klemm, H., Handbuch der metallographischen Âtzverfahren, Deutscher Ver-
lag für Grundstoffindustrie, Leipzig, Germany, 1984.
关46兴 Beraha, E. and Shipgler, B., Color Metallography, American Society for Materials, Materials
关47兴 Weck, E. and Leistner, E., “Metallographic Instructions for Colour Etching by Immersion, Part
I 共1982兲, II 共1983兲 and II 共1986兲,” Deutscher Verlag für Schweisstechnik GmbH, Düsseldorf,
Germany.
关48兴 Gräff, I., Practical Metallography, Vol. 36, 1999, pp. 669–684.
关49兴 Bühler, H. E. and Hougardy, H. P., Atlas of Interference Layer Metallography, Deutsche Gesell-
schaft für Materialkunde, Oberursel, Germany, 1980.
Part II:
Metallographic/Materialographic
Specimen Preparation—A Hands-On
Manual
10
Introduction
THE GOAL FOR ANY METALLOGRAPHIC/MATERIALOGRAPHIC PREPARA-
tion is a true microstructure, or at least a structure that makes a correct analysis of a
structure detail possible. It should be stressed that an examination with a subsequent
interpretation, using a light microscope or other method, is of no use if the prepared
microstructure is not correct.
This part of the book is made to guide the reader directly towards the correct
preparation of the microstructure for most materials and material groups. To obtain
more information on the true structure, a more detailed description of the total prepa-
ration process and the theories behind it, see Part I of this book.
Before starting a preparation process, two facts must be considered: Specimen
Material and Purpose of Examination.
10.1 Specimen Material

The specimen material, in the following material, is decisive for the choice of a prepara-
tion process. It is evident that soft, hard, ductile, brittle, homogenous, heterogeneous,
etc., materials cannot be treated the same way to obtain a correct result.
To find the correct preparation method for a given material, the reader shall review
Table 11.1 and find the material or group of materials corresponding to the given mate-
rial 共see below兲.
10.2 Purpose of Examination

Before a preparation method is selected, the purpose of examination, in the following
the purpose, should be considered. A given material can be prepared often electrolyti-
cally in a relatively short time for one purpose, and for another purpose, a longer me-
chanical preparation sequence should be performed. An example is medium carbon
steel. If the purpose of examination is the study of grain size, the electrolytic polishing
method El-01, Section 13.3.6, can be used, having a total preparation time of approxi-
mately 3 min, including grinding 共less than 3 min兲 and polishing/etching 共10– 12 s兲. If
the purpose is examination of inclusions, the mechanical methods, C-28 and T-28, Sec-
tion 13.2.3, are recommended with a total preparation time of 10– 12 min.
Based on the purpose, the user will select the correct process/method stated in the
Material/Preparation Tables. Other information connected to the purpose, such as
etchants, will be stated also.
10.3 Specimen Preparation

Modern specimen preparation is based on a systematic approach, and in this way se-
curing the reproducibility that is a must in both research and quality control. In the
Material/Preparation Tables, Section 13.2.3, the total preparation process is stated, in-
179
cluding sectioning, mounting, grinding/polishing methods 共mechanical and electro-

lytical兲, and etching. Mechanical polishing can be done by hand and is also described in
this part of the book, but for the indicated methods, a semiautomatic grinder/polisher
is recommended.
A section covering “trouble shooting” of all stages of the preparation process, and
how to analyze the used preparation method to avoid or overcome artifacts is also in-
cluded in Part II.
11
Specimen Material—Table 11.1
THE SPECIMEN MATERIAL, COMBINED WITH THE PURPOSE OF EXAMINA-
tion, is decisive for the choice of preparation process/method. Two physical properties,
hardness and ductility, are important in selecting a specific preparation method, but
conditions such as coatings or composites also play an important role.
In Table 11.1, Section 11.3, most materials and the most common material combi-
nations are indicated to guide the reader to a preparation process/method best suited
for a specific material stated in the Material/Preparation Tables, Section 13.2.3.
11.1 Classification of Materials

A classification of all available materials is needed to guide the reader to a specific ma-
terial in an efficient way. This is done by defining twelve main groups partly based on
material composition, such as “ceramics,” “ferrous metals,” etc., and on other impor-
tant features like “coatings,” “electronic components,” etc. The twelve main groups are
stated alphabetically 共see below兲.
The main groups are split into a number of subgroups. An example is the main
group Ceramics, which has five subgroups: Carbides, Nitrides, Oxides, Traditional Ce-
ramics, and Other Ceramics.
These subgroups lead to the specific material or material group, e.g., under Ceram-
ics, Oxides: Al2O3, BaTiO3, CaO, CeO2, Cr2O3, MgO, SiO, ZnO, ZrO2, and Other Oxides.
The twelve main groups 共alphabetic兲:
• Ceramics
• Coatings
• Composites and Reinforced Materials
• Electronic Components
• Ferrous Metals
• Mineralogical Materials
• Nonferrous Metals
• Organic Materials
• Polymers
• Powder Metals
• Sintered Carbides
11.2 How to Use Table 11.1

When a given material or material group should be found in the table, the main group
most likely will be evident such as Ceramics, Coatings, Ferrous Metals, Polymers, etc.
If in doubt, a look at the subgroups will often lead the way to the material or material
group. In the case of an alloy, the material should be found according to the component
with the highest content. Example: The superalloy: 48 % Ni, 25 % Co, 19 % Cr, 7.5 % Fe,
0.5 % Ti, is classified under the main group Nonferrous Metals, subgroup Nickel and
Nickel Alloys.
181
When the material 共material group兲 is found, two or more Methods with Method
Numbers are indicated in the same row. Now go to Section 13.2.3 and find the Material/
Preparation Tables with the same number. A number of purposes with corresponding
preparation methods are indicated here 共see Chapter 12兲, and the method correspond-
ing to the correct purpose is selected.
11.3 Table 11.1—Materials/Methods

TABLE 11.1—Materials/Methods.
Method
Material Group/Material (Alphabetical) (See Section 13.2.3/3.6)
Ceramics Bioceramics Hydroxyapatite Coating T-01, C-01
Bioceramics, Others T-05, C-05, T-06, C-06
Carbides B 4C T-02, C-02
CrC T-03, C-03
SiC T-02, C-02
TaC T-03, C-03
TiC T-03, C-03
WC T-03, C-03
Nitrides CBN T-03, C-03
Si3N4 T-04, C-04
TiN T-03, C-03
Other Ceramics T-03, C-03
Oxides Al2O3 T-05, C-05
BaTiO3 T-06, C-06
CaO T-06, C-06
CeO2 T-06, C-06
Cr2O3 T-05, C-05
MgO T-06, C-06
SiO T-06, C-06
UO2 T-68, C-68
ZnO T-06, C-06
ZrO2 T-06, C-06
Oxides, Others T-05, C-05, T-06, C-06
Borides T-06, C-06
Traditional Glasses, Optical Fibers T-07, C-07
Ceramics Porcelain T-06, C-06
Slag T-06, C-06
Tile T-06, C-06
Other Traditional Ceramics T-06, C-06
Coatings Electrolytically Anodized Coatings T-08, C-08
Deposited Galvanization—Plated Coatings T-09, C-09
Other Electrolytically Deposited T-09, C-09
Other Coatings CVD T-08, C-08
Diffusion Coatings T-09, C-09
Hot Dip Zn-Coating T-10, C-10
Other Zn-based Coatings T-10, C-10
PVD T-08, C-08
Chapter 11 Specimen Material 183
TABLE 11.1—(Continued.)
Method
Paint Layers T-11, C-11
Other Coatings T-09, C-09
Thermal Spray Flame T-12, C-12
Coatings HVOF (High Velocity Oxygen T-12, C-12
Fuel)
Plasma Spray Coatings— T-13, C-13
Metallic Layers
Plasma Spray Coatings— T-14, C-14
Ceramic Layers
Plasma Spray Coatings— T-15, C15
Composite Layers
Other Thermal Spray Coatings T-12, C-12
Composites SiC Fibers in Ti Matrix T-16, C-16
and Glassfiber Reinforced Plastic T-17, C-17
Reinforced Other Composite Materials T-18, C-18
Electronic Ceramic Capacitors T-19, C-19
Components Components Resistors T-19, C-19
Diodes T-19, C-19
YBCO Ceramic Super T-20, C-20
Conductors
Metallic Germanium, Silicon, Si Wafers T-21, C-21
Components Microelectronic Material C-22
(Semiconductor Device)
Resistors T-23, C-23
Solderballs T-24, C-24
Other Metal Components T-23, C-23
Polymer Capacitors, Other Electronic T-25, C-25
Components Components
Microelectronic Packages, T-24, C-24
Integrated
Circuits, Transistors T-26, C-26
PCB Coupon T-27, C-27
Other Microelectronic Devices T-26, C-26
Ferrous Carbon Steels High Carbon Steels T-28, C-28, E1-01
Metals Low Carbon Steels T-29, C-29, El-02
Medium Carbon Steels T-28, C-28, El-01
Cast Irons Gray Cast Iron, T-30, C-30, El-03
Lamellar
Cast Iron, T-30, C-30, El-03
Malleable
Cast Iron, T-31, C-31, El-03
Nodular
Cast Iron, White T-32, C-32, E1-03
Cast Iron, others T-28, C-28, El-03
Heat Treated Heat Treated, High-Alloy Steels T-33, C-33, El-04
Method
Steels Heat Treated, Low-Alloy Steels T-33, C-33, El-04
High-Alloy Stainless Steels T-34, C-34, El-05
Steels Super Alloys, Fe-Based T-35, C-35, El-06
Other High-Alloy Steels T-33, C-33, El-05
Low-Alloy High Strength Low-Alloy Steels T-36, C-36, El-04
Steels Other Low-Alloy Steels T-34, C-34, E1-04
Other Ferrous T-33, C-33, E1-02
Metals
Pure Iron T-34, C-34, El-07
Surface Treated Carbonitrided Steels T-37, C-37
Steels Carburized Steels T-37, C-37
Nitrided Steels T-37, C-37
Other Surface Treated Steels T-37, C-37
Tool Steels High Speed Steels T-38, C-38, El-08
Low-Alloyed Tool Steels T-38, C-38, El-09
Tool Steels, Others T-38, C-38, El-09
Mineralogical Constructed Portland Cement Clinker, T-39, C-39
Concrete
Materials Materials
Natural Minerals T-40, C-40
Ores T-40, C-40
Nonferrous Aluminum and Pure Aluminum T-41, C-41, El-10
Metals Al Alloys Cast Aluminum Alloys T-41, C-41
Wrought Aluminum Alloys T-43, C-43, El-10
Other Aluminum Alloys T-42, C-42, El-10
Americium See Material/
Preparation
Tables 68
Antimony and Pure Antimony T-44, C-44, El-10
Sb Alloys Antimony Bearing Alloys T–44, C-44, El-10
Other Sb Alloys T-44, C-44, El-10
Beryllium and T-45, C-45, El-10
Be Alloys
Bismuth and Bi T-44, C-44, El-10
Alloys
Cadmium See Material/
Preparation
Tables 68
Chromium and T-46, C-46, E1-11
Cr Alloys
Cobalt and Co Pure Cobalt, Cobalt Alloys T-47, C-47, El-12
Alloys Super Alloys, Cobalt-Based T-48, C-48, El-12
Copper and Cu Pure Copper T-50, C-50, El-13
Alloys Brass T-49, C-49, El-13
Bronze T-49, C-49, El-14
Method
Copper Bearings Alloys T-50, C-50, El-14
Other Copper Alloys T-49, C-49, E1-13
Germanium T-21, C-21
Gold and Au T-51, C-51
Alloys
Hafnium and T-62, C-62, El-11
Hf Alloys
Indium See Material/
Preparation
Tables 68
Iridium and Ir T-57, C-57
Alloys
Lead and Pb T-52, C-52, E1-15
Alloys
Magnesium T-53, C-53, E-16
and
Mg Alloys
Manganese and T-54, C-54, El-01
Mn Alloys
Mercury and See Material/
Amalgams Preparation
Tables 68
Molybdenum T-55, C-55, E1-01
and Mo Alloys
Neptunium See Material/
Preparation
Tables 68
Nickel, Ni T-56, C-56, El-17
Alloys and Ni-
Based Super
Alloys
Niobium and T-55, C-55
Nb Alloys
Osmium and T-57, C-57
Os Alloys
Palladium and T-57, C-57
Pd Alloys
Platinum and T-57, C-57
Pt Alloys
Plutonium See Material/
Preparation
Tables 68
Rare Earth See Material/
Metals Preparation
Tables 68
Rhenium and T-55, C-55
Method
Re Alloys
Rhodium and T-57, C-57
Rh Alloys
Ruthenium and T-57, C-57
Ru Alloys
Selenium See Material/
Preparation
Tables 68
Silicon T-21, C-21
Silver and Ag T-58, C-58, E1-18
Alloys
Tantalum and T-55, C-55
Ta Alloys
Tellurium See Material/
Preparation
Tables 68
Thallium See Material/
Preparation
Tables 68
Thorium See Material/
Preparation
Tables 68
Tin, Sn T-59, C-59, E1-19
Bearing
Alloys and
Other Sn
Alloys
Titanium and T-60, C-60, E1-20
Ti Alloys
Tungsten and T-55, C-55, E1-21
W Alloys
Uranium and T-68, C-68
Uranium
Dioxide
Vanadium and T-55, C-55, E1-22
V Alloys
Zinc and Zn T-61, C-61, E1-23
Alloys
Zirconium and T-62, C-62, E1-24
Zr Alloys
Zircalloy
Organic Biological T-63, C-63
Materials Materials
Bone
Teeth
Tissue
Method
Carbon, Coal, T-63, C-63
Graphite
Paper, T-63, C-63
Wood
Other Organic T-63, C-63
Materials
Polymers Elastomers Elastomers, Others T-64, C-64
EPDM Polymers T-64, C-64
Silicone T-64, C-64
Thermoplastics Acrylic (CS) T-64, C-64
Acrylonitril Butadicne Styrene T-65, C-65
(ABS)
Polyamid (PA) T-64, C-64
Polycarbonate (PC) T-65, C-65
Polyester, Saturated T-65, C-65
Polyethylene (PE) T-64, C-64
Polymethylmethacrylate T-65, C-65
(PMMA)
Polyoxymethylene (POM) T-65, C-65
Polypropylene (PP) T-64, C-64
Polystyrene (PS) T-64, C-64
Polyvinylchloride (PVC) T-64, C-64
Thermoplastics, Others T-64, C-64
Thermosetting Epoxy T-65, C-65
Plastics Phenolic Resins (PF) T-65, C-65
Polyester, Unsaturated T-65, C-65
Polyurethane (PUR) T-65, C-65
Other Thermosetting Plastics T-65, C-65
Powder Ferrous Powder
Metals Metals
Nonferrous T-66, C-66
Powder Metals
Sintered Cemented T-67, C-67, E1-25
Carbides Carbides,
(Cemented (Hard metals),
Carbides) Coated
Sintered
Carbides and
Other Sintered
Carbides
12
Purpose of Examination
12.1 Purpose in General
FOR A GIVEN MATERIAL SEVERAL PREPARATION METHODS WILL USU-
ally be available, however, the correct method should be chosen based on the purpose
of examination. For this reason, a number of relevant purposes are stated with each
material/method in the Material/Preparation Tables, 共see Section 13.2.3兲.
Table 12.1 shows a number of the most common “purposes of examination.” It is
expressed in the following text and in the table as “purpose.” Most of these purposes are
covered by one or more ASTM standards and, in this case, the standard共s兲 is indicated.
For a given material also microetching is performed in accordance with the pur-
pose of the examination, and therefore also chemical microetching with a list of
etchants 共Table 12.2兲 is stated in this chapter.
12.2 Purpose: ASTM Standards

A preparation is made very often to be able to make an examination according to an
ASTM standard. Section 12.4 lists all ASTM standards commonly used in metallogra-
phy and materialography and a Document Summary of each standard is indicated in a
CD-ROM included with this manual.
Other relevant standards 共ISO, BSI, DIN, etc.兲 are stated in Appendixes I and II. In
Table 12.1, the ASTM standards are shown relating to purpose.
12.3 Table 12.1: Purpose/ASTM Standards

Table 12.1indicates a number of common purposes of examination with the most im-
portant ASTM standards, if any. Not all applicable standards are listed in this table,
only some of the more pertinent ones.
As part of each Material/Preparation Tables 共Section 13.2.3兲, a similar table will be
stated, but only the purposes and the ASTM standards, relevant for the material de-
scribed in the Material/Preparation Tables, will be indicated.
12.4 ASTM Standards—Metallography
12.4.1 Introduction
The metallographic field is covered by ASTM with a number of documents of the fol-
lowing types:
Guide—a compendium of information or series of options that doesn’t recom-
mend a specific course of action.
Practice—a definitive set of instructions for performing one or more specific op-
erations or functions that does not produce a test result.
188
Chapter 12 Purpose of Examination 189
TABLE 12.1—Purpose/ASTM Standards.

Purpose (alphabetic): ASTM Standard (See Section 12.4)
Case or coating thickness/hardness B 487, B 578, B 748, B 931, B 933, B 934, C 664,
Surface layers E 1077
Perfect edge retention
Graphite in cast iron A 247
Grain size, grain boundaries B 390, E 112, E 930, E 1181, E 1382
Heat-influenced zone E 1077
Heat treatment
Image analysis, rating of inclusion content E 45, E 562, E 768, E 1077, E 1181,
High planeness E 1245, E 1268, E 1382, E 2109
Inclusions in steel B 796, E 45, E 768, E 1245
Microhardness, hardness B 578, C 730, C 849, C 1326, C 1327, E 10,
E 18, E 92, E 103, E 110, E 140, E 384, E 448
Microstructure A 247, A 892, B 657, B 665, E 3, E 45, E 112, E
407, E 562, E 768, E 883, E 930, E 1077, E 1122, E
1181, E 1245, E 1268, E 1351, E 1382, E 1558, E
1920, E 2015, E 2109, E 2283
Phase identification A 247, B 657
Porosity B 276, E 2109, F 1854
Structure changes (forging)
Thermal sprayed coatings: Distribution, porosity, E 1920, E 2109
unmelted particles
Specification—an explicit set of requirements to be satisfied by a material, prod-

uct, system, or service.
Terminology—a document comprising definitions of terms—explanation of sym-
bols, abbreviations, or acronyms.
Test Method—a definitive procedure that produces a test result.
Most of the standards covering metallography and materialography are published
in the Annual Book of ASTM Standards, Volume 03.01, Metals—Mechanical Testing;
Elevated and Low-Temperature Tests; Metallography 共ASTM Stock Number:
S030100兲.
The standards covering metallography, including Microindentation Hardness
Testing, are under the jurisdiction of ASTM Committee E4. Those covering other types
of hardness testing are under ASTM Committee E28.
Designation
Each standard has a serial designation prefixed to the following title, the number fol-
lowing the dash indicates the year of original adoption as a standard or, in the case of
revision, the year of the last revision. Thus, standards adopted or revised during the
year 2003 have as their final number, 03. A letter following this number indicates more
than one revision during that year, that is, 03a indicates the second revision in 2003,
03b, the third revision, etc. Standards that have been reapproved without change are
indicated by the year of last reapproval in parentheses as part of the designation num-
ber, for example, 共2003兲. A superscript epsilon indicates an editorial change since the
last revision or reapproval-␧1 for the first change, ␧2 for the second change, etc.
In this manual, only the serial designations are indicated because the following
numbers are continuously changed.
12.4.2 ASTM Standards in this Book

All ASTM standards mentioned under METALLOGRAPHY in Volume 03.01 and oth-
ers, relating to the subjects covered by this book, are listed below. Most of these will be
stated as DOCUMENT SUMMARY in Section 12.4.3. The listed standards should not
be considered as a complete list of standards covering the subject of metallography/
materialography and related subjects. Also, a few specifications covering materials are
shown as examples.
The standards listed are based on the situation as per October 2006, and this situa-
tion will change due to the development of new standards and the revision or deletion
of old standards.
ASTM Standards Listed by Subject „Alphabetically…
Coatings
Test Methods for:
B 487 Measurement of Metal and Oxide Coating Thickness by Microscopical Ex-
amination of a Cross Section
B 578 Microhardness of Electroplated Coatings
B 588 Measurement of Thickness of Transparent or Opaque Coatings by Double-
Beam Interference Microscope Technique
B 748 Measurement of the Thickness of Metallic Coatings by Measurement of
Cross Section with a Scanning Electron Microscope
C 664 Thickness of Diffusion Coating
Criteria for Metallographic Laboratory Evaluation, Safety, and

Management
Guide for:
E 1578 Laboratory Information Management Systems 共LIMS兲
E 2014 Metallographic Laboratory Safety
Grain Size
Test Methods for:
E 1181 Characterizing Duplex Grain Sizes
E 112 Determining Average Grain Size
E 930 Estimating the Largest Grain Observed in a Metallographic Section 共ALA
Grain Size兲
Practice for:
B 390 Evaluating Apparent Grain Size and Distribution of Cemented Tungsten
Carbides
Guides for:
E 1951 Calibrating Reticles and Light Microscope Magnifications
Inclusions
Test Methods for:
B 795 Determining the Percentage of Alloyed or Unalloyed Iron Contamination
Present in Powder Forges 共P/F兲 Steel Parts
B 796 Nonmetallic Inclusion Content of Powders Intended for Powder Forging

共P/F兲 Applications
E 45 Determining the Inclusion Content of Steel
Indentation Hardness Testing

Specifications for:
E 140 Hardness Conversion Tables for Metals. Relationship Among Brinell Hard-
ness, Vickers Hardness, Rockwell Hardness, Superficial Hardness, Knoop Hardness,
and Scleroscope Hardness. Please refer to ASTM E 140 in the CD-ROM included with
this manual.
Test Methods for:
C 730 Knoop Indentation Hardness of Glass
C 849 Knoop Indentation Hardness of Ceramic Whitewares
C 1326 Knoop Indentation Hardness of Advanced Ceramics
C 1327 Vickers Indentation Hardness of Advanced Ceramics
D 785 Rockwell Hardness of Plastics and Electrical Insulating Materials
D 1415 Rubber Property-International Hardness
D 2240 Rubber Property-Durometer Hardness
E 10 Brinell Hardness of Metallic Materials
E 110 Indentation Hardness of Metallic Materials by Portable Hardness Testers
E 103 Rapid Indentation Hardness Testing of Metallic Materials
E 18 Rockwell Hardness and Rockwell Superficial Hardness of Metallic Materials
E 92 Vickers Hardness of Metallic Materials
Practice for:
E 448 Scleroscope Hardness Testing of Metallic Materials
Microindentation Hardness Testing

Test Methods for:
B 578 Microhardness of Electroplated Coatings
B 931 Metallographically Estimating the Observed Case Depth of Ferrons Powder
Metallurgy 共P/M兲 Parts
B 933 Microindentation Hardness of Poweder Metallurgy 共P/M兲 Materials
B 934 Effective Case Depth of Ferrous Poweder Metallurgy 共P/M兲 Parts Using Mi-
croindentation Hardness Measurements
E 384 Microindentation Hardness of Materials
Practice for:
WK 382 Instrumented Indentation Testing
Porosity
Test Method for:
B 276 Apparent Porosity in Cemented Carbides
See also under Quantitative Metallography
Quantitative Metallography
Test Methods for:
D 629 Quantitative Analysis of Textiles
D 1030 Fiber Analysis of Paper and Paperboard
D 2798 Microscopical Determination of the Reflectance of Vitrinite in a Polished

Specimen of Coal
E 562 Determining Volume Fraction by Systematic Manual Point Count
E 1382 Determining the Average Grain Size Using Semiautomatic and Automatic
Image Analysis
E 1077 Estimating the Depth of Decarburization of Steel Specimens
E 2109 Determining Area Percentage Porosity in Thermal Sprayed Coatings
F 1854 Stereological Evaluation of Porous Coatings on Medical Implants
Practices for:
C-856 Petrographic Examination of Hardened Concrete
E 1268 Assessing the Degree of Banding or Orientation of Microstructures
E 1245 Determining the Inclusion or Second-Phase Constituent Content of Metals
by Automatic Image Analysis
E 2283 Extreme Value Analysis of Nonmetallic Inclusions in Steel and Other Mi-
crostructural Features
Sampling, Specimen Preparation and Photography

Test Methods for:
A 247 Evaluating the Microstructure of Graphite in Iron Castings
B 328 Density, Oil Content, and Interconnected Porosity of Sintered Metal Struc-
tural Parts and Oil-Impregnated Bearings
B 657 Metallographic Determination of Microstructure in Cemented Tungsten
Carbides
E 381 Macroetch Testing Steel Bars, Billets, Blooms, and Forgings
E 340 Macroetching Metals and Alloys
E 3 Preparation of Metallographic Specimens
Practices for:
B 665 Metallographic Sample Preparation of Cemented Tungsten Carbides
E 122 Calculating Sample Size to Estimate, with a Specified Tolerable Error, the
Average for Characteristic of a Lot or Process
E 178 Dealing with Outlying Observations
E 407 Microtching Metals and Alloys
E 1180 Preparing Sulfur Prints for Macrostructural Examination
E 768 Preparing and Evaluating Specimens for Automatic Inclusion Assessment
of Steel
E 1351 Production and Evaluation of Field Metallographic Replicas
Guides for:
A 892 Defining and Rating the Microstructure of High Carbon Bearing Steels
E 1558 Electrolytic Polishing of Metallographic Specimens
E 1920 Metallographic Preparation of Thermal Sprayed Coatings
E 2015 Preparation of Plastics and Polymeric Specimens for Microstructural Ex-
amination
E 883 Reflected-Light Photomicrography
Terminology
Terminology for:
E 7 Metallography
X-Ray and Electron Metallography „This subject is not included in this

Book.…
Test Methods for:
E 82 Determining the Orientation of a Metal Crystal
E 2142 Rating and Classifying Inclusions in Steel Using the Scanning Electron Mi-
croscope
Practices for:
E 766 Calibrating the Magnification of a Scanning Electron Microscope
E 963 Electrolytic Extraction of Phases from Ni and Ni-Fe Base Superalloys Using
a Hydrochloric-Methanol Electrolyte
E 81 Preparing Quantitative Pole Figures
E 986 Scanning Electron Microscope Beam Size Characterization Performance
Characterization
E 975 X-Ray Determination of Retained Austenite in Steel with Near Random
Crystallographic Orientation
Guides for:
E 1508 Quantitative Analysis by Energy-Dispersive Spectroscopy
ASTM Specifications—Examples
Standard Specification for:
A 1 Carbon Steel Tee Rails
A 3 Steel Joint Bars, Low, Medium, and High Carbon 共Non-Heat-Treated兲
A 36 Carbon Structural Steel
A 47 Ferritic Malleable Iron Castings
A 48 Gray Iron Castings
A 126 Gray Iron Castings for Valves, Flanges, and Pipe Fittings
A 159 Automotive Gray Iron Castings
A 197 Cupola Malleable Iron
A 220 Pearlitic Malleable Iron
A 242 High-Strength Low-Alloy Structural Steel
A 338 Malleable Iron Flanges, Pipe Fittings, and Valve Parts for Railroad, Marine,
and Other Heavy Duty Service at Temperatures Up to 650° F 共345° C兲
A 377 Ductile-Iron Pressure Pipe
A 439 Austenitic Ductile Iron Castings
A 532 Abrasion-Resistant Cast Irons
A 536 Ductile Iron Castings
A 572 High-Strength Low-Alloy Colombium-Vanadium Structural Steel
A 602 Automotive Malleable Iron Castings
A 656 Hot-Rolled Structural Steel, High-Strength Low-Alloy Plate with Improved
Formability
12.4.3 ASTM Standards—Document Summaries

For Document Summaries on the above mentioned standards please refer to the CD-
ROM included with this manual.
12.5 Chemical Microetching—Table 12.2—Table 12.3

The prepared specimen surface typically must be etched to reveal the microstructure
depending on the purpose of examination. Mostly this is done with chemical solutions,
etchants, developed for a specific material and often for a specific purpose.
In ASTM Practice for Microetching Metals and Alloys 共E 407兲共see Section 12.4.3兲 a
large number of etchants for metals are stated with the purposes 共uses兲. Based on Table
1 of the newest version of this practice 共ASTM E 407–99兲 and other sources, Refs. 2, 4,
and 9, Part I, etchants are stated according to their purpose on each Material/
Preparation Tables, Section 13.2.3. The etchant is identified with a number. This num-
ber is taken to Table 12.2, which states the composition and procedure for the etching
process. Table 12.2 is based on Table 2 of ASTM E 407–99 covering metals 共etchants
1–226兲 with additions 共etchants 901–950兲, mainly covering ceramics and plastics,
taken from Petzow, Ref. 2, 共Part I兲, ASM Handbook, Vol. 9, Ref. 4, 共Part I兲, and Vander
Voort, Ref. 9, 共Part I兲.
Attention: The ASTM Practice E 407 mentioned above is updated at different time
intervals and the reader should consult with the latest published version of the stan-
dard which can be found in Annual Book of Standards, Volume 03.01 共see Section
12.4.1兲.
For etchants not mentioned in this book, see references in Section 9.1, and Litera-
ture, Chapter 27.
Etchant Names: Some etchants have special names, like “Beraha.” These names
are stated in Table 12.3, indicating the etchant number so that the composition can be
found in Table 12.2. Table 12.3 is based on Table 3 of ASTM E 407.
Theory of Microetching: For chemical etching theory, different types of etching
and literature on etching see Chapter 9.
12.5.1 Etching Practice

Chemical etching is a straightforward, reasonably simple process. In most cases a rela-
tive small quantity of the etchant is placed in a shallow beaker, and the carefully
cleaned and dried specimen is immersed into the reagent. The specimen should always
be held with a pair of tongs, and preferably with the surface turning upwards to be able
to see the progress of the process. The specimen is moved gently to remove reaction
products on the surface. In some cases a swabbing with a saturated piece of cotton can
be recommended, but the cotton might scratch the surface and care should be taken
that the cotton is regularly recharged with reagent.
Safety Precautions: See Sections 9.3.4 and 26.2 and ASTM Guide for Metallo-
graphic Laboratory Safety 共E 2014兲. Please refer to E 2014 in the CD-ROM included
with this manual.
12.5.2 Table 12.2—Numerical List of Etchants
TABLE 12.2—Numerical list of etchants. (This table contains etchants mentioned in the Material/
Preparation Tables and other etchants, seeASTM E 407.)
Etchant Composition Procedure
1 1 mL HF (a) Swab with cotton for 15 s.
200 mL water (b) Alternately immerse and polish several
minutes.
(c) Immerse 3 – 5 s.
(d) Immerse 10– 120 s.
2 3 mL HF (a) Swab 10 s to reveal general structure.
100 mL water (b) Immerse 15 min, wash 10 min in water to form
film with hatching
which varies with grain orientation.
3 2 mL HF (a) Immerse 10– 20 s. Wash in stream of warm
3 mL HCl water. Reveals general structure.
5 mL HNO3 (b) Dilute with 4 parts water-colors constituents—
190 mL water mix fresh.
4 24 mL H3PO4 Electrolytic: Use carbon cathode raising d-c
50 mL Carbitol (diethylene glycol voltage from 0 – 30 V in 30 s. Total
monoethyl ether) etching time 3 min with agitation. Wash and cool.
4 g boric acid Repeat if necessary.
2 g oxalic acid
10 mL HF
32 mL water
5 5 g HBF4 Electrolytic: Use Al, Pb, or stainless steel cathode.
200 mL water Anodize 1 – 3 min,
20– 45 V d-c. At
30 V, etch for 1 min.
6 25 mL HNO3 Immerse 40 s at 70° C 共160° F兲. Rinse in cold
75 mL water water.
7 10– 20 mL H2SO4 Immerse 30 s at 70° C 共160° F兲. Rinse in cold
80 mL water water.
8 10 mL H3PO4 (a) Immerse 1 – 3 min at 50° C 共120° F兲.
90 mL water (b) Electrolytic at 1 – 8 V for 5 – 10 s.
9 3–4 9 sulfamic acid Use just prior to the last polishing operation.
5 drops HF It is not intended as a final etchant.
100 mL water The specimen is examined as polished even under
polarized light.
10 10 mL HF Immerse 10– 30 s.
90 mL methanol (90 %)
11 2 mL HF Immerse or swab few seconds to a minute.
100 mL water
12 20 mL HNO3 Use hood. Do not store. Immerse or swab 5 – 60 s.
60 mL HCl
13 10 g oxalic acid Electrolytic at 6 V:
100 mL water (a) 10– 15 s.
(b) 1 min.
(c) 2 – 3 s.
Use stainless steel cathode and platinum or
Nichrome connection to specimen.
Preparation Tables and other etchants, seeASTM E 407.)(Continued.)
14 10 mL HNO3 Immerse few seconds to a minute.
15 15 mL HNO3 Age before use. Immerse 5 – 30 s. May be used
15 mL acetic acid electrolytically.
60 mL HCl
15 mL water
16 5 – 10 mL HCl Electrolytic at 3 V for 2 – 10 s.
100 mL water
17 5 mL HCl Electrolytic at 6 V for few seconds.
10 g FeCl3
100 mL water
18 2 – 10 g CrO3 Electrolytic at 3 V for 2 – 10 s.
100 mL water
19 A Immerse in freshly mixed Solutions A + B (1:1) for
8 g NaOH 5 – 10 s.
100 mL water If surface activation is necessary, first use Etch
B #18, then rinse in water.
Saturated aqueous solution of KMnO4 While still wet, immerse in Solutions A + B (1:1).
Mixture of solutions A + B has 15 min useful life.
20 5 mL H2O2 (30 %) Use hood. Mix fresh. Immerse polished face up for
100 mL HCl few seconds.
21 1 g CrO3 Use hood. To mix, add the HCl to CrO3.
140 mL HCl Electrolytic at 3 V for 2 – 10 s.
22 100 mL HCl Use hood. Do not store.
0.5 mL H2O2 (30 %) (a) Immerse or swab 1 / 2 – 3 min. Add H2O2
dropwise to maintain action.
(b) Electrolytic, 4 V, 3 – 5 s.
23 5 mL HCl Electrolytic at 6 V for 10– 20 s.
95 mL ethanol (95 %) or methanol
(95 %)
24 5 mL HNO3 Use hood. Immerse few seconds.
200 mL HCl
65 g FeCl3
25 10 g CuSO4 Immerse or swab 5 – 60 s. Made more active by
50 mL HCl adding few drops of H2SO4 just before use.
50 mL water
26 5 g FeCl3 Swab 16– 60 s. Activity may be decreased by
10 mL HCl substituting glycerol for water.
50 mL glycerol
30 mL water
27 1 g KOH Dissolve KOH in water, then slowly add NH4OH
20 mL H2O2 (3 %) to solution. Add 3 % H2O2 last. Use
50 mL NH4OH fresh—immerse few seconds to a minute.
30 mL water
28 1 g FeNO3 Swab or immerse few seconds to a minute.
100 mL water
29 1 g K2Cr2O7 Add 2 drops of HCl just before using. Swab few
4 mL H2SO4 seconds to a minute.
50 mL water
30 25 mL NH4OH Mix NH4OH and water before adding H2O2. Must
25 mL water be used fresh. Swab 5 – 45 s.
50 mL H2O2 (3 %)
31 10 g ammonium persulfate (a) Swab or immerse to 5 s.
100 mL water (b) Immerse to 2 min to darken matrix to reveal
carbides and phosphides.
(c) Electrolytic at 6 V for few seconds to a minute.
(d) Immerse 3 – 60 s. Can be heated to increase
activity.
32 60 g CrO3 Saturated solution.
100 mL water Immerse or swab 5 – 30 s.
33 10 g CrO3 Add HCl just before use. Immerse 3 – 30 s. Phases
2–4 drops HCl can be colored by Nos. 35, 36, 37.
100 mL water
34 5 g FeCl3 (a) Immerse or swab few seconds to few minutes.
50 mL HCl Small additions of HNO3
100 mL water activate solution and minimize pitting.
(b) Immerse or swab few seconds at a time. Repeat
as necessary.
35 20 g FeCl3 Immerse or swab few seconds at a time until
5 mL HCl desired results are obtained.
1 g CrO3
100 mL water
100 mL water
10 mL HCl desired results are obtained
100 mL water
38 8 g FeCl3 Swab 5 – 30 s.
25 mL HCl
100 mL water
1 g CuCl2
0.1 g SnCl2
100 mL water
40 5 gFeCl3 16 ML HCl 60 mL Immerse or swab few seconds to few minutes.
ethanol (95 %) or methanol
(95 %)
41 2 g K2Cr2O7 Add the HCl just before using. Immerse 3 – 60 s.
8 mL H2SO4
4 drops HCl
100 mL water
42 10 g cupric ammonium chloride Add NH4OH to solution until neutral or slightly
100 mL water alkaline. Immerse 5 – 60 s.
NH4OH
43 20 mL NH4OH Immerse 5 – 30 s.
1 g ammonium persulfate
44 50 mL NH4OH Use fresh. Peroxide content varies directly with
20– 50 mL H2O2 (3 %) copper content of alloy to be etched.
0 – 50 mL water Immerse or swab to 1 min. Film on etched
aluminum bronze removed by No. 82.
45 1 g CrO3 Electrolytic at 6 V for 3 – 6 s. Use aluminum
100 mL water cathode.
46 15 mL NH4OH When mixing, add NaOH pellets last.
15 mL H2O2 (3 %) For best results use before pellets have dissolved.
15 mL water
4 pellets NaOH
47 5 g NaCN or KCN Use hood—Can give off extremely poisonous
5 g 共NH4兲2S2O2 hydrogen cyanide.
100 mL water Precaution—Also poisonous by ingestion as well
as contact.
48 10 g NaCN Use hood—Can give off extremely poisonous
100 mL water hydrogen cyanide.
Precaution—Also poisonous by ingestion as well
as contact. Electrolytic at 6 V:
(a) 5 s for sigma.
(b) 30 s for ferrite and general structure.
(c) to 5 min for carbides.
49 3 g FeSO4 Electrolytic at 8 – 10 V 共0.1 A兲 for 5 – 15 s.
0.4 g NaOH
10 mL H2SO4
190 mL water
50 5 mL acetic acid Use hood. Do not store. Electrolytic at 1.5 V for
10 mL HNO3 20 to 60 s. Use platinum wires.
85 mL water
51 2 g FeCl3 Immerse few minutes.
5 mL HCl
30 mL water
60 mL ethanol or methanol
52 1 g sodium dichromate Swab few seconds.
1 g NaCl
4 mL H2SO4
250 mL water
53 1 – 5 mL NH4OH Immerse 5 – 60 s.
100 mL water
54 1 g ammonium acetate Electrolytic at 0.3 A / cm2 for 5 – 30 s.
3 g sodium thiosulfate
7 mL NH4OH
1300 mL water
55 1 mL H2SO4 Swab gently 10– 15 s. Rinse with methanol and
15 mL HNO3 blow dry. Helps to chemically polish.
10 mL acetic acid If final etch is too even mild, follow with No. 98.
5 mL H3PO4
20 mL lactic acid
56 30 mL HNO3 Swab gently 5 – 15 s. Rinse with ethanol or
10 mL H3PO4 methanol and blow dry.
20 mL acetic acid
10 mL lactic acid
57 75 mL acetic acid Immerse 6 – 15 s.
25 mL H2O2 (30 %)
58 25 mL HF Swab 3 – 20 s.
25 mL HNO3
5 mL water
59 2 g AgNO3 Mix AgNO3 and water, then add HF and HNO3.
40 mL water Swab 1 / 2 – 2 min.
40 mL HF
20 mL HNO3
60 25 mL HNO3 Use hood. Let stand 1 / 2 h before using. Swab
15 mL acetic acid 3 – 20 s.
15 mL HF
5–7 drops bromine
61 60 mL HCl Use hood. Immerse few seconds to a minute.
40 mL HNO3
62 1 – 5 g CrO3 Vary composition of reagent and aging of reagent
100 mL HCl after mixing to suit alloy.
Swab or immerse few seconds to a minute.
63 0.1 g CrO3 Swab few seconds to a minute.
10 mL HNO3
100 mL HCl
64 5 mL HNO3 (a) Immerse 1 – 5 min.
25 mL HCl (b) Use hot. Will form chloride film on gold alloys
30 mL water if much silver is present.
Ammonia will remove film.
65 A Use hood—Can give off extremely poisonous
10 g ammonium persulfate hydrogen cyanide.
100 mL water Precaution—Also poisonous by ingestion as well
B as contact. Mix 1 + 1 mixture of Solutions A and B
10 g KCN just before use. (A mixture of 5 drops of each will
100 mL water cover the surface of a 1 in. dia. mount.)
Immerse 1 / 2 – 2 min.
66 30 mL HF Swab 3 – 10 s or immerse to 2 min.
15 mL HNO3
30 mL HCl
67 10 mL perchloric acid Precaution—Keep cool when mixing and use.
10 mL 2-butoxyethanol Electrolytic at 30– 65 V for 10– 60 s.
70 mL ethanol (95 %)
10 mL water
35 mL 2-butoxyethanol Electrolytic at 60– 150 V for 5 – 30 s.
60 mL methanol (absolute)
80 mL acetic acid Electrolytic at 20– 60 V for 1 – 5 min.
70 5 mL HF Swab for 5 – 60 s.
2 mL AgNO3 (5 %)
200 mL water
71 5 mL HF Add 5–10 drops of this solution on the final
95 mL water polishing wheel which has been charged
with the polishing solution. The specimen is
polished on this wheel until the surface
turns black. Distilled water is then slowly added to
the wheel and polishing continued
until the surface is bright. At this time the
specimen should be ready for examination
via polarized light.
Note—Use inert substance between cloth and
wheel to prevent attack of the wheel.
Wear gloves.
72 10 mL HF Swab for 5 – 20 s.
45 mL HNO3
45 mL water
73 20 mL HCl Electrolytic etch—use carbon cathode and
25 g NaCl platinum wire connection to specimen.
65 mL water (a) 6 V ac for 1 min.
(b) 5 V – 20 V ac for 1 – 2 min.
(c) 20 V ac for 1 – 2 min.
For etch-polishing, use shorter times. After etching,
water rinse, alcohol rinse, and dry.
74 1 – 5 mL HNO3 Etching rate is increased, sensitivity decreased with
100 mL ethanol (95 %) or methanol increased percentage of HNO3.
(95 %) (a) Immerse few seconds to a minute.
(b) Immerse 5 – 40 s in 5 % HNO3 solution. To
remove stain, immerse 25 s in 10 %
HCl-methanol solution.
(c) For Inconels and Nimonics, use 5 mL HNO3
solution—electrolytic at 5 – 10 V for 5–
20 s.
(d) Swab or immerse several minutes.
(e) Swab 5 – 60 s. HNO3 may be increased to
30 mL in methanol only depending on
alloy. (Ethanol is unstable with over 5 % HNO3).
Do not store.
75 5 g picric acid Immerse 1 – 2 s at a time and immediately rinse
8 g CuCl2 with methanol. Repeat as often as
20 mL HCl necessary. (Long immersion times will result in
200 mL ethanol (95 %) or methanol copper deposition on surface.)
(95 %)
76 4 g picric acid Composition given will saturate with picric acid.
100 mL ethanol (95 %) or methanol Immerse few seconds to a minute or
(95 %) more. Adding a wetting agent such as zepherin
chloride will increase response.
77 10 g picric acid Composition given will saturate the solution with
5 drops HCl picric acid. Immerse few seconds to
100 mL ethanol (95 %) or methanol a minute or more.
(95 %)
78 10 g potassium metabisulfite Immerse 1 – 15 s. Better results are sometimes
100 mL water obtained by first etching lightly with
No. 76 or 74.
79 40 mL HCl Swab few seconds to a minute.
5 g CuCl2
30 mL water
(95 %)
80 5 mL HCl Immerse or swab few seconds to 15 min. Reaction
1 g picric acid may be accelerated by adding a
100 mL ethanol (95 %) or methanol few drops of 3 % H2O2. Optional (for prior
(95 %) austenite grain boundaries)—temper
specimen at 600– 900° F prior to preparation.
81 2 g picric acid Composition given will saturate the should with
1 g sodium tridecylbenzene sulfonate picric acid.
100 mL water (a) Immerse few seconds to a minute.
(b) Immerse to 15 min with occasional swabbing
for heavy grain boundary attack.
82 5 g FeCl3 Immerse 5 – 10 s.
5 drops HCl
100 mL water
83 10 g CrO3 (a) Electrolytic at 6 V for 5 – 60 s. Attacks
100 mL water carbides.
(b) Electrolytic at 6 V for 3 – 5 s.
84 10 mL H2SO4 Precaution—Add H2SO4 slowly to water and cool,
10 mL HNO3 then add HNO3. Immerse 30 s.
80 mL water Swab in running water. Repeat three times and
repolish lightly.
85 2 g picric acid Immerse in boiling solution for 5 min. Precaution—
25 g NaOH Do not boil dry—anhydrous picric
100 mL water acid is unstable and highly explosive. Alternative:
Electrolytic at 6 V for 40 s (room
temperature). Use stainless steel cathode.
86 3 g oxalic acid Solution should be freshly prepared. Immerse
4 mL H2O2 (30 %) 15– 25 min when specimens or parts
100 mL water cannot be given usual metallographic polish.
Multiple etching may be required.
87 10 mL HNO3 Use hood—Can give off nitrogen dioxide gas.
20– 50 mL HCl Precaution—Mix HCl and glycerol
30 mL glycerol thoroughly before adding HNO3. Do not store.
Discard before solution attains a dark
orange color. Immerse or swab few seconds to few
minutes. Higher percentage of
HCl minimizes pitting. A hot water rinse just prior
to etching may be used to activate
the reaction. Sometimes a few passes on the final
polishing wheel is also necessary
to remove a passive surface.
88 10 mL HNO3 Use hood—Can give off nitrogen dioxide gas.
20 mL HCl Precaution—Discard before solution
30 mL water attains a dark orange color. Immerse few seconds
to a minute. Much stronger reaction
than No. 87.
89 10 mL HNO3 Use hood. Do not store. Immerse or swab few
10 mL acetic acid seconds to few minutes.
15 mL HCl
2–5 drops glycerol
90 10 mL HNO3 Immerse 2 – 10 s.
20 mL HF
20– 40 mL glycerol
91 5 mL HNO3 This etchant is equivalent to a 1 + 1 mixture of No.
5 mL HCl 80 and No. 74 (5 % HNO3). Swab
1 g picric acid for 30 s or longer.
(95 %)
92 10 mL HCl Immerse 5 – 30 min or electrolytic at 6 V for
100 mL ethanol (95 %) or methanol 3 – 5 s.
(95 %)
93 concentrated HNO3 Use hood. Electrolytic at 0.2 A / cm2 for few
seconds.
94 2 g CuCl2 Submerged swabbing for few seconds to several
40 mL HCl minutes. Attacks ferrite more readily
40– 80 mL ethanol (95 %) or methanol than austenite.
(95 %)
95 2 g CuCl2 Immerse or swab few seconds to few minutes.
40 mL HCl
40– 80 mL ethanol (95 %) or methanol
(95 %)
40 mL water
96 85 g NaOH Electrolytic at 6 V for 5 – 10 s.
50 mL water
97 45 g KOH Composition of solution is approximately 10 N.
60 mL water Electrolytic at 2.5 V for few seconds.
Stains sigma and chi yellow to red brown, ferrite
gray to blue gray, carbides barely
touched, austenite not touched.
98 10 g Fe共CN兲4 Use hood—Can give off extremely poisonous
10 g KOH or NaOH hydrogen cyanide. Precaution—Also
100 mL water poisonous by ingestion as well as contact. Use
fresh.
(a) Immerse or swab 15– 60 s. Stains carbides and
sigma. (To differentiate, No. 31
electrolytic at 4 V will attack sigma, but not
carbides. If pitting occurs, reduce voltage.)
(b) Immerse in fresh, hot solution 2 – 20 min.
Stains carbides dark, ferrite yellow,
sigma blue. Austenite turns brown on overetching.
(c) Swab 5 – 60 s. (Immersion will produce a stain
etch.)
Follow with water rinse, alcohol rinse, dry.
99 25 mL HCl Mix fresh. (For stock solution, mix first three items.
3 g ammonium bifluoride Add potassium metabisulfite just
125 mL water before use.) Immerse few seconds to a few
few grains potassium metabisulfite minutes.
100 10 g FeCl3 Immerse few seconds.
90 mL water
101 2 g CrO3 Immerse 5 – 60 s. (CrO3 may be increased up to
20 mL HCl 20 g for difficult alloys. Staining and
80 mL water pitting increase as CrO3 increased.)
102 concentrated NH4OH Use hood. Electrolytic at 6 V for 30– 60 s. Attacks
carbides only.
103 20 mL HNO3 Immerse 10– 60 s.
4 mL HCl
104 5 mL HNO3 Immerse 10 min or longer.
45 mL HCl
50 mL water
105 5 mL H2SO4 Use hood. Precaution—add H2SO4 slowly to HCl
3 mL HNO3 with stirring, cool; then add HNO3.
90 mL HCl Discard when dark orange color. Swab 10– 30 s.
106 7 mL HNO3 Use fresh to avoid pitting. Immerse or swab
25 mL HCl 10– 60 s.
107 10 mL H3PO4 Use hood. Precaution—Mix H3PO4 and HNO3
50 mL H2SO4 thoroughly, then add H2SO4 slowly
40 mL HNO3 with stirring. Use fresh, but allow to cool.
Electrolytic at 6 V for few seconds. Brown
discoloration will form at edges of specimen. To
slow reaction, add water (to 100 mL)
very carefully with stirring. Attacks bakelite
mounts.
108 3 – 10 mL H2SO4 Electyrolytic at 6 V for 5 – 10 s. Tends to pit with
100 mL water longer times.
109 50 mL HCl Make fresh but allow to stand 30 min to avoid
25 mL HNO3 plating out copper. Immerse few
1 g CuCl2 seconds to a few minutes.
150 mL water
110 10 mL HCl Immerse to several minutes until deeply etched.
5 mL HNO3 Follow with light repolish.
(95 %)
111 5 mL H2SO4 Electrolytic at 10 V 共0.2 A / cm2兲 for 5 – 30 s.
8 g CrO3 Reveals Ti- and Cb-rich areas at a faster
85 mL H3PO4 rate than grain boundaries.
112 60 mL acetic acid Immerse 8 – 15 s.
30 mL H2O2 (30 %)
113 15 mL acetic acid Do not store. Use fresh solution at 80° C 共176° F兲.
15 mL HNO3
60 mL glycerol
114 15 mL acetic acid Use fresh solution at 40– 42° C 共104– 108° F兲.
20 mL HNO3 Immerse 4 – 30 min depending on depth of
80 mL water worked metal layer. Clean with cotton in running
water.
115 100 mL acetic acid Immerse 10– 30 min depending on depth of
10 mL H2O2 (30 %) worked metal layer. Clean in HNO3 if
necessary.
116 5 – 10 g AgNO3 90 mL water Swab.
117 10 mL HCl (a) Immerse for 1 / 2 – 5 min. Follow with
90 mL water electrolytic etch at low current density in same
solution. If specimen has considerable surface flow,
immerse in concentrated HCl for
a few seconds, then follow above procedure.
(b) Immerse for 1 / 2 – 2 min.
118 1 mL HNO3 Swab 3 – 5 s for F and T6, 1 – 2 min for T4 and O
75 mL diethylene glycol temper.
25 mL water
119 1 mL HNO3 Swab 1 – 3 s for F and T6, 10 s for T4 and O
20 mL acetic acid temper.
60 mL diethylene glycol
20 mL water
120 10 mL HF Immerse with gentle agitation 3 – 30 s.
90 mL water
121 0.7 mL H3PO4 Composition critical.
4 g picric acid (a) Immerse with gentle agitation 10– 30 s.
100 mL ethanol (95 %) or methanol (b) To increase staining immerse and withdraw
(95 %) with a meniscus layer. Lightly apply
etchant over surface until dark stain develops.
122 2 g oxalic acid Swab.
100 mL water
123 60 mL H3PO4 Electrolytic: Use stainless steel cathode. Space
100 mL ethanol (95 %) electrodes 2 cm apart. Start at 3 V dc.
After 30 s maintain at 11 / 2 V.
124 5 mL acetic acid Immerse with gentle agitation 10– 60 s.
10 mL water
6 g picric acid
(95 %)
125 10 mL acetic acid Immerse with gentle agitation 15– 30 s.
6 g picric acid
(95 %)
126 30 mL acetic acid Immerse with gentle agitation 1 – 30 s.
15 mL water
6 g picric acid
(95 %)
127 20 mL acetic acid Immerse with gentle agitation 5 – 30 s.
20 mL water
3 g picric acid
(95 %)
128 8 mL HF Immerse with gentle agitation 5 – 15 s.
5 mL HNO3
200 mL water
129 10 mL HF Swab 10– 20 s. Vary HF to increase or decrease
30 mL HNO3 activity.
60 mL lactic acid
130 25 mL HCl Caution—Keep below 24° C 共75° F兲. Electrolytic
75 mL methanol at 30 V for 30 s.
131 5 mL H2SO4 Electrolytic at 50– 60 V for 10– 20 s.
1 mL HF
132 5 mL HF Use fresh.
10 mL HNO3 (a) Swab with heavy pressure for 5 – 10 s. Water
50 mL lactic acid rinse, alcohol rinse, dry, then etch
with No. 98c.
(b) Swab for 5 – 30 s.
133 50 mL HNO3 Use hood. Do not store. Mix fresh. Immerse or
50 mL acetic acid swab 5 to 30 s. Will chemically polish
with longer times. Sulfidized grain boundaries
etched before normal grain boundaries.
134 70 mL H3PO4 Electrolytic 5 – 10 V for 5 – 60 s. (Polishes at high
30 mL water currents.)
135 80 mL HNO3 Use hood. Warm specimen in boiling water prior to
3 mL HF immersion for 10 to 120 s.
136 20 mL H3PO4 Electrolytic at 10– 20 V for 10– 15 s.
80 mL water
137 10 g NaNO3 Electrolytic, 0.2 A / cm2, 1 min.
100 mL water
138 5 g FeCl3 Swab 10– 60 s.
2 mL HCl
100 mL ethanol (95 %) or
methanol (95 %)
139 5 g (95 %) KCN Use hood—Can give off extremely poisonous
100 mL water hydrogen cyanide. Precaution—Also
0.5 mL H2O2 (3 %) poisonous by ingestion as well as contact. Immerse
10– 100 s.
140 50 mL acetic acid Use hood. Do not store. Decomposes with possible
50 mL HNO3 explosion on standing. Immerse
50 mL acetone 10– 30 s.
141 3 g NH4Cl Swab 5 – 30 s. Do not store.
3 g CrO3
10 mL HNO3
90 mL water
142 5 mL HF Electrolytic at 2 – 3 V for 2 – 10 s.
10 mL glycerol
85 mL water
144 A Electrolytic in Solution A: specimen is cathode,
10 g sodium thiosulfate 10 V, 5 – 10 s. Then electrolytic in
100 mL water Solution B: specimen is anode, 10 V, 5 – 10 s.
B
10 mL HCl
90 mL water
145 2 mL H2SO4 Electrolytic at 3 – 10 V for 5 – 15 s. Use platinum
100 mL water wires. H2SO4 may be increased to 20
mL for deeper attack.
146 10 mL HF Immerse 30 s - 3 min.
100 mL HNO3
80 mL HCl
148 5 mL HNO3 Immerse 10– 30 s.
100 mL water
149 50 mL HCl Immerse 10– 30 s. Do not store.
2 mL H2O2 (30 %)
50 mL water
150 60 mL HCl Use hood. Do not store. Swab few seconds to a
20 mL HNO3 minute. Discard when solution turns
40 mL glycerol dark yellow.
151 10 mL HF Swab 5 – 30 s.
25 mL HNO3
150 mL water
152 85 mL NH4OH Immerse 5 – 15 s. Do not store—Decomposes.
15 mL H2O2 (30 %)
153 10 mL HNO3 Use hood. Do not store. Add HNO3 last. Discard
50 mL HCl when dark yellow. Immerse 10– 60 s.
60 mL glycerol Preheating specimen in boiling water hastens
reaction.
154 50 mL HCl Immerse 10– 100 s.
(95 %)
155 3 mL selenic acid Immerse 1 – 15 min. (Up to 30 mL of HCl may be
10 mL HCl used for more vigorous action.) Stable
100 mL ethanol (95 %)or methanol for 3 – 90 days, depending on HCl concentrations.
(95 %)
158 1 g thiourea Electrolytic, 0.005– 0.01 A / cm2, 1 – 2 min.
1 mL H3PO4
1000 mL water
157 25 g CrO3 Immerse 5 – 20 s.
150 mL HCl
50 mL water
158 10 mL HF Swab 5 – 15 s.
10 mL HNO3
20 mL glycerol
159 5 mL HF Swab 10– 30 s.
20 mL HNO3
50 mL acetic acid
160 20 mL HF Immerse to 5 min.
15 mL H2SO4
5 mL HNO3
50 mL water
161 25 mL HNO3 Immerse 5 – 120 s.
5 mL HF
162 A Swab 1 – 3 min in Solution A (acts as etch polish).
50 mL lactic acid To etch, swab with Solution B for 5 s.
30 mL HNO3 Repeat if necessary. The HF may be varied to give
2 mL HF more or less etching.
B
30 mL lactic acid
10 mL HNO3
10 mL HF
163 30 mL H2SO4 Immerse 5 – 60 s. Use this solution for alternate
30 mL HF etch and polishing.
3–5 drop H2O2 (30 %)
30 mL water
164 50 mL HNO3 Use hood. Swab 3 – 10 s.
30 g ammonium bifluoride
20 mL water
165 10 mL HCl (a) Electrolytic at 10 V for 30 s. Use carbon
90 mL ethanol cathode and platinum wire connection to
specimen. For etch-polishing, use shorter time.
(b) Electrolytic at 6 V for 10 s. Use stainless steel
cathode and platinum or Nichrome
wire contact to specimen.
20 g ammonium persulfate hydrogen cyanide. Precaution—Also
90 mL water poisonous by ingestion as well as contact. Mix 1
B + 1 ratio of Solution A and B just
20 g KCN before use. (A mixture of 5 drops of each will
90 mL water cover the surface of the 1 in. dia mount.)
Immerse to several minutes.
167 5 g NaCN Use hood—Can give of extremely poisonous
100 mL water hydrogen cyanide. Precaution—Also
poisonous by ingestion as well as contact.
Electrolytic at 1 – 5 V ac for 1 – 2 min. Use
platinum cathode.
168 20 mL HCl Composition given will saturate the solution with
35 g NaCl NaCl. Electrolytic at 11/2 V ac for 1
80 mL water min.
169 5 mL HNO3 Electrolytic at 0.05 A / cm2 for 2 min. Use stainless
50 mL ethylene glycol steel cathode.
(95 %)
170 1 mL HF (a) Swab 5 – 30 s. Follow with water rinse, alcohol
30 mL HNO3 rinse, dry.
30 mL lactic acid (b) Swab for 10 s intervals. Increase HF to
exaggerate grain boundaries.
171 concentrated HCl Use hood. Electrolytic at 5 V ac for 1 – 2 min. For
etch-polishing, use shorter times.
Follow with water rinse, alcohol rinse, and dry.
5 g ammonium persulfate hydrogen cyanide. Precaution—Also
10 mL water poisonous by ingestion as well as contact. Prepare
B 1 + 1 mixture of Solutions A and B just before use.
5 g KCN (A mixture of 5 drops of each will cover the
100 mL water surface of a 1 in. dia
mount.) Immerse 1 – 2 min.
173 50 mL NH4OH Immerse few seconds to a minute.
10– 30 mL H2O2 (50 %)
174 A Prepare 1 + 1 mixture of Solutions A and B. Apply
25 mL HNO3 with camel’s hair brush.
1 g K2Cr2O7 Nonadherent film of silver chromate should form.
1000 mL water If film adheres, add more of solution
B A, if none forms, add Solution B.
40 g CrO3
3 g Na2SO4
200 mL water
175 1 g CrO3 Immerse to 1 min.
1 mL H2SO4
100 mL water
176 2 g FeCl3 Immerse 5 – 30 s.
100 mL water
177 10 g NaOH Swab or immerse 5 – 15 s.
100 mL water
178 20 mL HF Swab for 5 – 20 s.
20 mL HNO3
60 mL lactic acid
179 A Use hood—Mix Solution B very slowly. Solution
10 mL HF A is used as a chemical polish, though
10 mL HNO3 some etching will occur. Swab 2 or more minutes
30 mL lactic acid for desired surface. If surface is
B insufficiently etched use Solution B electrolytically
10 mL HF at 1 / 2 – 1 V / in.2 of specimen. Use
10 mL HF carbon cathode and platinum wire connection to
90 mL H2SO4 specimen. Discard Solution B after 1
h.
180 10 mL HNO3 Immerse for 1 / 2 – 10 min at 38 to 42° C
30 mL acetic acid 共100– 108° F兲.
50 mL glycerol
181 2 mL HCl Swab for 1 – 3 min.
(95 %)
182 10 mL HNO3 Immerse for 1 / 2 – 10 min at 38 to 42° C
10 mL acetic acid 共100– 108° F兲
80 mL glycerol
183 2 drops HF Immerse for 1 min.
1 drop HNO3
25 mL glycerol
184 10 g FeCl3 1
Immerse for – 5 min.
2 mL HCl 2
100 mL water
185 10 mL HF Swab for few seconds.
10 mL HNO3
186 10 mL HF Swab 3 – 2 s.
5 mL HNO3
85 mL water
187 10 mL HF Swab 3 – 20 s.
30 mL HNO3
50 mL water
188 1 mL HF Swab until stain is removed.
50 mL HNO3
50 mL H2O2 (30 %)
50 mL water
189 10 mL HF Swab 3 – 20 s.
25 mL HNO3
45 mL glycerol
20 mL water
190 8 g KOH Swab 3 – 20 s.
10 mL H2O2 (30 %)
60 mL water
191 25 mL HF Swab 3 – 20 s.
18 g benzalkonium chloride
40 mL glycerol
192 1 – 3 mL HF Swab 3 – 10 s or immerse 10– 30 s. (HF attacks
2 – 6 mL HNO3 and HNO3 brightens the surface of
100 mL water titanium. Make concentration changes on this
basis.)
193 2 drops HF Swab 3 – 20 s.
1 drop HNO3
3 mL HCl
25 glycerol
194 20 mL HF Immerse 5 – 30 s.
20 mL HNO3
60 mL glycerol
195 30 mL H3PO4 Electrolytic at 18– 20 V 共0.03 A / cm2兲 for
30 mL ethylene glycol 5 – 15 min.
196 18 g CrO3 Dissolve CrO3 in hot water and cool before adding
75 mL acetic acid acetic acid. Keep solution below
20 mL water 2 ° C 共35° F兲 during use. Electrolytic at 80 V for
5 – 30 min. Do not store.
197 5 g oxalic acid Electrolytic at 6 V for 5 – 20 s.
100 mL water
198 30 mL HF Swab for 60 s.
30 mL HNO3
30 mL glycerol
199 2 mL HF Swab for 5 s
5 g AgNO3
100 mL water
200 A Immerse in Solution A with gentle agitation for
40 g CrO3 several seconds. Rinse in Solution B.
3 g Na2SO4
200 mL water
B
40 g CrO3
200 mL water
201 A Immerse in Solution A with gentle agitation for
40 g CrO3 several seconds. Rinse in Solution B.
1.5 g Na2SO4
200 mL water
B
40 g CrO3
200 mL water
202 A Immerse in Solution A for 2 – 5 s. Rinse in
10 g CrO3 Solution B.
1 g Na2SO4
200 mL water
B
40 g CrO3
200 mL water
203 20 g CrO3 Electrolytic at 0.2 A / cm2 for 5 s.
100 mL water
10 mL glycerol Electrolytic at 15– 50 V for 15– 60 s.
10 mL water
205 5 mL HF Swab vigorously for 10– 60 s. Wet cotton
2 mL AgNO3 (5 %) frequently.
100 mL water
206 5 mL HF Precaution—Discard after use. Solution
10 mL HNO3 decomposes on standing. Electrolytic at 9–12
10 mL glycerol V for 1 – 10 min.
207 30 mL HNO3 Swab for 5 – 30 s.
30 mL acetic acid
30 mL water
208 1 mL NH4OH Immerse or swab few seconds to a minute.
3 g ammonium persulfate
10 mL water
3 mL HF
80 mL water
210 50 mL water (cold) saturated with First ingredient in stock solution. Add potassium
sodium metabisulfite before use. Solution
thiosulfate good for several days, or longer. Immerse face up,
1 g potassium metabisulfite gently agitate until coloration
begins, allow to settle. Stop etch when surface is
red-violet. Etch time varies with
material. Colors matrix phases.
211 3 g potassium metabisulfite Use fresh solution. Immerse specimen face up,
10 g sodium thiosulfate gently agitate solution until coloration
100 mL water begins, allow to settle. Stop etch when surface is
red-violet. Etch time varies with
material. Colors matrix phases.
212 10–50 % HCl in water For more corrosion resistant alloys. Increase the
0.5– 1.0 g potassium metabisulfite per HCl and potassium metabisulfite
100 mL of aqueous HCl solution contents. Use optional ingredients to improve
Optional: 1 g CuCl2 coloration, if needed. Colors matrix
1 – 3 g FeCl3 phases. Use by immersion only.
2 – 10 g ammonium bifluoride
213 2 – 10 mL HCl For more corrosion resistant alloys, increase the
0.5– 3 mL selenic acid HCl and selenic acid content. For highly
100 mL ethyl alcohol (95 %) corrosion-resistant alloy, use 20– 30 mL HCl.
Colors second phase
constituents. Use by immersion only.
214 1 g sodium molybdate Add nitric acid to lower the pH to 2.5–3. Add
100 mL water 0.1– 0.5 g ammonium bifluoride for carton
steels. Use by immersion only. Colors carbides.
Immerse about 15 s.
215 240 g sodium thiosulfate Mix in order given. Store in a dark bottle at least
30 g citric acid 24 h before use at 20° C. Lightly pre-
24 g lead acetate etch specimen before use. Use small portion of
1000 mL water stock solution for 4 h max. Pre-etch
steel specimens with nital before tinting the MnS
(add 0.2 g sodium nitrite to 100 mL
of etch) white. Colors phosphides in cast iron.
Colors matrix of Cu alloys.
216 8 – 15 g sodium metabisulfite Do not store. Mix fresh. Immerse specimen face
100 mL water up. Agitate solution gently until
coloration begins, allow to settle. Stop when
surface is dark. use crossed polarized
light and sensitive tint to improve coloration.
217 5 g ammonium bifluoride Mix fresh, use plastic coated tongs and
100 mL water polyethylene beaker. Immerse until surface is
colored.
218 3 g ammonium bifluoride Mix fresh, use plastic coated tongs and
4 mL HCl polyethylene beaker. Immerse until surface is
100 mL water colored. Works best with attack-polished
specimens.
219 60 mL HNO3 Electrolytic etch, does not reveal twins in ␥
40 mL water stainless steel. Excellent grain boundary
etch for ferritic stainless steels. Use at 1 V dc,
120 s, with stainless cathode; 0.6 V dc
with platinum cathode.
220 20 g NaOH Electrolytic etch, colors ␦-ferrite in stainless steel.
100 mL water Use at 2 – 20 V dc, 5 – 20 s,
stainless steel cathode. If ␦ is not colored, increase
NaOH to 40 g.
221 50 mL water Use by immersion. Will not attack sulfides in
50 mL ethyl alcohol stainless steels.
50 mL methyl alcohol
50 mL HCl
1 g CuCl2
2.5 g FeCl3
2.5 mL HNO3
222 8 g Na2SO4 (a) Few seconds to 1 minute.
100 mL water (b) Pre-etch 2 s in No. 74, rinse, and etch 20 s.
223 A Mix equal volumes of Solutions A and B just
8 g oxalic acid before use. Etch 2 – 3 s; 3 s pre-etch in
5 mL H2SO4 No. 74 may be needed.
100 mL water
B
H2O2 (30 %)
224 10 mL H2O2 (30 %) Immerse 10 s at 20° C 共68° F兲.
20 mL 10 % aqueous NaOH
225 4 g NaOH Immerse 10 s at 20° C 共68° F兲.
100 mL saturated aqueous KMnO4
226 15 mL HCl Use hood—Can give off nitrogen dioxide gas.
10 mL acetic acid Precaution—Mix HCl and glycerol
5 mL HNO3 thoroughly before adding HNO3. Do not store.
2 drops glycerol Discard before solution attains a dark
orange color. Use fresh or age up to 1 min.
Immerse or swab few seconds to few
minutes. Can increase HNO3 to increase strength.
Sometimes a few passes on the
final polishing wheel is also necessary to remove a
passive surface.
901 1 g KOH Electrolytic: Use stainless steel cathode. 40 V
100 mL water DC at 3 A / cm2 in 30– 60 s
902 Plasma etching with CF4 gas and O2 3 – 5 min, 60– 80 W
gas (1:1)
903 See etchant 98 (Murakami’s reagent) Use hot, 30– 40 min for SiC with 1 % B4C or
boiling for B-doped SiC
904 30 g K3Fe共CN兲6 Immerse 5 – 30 min at 110° C 共230° F兲
3 g NaOH
60 mL water
905 10 g K3Fe共CN兲6 Immerse 5 – 10 min
10 g NaOH
20 mL water
906 10 g K3Fe共CN兲6 Immerse 10– 20 min
10 g NaOH
80 mL water
907 10 mL HNO3 (65 %) Immerse 30– 40 min at 60° C 共140° F兲
10 g K3Fe共CN兲6
100 mL water
908 30 g K3Fe共CN兲6 Immerse 8 – 15 min. Use boiling
3 g NaOH
60 mL water
909 10 mL HNO3 (65 %) Immerse seconds to min
10 mL HF (40 %)
10 mL water
910 10 mL HF (40 %)
50 mL lactic acid
30 mL HNO3 (65 %)
911 10 mL HF (40 %) Immerse 2 min
30 mL HNO3 (65 %)
912 10 mL HCl (32 %) Immerse seconds to min
10 mL H2O2 (30 %)
913 Plasma etching 1 – 5 min, 60– 80 W
CF4 gas and O2 gas (2:1)
914 H3PO4 (85 %) Use boiling up to 15 min
915 Molten NaOH (free of water) 20 s to 3 min at 300– 350° C 共570– 660° F兲, 2–3
samples per melt
916 10 mL 10 % aqueous NaH solution Immerse 30 min at 100° C 共212° F兲)
10 mL 10 % aqeous potassium
ferricyanide solution
50 mL water
(Modified Murakami, see etchant 98)
917 Thermal etch in air 1100– 1500° C 15– 20 min at 1300– 1400° C 共2370– 2550° F兲
(Etch temperature is approximately 150° C
共300° F兲 below sintering temperature
918 H3PO4 (85 %) 5 s to 3 min at 250° C 共480° F兲
919 HCl (32 %) Immerse 3 – 6 min
920 Sat. aq. Na2S Immerse up to 1 min
921 20 mL HNO3 (65 %) Immerse up to 15 min
10 mL HF (40 %)
20 mL water
922 45 mL HNO3 (65 %) Immerse up to 15 min agitate
5 mL HF (40 %)
50 mL water
923 KHSO4, molten Immerse 15– 20 s at 300° C
924 15 mL HNO3 (65 %) Immerse 3 – 5 min at 25– 60° C 共77– 140° F兲
100 mL water
925 10 g NaOH Immerse seconds to minutes
10 g K3Fe共CN兲6
100 mL water
926 Thermal etch in air Minutes to 1 h at 1300– 1400° C 共2370– 2550° F兲
(according to sintering temperature)
927 H3PO4 (85 %) Immerse 3 s to 2 min at 250° C 共480° F兲
928 Thermal etch in air 30– 60 min at 1200° C 共2190° F兲 5 s to 2 min
929 3 mL HCl (32 %) Immerse 5 s to 2 min
2 mL HF (40 %)
95 mL water
930 2 mL HF (32 %) Immerse 10– 15 min
98 mL water
931 5 mL HNO3 (65 %) Immerse, up to 20 s
5 mL HF (40 %)
90 mL water
932 10 mL HNO3 (65 %) Immerse up to a few min
10 mL HF (40 %)
933 50– 100 g NaOH Immerse up to a few min
100 mL water
934 15 mL HCl (32 %) Immerse up to a few min
10 mL HF (40 %)
90 mL water
5 mL H2O2 (32 %)
70 mL water
936 30 mL CH3COOH (glacial acetic acid) Immerse up to a few min
10 mL H2O2 (30 %)
2 g FeCl3
100 mL water
938 25 mL HCl (32 %)
8 g FeCl3
100 mL water
939 15 mL HCl (32 %) Add CrO3 just before use
50 mL aq. sodium thiosulfate (16 %)
3 mL aq. CrO3 (10 %)
30 mL water
940 50 mL HCl (32 %) Immerse 1 – 10 min
50 mL water
941 25 down to 9 mL Immerse s to min
HNO3 (65 %)
25 down to 9 mL CH3COOH (glacial
acetic acid)
100 mL glycerol (87%)
942 200 mL acetyl acetone Immerse 2 – 18 min in ultrasonic bath to break up
1 – 2 mL nitric acid (65 %) the oxide layer
943 100 mL HNO3 (65 %) Immerse in 2 min at 70° C, time varies
100 mL H2SO4 + CrO3
(chromosulfuric acid)
(Variable concentration)
944 60 g CrO3 (chromium (VI)oxide) Immerse several hours at 70° C
100 mL water
945 HNO3 (65 %) Polyethylene (PE): Immerse in seconds to
minutes
Polyoxymethylene (POM) and polypropylene
(PP): Immerse in 10 min
946 C6H4共CH3兲2 (xylol) (99.8 %) Polyethylene, polypropylene: Immerse 3 days at
70° C
Polyamid, polyethylene: 70° C
for 60 s. Nylon 6: 65– 70° C for 2 – 3 min. Nylon
6,6: 75° C for 3 – 4 min
947 C6H15N (triethylamine (99 %) Immerse seconds to minutes
948 30 mL HCl (32 %) Immerse 20 s
100 mL distilled water
949 A: Freshly prepared mixture of equal Etch in mixture A at approx. 20° C for 2 – 10 s.
ASTM quantities of 10 % (mass/mass) Flush the test-piece section with water
Standard aqueous solutions of K3Fe 共CN兲6 (III) immediately, without removing the oxide layer.
B 657, (potassium ferricyanide and Dry the surface carefully with acetone or alcohol
Etching potassium or sodium hydroxide) without wiping
Technique
1
950 A: same as A (949) Etch at approx. 20° C in mixture A for 3 – 4 min..
ASTM B: A mixture of equal volumes of then wash in water and etch in mixture B for
Standard concentrated hydrochloric acid and approx. 10 s. Next wash in water, then in alcohol
B 657, water and dry the test-piece section. Finally, etch in
Etching mixture A for approx. 20 s
Technique
2
951 A: same as A (949) Etch in mixture A at approx. 20° C for 3 – 6 min
ASTM
Standard
B 657,
Etching
Technique
3
12.5.3 Table 12.3—Etchant Names
TABLE 12.3—Etchant names. (This table was taken fromASTM E 407.)

Common Name No. Common Name No.
Acetic glyceregia 89, 226 Groesbeck’s 19
Alkaline Sodium Picrate 85 Hatch 2
Aqua regia 12 Howarth’s 84
Barker’s 5 Kalling’s 1 95
Beraha’s 99, 155, 211–215 Kalling’s 2 94
Carapella 138 Keller’s 3
Chrome regia 101 Klemm’s 210
Contrast 141 Kroll’s 192, 187
CP 4 60 Marble’s 25
El-1R 107 Marshall’s 223
Flat 133 Murakami’s 98
Flouregia 90, 158 Nital 74
Frank’s 104 Palmerton 200
Fry’s 79 Phoschromic 111
G 107 Picral 76
Glyceregia 87 Ralph’s 221
Gorsuch 75 Super Picral 77
Grard’s No. 135 Vilella’s 80
Green contrast 94 92-5-3 105
13
Specimen Preparation
13.1 Introduction
THIS CHAPTER COVERS THE PRACTICAL PREPARATION OF THE MATER-
ials stated in Table 11.1 for each material two different methods of the mechanical
preparation process are stated in 68 Material/Preparation Tables. These tables also
contain specific information on ASTM standards and etching described in Chapter 12.
Electropolishing is covered by 25 methods.
At the end of the chapter, Section 13.5 covers Trouble Shooting regarding the pro-
cess and the results.
The background for the preparation process, including general advice and hints
for wet abrasive cutting and mounting can be found in Part I. Advice and hints for the
total preparation process covering specific materials will be stated on each Material/
Preparation Table and in Section 13.5.
13.2 Mechanical Preparation—The “Traditional” and

“Contemporary” Methods
As described in Part I, two basic methods are available for the metallographer, one is
based on SiC grinding paper or other “traditional” grinding media, referred to as the
“traditional” method with a T-number, and another method, based on rigid composite
disks 共RCDs兲, referred to as the “contemporary” method, with a C-number.
Both methods will be stated side-by-side in the Material/Preparation Tables, Sec-
tion 13.2.3.
13.2.1 Material/Preparation Tables

Each sheet of Material/Preparation Tables has a number starting with 1–68. The two
Method Tables, one for the C-Method and one for the T-Method are part of the Material/
Preparation Tables and have the same number as the sheet, for example, C-01 and T-01.
Each sheet with tables can be from three to six pages, depending on the amount of text.
The tables include as far as possible all relevant information for the preparation pro-
cess of the given material or material group.
The text is in the following order:
Material or Material Group, see Section 11.2 and Table 11.1.
Material Properties: For most materials, four basic properties are stated: Crystal
Structure, Density in g / cm3, Melting Point in °C 共°F兲, and Hardness, 共for nonferrous
metals the figures for hardness are taken from ASM Handbook, Vol. 02, Properties and
Selection: Nonferrous Alloys and Special-Purpose Materials, ASM International, Materi-
als Park, Ohio, USA, 1990. The hardness can be in HB, HK, HRC, HV, and Moh 共in some
cases, no hardness is indicated兲.
Comments on Material: Basic information on the material and the preparation
of the material.
General Comments on:
218
Chapter 13 Specimen Preparation 219
Sectioning
Mounting
Grinding
Polishing
Etching
Purpose: A table indicating relevant methods relating to the purpose of examina-
tion and ASTM standards 共see Section 12 and Table 12.1兲.
Preparation Process:
Sectioning: Specific indications.
Mounting: Specific indications. Attention: In most cases several types of mount-
ing materials can be used. In these cases only examples, “bakelite” 共hot mounting兲 and
“acrylics” 共cold mounting兲 are stated.
Grinding: Specific indications.
Polishing: Specific indications.
Contemporary Method: Method Table.
Traditional Method: Method Table.
Etchants: Table with relevant etchants.
13.2.2 Method Tables—Generic Methods—Parameters/Consumables—

Table 13.1
Generic Methods
The Method Tables covering the C- and T-methods contain a number of parameters
and consumables. The methods should be considered “generic,” and state a basic pro-
cedure for a given material, using a standard semiautomatic grinder/polisher with ex-
changeable grinding/polishing disks. The specimens are either “single specimens” or
“fixed specimens” in a holder on a 300 mm 共12 in兲 grinding/polishing disk. If material
or equipment/consumables vary, the data must be changed accordingly 共see below un-
der “Force per Specimen” and “Time”兲.
The time stated for each step can in some cases be shortened with the stated times
being to the “safe side.” This is because the preparation time normally is the only indi-
cation we have of “material removal.” During the preparation a certain amount of ma-
terial should be removed. The best would be a direct measurement, but in normal prac-
tice only the process time can be measured, giving an indication of material removal
based on experience. Variation in polishing cloths, abrasives, etc., justifies the rela-
tively long times indicated to secure a sufficient material removal, but often the metal-
lographer with experience will be able to shorten these times.
Steps
The method is divided into a number of steps:
PG 共plane grinding兲. This is the first step and is usually performed with one or sev-
eral sheets of 220 grit SiC grinding paper. In the row, Time 共see below兲 normally “Until
plane” is stated, indicating that a sufficiently prepared surface, coplanar to the surface
of the paper and with a regular “220” scratch pattern covering the whole specimen sur-
face is obtained.
In some cases a coarser grain like grit 180 can be used before grit 220, but 220
should always be used as the last paper for PG. This ensures the reproducibility of the
method.
For some materials 共very hard or soft兲, grit 220 grinding paper is not stated for PG;
TABLE 13.1—Comparison Between Surfaces for Grinding and Polishing from a Number of Suppliers with
Abbreviations Used in Method Tables.
Allied
High Mark Lap-
Suppliers Buehler Struers Leco Tech V master
Abbreviations in
Method Tables
Dia, pad, bak or Ultra-Prep Diamond Diamond Bonded Flex
met Pad Spot Diamond Diamond
Pattern Disk Disk
Dia, disk, fixed, Apex DGD MD-Piano Cameo
res Platinum
RCD, hard ApexHerculesH MD- Cameo
Allegro Silver
RCD, soft ApexHercules S MD-Largo Cameo
Gold
Cloth, napless, Ultra-Pad DP/MD- Plan
v. hard, wov, Plan Cloth
syn
Cloth, napless, Texmet 2000 DP/MD- Leco Pol Kempad Met-X Pan-W
hard, nonwov Texmet 1000 Pan Pan-W Pan-B
syn
Cloth, napless, Ultra-Pol DP/MD- Silk Silk Silk Silk
hard, wov, silk Dur
Cloth, napless, Trident DP/MD- Gold Gold RAM ASR
hard, wov, syn Nylon Dac Technotron Label Nylon Nylon
Nylon Nylon
Cloth, napless, DP/MD- Broad Micro
med hard, wov, Mol cloth LP
wool
Cloth, med nap, Microcloth DP/MD- Lecloth Spec- Alpha NTR
soft, syn Nap Cloth A
Cloth, napless, Chemomet OP/MD- Black Chem-Pol Supreme
soft, porous, syn Chem Technotron
in these cases, PG, possibly made in several steps, shall end with the Disk/Cloth stated
in the Method Table.
See also Time below.
FG 共fine grinding兲. This can be in several steps indicated with a number, e.g., FG 1.
P 共polishing兲. This can be in several steps, indicated with a number, e.g., P 1. In
most methods, the last step indicated is with silica/alumina. Often this step can be
omitted, depending on the purpose of the preparation.
Parameters
Each step contains a number of parameters:
Disk/Cloth: The surface covering the rotating disk of the grinding/polishing ma-
chine.
Abrasive Type: The abrasive used for grinding and polishing.
Grit/Grain Size: Grit, indicated with a P- number corresponding to the FEPA stan-
dard 共see Table 6.2 for comparison to American standard兲. In case of diamond or an-
other abrasive, the grain size is indicated in ␮m.
Lubricant Type: The type of medium used for lubrication during the process.
Rotation Disk/Holder, Comp/Contra: rpm of grinding/polishing disk and speci-
men holder. “Comp” means complementary: The disk and holder rotates in the same
direction. “Contra” means counter rotation: The disk and the holder rotates in opposite
directions.
Force per Specimen: The force in N and lb per specimen. Attention: The force is
based on a 30 mm 共1.25 in兲 mounted specimen with the specimen totaling approxi-
mately 50 % of the mount. At 25 mm 共1 in兲 specimens the force should be reduced with
the factor 0.7. At 40 mm 共1.50 in兲 only increase the force up to a maximum of 50 N
共11 lb兲 and as compensation, to obtain the necessary material removal, extend the
preparation time with 1 – 4 min. This is to avoid a possible overheating of the polishing
cloth that can take place at a force on each specimen of more than 50 N 共11 lb兲. With
SiC grinding paper, a very high force might create heavy damage to the specimen 共see
Section 6.6兲 and the paper, if not glued to the disk, might be torn away.
Be aware that the values indicated are for a single specimen. When using a holder
with say six fixed specimens, the value should be increased with a factor 6.
Time: The number of minutes the specimens are in contact with the disk. Atten-
tion: For specimens larger than 30 mm 共1.25 in兲 the time should be extended 共see
Force per Specimen above兲. Also, if the grinding/polishing disk is smaller than
300 mm 共12 in兲, the time should be extended. At PG, until plane indicates that the
specimen surface should be uniformly covered with a regular scratch pattern. The time
used depends on the quality of the sectioning and the alignment of the specimens if a
specimen holder with several fixed specimens is used.
Consumables—Abbreviations—Table 13.1
The methods are based on the use of a number of consumables which are described in
the Method Tables with abbreviations. These consumables have different names from
the different suppliers. For this reason a description is given below for each type of
consumable. Based on this, the user should be able to choose the correct consumable
from any supplier.
The surfaces used for grinding and polishing can be difficult to describe. For this
reason, a list of surfaces from a number of suppliers is stated in Table 13.1.
The descriptions are given according to the abbreviations used in the Method
Tables, stated alphabetically.
For a more detailed description of consumables see Part I.
Abbreviations Used in Method Tables—Description of Consumables

Alco: Alcohol-based lubricant. This lubricant should be phased out if possible and re-
placed with water-based lubricant because ethyl alcohol 共ethanol兲 is considered a dan-
ger to health in certain countries.
Alumina: Al2O3 suspension as abrasive.
Bak: The abrasive is fixed in a bakelite bond.
Cloth: A surface made of a textile or other flexible material fixed to the polishing
disk with adhesive backing or magnetically.
Disk: A surface for grinding/polishing made of a material with a “rigid” surface
normally fixed to the polishing disk like a cloth, or in some cases a solid disk taking the
place of the polishing disk.
Dia: Diamond as abrasive. This is followed by spr or susp, or both 共see below兲.
Diamond: Diamond as abrasive.
Fixed: The abrasive is fixed in the surface of the disk.
Hard: A hard rigid composite disk 共RCD兲 or polishing cloth with a relatively hard,
aggressive surface. A hard cloth could be satin woven, very thin or compact 共see “V.
hard”兲 without nap and with a very low resilience.
Low nap: Polishing cloth with a very short nap could be synthetic material. Low
resilience.
Med„ium… hard: Polishing cloth, napless, with a low resilience.
Med„ium… nap: Polishing cloth with a medium nap could be a flocked cloth with
relatively high resilience.
Met: The abrasive is fixed in a metal bond.
Napless: Polishing cloth without nap 共see Hard above兲.
Nonwov: Polishing cloth made of a nonwoven material.
Oil: Oil-based suspension or lubricant. This type should be avoided because oil-
based products are considered dangerous to health in certain countries. Oil-based dia-
mond suspensions are only stated in the T-methods. Lubricants based on oil emulgated
with water 共see below兲.
Pad: Diamond pad 共disk兲 with either metal or bakelite bond.
Porous: Polishing cloth with a porous surface mostly used for oxide polishing.
RCD: Rigid Composite Disk.
Res: The abrasive is fixed in a resin bond like epoxy, different from bakelite.
SiC paper: SiC wet grinding paper, normally with a C weight backing, and nor-
mally used with plain backing 共see Section 13.2.4兲. In certain cases it is an advantage to
use paper with an adhesive back for “heavy” automatic grinding.
Silica: Colloidal silica 共SiO2兲 as abrasive.
Silk: Polishing cloth made of silk.
Soft: A soft RCD or cloth with a relatively soft, less aggressive surface. For a cloth,
soft indicates a certain relative resilience, and can be with “Nap” or “Napless.”
Spr: Diamond spray.
Susp: Diamond suspension.
Syn: Polishing cloth made of synthetic material.
V.hard: A very hard cloth with an aggressive surface mostly used for “fine grind-
ing” 共see “Hard” above兲.
Wat: Water-based suspension or lubricant. This type should be preferred because
alcohol- and oil-based products are considered dangerous to health in certain coun-
tries.
Water: Normal tap water or recirculated water, with or without an additive.
Wat-oil: Lubricant based on water with an in-mixed oil forming an emulsion.
Wool: Polishing cloth made of wool.
Wov: Polishing cloth made of a woven material.
13.2.3 Material/Preparation Tables—Methods C-01/T-01 to C-68/T-68

This section contains 68 numbered sheets with Material/Preparation Tables 共M/PT兲
that include material/process information and two Method Tables.
To find the correct M/PT use Table 11.1
Using these tables should guide the user to obtaining a satisfactory preparation
result based on the material and the examination purpose.
The data stated in the Method Tables are based on a specimen of 30 mm 共1.25 in兲
diameter, clamped in a specimen holder on a 300 mm 共12 in兲 grinding/polishing disk.

Using a smaller disk diameter might prolong the preparation time. The specimen area
should be approximately 50 % of the mount.
The force indicated is per specimen and should be multiplied with the number of
fixed specimens in the holder.
The dosing levels for lubricant and abrasives are to be adjusted individually be-
cause temperature, humidity, etc., has a significant influence on the preparation pro-
cess. Take care that the surface of the polishing cloth/RCD is just “moist” when touched
with a fingertip, not “wet.”
For manual preparation see Section 13.2.4; often the data indicated in the
T-methods and some of the C-methods are suited for preparation by hand.
For electrolytic polishing see Section 13.4.2.
Material/Preparation Tables 01
Material: Hydroxyapatite „HA… coating
Material Properties: HA: Ca10共PO4兲6共OH兲2

Comments on Material: Ceramic materials that are specially developed for use as
medical and dental implants are called bioceramics. They include alumina and
zirconia, bioactive glasses, glass-ceramics, coatings and composites,
hydroxyapatite 共HA兲, tricalcium phosphate 共TCP兲 and other calcium phosphates
and radiotherapy glasses. The most used bioceramics are calcium phosphate
compounds, especially HA and TCP. This is because they have almost the same
compositions as the skeleton 共69 % of bone is HA兲 and they have excellent
biocompatibility. When these ceramics are implanted into the living body 共in vivo兲
for a range of time, it is found that they have a strong chemical bond with bone
tissue and finally become a firm attachment. Ceramics are brittle and they are less
suited for load-bearing applications. Therefore, a calcium phosphate like HA is
used as a coating on materials such as titanium alloys or stainless steel where it
can contribute its bioactive properties, while the metallic component bears the
load. Also the coating gives a relatively rough surface that increases the
mechanical fixation of the component. The accepted method of applying HA
coatings to metallic implants is plasma spraying. The coatings with HA and TCP
are made with a controlled porosity. This porosity and other features like the
contact between base material 共substrate兲 and coating should be
materialographically examined.
For preparation of other bioceramics see Material/Preparation Tables 共M/PT兲 05
and 06, and for other ceramic coatings see M/PT 14.
Sectioning: HA/TCP are very sensitive materials and should be kept free of
contamination during the cutting. This can be done by masking the areas of
concern using plastic film and tape. It is important that the specimen is mounted
and vacuum impregnated before sectioning takes place to avoid damaging the
brittle ceramic layer 共see below兲. The sectioning should be done on a precision
cutter with a cut-off wheel suited for the base material 共substrate兲. The specimen
should be oriented so that the coating is compressed into the substrate during the
cutting 共see also M/PT 08兲. The thinnest possible cut-off wheel should be used and
the feed speed should be low.
Mounting: Before sectioning a careful vacuum infiltration of the specimen should
take place 共see M/PT 02 and Section 3.10兲. It is important that all open pores are
filled with epoxy so that the coating cannot be contaminated or damaged during
the following preparation. The sectioned specimen should possibly be vacuum
impregnated after the sectioning and carefully mounted in epoxy to secure a good
edge retention.
Grinding: In Methods C-01 and T-01 it is an assumption that the base material
can be ground with SiC grinding paper. For grinding surfaces for the harder
ceramics see M/PT 02–06.
Grinding times should be kept at a minimum.
Polishing: Also, polishing times should be as short as possible to secure a good
edge retention.
Etching: Normally the HA/TCP layer is not etched, but relief polishing, creating a
“physical etching” can be used 共see Section 9.6兲. For other ceramics see M/PT 02
to 06.
Purpose ASTM Standard 共See Section 12.4兲 Method

Case or coating thickness/hardness, C-01
surface layers
Grain size, grain boundaries E 562, E 1245, C-01
E 1268, E 1382
Image analysis, rating of inclusion E 562, E 1245, C-01
content E 1268, E 1382
High planeness
Microhardness, hardness C 730, C 849, C 1326, C-01,
C 1327, E 384 T-01
Microstructure E 3, E 562, E 883, C-01,
E 1245, E 1268, E 1382 T-01
Phase identification C-01,
T-01
Porosity C-01
Thermal spray coatings: Distribution, C-01
porosity, unmelted particles
Preparation Process 01
Sectioning
Cut-Off Wheel Al2O3 or SiC, backlite bond or diamond, metal bond
Mounting
Hot Resin Cold Mounting Resin Epoxy

Compression Time Time 6 – 12 h
Mounting Minutes Minutes/Hours
Grinding
Attention: In C-methods when using RCD: The disk turns concave during use.
When the difference is more than 100– 150 ␮m between the center and the
periphery, the disk is either discarded or trued.
Polishing
C-01: In some cases a step with a napless, hard, wov, silk cloth and 1 ␮m
diamond, other parameters like step P 2 in method T-01, can be added as P 1,
making the shown P 1 to P 2.
Contemporary Method C-01 共For definitions of parameters and consumables see

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 P1
Polishing
Disk/Cloth SiC paper SiC paper RCD, Cloth, napless
soft soft, porous, syn
Abrasive Type SiC SiC Dia, spr Silica
or susp
Grit of Grain 320 500 9 0.04
Size ␮m
Lubricant Type Water Water Alco/wat
Rotation 300/ 150 300/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp Comp Comp Contra
Force per 30 共7兲 30 共7兲 40 共9兲 15 共3.3兲
Specimen
N 共lb兲
Time Until plane 1 5–6 2–4
Minutes
Traditional Method T-01 共For definitions of parameters and consumbles see

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 FG 3 P1 P2 P3
Polishing
Disk/Cloth SiC SiC SiC SiC Cloth, Cloth, Cloth,
Paper Paper Paper Paper napless, napless, napless,
hard, wov, hard, soft,
silk wov, porous,
syn syn
Abrasive SiC SiC SiC SiC Dia, spr or Dia, spr Silica
Type susp or susp
Grit or P220 P320 P500 P1000 6 3 0.04/ 0.05
Grain
Size 共␮m兲
Lubricant Water Water Water Water Alco or Alco or
Type wat wat
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/ Comp or Comp or Comp Comp Comp Comp Contra
Contra contra contra or or
contra contra
Force per 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 10 共2.2兲
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 6 3 1–2
Minutes plane
Material: Boron carbide, B4C. Silicon carbide, SiC. Other carbides
Material Properties: B4C: Rhombohedral, 2.52 g / cm3, 2450° C 共4442° F兲, HV

3400–3800
SiC: Hexagonal/cubic, 3.21 g / cm3, 2300° C 共4172° F兲, HV 2800–3600
Comments on Material: High-performance ceramics can roughly be characterized
by structure and function. They can be divided roughly into two categories,
structural and functional ceramics. For those structural ceramics like silicon
nitride, silicon carbide, some types of zirconium dioxide, and a number of mixed
ceramics based on Al2O3, the properties are directed towards mechanical strength
and other mechanical properties. For those functional ceramics like barium
titanate, zinc oxide, and titanate the properties are directed towards electric,
magnetic, dielectric, and optical properties. Some ceramics like aluminum oxide
共the most important high-performance ceramic兲 and zirconium dioxide can be
optimized towards either structural or functional properties. For in-depth
information on ceramics and preparation of ceramics see Carle et al. Ref. 26, 共Part
I兲 and Elsner et al. Ref. 27, 共Part I兲.
In contrast to metals, the evaluation of ceramic materials with light microscopy
can be carried out both by reflected light and 共with some exceptions兲 on thin
sections by transmitted light. For economic reasons, however, the more simple
preparation of specimens for reflected light is preferred for routine examination.
For preparation of thin sections see Section 7.13.1.
Compared to metals, ceramics have a high to very high hardness, a low ductility,
and a high brittleness. The high hardness influences the preparation to a high
degree, but other factors like porosity and brittleness also makes the preparation
difficult.
Brittleness: This might cause pull-outs during cutting and grinding, the ceramic
grains being removed by the abrasive. Pull-outs are especially critical in materials
with a vitreous 共amorphous兲 phase between the grains. Also cracks and surface
stress can develop during sectioning and grinding 共see Sections 6.3.2 and 13.6兲.
Porosity: Often the following should be determined: Total porosity, pore type,
shape, size, and pore size distribution. Pull-outs are often made during the first
stages of the preparation. These pull-outs can be observed as pores and often will
disturb the analysis of grains, etc. Also, the edges of the original pores will be
damaged and rounded after grinding and fine grinding. In case of differences in
hardness between phases, material can be smeared into the original pores 共see also
Section 13.6兲.
Preparation methods: Due to the large variations in ceramic materials, five Material/
Preparation Tables, 02–06, with ten methods, are stated in the following.
Preparation times: A wide variation in time is provided in the method tables. This
is due to the large variations in ceramic materials which in some cases call for
long times, especially in the case of a high porosity.
Sectioning: The bond of the diamond cut-off wheel, its thickness and also the
type, size, and concentration of the abrasive grains are mainly responsible for the
quality of the cut surface. Both metal bond 共bronze兲 and bakelite bond can be
used. Bakelite bond will give the least damage to the surface and should be used
on brittle/porous materials. Depending on the material properties, feed rate and
rotational speed of the cut-off wheel should be adjusted. The higher porosity and
risk of pull-outs of a material, the slower the feed rate. The rotational speed
should not exceed 2000 rpm and often a lower speed should be used. The surface
quality can normally be improved by using a cut-off wheel with small grain size,
giving a drawback when cutting large specimens as the cutting time is prolonged.
The concentration of diamonds in the bond should not be too high, causing the
wheel to “press” and “pinch,” which will create pull-outs and micro and
macrocracks 共see Section 2.4.2兲. The same types of material damage develop with
a very hard bond. As a rule the cutting should be made with a thinnest possible
wheel with a grain size around 94 ␮m. Special care should be taken when
clamping specimens. Pressure spots induce high stress which might fracture the
material prior to cutting. In case of very brittle and porous materials, an
impregnation before cutting can be necessary 共see below and also Section 13.6兲.
Mounting: Vacuum impregnation: If the porosity is higher than 5 % it is advisable
to impregnate under vacuum in a special apparatus using epoxy of low viscosity
and possibly a dye 共see Section 3.10兲. Impregnation should often be repeated after
grinding to close pores that have been opened.
Mounting: Dense ceramic specimens with porosity under 5 % can be prepared
unmounted, clamped in a holder, if the shape permits. Ceramics with a porosity
over 5 % should be impregnated as described above and mounted in a cold
mounting material, preferably epoxy having an addition of hard filler to increase
the hardness of the mounting material. For very stable ceramics that will not be
damaged by the pressure, hot compression mounting in a mineral filled epoxy is
preferred because it provides a mount with a hardness matching the ceramic. In
certain cases hot mounting can be made with acrylic that can be used virtually
without pressure 共see Section 3.4兲.
Grinding: Plane grinding 共PG兲 is normally done with grinding disks with diamond
共see Sections 6.6.1 and 6.7.2兲. PG is causing relatively heavy damage to the
specimen surface; for this reason the finest possible grain size should be chosen. If
using diamond pads, the metallic bond will be the most aggressive, giving short
times but with strong damage. For sensitive ceramics the less aggressive bakelite
bond should be used. If the ceramic is not too hard 共functional ceramics兲, SiC
grinding paper might be used.
Fine grinding 共FG兲 normally takes place using diamond but in relatively soft,
brittle materials, sensitive to pull-outs, SiC paper can be used down to P4000.
Fine grinding 共FG兲 can be done on different surfaces stated in the Method Tables.
In case of brittle materials the pressure when using RCDs should be kept at 25 N
共5.7 lb兲. On materials with many pores the swarf from the RCD might be forced
into the pores, making examination very difficult. In this case a napless very hard,
woven, synthetic cloth is used for FG.
Polishing: The 6 ␮m and 3 ␮m diamond steps are very important for most
ceramics, removing the heavy deformations from grinding. In the case of pores a
1 ␮m diamond step can be useful to establish the edges of the pores. Oxide
polishing gives chemical mechanical action on ceramics. The effect can often be
increased by adding small quantities of H2O2 共32 %兲 and ammonia solution 共25 %兲
to the colloidal silica. This polishing can be used for relief polishing 共see Section
9.6兲.
Etching: Ceramic materials may often be difficult to examine under the

microscope since reflection differences in the structure are very slight. Various
etching and contrast methods can be used. Oxide materials are often contrasted by
thermal etching in air, vacuum, or various gases. The temperature range is usually
between 1200 and 1650° C 共2200 and 3000° F兲共Approximately 150° C 共300° F兲
below sintering temperature in air.兲 Etching time can be from 15 minutes to
several hours. Chemical etching mostly takes place only with hot 共boiling兲 acid
mixtures or molten metal salts. All etching shall take place under a fume hood
with extreme care. Often optical etching like dark field and DIC can be used on the
specimen surface taken directly from the preparation 共relief polishing兲. Also
plasma etching and ion etching are used 共see Chapter 9兲.
Purpose ASTM Standard 共See Section 12.4兲 Methods

surface layers
Grain size, grain boundaries E 112, E 930, C-02, T-02
E 1181, E 1382
Image analysis, rating of inclusion E 562, E 1245, C-02
content E 1268, E 1382
High planeness
Microhardness, hardness C 730, C 849, C 1326, C-02, T-02
C 1327, E 384
Microstructure E 3, E 562, E 883, E 1245, C-02, T-02
E 1268, E 1382
Phase identification C-02, T-02
Porosity C-02
Sectioning
Cut-Off Wheel Diamond, metal bond, or bakelite bond

Mounting
Hot Compression Resin Epoxy with Cold Mounting Resin Epoxy

Mounting Mineral Filler
Time Minutes 9 Time 6–8 h
Minutes/
Hours
Grinding
C-02: Often the FG2 step can be omitted.

T-02: Often the PG step can be omitted.
T-02: PG and FG1: Often both steps or only FG1 should be changed to
bakelite bond. Also, conventional diamond disks, preferably with bakelite bond
can be used 共see Section 6.6.1兲.
Attention: In C-methods, when using RCD: The disk turns concave during use.
Polishing
C-02: Often P 2 can be changed to a napless, hard, silk cloth or be omitted.

C-02, T-02: Final polishing step: Chemical mechanical polishing can be used by
adding small quantities of H2O2 共32 %兲 and ammonia solution 共25 %兲 to the
colloidal silica.
Etching
Etchants for oxides see Material/Preparation Tables 05/06.

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 P1 P2 P3
Polishing
Disk/Cloth Dia. disk, Dia. disk RCD, Cloth, Cloth, med Cloth,
fixed, res fixed, res soft napless, nap, syn napless,
hard, soft,
wov, syn porous
Abrasive Type Diamond Diamond Dia.spr Dia.spr Dia.spr Silica
or susp or susp or susp
Grit or Grain P220 P1200 9 3 1 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Alco or Alco or Alco or
wat wat wat
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp Comp Comp Comp Contra
contra
Force per 25 共6兲 25 共6兲 30 共7兲 30 共7兲 25 共6兲 15 共3.4兲
Specimen
N 共lb兲
Time Until 2 8–15 10–120 2–10 1–6
Minutes plane
Traditional Method T-02 共For definitions of parameters and consumables see

Section 13.2.2.兲
Polishing
Disk/Cloth Dia Dia Cloth, Cloth, Cloth, Cloth, Cloth,
pad, pad, napless, napless, napless, napless, napless,
met met v. hard, v. hard, hard, hard soft,
nonwov/ non non wov, porous
wov, wov/ wov, silk
syn wov, syn
syn
Abrasive Diamond Diamond Dia, Dia, Dia, Dia, Silica
Type spr or spr or spr spr
susp susp or susp or susp
Grit or 125 40 15 9 6 3 0.04/ 0.05
Grain
Size ␮m
Lubricant Water Water Alco/wat Alco/wat Alco/wat Alco/wat
Type
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/rpm
Comp/ Comp Comp Comp Comp Comp Comp Contra
Contra
Force per 30 共7兲 30 共7兲 30 共7兲 30 共7兲 30 共7兲 20 共4.5兲 10 共2.2兲
Specimen
N 共lb兲
Time Until 2–10 6–15 6–15 5–30 10–60 1–10
Minutes plane
Etchants
Material Etchants 共see Table 12.2兲 Uses

B 4C 901 General structure
SiC with 5–15 % 902 Secondary phase
oxide additions remain
SiC with 1 % B4C 903 Grain boundaries
SSiC 904 Alpha/alpha 共␣ / ␣兲
grain boundaries
Alpha/beta 共␣ / ␤兲
phase boundaries
SSiC doped 905 Grain boundaries
with B
SSiC doped 906 Grain boundaries
with Al
SiC with B4C 907 Grain boundaries
SiSiC 908 Grain boundaries
Material: Chromium carbide, CrC. Titanium carbide, TiC.
Titanium nitride, Tin Cubic boron nitride, CBN. Tungsten
carbide, WC. Other ceramics
Material Properties:
TiC: Face-centered cubic, 4.93 g / cm3, 3140° C 共5684° F兲, HV 2800–3500
TiN: Face-centered cubic, 5.4 g / cm3, 2950° C 共5342° F兲, HV 2450
CBN: Face-centered cubic, 3.48 g / cm3, 1700° C 共3092° F兲, HV 4500
WC: Hexagonal, 15.7 g / cm3, 2780° C 共5036° F兲, HV 2400
Comments on Material: See Material/Preparation Tables 02.
Preparation times: A wide variation in time is provided in the Method Tables. This
long times, especially in the case of high porosity.
Sectioning: See Material/Preparation Tables 02.
Mounting: See Material/Preparation Tables 02.
Grinding: See Material/Preparation Tables 02, and directions for specific materials
below.
Polishing: See Material/Preparation Tables 02, and directions for specific materials
below.
Etching: See below and Material/Preparation Tables 02.

surface layers
Grain size, grain boundaries E 112, E 930, C-03,

E 1181, E 1382 T-03
Image analysis, rating of E 562, E 1245, C-03
inclusion content E 1268, E 1382
High planeness
Microhardness, hardness C 730, C 849, C 1326, C-03,
C 1327, E 384 T-03
Microstructure E 3, E 562, E 883, C-03,
E 1245, E 1268, E 1382 T-03
T-03
Porosity C-03
Sectioning
Cut-Off Wheel Diamond, metal bond, or bakelite bond
Mounting
Hot Compression Resin Epoxy with Cold Mounting Resin Epoxy

Mounting Mineral Filler
Time 9 Time 6–8 h
Minutes Minutes/Hours
Grinding
C-03: PG: If the surface is very rough, start with Dia, disk, fixed res, P120.
T-03: The PG step can often be omitted.
T-03: PG and FG 1: Often both steps or only FG 1 should be changed to bakelite
bond. Also conventional diamond disks, preferably with bakelite bond can be
Polishing
Tungsten carbide: C-03: FG 2 can be omitted, P 1 can be changed to a napless,

hard, wov silk cloth and a P 2 step from Method C-02 can be included before the
final step 共see also Method C-67兲.

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 P1 P2
Polishing
Disk/Cloth Dia, disk, RCD, hard RCD, Cloth, Cloth,
fixed, res soft napless, napless,
hard, soft,
wov, syn porous,
syn
Abrasive Type Diamond Dia, spr or Dia, spr or Dia, spr or Silica
susp susp susp
Grit or Grain P220 9 3 3 0.04/ 0.05
Size ␮m
Lubricant Type Water Alco or wat Alco or wat Alco or wat
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp Comp Comp Contra
contra
Force per 35 共8兲 35 共8兲 35 共8兲 25 共5.5兲 10 共2.2兲
Specimen N 共lb兲
Time Until plane 5–6 10–15 8–10 2
Minutes

Section 13.2.2.兲
Grinding/ FG 3 P1 P2 P3
Polishing PG FG 1 FG 2
Disk/Cloth Dia, Dia, Cloth, Cloth, Cloth, Cloth, Cloth,
pad, pad, napless, napless, napless, napless, napless,
met met v. hard, v. hard, hard, hard, soft,
wov, wov, non wov, porous,
syn syn wov, silk syn
syn
Abrasive Diamond Diamond Dia, Dia, Dia, Dia, Silica
Type spr/ spr/ spr/ spr/
susp susp susp susp
Grit or 125 40 15 9 6 3 0.04/ 0.05
Grain
Size ␮m
Lubricant Water Water Alco Alco Alco Alco
Type
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm

Contra contra contra
Specimen
N 共lb兲
Time Until 2 6–8 6–8 5–6 5–6 2
Minutes plane
Etchants
CrC, HfC, TiC, VC 909 General structure
TaC 910, 911 General structure
WC 912 General structure
Material: Silicon nitride, Si3N4
Material Properties: Si3N4: Hexagonal, 3.18 g / cm3, 1900° C 共3452° F兲, HV 800–
1900
Grinding: See Material/Preparation Tables 02.
Polishing: See Material/Preparation Tables 02.

Case or coating C-04
thickness/hardness,
surface layers
Grain size, E 112, E 930, C-04, T-04
grain boundaries E 1181, E 1382
High planeness
C 1327, E 384
E 1268, E 1382
Porosity C-04
Sectioning
Cut-Off Wheel Diamond, metal bond
Mounting
Hot Compression Resin Epoxy Cold Mounting Resin Epoxy

Mounting with Filler
Time 9 Time 6–8 h
Grinding
C-04: PG: If the surface is very rough, start with Dia, disk, fixed, res, P120.
T-04: PG with 125 ␮m diamond can often be omitted.
Polishing
C-04: P 1 can often be omitted so that FG 3 is the last step. In some cases also
FG 3 can be omitted.

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 FG 3 P1
Polishing
Disk/Cloth Dia, disk, RCD, soft RCD, soft RCD, soft Cloth,
fixed, res napless,
soft, porous,
syn
susp susp susp
Grit/Grain P220 9 3 0.25 0.04/ 0.05
Size ␮m

Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen
N 共lb兲
Time Until 7–8 7–8 6–8 1
Minutes plane

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, pad, Dia, pad, Cloth, Cloth, Cloth, Cloth,
met met napless, napless, napless, napless.
v. hard, hard, hard, soft,
non wov, non wov, porous,
syn wov, silk syn
syn
Abrasive Type Diamond Diamond Dia, spr or Dia, spr or Dia, spr or Silica
susp susp susp
Grit or 125 30 9 6 3 0.04/ 0.05
Grain
Size ␮m
Lubricant Water Water Alco or Alco or wat Alco or
Type wat wat
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen
N 共lb兲
Time Until 4 8–10 5–6 5–6 2
Minutes plane
Etchants
Si3N4 913 General structure
Si3N4 914 Grain boundaries
Si3N4 915 Grain boundaries
AlN-Al2O3 916 Grain boundaries
Material: Aluminum oxide, Al2O3. Chromium oxide, Cr2O3
Material Properties: Al2O3: Trigonal 共rhombohedral兲, 4.0 g / cm3, 2050° C

共3722° F兲, HV 2500–2800
Cr2O3: Hexagonal, 5.12 g / cm3, 2340° C 共4244° F兲, HV 2900
Grinding: See Material/Preparation Tables 02 and directions for specific materials
below.
Polishing: See Material/Preparation Tables 02 and directions for specific materials
below.

surface layers
E 1181, E 1382
High planeness
C 1327, E 384
Microstructure E 3, E 562, E 883, C-05, T-05
E 1245, E 1268, E 1382
Porosity C-05
Sectioning

Mounting
Hot Compression Resin Epoxy with Filler Cold Mounting Resin Epoxy
Mounting Time 9 Time 6–8 h
Minutes Minutes/
Hours
Grinding
T-05: The PG step with 125 ␮m diamond and FG 2 can often be omitted.
Very hard oxides: Use C-03.
Polishing
C-05: Cr2O3: The steps FG 1 and P 2 can be omitted.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, Dia, disk, RCD, Cloth, Cloth, med Cloth,
fixed, res fixed, res soft napless, nap, napless,
hard, soft, soft,
wov, syn porous,
syn syn
Abrasive Type Diamond Diamond Dia, spr Dia, spr Dia, spr Silica
or susp or susp or sup
Grit or P220 P1200 9 6 1 0.04/ 0.05
Grain Size ␮m
Lubricant Type Water Water Alco Alco Alco
or wat or wat or wat
Rotation 150/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp or Comp Comp Comp Contra
contra contra
Force per 35 共8兲 35 共8兲 35 共8兲 30 共6.6兲 25 共5.5兲 25 共5.5兲
Specimen
N 共lb兲
Time Until 1 9–10 8 2–3 1–2

Minutes plane

Section 13.2.2.兲
Polishing
Disk/Cloth Dia Dia Cloth, Cloth, Cloth, Cloth, Cloth,
pad, pad, napless, nap- napless, napless, napless,
met met v. hard less, hard, hard, soft,
wov, v. hard, non wov, porous,
syn wov, syn wov, silk syn
syn
Abrasive Diamond Diamond Dia, spr/ Dia, spr Dia, spr Dia, spr Silica
Type susp or or susp or susp
susp
Grit or 125 40 15 9 6 3 0.04/ 0.05
Grain
Size ␮m
Lubricant Water Water Alco or Alco or Alco or Alco or
Type wat wat wat wat
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Specimen
N 共lb兲
Time Until 2 6–7 6–7 5–6 5–6 2
Minutes plane
Etchants
Material Etchants 共see Tables 12.2兲 Uses
Al2O3 917 Grain boundaries
and small grains
Al2O3 918 Grain boundaries
Cr2O3 923 General structure
Material: Barium titanate, BaTiO3. Calcium oxide, CaO. Cerium
oxide, CeO2. Magnesium oxide, MgO. Silicon oxide, SiO2.
Zirconium dioxide, ZrO2. Zinc oxide, ZnO. Other oxides. Borides.
Porcelain Tile. Slag. Other traditional ceramics
CeO2: Cubic, 7.28 g / cm3
MgO: Cubic, 3.5 g / cm3, 2800° C 共5072° F兲, HV 1130
SiO2: Hexagonal, 2,2-2,65 g / cm3, 1710°C 共3100°F兲, HV 1000—1250
ZrO2: Monoclinic, 5.7– 6 g / cm3, 2690° C 共4874 °F兲, HV 1500–1900
Grinding: See Material/Preparation Tables 02 and directions for the specific
materials below.
Polishing: See below and Material/Preparation Tables 02 and directions for the
specific materials below.

surface layers
E 1181, E 1382
High planeness
C 1327, E 384
Microstructure E 3, E 562, E 883, C-06, T-06
E 1245, E 1268, E 1382
Porosity C-06
Sectioning
Cut-Off Wheel Diamond, metal bond or SiC, bakelite bond

Mounting
Minutes Minutes/
Hours
Grinding
Borides: T-06: FG 4 can be changed to grit 4000 SiC paper and P 1 can be
changed to FG 3 in C-06.
Calcium oxide: C-06: PG can be done with SiC paper grit 500, FG 1 and FG 3
can be omitted by changing FG 2 to 9 ␮m diamond.
Zirconium dioxide: The methods C-02 and C-05 can also be used. Often the step
P 3 in C-05 can be omitted.
Porcelain and traditional ceramics: The step FG 2 can be omitted and FG 3
can be prolonged to 10 min
Tile, slag: Method C-02 can be used with SiC paper grit 220 for PG and FG 1
and P 3 omitted.
T-06: FG 3 and FG 4 can be omitted if a 6 ␮m step is performed 共see below兲.
Polishing
T-06: In some cases a P 1 step with 6 ␮m diamond and a napless, hard, wov, silk
cloth should be added with further data like P 1 indicated below. In this case FG
3 and FG 4 may be omitted.
T-06: Often the step P 2 can be omitted.

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 FG 3 P1 P2
Polishing
Disk/Cloth Dia, disk, RCD, RCD, RCD, soft Cloth, Cloth,
fixed, res hard soft napless, napless,
hard, soft,
wov, porous,
syn syn
Abrasive Diamond Dia, spr or Dia, spr or Dia, spr Dia, spr or Alumina
Type susp susp or susp susp
Grit or P220 9 6 3 3 0.02/ 0.05
Grain
size ␮m
Lubricant Water Alco or Alco or Alco or Oil-wat

Type wat wat wat
Rotation 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/rpm
Comp/ Comp or Comp Comp Comp Comp Contra
Contra contra
Force per 30 共7兲 40 共9兲 35 共8兲 35 共8兲 20 共4.4兲 15 共3.4兲
Specimen
N
共lb兲
Time Until 5–6 5–6 5–6 5–6 3–5
Minutes plane

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 FG 3 FG 4 P1 P2 P3
Polishing
Disk/ SiC SiC SiC SiC SiC Cloth, Cloth, Cloth,
Cloth paper paper paper paper paper napless, napless, napless,
hard, hard, soft,
wov, wov, porous,
syn silk syn
Abrasive SiC SiC SiC SiC SiC Dia, Dia, Silica
Type spr spr
or or
susp susp
Grit or P220 P320 P500 P1200 P2400 3 1 0.04
Grain / 0.05
Size ␮m
Lubricant Water Water Water Water Water Alco Alco
Type or wat or wat
Rotation 100/150 300/150 300/150 150/150 150/150 150/150 150/150 150/150
Disk/
Holder
rpm/rpm
Comp/ Comp Comp Comp Comp Comp Comp Comp Contra
Contra or or or
contra contra contra
Force per 30 共7兲 30 共7兲 30 共7兲 30 共7兲 20 共4.5兲 25 共5.5兲 25 共5.5兲 15 共3.4兲
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 5–8 5–15 3–5
Minutes plane
Etchants
CaO 919, 920, 921, 922, 923 General structure
MgO 919, 924 General structure
Porcelain 930 General structure
ZnO 925 Grain boundaries
ZrO2 926, 927 Grain boundaries
Ba TiO3 928, 929 Grain boundaries
Material: Glasses. Optical fibers
Comments on Material: There are many different types of glass with different
chemical and physical properties. Glass can be defined as an amorphous solid. A
material is amorphous when it has no long-range order, that is, when there in no
regularity in the arrangement of its molecular constituents on a scale larger than a
few times the size of these groups. For example, the average distance between
silicon atoms in vitreous silica 共SiO2兲 is about 3.6 Å, and there is no order between
these atoms at distances above about 10 Å. A solid is a rigid material that does not
flow when it is subjected to moderate forces. This definition is not totally agreed
upon. In the ASTM standard for glass, the material is described as “glass is an
inorganic product of fusion which has been cooled to a rigid condition without
crystallization.” This description is based on the fact that most glass is made by
cooling a liquid in such a way that it does not crystallize. The difficulty with this
view is that glasses can be prepared without cooling from the liquid state. Glass
coatings are deposited from the vapor or liquid solution, sometimes with chemical
reactions. Sodium-silicate glass made by evaporation and baking is
indistinguishable from sodium-silicate glass made by cooling from the liquid.
The main types of glass and their used are: Soda lime 共containers, windows, lamp
bulbs兲, pyrex borosilicate 共headlamps, cookware, laboratory ware兲 vitreous silica
共semiconductor crucibles, lamps, optical components, optical fibers兲, alkali lead
共lamp tubing, sealing兲, “E” lime aluminosilicate 共fibers兲, lime magnesia
aluminosilicate 共high temperatures, cookware兲.
Optical fibers are coated strands of optically pure glass with a thickness of
9 – 62.5 ␮m that carry digital information over long distances. They are also used
in medical imaging and mechanical engineering inspection.
Preparation of glass is not difficult; if planeness is important, the use of Method
C-07 should be preferred. Glass being a very brittle material can be prepared by
lapping 共see Section 6.7.7兲 and Method T-39. As the surface of glass is softened by
water, this liquid should be used to carry the lapping abrasive to obtain the highest
removal rate. Also at polishing a hydrated layer is formed by chemical reaction
and the process can be described as chemical mechanical polishing 共CMP兲, the
polishing abrasive only removing the soft reaction layer 共see Section 7.12兲.
Sectioning: Wet abrasive cutting with a diamond metal bond cut-off wheel
preferably on a precision cut-off machine. Because of the brittleness of the glass,
the feed rate should be low and the use of a thin cut-off wheel should be
preferred. In the case of examination of a coating, the area to be examined should
be under compression when the cut-off wheel enters the work piece 共see also
Material/Preparation Tables 08–10兲.
Mounting: In general, hot compression mounting cannot be recommended due to
the risk of cracking because of the pressure and thermal cycle in the mounting
press. If considered possible, the hot compression mounting should be with epoxy
with a filler to obtain a high hardness of the mounting material. Cold mounting
can be with acrylics 共with a filler兲, epoxy, and polyester.
Grinding: Most glasses can be ground with SiC grinding paper. As an alternative,
diamond disks with fixed abrasives in a resin bond should be used combined with
an RCD 共see Method C-07兲 if a very plane surface is needed. Also lapping 共see
Method T-39兲 and diamond lapping film can be used 共see Section 6.7.6兲.
Polishing: Polishing can be done with diamond, silica, and alumina. The methods
mentioned below may be extended as indicated. To increase the CMP, an acidic
suspension can be used for the final polishing step by adding a few drops of nitric
acid.
Etching: Normally glasses are not etched.
Purpose 共alphabetic兲: ASTM Standard 共See Section 12.4兲 Methods

thickness/hardness,
surface layers
Image analysis, rating of C-07
inclusion content
High planeness
Microhardness, hardness C 730 C-07, T-07
Microstructure C-07, T-07
Porosity C-07
Sectioning
Mounting
Hot Compression Resin Cold Mounting Resin Acrylics/Epoxy

Mounting Time Time 6 – 10 min/ 6 – 8 h
Grinding
C-07: FG 1 can be omitted and FG 2 changed to 9 ␮m diamond. In this case two

polishing steps are added 共see below兲.
Medium hard materials: C-07: PG can be changed to SiC paper grit 500
followed by the three steps mentioned above and below.
Polishing
C-07: A polishing step like P 1 in Method T-07 can be added. If FG 1 is omitted

and FG 2 is changed as mentioned above, two polishing steps, P 1 from C-06 and
P 1 from T-07 are added.
T-07: A step like P 2 in Method T-06 can be used between FG 4 and P 1 to secure
a good edge retention. A few drops of HNO3 can be added to the final polishing
step 共see above兲.

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2
Polishing
Disk/Cloth Dia, disk, Dia, disk RCD, soft
fixed, res fixed, res
Abrasive Type Diamond Diamond Dia, spr, or susp
Grit or Grain size ␮m P220 P1200 1
Lubricant Type Water Water Wat
Rotation Disk/Holder 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp Comp Comp
Force per Specimen N 共lb兲 30 共7兲 30 共7兲 35 共8兲
Time Until plane 3–5 7
Minutes

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 FG 3 FG 4 P1
Polishing
Disk/Cloth SiC paper SiC paper SiC paper SiC paper SiC paper Cloth,
napless,
soft,
porous
syn
Abrasive Type SiC SiC SiC SiC SiC Silica
Grit or P320 P400 P800 P1000 P4000 0.04/

Grain Size 0.05
␮m
Lubricant Water Water Water Water Water
Type
Rotation 300/ 150 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp Comp Comp Comp Comp Contra
Force per 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 15 共3.4兲
Specimen N
共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 2
Minutes plane
Material: Anodized coatings. CVD coatings. PVD Coatings
Material Properties: See below.
Comments on Material: Anodizing is used for surface treatment of aluminum
products. The work piece is placed as an anode in an electrolytic bath, and an
aluminum oxide layer is developed. It consists of a solid layer of typically
0.005– 0.04 ␮m towards the work piece and further a layer with pores 5 – 25 ␮m
thick.
Solid aluminum oxide has a hardness in the range of 2000 HV, the hardness of the
porous layer is normally higher than 1000 HV. Hard anodizing is performed at low
temperatures around 5 ° C 共41° F兲 and gives a coating with few small pores and
thickness up to 50– 100 ␮m. Anodizing is mainly used for decorative finishing and
protection against wear and corrosion. Metallographic/materialographic
examination is mainly made for measurement of the thickness, microhardness,
and the quality of the coating.
Chemical vapor deposition 共CVD兲 is a method of forming dense structural parts or
coatings using the decomposition of relatively high vapor pressure gases. Coatings,
which are the most common application of CVD, generally fall into one of two
categories, electronic materials or protective coatings, and are applied either as
conversion coatings or as deposited coatings. Conversion coatings involve the
surface formation of a compound where one of the elemental components is
already present on the surface. At deposited coatings all the elemental constituents
of the coating comes from the vapor phase Protective coatings are deposited onto
a work piece 共substrate兲 to provide wear, corrosion or erosion protection, or both.
A high number of materials, metals, and ceramics can be used for coatings.
Metallographic/materialographic examination includes the purposes mentioned
above and the adhesion between coating and work piece 共substrate兲.
Physical vapor deposition 共PVD兲 is a method of depositing a coating using a

vacuum chamber and an electric current between the material source and the
work piece. The material source can consist of any electrically conductive metal.
The coating has a thickness of 3 – 5 ␮m and the hardness can go up to 5000 HV
using AlTiN as the coating material. Used coating materials are Cr, CrN, Ni, Ag, Ti,
TiAlCN, TiCN, AlTiN, TiO, TiN, and ZrN. The coatings are made for corrosive
protection, decoration, high hardness, improved wear resistance, and reduced
friction.
The metallographic/materialographic examination includes the purposes
mentioned above.
Sectioning: It is important that the cutting takes place perpendicular to the
surface to be prepared. If the plane of the cross section is not perpendicular to the
plane of the coating, the measured thickness will be greater than the true
thickness. For example, an inclination of 10° will contribute a 1.5 % error.
The cutting should preferably take place on a precision cut-off machine using the
thinnest possible cut-off wheel with a bakelite bond, the wheel suited for the work
piece material, not the coating material. The wheel speed should be in the range of
25 m / s 共82 ft/ s兲. Diamond cut-off wheels should only be used for very hard work
piece materials like ceramics. It is very important that the cut-off wheel is entering
the work piece through the coating at the area later to be examined so that the
coating is compressed into the work piece. This reduces the risk that the true
condition of the coating 共adherence to substrate material兲 is disturbed. For this
reason also the feed speed should be low.
If shearing is used for sectioning of plate material, the grinding time should be
prolonged to remove damaged material and possible cracks between base material
and coating caused by the shearing 共see Section 2.7.3兲
Mounting: It is very important that edge rounding and gaps between sample and
mounting material are avoided. Therefore, a mounting material without shrinkage
should be used, preferably epoxy. On very hard coatings hot mounting with epoxy
with a filler should be preferred if heat and pressure can be tolerated.
Also a phenolic resin with carbon fibers can be of advantage. In hot mounting a
special application can be made to secure the edge: Tightly wrap up the specimen
in Al-foil 共household type兲. This gives a good separation between mounting
material and coating. Choose a mounting material with hardness as close as
possible to the hardness of the coating. As an alternative cold mounting with
epoxy can be used, and in case of porosity, vacuum impregnation can be an
advantage 共see Section 3.10兲.
Grinding: The preparation process should secure the highest possible edge
retention. This means that all grinding, either on SiC grinding paper or rigid
composite disks 共RCDs兲, should be as short as possible.
Polishing: Also the polishing steps should be kept as short as possible.
Etching: For most examinations no etching is needed.

Case or coating B 487, B 578, B 681, B 748 C-08
thickness/hardness,
surface layers
Grain size, grain boundaries B 390, E 112, E 930, C-08, T-08
E 1181, E 1382
Heat influenced zone C-08, T-08
Image analysis, rating E 562 C-08
of inclusion E 1245, E 1268, E 1382
content
High planeness
Microhardness, hardness B 578, C 730, C 849, C-08, T-08
C 1326, C 1327, E 10,
E 18, E 92, E 103,
E 110, E 140, E 384,
E 448
Microstructure E 3, E 407, E 883 C-08, T-08
Porosity C-08, T-08
Sectioning
Cut-Off Wheel Bakelite, Al2O3 or SiC depending on the work piece

共substrate兲 material 0.5 mm 共0.019 in兲 thickness
Mounting
Minutes Minutes/
Hours
Grinding
C-08, T-08: If possible make PG step with SiC paper grit 500.
C-08: FG 1 and FG 3: Often these two steps can be omitted.
C-08: For CVD coating and PVD coatings on a hard substrate change PG and FG
1 to PG from Method C-09.
C-08: For preparation of CVD and PVD coatings, use shortest times stated.
Polishing
C-08: For preparation of anodized coatings, the P 1 step can be changed to a

napless, hard, wov, silk cloth.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper Sic paper RCD, soft RCD, soft Cloth, Cloth,
napless, napless,
hard, soft,
wov, syn porous,
syn
Abrasive Type SiC SiC Dia, spr or Dia, spr Dia, spr Silica
susp or susp or susp
Grit/Grain P320 P500 9 3 3 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Alco or Alco or Wat-oil
wat wat
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen
N 共lb兲
Time Until 0.5–1 3–8 3–7 1.5–5 0.5–1
Minutes plane

Section 13.2.2.兲
Polishing
paper paper paper paper napless, napless, napless,
hard, hard, soft,
non wov, porous,
wov, syn syn
syn
Abrasive SiC SiC SiC SiC Dia, Dia, Silica
Type spr spr
or or
susp susp
Grit or P220 P320 P500 1200 6 3 0.04/ 0.05

Grain
Size ␮m
Type wat wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
r/min/r/min
Contra or or or
Force per 25 25 25 25 20 共4.3兲 20 共4.3兲 10 共2.3兲
Specimen 共5.7兲共5.7兲共5.7兲共5.7兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 3–5 2–5 0.5–1
Minutes plane
Material: Electrolytically deposited coatings: Galvanization,
plated coatings, other coatings. Diffusion coatings. Other
coatings

Comments on Material: Electrolytically deposited coatings are produced by
electrolysis, the work piece 共substrate兲 placed as a cathode in an electrolyte with
an anode of the coating material. In galvanization, zinc is used as the coating
material and in electroplating 共plating兲 other metals like chrome may be used. For
Zn coatings also see Material/Preparation Tables 10.
Diffusion coating is a process in which the work piece is either coated with
another material and heated to a sufficient temperature in a suitable environment
or exposed to a gaseous or liquid medium containing the other material, causing
diffusion of the coating material into the work piece surface resulting in a change
of the composition and properties of the surface 共see also Material/Preparation
Tables 37兲.
An example of other coatings is electroless plating in which metal ions in a dilute
aqueous solution are plated out on the work piece by means of an autocatalytic
chemical reduction.
Typical examples of metallographic/materialographic examination of coatings are
the layer thickness, porosity of coating, cracks, adherence to base material, and
the diffusion zone between substrate 共work piece兲 and coating.
Mounting: See Material/Preparation Tables 08. As an alternative to epoxy for cold
mounting, acrylics with a filler can be used.
Polishing: See Material/Preparation Tables 08. For zinc coatings, see Material/
Preparation Tables 10.
Etching: For most examinations, etching is not needed, but an etchant for Sn
coating on steel is stated below and etchants for Zn coatings are stated in Material/

Case or coating B 487, B 587, B 748, B 931, B 933, B 934 C-09
thickness/hardness
surface layers
Grain size, grain boundaries B 390, E 112, E 930, E 1181, E 1382 C-09, T-09
Image analysis, rating E 562, E 1245, E 1268, E 1382 C-09
of inclusion
content
High planeness
Micohardness, hardness B 578, C 730, C 849, C 1326, C-09, T-09
C 1327, E 10, E 18, E 92, E 103,
E 110, E 140, E 384, E 448
Porosity C-09, T-09
Sectioning
Cut-Off Wheel Al2O3 or SiC according to base material, bakelite

bond, 0.5 mm 共0.019 in兲 thickness
Mounting
Hot Compression Resin Epoxy Cold Mounting Resin Epoxy

Mounting Time 8–10 Time 6–8 h
Grinding
Plated coatings: C-09: Use SiC paper grit 500 for PG.
Diffusion coatings: C-09: FG 1: RCD, soft can be changed to a napless v. hard,
wov, syn cloth.
C-09: PG: SiC paper grit 220 or grit 320 can be used instead of a diamond disk.
C-09: For some Zn coatings where water sensitivity is suspected, diamond spray
and alcohol-based lubricants are preferred at the step FG 1 and P 1. If silica in P
2 is too alkaline use alumina, pH 7-7.5.
C-09: P 2: For sensitive layers this step can be changed to a napless, hard, wov,
silk cloth with 1 ␮m diamond spray and alcohol-based lubricant.
When the difference is more than 100– 150 ␮m
between the center and the periphery, the disk is either discarded or trued.
Polishing
C-09: A step like P 3 in Method T-17 can be added before the final step.

Section 13.2.2.兲
Grinding/ PG FG 1 P1 P2
Polishing
Disk/Cloth Dia, disk, RCD, Cloth, Cloth,
hard, soft,
wov, syn porous,
syn
Abrasive Type Diamond Dia, spr Dia, spr Silica
or susp or susp
Grit/Grain Size ␮m P220 9 3 0.04/ 0.05
Lubricant Type Water Alco or wat Alco or wat
Rotation Disk/Holder 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp or Comp Comp Contra
contra
Force per Specimen N 共lb兲 25 共5.7兲 25 共5.7兲 25 共5.7兲 15 共3.4兲
Time Until plane 3–5 3–5 0.5–1
Minutes

Section 13.2.2.兲
Grinding/ PG FG 1 Fg 2 FG 3 P1 P2
Polishing
Disk/Cloth SiC SiC SiC SiC Cloth, Cloth,
paper paper paper paper napless, napless,
hard, soft,
wov, porous,
syn syn
Abrasive Type SiC SiC SiC SiC Dia, spr Silica
or
susp
Grit or Grain Size ␮m P220 P320 P500 P1200 3 0.04/ 0.05
Lubricant Type Water Water Water Water Wat-oil
Rotation Disk/Holder 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
or or or
Force per Specimen 30 共7兲 30 共7兲 30 共7兲 30 共7兲 30 共7兲 15 共3.4兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 2–3 1
Minutes plane
Etchants
Material Etchants 共see Table Uses
12.2兲
Sn coating on steel 183 General structure
Zn coatings, see M/PT-10
Material: Hot dip zinc coatings. Other Zn coatings

Comments on Material: In hot dipped zinc coating the work piece is dipped into
molten zinc. This is a very efficient way to apply a sufficient thickness of zinc to
obtain a very good corrosion protection.
Other Zn coatings include electrolytically deposited coatings mentioned in Material/
Preparation Tables 09, and the below stated methods should be seen as
alternatives to Methods C/T-09.
The metallographic/materialographic examination of Zn coatings includes
thickness measurement of the coating, adhesion of coating to base material,
microstructure of base material, and coating and failure analysis like cracks in the
coating.
Mounting: See Material/Preparation Tables 08. It is very important that mounting
is done without gaps between sample and mounting material because the water
sensitive zinc is strongly influenced by water bleeding from the gap. Degrease the
specimen in acetone before mounting. Place the specimen in clips to keep it
upright. Use epoxy for cold mounting or bakelite with a carbon filler for hot
mounting. In case of having many pieces of coated sheets in the same mount,
gluing the sheets together with instant glue and hot mounting give good results
without bleeding of liquid from the gaps between the sheets.
Grinding: Pure zinc is very soft and sensitive to water. The purer the zinc of the
coating is, the softer and the more water-sensitive it becomes. Therefore, plain, hot
dipped, and electrolytically deposited coatings are soft and prone to mechanical
deformation and they cannot be cleaned with water. Ethanol or isopropanol
should be used for cleaning. It is important that the grinding steps are properly
performed to avoid excessive damage that is very difficult to remove during the
polishing.
Polishing: Water-free suspensions and lubricants should be used for polishing of
zinc coatings. The polishing can be finished with a cleaning step 共see below兲.
Etching: Etching times should be short and concentration of etchant low to avoid
over-etching 共see below兲.

Case or coating thickness/hardness, B 487, B 578, B 748 C-10
surface layers
Grain size, grain boundaries E 112, E 930, E 1181, E 1382 C-10, T-10
Image analysis, E 562, E 1245, E 1268, E 1382 C-10
rating of inclusion
content
High planeness
Microhardness, hardness B 578, C 730, C 849, C 1326, C-10, T-10
C 1327, E 10, E 18, E 92,
E 103, E 110, E 140, E 384,
E 448
Porosity C-10, T-10
Sectioning
Cut-Off Wheel Al2O3 or SiC according to base material, bakelite

Mounting
Hot Compression Resin Bakelite with Cold Mounting Resin Epoxy

Mounting Carbon Filler
Time 8–10 Time 6–8 h
Minutes Minutes/
Hours
Grinding
Polishing
C-10: P 1 can be changed to a hard silk cloth as used in P 2 and P 3 can be

omitted.
C-10 and T-10: The polishing can be finished with a cleaning step 共see P 3 in
Method C-10兲. This is to avoid contact with water to the finished surface. For all
other cleaning alcohol should be used.
In the case of very sensitive Zn coatings, water free suspensions and lubricants
should be used with Method C-10.

Section 13.2.2.兲
Grinding/ PG FG 1 P1 P2 P3
Polishing
Disk/Cloth SiC paper RCD, soft Cloth Cloth, Cloth,
napless, napless, napless,
hard, hard, soft,
wov, syn wov, porous,
silk syn
Abrasive Type SiC Dia, spr or Dia, spr or Dia, spr or See
susp susp susp above
Grit/Grain Size ␮m P320 9 3 1
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp Comp Comp Comp
contra
Force per 30 共7兲 30 共7兲 25 共5.7兲 20 共4.5兲 10 共2.2兲
Specimen N 共lb兲
Time Until plane 4 4–6 4–6 15– 20 s
Minutes

Section 13.2.2.兲
Grinding/ PG FG 1 Fg 2 FG 3 P1 P2
Polishing
hard, wov, med
silk hard,
wov,
wool
Abrasive Type SiC SiC SiC SiC Dia, spr or Dia,
susp spr or
susp
Grit or P220 P320 P500 P1200 3 1
Grain
Size ␮m
Lubricant Water Water Water Water Alco Wat-oil
Type
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp or Comp or Comp Comp Comp
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 4–6 1–2
Minutes plane
Etchants
Zn-Fe 74a Structure of galvanized sheet
Material: Paint layers
Comments on Material: Paint layers can be very different, either charged directly
on the base material of the work piece or on a coating.
The metallographic/materialographic examination includes measurement of layer
thickness, adhesion to work piece surface, and failures in the paint.
Sectioning: Sectioning shall take place as mentioned for coatings, see Material/
Grinding: See Material/Preparationn Tables 08.
Polishing: See Material/Preparation Tables 08. The paint coat normally is very soft
compared to the base material. This increases the risk of edge rounding and the
polishing times should be kept to a minimum, depending on the base material.
Etching: For etching, an etchant suited for the base material should be used.

Case or coating B 487, B 578, B 748 C-11
thickness/hardness,
surface layers
E 1181, E 1382
Image analysis, rating E 562, E 1245, C-11
of inclusion content E 1268, E 1382
High planeness
C 1326, C1327, E 10,
E 18, E 92, E 103,
E 110, E 140, E 384,
E 448
Porosity C-11, T-11
Sectioning
Cut-Off Wheel Al2O3 or SiC, bakelite bond, 0.5 mm 共0.019 in兲

thickness
Mounting
Hot Compression Resin Bakelite or Epoxy Cold Mounting Resin Epoxy

Minutes Minutes/
Hours
Grinding
T-11: FG 1: This step with grit 320 is only needed at hand preparation.
Attention: In C-methods, when using RCD: The disk concave during use. When
the diffenence is more than 100– 150 ␮m between the center and the periphery,
the disk is either discarded or trued.
Polishing
C-11: P 2 can changed to step P 2 in Method T-11.

T-11: P 2 can be changed to P 2 in Method C-11.
Contemporary Method C-11 共For definitions of parameters and consumable see

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper SiC paper RCD, soft Cloth, Cloth,
napless, napless,
hard, soft, porous,
wov, silk syn
Abrasive Type SiC SiC Dia, spr Dia, spr Silica
or susp or susp
Grit or Grain 220 500 9 3 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Alco or Alco or wat
wat
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen
N 共lb兲
Time Until 0.5–1 4–6 2–6 1
Minutes plane
Traditional Method T-11 共For definition of parameters and consumables see

Section 13.2.2.兲
Polishing
hard, med
wov, hard,
syn wov,
wool
Abrisive Type SiC SiC SiC SiC
Dia, spr Dia, spr
or susp or susp
Grit or Grain Size ␮m P320 P500 P1200 P4000 3 1
Lubricant Water Water Water Water Alco or Wat-oil
Type Wat
Rotation Disk/Holder 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150
rpm/rpm
Comp/Contra Comp Comp Comp Comp Comp Comp
or
contra
Force per Specimen 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 15 共3.4兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 2–5 1–3
Minutes plane
Material: Thermal spray coatings: Flame, HVOF „High Velocity
Oxygen Fuel… and other coatings

Comments on Material: Thermal spraying is a group of processes in which finely
divided metallic or nonmetallic surface materials are deposited in a molten or
semimolten condition on a substrate to form a spray deposit. The surfacing
material may be in the form of powder, rod, cord, or wire. A common feature of
all thermal spray coatings is their lenticular grain structure resulting from the
rapid solidification of small globules, flattened from striking a cold surface at high
velocities.
Flame spraying or the combustion wire thermal spray process is basically the
spraying of molten metal 共ceramics and cements can be used in rod or composite
form兲 onto a surface to provide a coating.
Material in wire form is melted in a flame and atomized using compressed air to
form a fine spray. This flame spray process is called a “cold process” 共relative to
the work piece material being coated兲, as the substrate 共work piece兲 temperature
can be kept low during the processing, avoiding damage, metallurgical changes,
and distortion to the substrate material. Flame spraying is used for improvement
of wear resistance, etc., at machine elements and for anticorrosion coatings.
HVOF/HVAF 共high velocity oxygen fuel/high velocity air fuel兲 and LVOF 共low
velocity oxygen fuel兲 are spraying processes using material in powder form which
is melted in a flame to form a fine spray. In HVOF the spray velocity is extremely
high and the coatings are very dense, strong, and show low residual tensile stress
or in some cases compressive stress. This enables very much thicker coatings to be
applied than possible with other spray processes.
Metallography/materialography is used for examination of a number of features,
decisive for the quality of the coating, described below.
Bond: The bonding at the thermal spray coating/substrate interface and between
the particles in the spray coating should be such that both mechanical interlocking
and diffusion bonding occur. A number of factors like cleanliness, temperature,
time, velocity, and physical/chemical properties influence the bonding.
Microstructure: The coatings show lamellar or flattened grains appearing to flow

parallel to the substrate. The structure is heterogeneous that is due to the
variations in the condition of the individual particle on impact. An important
feature is the presence of unmelted particles and also whether the coating contains
some porosity.
Porosity: This is present in most thermally sprayed coatings due to a lack of fusion
between sprayed particles or the expansion of gases generated during the spraying
process. A porosity of 1 to 25 % is normal but can be influenced by changes in
process and materials.
Linear detachment: Cooling and solidification of most materials is accompanied by
contraction or shrinkage. This generates a tensile stress within the particle and a
compressive stress within the surface of the substrate. As the coating is built up,
so are the tensile stresses in the coating. At a certain point the thickness will be
reached while the tensile stresses will exceed that of the bond strength or cohesive
strength and linear detachment will occur.
Oxides: Most metallic coatings suffer oxidation during normal thermal spraying in
air. The products of oxidation are usually included in the coating. Oxides are
generally much harder than the coating metal. Oxides in coatings can be
detrimental towards corrosion, strength, and machinability. During metallographic/
materialographic examination it is important to be able to discriminate between
oxides and pores 共voids兲. Other features to be examined are coating thickness,
hardness, and microhardness.
Metallographic/materialographic preparation: Preparation of thermal spray
coatings is more difficult than the average specimen. This is due to the difference
in coating material and substrate 共work piece兲 material, the complicated nature of
the coating, etc. All stages in the preparation process should be carefully executed
to obtain a sufficient result; a special problem is to reveal the true porosity 共see
Section 13.6.4, “Pull-Outs—False Porosity”兲. As the preparation process has this
very important influence on the microstructure, it is important that a systematic
and reproducible process is maintained. The preparation process is described
below, and two ASTM standards cover specifically the preparation and
examination of thermal sprayed coatings:
Standard Guide for Metallographic Preparation of Thermal Sprayed Coatings 共E
1920兲 and Test Method for Determining Area Percentage Porosity in Thermal
Sprayed Coatings 共E 2109兲.
Sectioning: Care must be exercised to avoid affecting the soundness of the coating
and the interface between the coating and the substrate. Friable, porous, or brittle
coatings may be vacuum impregnated with epoxy before sectioning to protect the
specimen 共see Section 3.10兲. Specimens should always be sectioned such that the
coating is compressed into the substrate. If the coating or interface is placed under
tension, it may cause the coating to be pulled away from the substrate or result in
delamination of the coating. If a part of the specimen has been under stress, this
part should not be included in the examination of the specimen. Sectioning
methods creating strong damage to the specimen, even wet cutting with a normal
cut-off wheel, should be avoided. Preferably precision cutting should be used with
the thinnest possible cut-off wheel, using Al2O3 or SiC in a bakelite bond
according to the substrate material. Only in case of very thick ceramic layers a
diamond wheel should be used. The cut-off wheel speed should be in the range of
25 m / s 共82 ft/ s兲 and the feed speed should be low to minimize the damage.
should be used, preferably epoxy. At very hard coatings hot mounting with epoxy
with a filler should be preferred if heat and pressure can be tolerated. Also, a
phenolic resin with carbon fibers can be an advantage. However, only cold
mounting with epoxy should be used in the initial determination of the true
characteristics of a coating before considering the use of any other mounting
material because hot mounting might influence the microstructure. As a rule hot
mounting should only be used for mounting of dense, nonfriable coatings with
substrates a minimum of 1.5 mm 共0.06 in兲 thick. Choose a mounting material with
hardness as close as possible to the hardness of the coating. In case of porosity,
vacuum impregnation can be required 共see Section 3.10兲 and often the use of a dye
can be of advantage 共see Section 3.10.1兲.
Grinding: Grinding may have a strong influence on the edge retention and a
number of artifacts like false porosity and smearing 共see below兲. Due to the many
different types of thermal coatings and substrate materials, the grinding sequence
will vary, but it should be possible to find a useable method among the methods
described in the Material/Preparation Tables 12–15.
Polishing: It is very important to evaluate the type of coating and substrate before
the start of the preparation because of the high variety of coatings and substrate
materials. Two important features are whether one or more of the components in
the microstructure are brittle or ductile. In case of a brittle component, often
pull-outs will take place during the grinding, causing a “false porosity” that can
only be removed with a prolonged polishing. In case of a ductile component this
might be smeared into the existing pores 共voids兲 and a too dense microstructure
might appear. To avoid this the use of SiC grinding paper should be reduced and
grinding on rigid composite disks 共RCDs兲 or very hard cloths followed by at least
two polishing steps should be used. See Section 13.6.4, “Pull-Outs—False Porosity,”
where a number of thermal spray coatings are shown.
Etching: The thermally sprayed coating is usually not etched, but etchants for the
substrate material can be used, mentioned under this material.

Case or coating B 487, B 748 C-12
thickness/hardness,
surface layers
Grain size, grain E 112, E 930, E 1181 C-12, T-12
boundaries
Image analysis, rating E 45, E 562, E 768, C-12
content
High planeness
Microhardness, B 578, C 730, C 849, C-12, T-12
hardness C 1326, C 1327, E 10,
E 18, E 92, E 103,
E 110, E 140, E 384, B 448
E 768, E 883, E 1245,
E1920
Porosity E 2109 C-12
Thermal spray coatings: E 1920, E 2109 C-12, T-12
Distribution, porosity,
unmelted particles
Sectioning

thickness
Mounting
Hot Compression Resin Epoxy or Bakelite Cold Mounting Resin Epoxy

Minutes Minutes/
Hours
Grinding
Polishing
C-12: At certain thermal spray coatings where longer polishing times are needed,
the P 1 step can be changed to diamond with grain size 6 ␮m and the P 1 and P
2 steps shown will be “P 2” and “P 3.”

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, Dia, disk RCD, Cloth, Cloth,
fixed, res fixed, res soft napless, napless,
hard, wov, soft,
syn porous,
syn
Abrasive Type Diamond Diamond Dia, spr or Dia, spr or Alumina
susp susp
Grit/Grain Size ␮m P220 P1200 9 3 0.02/ 0.05
Lubricant Type Water Water Alco or wat Alco or wat
Rotation Disk/Holder 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
rpm/rpm
contra
Force per 25 共5.7兲 30 共7兲 30 共7兲 25 共5.7兲 10 共2.2兲
Specimen N 共lb兲
Time Until plane 2 5–7 4–6 1
Minutes

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 FG 3 FG 4 P1 P2
Polishing
Disk/Cloth SiC SiC SiC SiC SiC Cloth, Cloth,
paper paper paper paper paper napless, med.
hard, nap,
wov, syn soft,
syn
Abrasive SiC SiC SiC SiC SiC Dia, spr Dia, spr
Type or susp or susp
Grit or P220 P320 P500 P1200 P2400 3 1
Grain Size
␮m
Lubricant Water Water Water Water Water Alco or Alco or
Type wat wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Contra or or or
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 3 0.5–1
Minutes plane
Material: Plasma spray coatings: Metallic layers
Comments on Material: Plasma spraying is a thermal spraying process in which a
nontransferred arc is utilized as the source of heat that ionizes a gas that melts
and propels the coating material to the work piece 共substrate兲. Compared to
combustion 共flame兲 spraying the plasma spraying provides rapid heating, low
particle flight time, more inert flame and higher velocity, resulting in a finer,
denser microstructure with less oxide inclusions. For further information see
Material/Preparation Tables 12.
Etching: See Material/Preparation Tables 12.

thickness/hardness,
surface layers
Grain size, grain boundaries E 112, E 930, E 1181 C-13, T-13
Image analysis, E 45, E 562, E 768, E 1245, C-13
rating of inclusion E 1382, E 2109
content
High planeness
Microhardness, B 578, C 730, C 849, C 1326, C-13, T-13
hardness C 1327, E 10, E 18, E 92,
E 103, E 110, E 140, E 384, E 448
E 768, E 883, E 1245,
E 1920

Distribution, porosity,
unmelted particles
Sectioning

thickness
Mounting

Minutes Minutes/
Hours
Grinding
C-13: PG: Grit 320 should be used if possible.

Polishing
C-13: P 2: Can be changed to P 2 from Method T-12.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper RCD, soft RCD, Cloth, Cloth,
soft napless, napless,
hard, soft,
wov, porous,
silk syn
Abrasive Type SiC Dia, Dia, Dia, Silica
spr or spr or spr or
susp susp susp
Grit/Grain P220 9 3 3 0.04/ 0.05
Size ␮m
Lubricant Water Alco or wat Alco or wat Alco or wat
Type
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Force per 25 共5.7兲 25 共5.5兲 25 共5.5兲 25 共5.5兲 10 共2.3兲
Specimen N
共lb兲
Time Until 4–6 5–7 3–4 0.5–1
Minutes plane

Section 13.2.2.兲
Polishing
paper paper paper paper paper napless, napless,
hard, soft,
wov, porous,
silk syn
Abrasive SiC SiC SiC SiC SiC Dia, spr Alumina
Type or susp
Grit or P220 P320 P550 P1200 P4000 3 0.02/ 0.05
Grain Size
␮m
Lubricant Water Water Water Water Water Alco or
Type wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp or Comp or Comp Comp Comp Contra
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 3–4 0.5–1
Minutes plane
Material: Plasma spray coatings: Ceramic layers

Comments on Material: See Material/Preparation Tables 12 and 13.
Sectioning: Depending on the substrate an Al2O3 or SiC, bakelite bond, or
diamond metal bond, 0.5 mm 共0.019 in兲 thickness cut-off wheel should be used. In
case of very brittle coatings a diamond wheel with bakelite bond should be used,
see Material/Preparation Tables 12.
Grinding: Remove at least 500 ␮m during the PG step to ensure that all damage
from the cutting is removed. Pull-outs will be developed during the grinding,
resembling pores 共see below兲.
See also Material/Preparation Tables 12.
Polishing: Polishing must be performed until the pull-outs made during the
grinding are removed. Check the porosity and go on polishing with the P 1 step
until the porosity level is constant.
See also Material/Preparation Tables 12.

thickness/hardness,
surface layers
content
High planeness
C 1326, C 1327, E 10,
E 18, E 92, E 103,
E 110, E 140, E 384,
E 448
E 768, E 883, E 1245,
E 1920
Distribution,
porosity, unmelted particles
Sectioning
Cut-Off Wheel Al2O3 or SiC, bakelite bond, or diamond metal or

bakelite bond, 0.5 mm 共0.019 in兲 thickness
Mounting
Hot Compression Resin Epoxy or Cold Mounting Resin Epoxy 共vacuum

Mounting Bakelite impregnation兲
with Filler
Minutes Minutes/
Hours
Grinding
The PG step is very important 共see above兲.

C-14, T-14: PG: At thin or brittle layers, or both, change to PG from Methods
T-13.
C-14: FG 1: For very hard ceramic layers, the disk should be changed to RCD,
hard.
Polishing
C-14, T-14: The time for the step, P 1 depends on the porosity level 共see M/PT 12兲.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, RCD, Cloth, Cloth,
fixed, res soft soft napless, napless,
hard, wov, soft,
silk porous,
syn
susp susp susp
Grit/Grain Size ␮m P220 9 3 3 0.04/ 0.05
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Force per 30 共7兲 40 共9兲 35 共8兲 35 共8兲 15 共3.4兲
Specimen N 共lb兲
Time Until 4–5 3 3–4 1
Minutes plane

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, pad, met Cloth, napless, Cloth, napless, Cloth,
v. hard, non hard, napless,
wov/wov, syn non-wov, syn soft,
porous,
syn
Abrasive Type Diamond Dia, spr or susp Dia, spr or susp Alumina
Grit or Grain Size ␮m 40 9 3 0.02/ 0.05
rpm/rpm
contra
Force per 25 共5.7兲 25 共5.7兲 25 共5.7兲 20 共4.5兲
Specimen N 共lb兲
Time Until plane 6–7 3–4 1–2
Minutes
Material: Plasma spray coatings: Composite layers
Material Properties: See Material/Preparation Tables 12 and 13.

Comments on Material: See Material/Preparation Tables 12 and 13.
Sectioning: See Material/Preparation Tables 12 and 14.
Grinding: See Material/Preparation Tables 12 and 14.
Polishing: See Material/Preparation Tables 12 and 14.

thickness/hardness,
surface layers
Grain size, grain E 112, E 930, E 1181 C-15,

boundaries T-15
Heat influenced zone C-15,
T-15
Image analysis, E 45, E 562, E 768, E 1245, C-15
rating E 1382, E 2109
of inclusion
content
High planeness
Microhardness, B 578, C 730, C 849, C 1326, C-15,
hardness C 1327, E 10 T-15
E 18, E 92, E 103, E 110,
E 140, E 384, E 448
Microstructure E 3, E 45, E 407, E 562, C-15,
E 768, E 883, E 1245, T-15
E 1920
T-15
Thermal spray E 1920, E 2109 C-15,
coatings: T-15
Distribution,
porosity, unmelted
particles
Sectioning
Cut-Off Wheel Al2O3 or SiC, bakelite bond, or diamond metal bond,

0.5 mm 共0.019 in兲 thickness
Mounting

Minutes Minutes/
Hours
Grinding
C-15: PG: For softer composites this can be changed to PG or FG 1 in Method

T-15
C-15: FG 2 and FG 3: It is important that the true level of pores is obtained at
these steps.
C-15: FG 1: If the composite layer is very hard 共ceramic兲, the disk can be
changed to RCD, hard. During the FG 2 step the level of porosities should be
evaluated, and FG 2 shall go on until the level stays constant.
T-15: If the composite layer contains hard ceramics 共⬎800 HV兲, SiC paper
should be changed to diamond pads. PG: 40 ␮m, met, FG 1: Diamond pad
10 ␮m, bak. See also Method T-14.
Polishing
C-15 and T-15: The last step can be changed to P 2 from Method T-12.
T-15: P 1 and P 2: It is important that the true level of pores is obtained at these
steps. During the P 2 step the level porosities should be evaluated, and P 2 shall
go on until the level stays constant.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk RCD, soft RCD, Cloth, Cloth,
hard, wov, soft, porous,
silk syn
susp susp susp
Grit/Grain P220 9 3 3 0.04/ 0.05
Size ␮m
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen
N 共lb兲
Minutes

Section 13.2.2.兲
Polishing
Disk/ SiC SiC SiC SiC Cloth, Cloth, Cloth,

Cloth paper paper paper paper napless, napless, napless,
v. hard, soft,
hard, wov, porous,
nonwov/ syn syn
wov,
syn
Type spr, spr
or or
susp susp
Grit or P220 P320 P500 P1000 6 3 0.04/
Grain 0.05
Size ␮m
Lubricant Water Water Water Water Alco Alco
Type or or
wat wat
Rotation 300/ 300/150 300/150 150/150 150/ 150/ 150/
Disk/Holder 150 150 150 150
rpm/rpm
Contra or
contra
Force per 30 共7兲 25 共4.5兲 25 共4.5兲 25 共4.5兲 20 20 10
Specimen 共4.5兲共4.5兲共2.2兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 15–20 10 0.5–1
Minutes plane
Material: Composites: SiC fibers in Ti matrix

Comments on Material: A composite material is characterized as consisting of
two or more different components. Depending on the bonding component used, a
distinction is made between metal matrix composites, ceramic matrix composites,
and plastic matrix composites. The intention behind a composite material is to
combine the favorable properties of various materials and, at the same time,
compensate for less favorable properties. The required combination of properties
determines the choice of materials. Another vital factor in achieving a material
with favorable properties is whether the various components “work together.” For
example, good bonding between the components is important and no
unintentional component alterations may occur during the production process. In
the area of metal matrix composites, cermets, the high hardness of ceramic
particles or the extreme strength of ceramic fibers, will typically be combined with
the toughness of the metal.
Metallographic/materialographic examination includes separation between

components, porosity, and transitions between components. Due to the very wide
variety of composite materials it is only possible to indicate six basic methods in
the Material/Preparation Tables 16 to 18, and these should be changed according
to the given material following the comments stated for each stage/step in the
preparation process.
The most common problems with the preparation of composites are related to
relief and unplaneness between the different components, often combined with
smearing of material from a soft component covering pores, etc., of the other
components.
Sectioning: Depending on the hardness of the components of the composite,
sectioning should be made as wet abrasive cutting with an Al2O3 / SiC, bakelite
bond cut-off wheel or a diamond wheel. If the bond between the components in
the composite is sufficiently high, a diamond wheel with metal bond can be used.
If the bond is not adequate or one of the components is very hard and brittle, or
both, bakelite bond should be used. The sectioning should be performed with
great care, and often it is an advantage to use a precision cutting machine for the
cutting using thin wheels 共see Material/Preparation Tables 12兲. A band saw should
only be used for cutting of a large piece, later to be cut with a cut-off wheel.
Mounting: As composite materials often have very high differences in hardness,
mounting in a relatively hard mounting material is of advantage. In the case of
porosity in one or more of the components, vacuum impregnation may be needed
共see Section 3.10兲.
Grinding: In case of very high differences in hardness, SiC grinding paper may be
less suited for grinding, removing too much material from the soft component
creating relief. In case of ceramic components, diamond disks should be used for
grinding.
Polishing: As a general rule, both grinding and polishing times should be kept as
short as possible to secure the planeness. It is important, however, that the hardest
component is correctly ground/polished at each step before going on to the next
finer step.
Etching: Etching is performed according to the components of the composite.

thickness/hardness,
surface layers
Image analysis, rating E 562, E 1245, E 1382 C-16
of inclusion content
High planeness
C 1326, C 1327, E 10,
E 18, E 92, E 103, E 110,
E 140, E 384, E 448

E 1245, E 1382
Porosity C-16
Sectioning
Mounting

Minutes Minutes/
Hours
Grinding
The material is relatively difficult to prepare because of the very hard SiC and
the relatively soft and tough Ti. It is important that the SiC phase is “finished” in
each step, before going to the next finer step.
Polishing
Ti may be chemically-mechanically polished: C-16: P 2 and T-16: P 3: Use the

solution: 96 mL silica, 2 mL H2O2 共30 %兲, 2 mL NH3 solution 共25 %兲.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk Dia, disk RCD, RCD, Cloth, Cloth,
fixed, res fixed, res soft soft napless, napless,
hard, wov, soft,
silk porous,
syn
Abrasive Type Diamond Diamond Dia, spr Dia, spr Dia, spr Silica
orsusp or susp orsusp See note
Grit/Grain P220 P600 9 3 1 0.04/ 0.05
Size ␮m
Lubricant Water Water Alco or Alco or Alco or

Type wat wat wat
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen N
共lb兲
Time Until 2 4 5 3 1
Minutes plane

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, Dia, Cloth, Cloth, Cloth,
pad, pad, napless, napless, napless,
met bak v. hard, hard, soft,
nonwov/ wov, porous,
wov, syn silk syn
Abrasive Type Diamon Diamond Dia, spr or Dia, spr or Silica
susp susp See note
Grit or Grain 40 10 6 1 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Alco or wat Alco or wat
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Force per 30 共7兲 25 共4.5兲 20 共4.5兲 20 共4.5兲 10 共2.2兲
Specimen
N 共lb兲
Time Until plane 3 5 3 1–2
Minutes
Material: Composites: Glass fiber reinforced plastic
Comments of Material: See Material/Preparation Tables 16. No “contemporary”
method is developed for this kind of material, instead, Method C-17 describes a
method using SiC grinding paper. See also the Material/Preparation Tables 64 and
65 covering polymers.


Case or coating C-17, T-17
thickness/hardness,
surface layers
Image analysis, rating E 45, E 562, E 768, C-17, T-17
of inclusion E 1245, E 1382
content
High planeness
Microhardness, hardness B 578, C 730, C849, C 1326, C-17, T-17
C 1327, E 10, E 18, E 92,
E 103, E 110, E 140, E 384,
E 448
Microstructure E 3, E 45, E 407, E 562, E 768, C-17, T-17
E 883, E 1245
Porosity C-17, T-17
Sectioning
Cut-Off Wheel Al2O3 or SiC, bakelite bond or diamond, metal bond

or bakelite bond
Mounting
Hot Compression Resin Cold Mounting Resin Epoxy

Mounting Time Time 6–8 h

Section 13.2.2.兲
Polishing
Disk/Cloth SiC SiC Cloth, Cloth, Cloth,

paper paper napless, napless, napless,
hard, wov, medium soft,
syn hard, porous,
wov, wool syn
Abrasive Type SiC SiC Dia, spr Dia, spr Silica
orsusp orsusp
Grit/Grain P220 P1200 3 1 0.04/ 0.05
Size ␮m
Lubricant Water Water Alco or Alco or
Type wat wat
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen
N 共lb兲
Time Until 0.5–1 3–5 3 1
Minutes plane

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 P1 P2 P3 P4
Polishing
Disk/Cloth SiC SiC SiC Cloth, Cloth, Cloth, Cloth,
paper paper paper napless, napless, napless, napless,
hard, hard, hard, soft,
wov, silk wov, silk wov, porous,
silk syn
Abrasive Type SiC SiC SiC Dia, spr Dia, spr Dia, spr Silica
Grit or P220 P320 P500 9 3 1 0.04/ 0.05
Grain
Size ␮m
Lubricant Water Water Water Alco or Alco or Alco or
Type wat wat wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp Comp Comp Comp Comp Contra
contra
Force per 30 共7兲 25 共4.5兲 25 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 10 共2.2兲
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 4 4 4 2–3

Minutes plane
Material: Composites. Other composite materials


thickness/hardness,
surface layers
Grain size, grain E 112, E 930, E 1181 C-18, T-18
boundaries
of inclusion E 1245, E 1382
content
High planeness
Microhardness, hardness B 578, C 730, C 849, C 1326, C-18, T-18
C 1327, E 10, E 18, E 92,
E 103, E 110, E 140, E 384,
E 448
E 883, E 1245
Porosity C-18
Sectioning
Cut-Off Wheel Al2O3 or SiC, bakelite bond or diamond, metal bond

or bakelite bond
Mounting

Minutes Minutes/
Hours
Grinding
T-18: At composites with ceramics, SiC grinding paper may not be used; use
diamond for grinding 共see Method T-16 or use Method C-18兲.
Polishing
C/T-18: Polishing step with silica: Depending on the matrix of the material,
alumina is used instead of silica. See under the actual material. Also the silica
step can be changed to P 2 from Method T-12.
T-18: P 2: Can be changed to step P 2 from Method T-12 as final step.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, Cloth, Cloth,
fixed, res soft napless, hard, napless,
wov, syn soft, porous,
syn
Abrasive Type Diamond Dia, spr or Dia, spr or Silica
susp susp
Grit/Grain Size ␮m P220 9 3 0.04/ 0.05
Rotation 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm Comp or Comp Comp Contra
Comp/Contra contra
Force per Specimen N 共lb兲 30 共7兲 40 共9兲 40 共9兲 10 共2.2兲
Time Until plane 4–6 3–5 1
Minutes

Section 13.2.2.兲
Polishing
hard, hard, soft,
wov, wov, porous,
silk silk syn
Type spr spr
or or
susp susp
Grit or P220 P320 P500 P1200 3 1 0.04/ 0.05
Grain
Size ␮m
Type or or
wat wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm Comp Comp Comp Comp Comp Comp Contra
Comp/Contra or
contra
Force per 30 共7兲 25 共5.5兲 25 共5.5兲 25 共5.5兲 20 20 10
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 4–5 3 0.5–1
Minutes plane
Material: Ceramic capacitors. Ceramic resistors. Diodes
Comments on Material: In ceramic capacitors, ceramic resistors, and diodes we

have the hard, brittle ceramic or glass phases combined with softer materials like
silicon and metals. Delamination, voidage, and cracks are typical processing
defects which can be assessed by materialography/metallography. Also
materialography/metallography can be used for dimension analysis.
The monolithic ceramic capacitor consists of ceramic plates, often barium
titanate, coated with layers of a silver-palladium alloy and with terminations in
silver. The barium titanate being very brittle and sensitive to mechanical stress
must be prepared very carefully with Method T-19 below; only the two grinding
steps PG and FG 1 should be omitted so that the preparation starts with grit P500
grinding paper.
Ceramic resistors are normally made with a less brittle and harder ceramic
共alumina兲 and Method C-19 can be recommended.
Glass and silicon of the diodes are very brittle materials and very careful
preparation is necessary. Method T-19 is considered the most suitable.
A number of artifacts can be developed during the preparation, like pull-outs,

cracks, delaminations, and relief 共see Section 13.5兲. The correct mounting
共encapsulation兲 is important; uncorrect mounting may create voids and gaps
between mounting material and the single constituents, leaving the constituent
unsupported causing rounding and possibly cracking.
Methods C-19 and T-19 may also be used for preparation of other electronic/
microelectronic devices like integrated circuits 共see also Material/Preparation
Tables 26兲.
Sectioning: Wet abrasive cutting with a diamond metal bond cut-off wheel as thin
as possible. This should preferably take place on a precision cut-off machine, both
to obtain the smallest possible stress to the specimen and to be able to cut
reasonably precise in the correct distance from the site 共target兲 to be investigated.
This distance should be so that neither the damages from the cutting and from the
rough grinding steps will influence the surface at the site of interest 共target兲.
In case the part 共capacitor兲 is relatively small, the part can be encapsulated
共mounted兲共see below兲 and a sectioning is not necessary; the inspection plane
共target兲 can be reached by grinding.
Mounting: The lowest possible heating of the specimen should take place during
mounting, so hot mounting should be avoided. Cold mounting in epoxy is
recommended because of the low viscosity, the low peak temperature, and the
possibility of vacuum impregnation 共see Section 3.10兲.
Grinding: It is important that the very brittle materials are not damaged too much
by the rough grinding papers and often, as mentioned above, the grinding should
start with the grits P320 or P500. If a relief between areas with a high difference
in hardness should be avoided, Method C-19 should be used if possible.
Polishing: Polishing times should be kept as short as possible to avoid relief, but
often long times are needed to remove deformation and other artifacts developed
during the grinding. Often a water-oil based lubricant should be used for the final
diamond steps.
Etching: Normally no chemical etching takes place, but physical etching, like
relief polishing can be used 共see Section 9.6兲.

surface layers
Grain size, grain boundaries E 112, E 1382 C-19, T-19
Image analysis, rating of inclusion E 562, E 1245, E 1382 C-19, T-19
content
High planeness
Microhardness, hardness E 92, E 384 C-19, T-19
1245, E 1382
Porosity C-19, T-19
Sectioning
Cut-Off wheel Diamond, metal bond, 0.5 mm 共0.019 in兲 thickness
Mounting
Hot Compression Mounting Resin Cold Mounting Resin Epoxy

Time Time 12– 24 h
Grinding
C-19 and T-19: For very sensitive materials it is recommended not to use the PG
step with grit P220 grinding paper, but start with grit P320 or P500.
Diodes: C-19: It is recommended to use SiC paper grit P220 for PG and grit
P500 for FG 1 so that FG 1 共RCD, soft兲 is changed to
FG 2.
Polishing
C-19: P 2: At materials with less tendency for relief, the cloth can be changed to
med nap, soft, syn.
Diodes: C-19: The cloth for the step P 1 is changed to napless, hard, wov, syn,
and the cloth for P 2 is changed to med nap, soft, syn.
C-19: In case of sensitive materials like constituents of soft metals 共diodes兲, the
lubricant for 3 ␮m and 1 ␮m diamond-polishing steps should be water-oil based.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, Cloth, Cloth, Cloth,
res soft napless, napless, napless,
hard, hard, soft,
wov, silk wov, silk porous,
syn
Abrasive Type Diamond Dia, Dia, Dia, Silica
spr or spr or spr or
susp susp susp
Grit/Grain P220 9 3 1 0.04/ 0.05
Size ␮m
Lubricant Type Water Alco or Alco or wat Alco or wat

wat
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm Comp or Comp Comp Comp Contra
Comp/Contra contra
Specimen
N 共lb兲
Time Until plane 4–6 1–2 1–2 0.5–1
Minutes

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 FG 3 P1 P2 P3 P4
Polishing
Disk/ SiC SiC SiC SiC Cloth, Cloth, Cloth, Cloth,
Cloth paper paper paper paper nap- nap- nap- nap-
less, less, less, less,
wov, wov, wov, porous
silk silk silk
Abrasive SiC SiC SiC SiC Dia, Dia, Dia, Silica
Type spr spr spr
or or or
susp susp susp
Grit or P220 P320 P500 P1200 9 6 1 0.04/ 0.05
Grain
size ␮m
Lubricant Water Water Water Water Alco Wat-oil Wat-oil
Type or wat
Rotation 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/rpm
Contra
Force 15 共3.4兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 10 共2.2兲
per
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 10–15 5–10 2 0.5–1
Minutes plane
Material: YBCO ceramic super conductors
Comments on Material: A superconductor is an element, intermetallic, or

compound that will conduct electricity without resistance below a certain
temperature, Tc. However, this applies only to direct current 共dc兲 electricity and to
finite amounts of current. All known superconductors are solids, and all require
extreme cold to enter a superconductive state. Once set in motion, current will
flow forever in a closed loop of superconducting material—making it the closest
thing to perpetual motion in nature. Tc is the critical transition temperature below
which a material begins to superconduct, and research is going on to find the
material with the highest Tc. Superconductors are categorized in Type 1 and Type
2. Type 1 category is mainly comprised of metals and metalloids that require
extremely low temperatures, Tc, up to a few K, to become superconductive. The
Type 2 category is comprised of metallic compounds and alloys, of which the
“perovskites,” metal-oxide ceramics like the so-called YBCO compounds composed
of yttrium, barium, copper, and oxygen, are important because they have a Tc
higher than 90 K.
In general, YBCO materials are very brittle and porous, so pull-outs and
microcracks can be introduced during the sectioning and grinding stages. The
Method T-20 is developed for YBa2Cu3O7+, and in case of materials too hard for
SiC grinding paper, or an extremely plane specimen is wanted, Method C-20 can
be used.
Sectioning: Sectioning should take place with utmost care because of the brittle
and porous material. Wet abrasive cutting can be done with a thin diamond cut-off
wheel, metal bond, or, if damage should be reduced, with bakelite bond on a
precision cut-off machine. The cut-off wheel should be as thin as possible and for
some softer materials, a thin SiC bakelite bond wheel, 0.5 mm 共0.02 in兲 can be
used. The feed rate should be low and the wheel speed in the range of 1000 rpm.
If the porosity is high, it can be recommended to vacuum impregnate the
specimen before cutting 共see below兲. The clamping of the specimen during cutting
should be so that pressure spots are avoided, as these can cause fractures in the
material. Very sensitive materials can be glued to a piece of nonmetallic base
material which is then clamped in the machine.
When water is used for cutting, place the cut specimen in alcohol for one hour if
the material is water sensitive.
Mounting: If the porosity is above 5 % it is advisable to vacuum impregnate the
sectioned specimen with epoxy possibly using a dye 共see Section 3.10兲. The
material should not be hot mounted, but mounting after impregnation should be
with a slow curing epoxy. To balance the hardness of the epoxy a filler can be
added 共see Section 3.11.2兲.
Grinding: As grinding with rough grinding papers causes pull-outs and
microcracks, the PG step with grit P220 grinding paper may be changed to grit
P320 if the surface after cutting seems relatively little damaged. Water should be
avoided for water sensitive materials 共see below兲.
Polishing: To remove pull-outs and microcracks polishing may be carried out at
low pressure over relatively long times 共see methods below兲.
Etching: No etchants are stated below, but contrast can be developed as indicated.

thickness/hardness,
surface layers
High planeness
Microhardness, hardness E 384 C-20, T-20
E 1268, E 1382
Porosity C-20, T-20
Sectioning
Cut-Off Wheel Diamond, metal bond 共bakelite bond兲, or SiC bakelite

Mounting
Hot Compression Resin Cold Mounting Resin Epoxy 共with filler兲

Mounting Time Time 12– 24 h
Grinding
C-20: FG 1 and FG 2: If material is highly sensitive to water use a water-free

diamond suspension.
T-20: If the material is not water sensitive, water should be used as a cooling
fluid for the steps PG and FG 1 to FG 4.
Polishing
C-20: P 1: If the material is water sensitive, use P 1 and P 2 from T-20.

T-21: If material is water sensitive, use water-free diamond suspension or spray

for P 1 and P 2 as indicated.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper RCD, soft RCD, soft Cloth,
napless,
soft,
porous,
syn
Abrasive Type SiC Dia, spr Dia, spr Silica
or susp or susp
Grit or Grain Size ␮m P220 9 3 0.04/ 0.05
Lubricant Type Water/dry Alco, water-free Alco, water-free
rpm/rpm
Comp/Contra Comp Comp Comp Contra
Force per Specimen N 共lb兲 15 共3.4兲 25 共5.7兲 25 共5.7兲 20 共4.5兲
Minutes

Section 13.2.2.兲
Polishing
hard, hard,
wov, silk wov, silk
Abrasive Type SiC SiC SiC SiC SiC Dia, spr Dia, spr
or susp or susp
Grit and P220 P500 P1200 P2400 P4000 1 0.25
Grain Size
␮m
Lubricant Type Dry Dry Dry Dry Dry Alco, Alco,
water water-
free free
Rotation 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp Comp Comp Comp Comp Comp Comp
Force per 15 共3.4兲 15 共3.4兲 15 共3.4兲 15 共3.4兲 15 共3.4兲 10–15 10–15
Specimen 共2.–3.4兲共2.3–3.4兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 4–20 5–15

Minutes plane
Etchant
YiBa2Ca3O7+ Contrast can be made by:
a兲 vapor depositing of interference layer 共e.g., iron oxide兲
b兲 Observation of the polished specimen in polarized light
Material: Germanium. Silicon. Si wafers. Other semiconductors
Material Properties: Germanium: Face-centered cubic, 5.3 g / cm3, 937.4° C

共1719° F兲.
Silicon: Face-centered cubic, 2.42 g / cm3, 1420° C 共2588° F兲.
Comments on Material: Germanium and silicon are metalloids and belong to the
group of materials, semiconductors. Silicon is the most commonly used material
and is often prepared as a chip 共see Material/Preparation Tables 22 and 26兲 or as a
wafer/solid piece, which is discussed here. It is, however, only the preparation for
metallographic/materialographic examination, the polishing 共thinning兲, which is
part of the production process, is outside the scope of this book. The
semiconductors are brittle materials that fracture easily, and especially as thin
wafers, the specimens should be handled with great care.
Sectioning: Wet abrasive cutting with a diamond metal bond cut-off wheel,
0.5 mm 共0.02 in兲 thick or thinner. The cutting should be done on a precision
cut-off machine to obtain the most controlled cutting with a low feed speed. The
clamping should not be directly on the specimen, but with elastic material as
spacers. Often it can be of advantage to encapsulate the specimen before cutting.
Sectioning for production of wafers is outside the scope of this book.
Mounting: For preparation of the flat side of a wafer, the wafer or a piece of the
wafer is temporarily glued with wax to a support disk which can be placed in the
specimen holder. In the case of a cross section of the wafer, the specimen is cold
mounted and placed in the mounting mold supported by clips to hold it in an
upright position 共see Section 3.9兲. Due to the brittle nature of the semiconductors
these should not be hot mounted, but cold mounted, preferably with epoxy.
Grinding: The rough grits of SiC grinding papers will damage silicon and other
semiconductors rather strongly, and therefore the grits P220 and P320 should only
be used if relatively much material should be removed. If the cut surface is of a
good quality, the plane grinding should be done with a grit P500 grinding paper if
possible. To avoid SiC grinding paper for fine grinding, use Method C-21. As an
alternative to SiC grinding papers, Al2O3/diamond lapping films can be used 共see
Section 6.7.6 and Material/Preparation Tables 22兲.
Polishing: Polishing times should be as short as possible to avoid edge rounding.
The semiconductor materials respond very well to chemical mechanical polishing
with colloidal silica, but also here the time should be as short as possible.
Etching: See Etchants below.

surface layers
Grain size, E 112, E 930, E 1382 C-21, T-21
grain boundaries
Image analysis, rating E 562, E 1245, E 1382 C-21
High planeness
E 1382
Porosity C-21, T-21
Sectioning
Cut-Off Wheel Diamond, metal bond, 0.5 mm 共0.02 in兲 or thinner
Mounting

Mounting Time Time 12– 24 h
Grinding
C-21 and T-21: Plane grinding with grit P220 or P320, or both, should be
avoided if possible.
C-21: PG: Grit P500 SiC paper can be used.
Polishing
C-21 and T-21: Polishing times should be kept as short as possible.

C-21 and T-21: P 1: This step can be changed to step P 2 in Method T-21.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, soft RCD, soft Cloth, Cloth, nap-
fixed, res napless, less, soft,
hard, wov, porous, syn
syn
Abrasive Diamond Dia, spr or Dia, spr or Dia, spr or Silica
Type susp susp susp
Grit or P500 9 3 3 0.04/ 0.05
Grain Size
␮m
Type
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/rpm
Comp/ Comp Comp Comp Comp Contra
Contra
Specimen
N 共lb兲
Minutes

Section 13.2.2.兲
Polishing
hard, hard, soft,
wov, silk wov, porous
silk
Abrasive Type SiC SiC SiC SiC Dia, spr Dia, spr Silica
or susp or susp
Grit or Grain P500 P1000 P2400 P4000 3 1 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Water Water
Alco or Alco or
wat wat
Rotation 300/150 300/150 300/150 300/150 150/150 150/150 150/150
Disk/Holder
rpm/rpm
Comp/Contra Comp Comp Comp Comp Comp Comp Contra
Force per 15–25 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 10–15
Specimen 共3.4–5.7兲共2.2–3.4兲
N 共lb兲
Time Until 1.5–2 1.5–2 1.5–2 4 3 1–3

Minutes plane
Etchants
Material Etchants 共see Table Uses
12.2兲
Si, Si alloys 931 General structure
Si, Si alloys 932 General structure
Si 933 General structure
Si 934 To reveal SiO2
Material: Microelectronic material „semiconductor device…
Preparation of cross section of a semiconductor device using a tripod fixture for

hand preparation on a grinder/polisher with a 200 mm 共8 in兲 polishing disk and
variable speed 0 – 150 r / min.
Comments on Material: Nonencapsulated cross sections through microelectronic
material 共semiconductor devices兲 serve two main functions. Cuts through
representative structures within an IC show relationships of layers and features,
such as step coverage, interfaces between layers, and possibly embedded defects or
voids. Precision cross sections through specific defects often lead to the process
step or mechanism which produced the defect 共see Section 7.10.2兲.
The preparation of a nonencapsulated cross section of microelectronic material is
described below. The method is considered a “C-Method,” using a combination of
SiC grinding papers and Al2O3/diamond lapping films 共see Section 6.7.6兲, and no
“T-Method” is stated.
Sectioning: The specimen should be a piece of silicon roughly 5 mm 共0.20 in兲
square. The desired cross section target should be within 50 ␮m from the edge.
The specimen can be cut out with a thin diamond cut-off wheel on a precision
cut-off machine medium speed or cleaved. Determine the desired cross section line
共target兲. If suitable landmarks do not exist, create visible marks with a laser or
mechanical probe.
Mounting: Heat up a sample mount to approximately 125° C 共250° F兲. Apply a dot
of wax and mount the specimen in cantilever fashion on the sample mount. The
target cross section line must extend beyond the end of the sample mount 共see
Section 7.10.2兲. Place the sample mount with specimen in the tripod fixture.
Grinding: The purpose of grinding is to rapidly achieve a surface 1 ␮m away from
and parallel to the desired cross section line. If more than 40 ␮m of material
should be removed to reach the final cross section line, begin grinding with SiC
paper grit P1200 共see step PG below兲. If the distance to line is 20 ␮m or less, start
with step FG 1 below.
FG 3 and FG 4 uses Al2O3 and diamond lapping film plane back, placed with
water as a “glue” on a plane, smooth surface 共glass/metal plate兲 on the polishing
disk.
Diamond lapping film can be used as an alternative to SiC paper, and Al2O3
lapping film in the steps PG and FG 1, 2, 3, and 4; this is stated in the Method
Table below. Step FG 5 shall always be with diamond lapping film. Attention:
Always let the grinding/polishing disk rotate into the edge containing the target,
except at the last polishing step 共reverse position兲.
Polishing: The completed cross section should be exactly centered on the contact,
via, or other feature in the target. Polishing will only remove very little material 共
2 ␮m or less兲 and cannot remove deep scratches or damage created by grinding
too close to the desired finish with coarse abrasives. Polishing is most important
when the cross section is to be viewed in a high-resolution field emission SEM.
Type of “polishing” depends on the composition of the specimen: Si, SiO2, and Al
with/without thin barrier layers: Repeat step FG 4 after step FG 5, only with
0.05 ␮m Al2O3 lapping film in 0.5 min or longer until the diamond scratches are
removed. Finish with 0.5 min holding the fixture in reverse position 共see Section
7.10.2兲.
Si, SiO2, and metallization including tungsten plugs or layers: Use step P 1 below,
holding the fixture in reverse position 共see Section 7.10.2兲.
Etching: Normally no etching is used.
Sectioning
Cut-Off Wheel Diamond wheel metal bond 0.5 mm 共0.019 in兲

thickness or by cleaving
Mounting
Hot Compression Resin See above Cold Mounting Resin See above
Mounting Time Time

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 FG 3 FG 4 FG 5 P1
Polishing
Disk/Cloth SiC SiC SiC Al2O3 Al2O3 Diamond Cloth,
paper paper paper or or lapping napless,
or or or diamond diamond film hard,
diamond diamond diamond lapping lapping wov, syn
lapping lapping lapping film film
film film film
Abrasive SiC or SiC or SiC or Al- Al-oxide Diamond Dia, susp
Type diamond diamond diamond oxide
Grit/Grain P1200 P2400 or P4000 or 1 0.3 0.1 0.1
Size ␮m or 15 8 3
Lubricant Water Water Water Water Water Water Alco

Type
Rotation 60/ 100 60/ 100 60/ 100 60/ 100 30 30 70/ 100
Disk/
Holder
rpm/
rpm
Comp/
Contra
Force per Weight Weight Weight Weight Weight Weight Weight
Specimen of of of of of of fixture of fixture
N 共lb兲 fixture fixture fixture fixture fixture
Time Until Until Until Until Until Until 0.5–1,
Minutes within within within 7 within 3 within 2 within 1- until
22 ␮m 12 ␮m ␮m ␮m 1.5 ␮m target
from ␮m from from from from
target from target target target target
line target line line line line
line
Material: Resistors. Other electronic metal components
Comments on Material: Metal film resistors and other metal-based electronic

components often consist of several very different types of material that range
from a very soft metal to a very hard ceramic. The methods stated below should
be considered as supplement to the methods stated in Material/Preparation Tables
19 and 26.
Sectioning: See Material/Preparation Tables 19 and 26.
Mounting: See Material/Preparation Tables 19 and 26.
Grinding: See Material/Preparation Tables 19 and 26.
Polishing: See Material/Preparation Tables 19 and 26.

surface layers
Image analysis, rating of inclusion E 562, E 1382 C-23, T-23
content
High planeness

E 1245, E 1382
Porosity C-23, T-23
Sectioning
Cut-Off Wheel Diamond wheel metal bond or SiC bakelite bond,

0.5 mm 共0.019 in兲 thickness.
Mounting
Hot Compression Resin Cold Mounting Resin Acrylics with a

Mounting Filler/Epoxy
Time Time 6 – 15 min/ 12– 24 h
Grinding
C-23: In the case of a high amount of ceramics in the specimen, PG may be

changed to a diamond pad, 30 ␮m, bakelite bond. See also Methods C/T-19.
Polishing
T-23: The step P 1 can be followed by a step like P 1 in Method C-23.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper RCD, soft RCD, soft Cloth, nap-
less, soft,
porous, syn
or susp or susp
Grit or Grain Size ␮m 320 9 3 0.04/ 0.05
rpm/rpm
contra
Force per Specimen N 共lb兲 35 共8兲 35 共8兲 35 共8兲 20 共4.5兲
Time Until 3–4 3 0.5–1

Minutes plane

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper SiC paper SiC paper SiC paper Cloth,
napless,
hard,
wov, syn
Abrasive Type SiC SiC SiC SiC Dia,
spr or
susp
Grit or Grain P220 P320 P500 P1200 3
Size ␮m
Lubricant Type Water Water Water Water Alco
or wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp or Comp or Comp Comp
Contra Contra Contra
Force per 30 共7兲 30 共7兲 30 共7兲 30 共7兲 30 共7兲
Specimen N 共lb兲
Time Until plane 0.5–1 0.5–1 0.5–1 3
Minutes
Material: Solder balls. Microelectronic packages
Comments on Material: The tin-lead solders used for solder balls often have to be
prepared together with other components like printed circuit boards 共PCBs兲,
ceramics, plastics, etc. 共see Section 7.10.3兲. This means that the ideal preparation
of the soft solder is not possible if the other components also should be prepared
in an acceptable way. For soft solders the main problem is embedding of abrasive
grains and particles from the preparation process 共see below and Section 13.5/6兲.
In case of soldered joints, cracks may develop after the preparation due to stress,
and for this reason the specimen should be examined and documented
immediately after preparation. For preparation of PCBs see Material/Preparation
Tables 27. For microelectronic packages see also Material/Preparation Tables 19
and 26.
Sectioning: Sectioning often involves cutting through components of very

different hardness. Wet abrasive cutting should be done with a diamond metal
bond cut-off wheel if the sectioning involves ceramics, and a SiC bakelite wheel if
cutting involves only softer materials 共see also Material/Preparation Tables 26兲.
Cutting should be done on a precision cut-off machine to secure a precise cut and
make the use of a thin wheel, 0.5 mm 共0.02 in兲 or thinner, possible. In case of
component-mounted boards, take care that all specimens are properly identified
before they are sectioned from the PCB. The cut should be in a certain distance
from the level of investigation so that damage from the cutting can be removed at
grinding and polishing.
Often the section to be investigated should be encapsulated 共mounted兲 in epoxy
prior to cutting to ensure the integrity of delicate joints/components.
Mounting: The specimen should be carefully cleaned in acetone and preferably
ultrasonics before mounting. Hot mounting cannot be recommended. Cold
mounting with epoxy and vacuum impregnation is recommended so that all voids
are filled with epoxy 共see Section 3.10兲.
Grinding: For specimens containing ceramics the Method C-24 should be used
with Method C-19 as an alternative.
Polishing: In case of embedded abrasive grains, the use of diamond paste can be
tried out for the 3 and 1 ␮m steps; also the use of only small amounts of lubricant
may prevent embedding of particles.
Etching: Normally no etching is made, but in case of etching, see Material/

thickness/hardness,
surface layers
Grain size, grain boundaries C-24, T-24
Image analysis, rating C-24, T-24
High planeness
Sectioning
Cut-Off Wheel Diamond, metal bond or SiC, bakelite bond, thinnest

possible
Mounting

Grinding
C-24: FG 1 and T-24: FG 3: Grind until solder balls are visible, being close to
target.
Polishing
C-24, T-24: In case of embedded diamonds, diamond paste may be used instead
of spray/suspension for the 3 ␮m and 1 ␮m steps.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper SiC paper RCD, soft Cloth, nap- Cloth,
less, medium napless,
hard, soft,
wov, wool porous,
syn
Abrasive Type SiC SiC Dia, spr or Dia, spr or Silica
susp susp
Grit or Grain 220 320 9 3 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Alco or wat Wat-oil
rpm/rpm
Comp/Contra Comp or Comp or Comp Comp Contra
contra contra
Force per Specimen 20 共4.5兲 15 共3.4兲 20 共4.5兲 20 共4.5兲 15 共3.4兲
N 共lb兲
Time Until plane To target 2 1–2 1
Minutes

Section 13.2.2.兲
Polishing
paper paper paper paper napless, napless, nap-
hard, hard, less, soft
nonwov, wov, silk porous,
syn syn
Abrasive SiC SiC SiC SiC Dia, spr Dia, spr Silica
Size ␮m
Lubricant Water Water Water Water Wat-oil Wat-oil
Type
Rotation 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Force per 30 共7兲 30 共7兲 30 共7兲 30 共7兲 20 共4.5兲 20 共4.5兲 15 共3.4兲
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 4 2 0.5–1
Minutes plane
Material: Capacitors. Other polymer electronic components
Comments on Material: Film capacitors often incorporate two layers of dielectric

film that have each been metallized on one side; these strips are stacked and
rolled. The assembly may be packaged in a polymeric conformal coating or in a
molded polymeric housing.
Grinding: If the specimen contains phases of very different hardness, Method C-25
should be preferred.
Polishing: Polishing times should be kept as short as possible to avoid relief.
Etching: Normally no etching is done.

surface layers
Grain size, grain boundaries E 112, E 1382 C-25,

T-25
Image analysis, rating of inclusion E 562, E 1245, E 1382 C-25,
content T-25
High planeness
Microhardness, hardness E 92, E 384 C-25,
T-25
E 1245, E 1382 T-25
T-25
Porosity C-25,
T-25
Sectioning
Cut-Off Wheel Diamond, metal bond or SiC, bakelite bond, 0.5 mm

共0.02 in兲 thick
Mounting

Mounting Time Time 6 – 10 min/ 8 – 12 h
Grinding
C-25: PG step: In the case of little or no ceramic material, SiC paper can be
used.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, soft Cloth, nap- Cloth, Cloth,
res less, hard, napless, napless,
wov, silk hard, wov, soft,
silk porous,
syn
susp susp susp
Grit or P220 9 6 1 0.04/ 0.05

Grain Size ␮m
Lubricant Water Alco or wat Wat-oil Wat-oil

Type
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp Comp Comp
contra
Specimen N 共lb兲
Time Until plane 5 1–2 0.5–1 0.5
Minutes

Section 13.2.2.兲
Polishing
v. hard, hard, soft
wov, syn wov, silk porous,
syn
or susp or susp
Size ␮m
Type wat wat
Rotation 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 3 2 0.5–1
Minutes plane
Material/Preparation Table 26
Material: Microelectronic packages. Integrated circuits.
Transistors. Other microelectronic devices
Comments on Material: As an introduction to preparation of microelectronic

packages Section 7.10.3 should be studied to get an impression of the problems
involved.
Electronic and microelectronic devices and packages are complex material
composites. Imaging and analysis of the various material microstructures, layered
structures, and interfaces are necessary for a number of reasons, including
package qualification, monitoring of the manufacturing process, incoming quality
control, and failure analysis. The dimensions of the individual features range from
fractions of a micron to several cm 共fraction of an in兲. Due to the close packing of
the various materials within a small volume, all materials having very different
properties; materialographic preparation faces the problem of making all the
materials suited for proper analysis. It is essential to have a general understanding
of the physical properties of all materials used in the construction of the package
共see Table 7.1兲. As a rule the preparation is tailored to the predominant component
material to be analyzed, but often all materials must be considered to obtain a
satisfactory result. Ignoring the unique interfaces that are present in a
microelectronic package will likely result in artifacts induced during the
preparation process. Such artifacts may be edge rounding, relief, embedding of
abrasive grains, smearing and fracturing, and introduction of microcracks. Several
of these artifacts could be misinterpreted as defects in the package developed
during the production or in other ways.
Making a cross section of a microelectronic package is a destructive test; it is
important that as much information as possible about the device is gathered
before the preparation starts. Such information is important to decide on the
target of the preparation and may be important to be able to decide whether a
defect was pre-existing or induced during the preparation. Also, this information is
important in case of failure analysis. The information can be obtained through a
number of analysis techniques like radiography, ultrasonic imaging, and
macrophotography. Based on the available information, the
preparation process is decided upon as either one of the two methods indicated
below or other methods stated in Material/Preparation Tables 19, 22, 23, and 25,
with the Methods C-19 and T-19 as the first choice.
Sectioning: Wet abrasive cutting with a diamond metal bond cut-off wheel,
0.5 to 1 mm 共0.02 to 0.04 in兲 thick on a precision cut-off machine with
1500 to 2000 rpm. Often an electroplated diamond wheel can be used with
advantage, and in the case of very hard components a diamond wheel with
bakelite bond should be used. In certain cases depending on the materials, SiC
bakelite bond cut-off wheel can be used.
Cutting before encapsulation: In some cases the package should be opened to be
able to make the encapsulation 共mounting兲. This can be done with wet abrasive
cutting as mentioned or with grinding away the material or by other means. It is
important that this process takes place at a safe distance to the site to be
investigated.
Cutting after encapsulation: Wet abrasive cutting as stated above is recommended.

It is important that the specimen is oriented, with respect to wheel rotation, such
that the brittle material in the specimen, like silicon, is cut in compression. Doing
this will minimize delamination or fracturing, or both, of the brittle component
material. Also the specimen should be positioned so that the wheel cuts into the
smallest dimension of the critical parts in the package. To shorten the following
preparation process, the cutting should be done in a plane relatively close to the
site of investigation with this under the condition that the damage caused by the
cutting is “under control.”
Mounting: Microelectronic packages cannot be subjected to pressure and heat, so
only cold mounting, most often as an encapsulation in epoxy under vacuum, is
recommended.
Encapsulation: It is very important that the package is carefully cleaned to secure
a complete adhesion by the epoxy during the encapsulation. This can be done in
acetone, preferably in a beaker in an ultrasonic bath. Drying should be done with
N2 gas or absolutely pure compressed air; normal compressed air should
be avoided. The cleaned part should be handled with a pair of tweezers and dried
in an oven at 50° C 共122° F兲. The package is placed in the mounting mold so that
the plane of interest will ultimately be parallel to the cutting wheel. If needed, the
specimen is supported with clips or by other means. It is important that the
mounting material adheres to all constituents and that all topographical features
of the package is filled with mounting material. This can best be provided with an
epoxy with a low viscosity and impregnation under vacuum 共see Section 3.10兲.
Also a pressure vessel can be used for securing a good encapsulation 共see Section
3.7兲.
Grinding: Considering the often very brittle materials in the specimen, plane
grinding with rough SiC grinding papers should be avoided. In the methods stated
below plane grinding is with grit P320 grinding paper, but this paper should only
be used if the plane grinding is in a plane relatively far from the site of interest
共target兲. If possible, depending on the surface established by the sectioning, the
plane grinding should be done with an RCD stated in Method C-26, step FG 2,
below. In case of packages with many soft, ductile materials, Method T-26 below
may have the best grinding steps.
Polishing: It is very important that the deformation and other damage developed
during the grinding is removed during the rough polishing step. Often step P 2 in
Method T-26 can be omitted. For packages containing predominantly soft
materials 共plastics兲, it can be of advantage to use a mixture of 50 % colloidal silica
and 50 % deagglomerated alumina 共0.05 ␮m兲 for the final polishing step.
Etching: Normally no chemical etching takes place, but physical etching, like
relief polishing and methods like deposition of layers can be used 共see Section 9.6兲.

surface layers
content
High planeness
E 1245, E 1382
Porosity C-26, T-26
Sectioning
Cut-Off Wheel Diamond, metal bond or SiC, bakelite bond,

0 to 1 mm 共0.02 to 0.04 in兲 thick, see also above.
Mounting

Grinding
C-26, T-26: Only use rough grits of SiC grinding paper, when not close to target.
Polishing

C-26: P 2: Often the cloth can be changed to a med nap, soft, syn, if the
difference in hardness of the components materials is not high.
C-26 and T-26: For predominantly soft materials use a mixture of 50 % colloidal
silica and 50 % deagglomerated alumina 共0.05 ␮m兲 for the final polishing step.
C-26 and T-26: For the steps with 6, 3, and 1 ␮m diamond, colloidal silica can
be used as lubricant.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper SiC paper RCD, soft Cloth, nap- Cloth, Cloth,
less, hard, napless, napless,
wov, syn hard, wov, soft,
silk porous,
syn
Abrasive SiC SiC Dia, spr or Dia, spr or Dia, spr or Silica
Type susp susp susp
Grit or Grain 220 320 9 3 1 0.04/ 0.05
Size ␮m
Lubricant Water Water Alco or Wat-oil Wat-oil
Type wat
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra contra
Force per 25 共5.7兲 25 共5.7兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 10–15
Specimen 共2.2–3.4兲
N 共lb兲
Time Until 0.5–1 2–15 1–5 1–4 0.5–1
Minutes plane 共Close to
target兲

Section 13.2.2.兲
Grinding/ FG 3 P1 P2 P3 P4
Disk/ SiC SiC SiC SiC Cloth, Cloth, Cloth, Cloth,
Cloth paper paper paper paper nap- nap- nap- nap-
less, less, less, less,
wov, wov, wov, por-
silk syn silk ous,
syn
Abrasive SiC SiC SiC SiC Dia, Dia, Dia, Silica
Type spr spr spr
or or or
susp susp susp
Grit or P320 P500 P800 P1200 6 3 1 0.04/
Grain 0.05
Size ␮m
Lubricant Water Water Water Water Wat-oil Wat-oil Wat-oil
Type
Rotation 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/
rpm
Contra or
contra
Force per 30 共7兲 30 共7兲 30 共7兲 30 共7兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 10–15
Specimen 共2.2–
N 共lb兲 3.4兲
Time Until 0.5–1 0.5–1 0.5 –1 5–15 1–2 1–4 0.5–1
Minutes plane 共Close
to
target兲
Material: PCB coupon
Comments on Material: For a description of PCB coupons with reference holes

and their preparation, see Section 7.10.1.
A “contemporary” method is not developed for this type of preparation; therefore,
Method C-27 is a “traditional” method using SiC grinding paper.
Sectioning: The coupon is normally cut out with a router or punched out. A
precision cut-off machine with a diamond cut-off wheel, metal bond, can also be
used.
Mounting: Two to six coupons are mounted with a cold mounting material like
acrylics in a special mounting mold to be placed in a special holder, with reference
pins, to obtain a controlled material removal.
Grinding: Grinding is done in two steps against adjustable stops mounted on the
specimen holder to stop material removal before the center of the holes to be
inspected.
Polishing: The polishing steps P 3 and even P 2 in Methods C-27 and T-27 may be
omitted according to the type of PCB and the purpose of examination.
Etching: If an etching is wanted this can be done in the polishing step P 3: Use
96 mL colloidal silica, 2 mL H2O2 共30 %兲 and 2 mL ammonia solution 共25 %兲.
Sectioning
Cut-Off Wheel Diamond, metal bond, if not routed or punched, see

above.
Mounting
Hot Compression Mounting Resin Cold Mounting Resin Acrylics

Time Time 8 – 10 min
Grinding
C-27, T-27: Grinding is performed against adjustable stops 共see above兲.

Polishing
C-27, T-27: Etching can be done through chemical mechanical polishing with
96 mL colloidal silica, 2 mL H2O2 共30 %兲 and 2 mL ammonia solution 共25 %兲.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper SiC paper Cloth, Cloth, Cloth,
hard, hard, wov, soft,
wov, syn wool porous,
syn
susp susp
Grit or Grain Size ␮m P220 P1200 3 1 0.04/ 0.05
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Force per Specimen N 共lb兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 15 共3.4兲 10 共2.2兲
Time See above See above 2 2 0.5
Minutes

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper SiC paper Cloth, Cloth, Cloth,

hard, hard, soft,
wov, syn wov, silk porous,
syn
susp susp
Grit or Grain P220 P1200 6 1 0.04/ 0.05
Size ␮m
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen N 共lb兲
Time See above See above 2 2 0.5
Minutes
Material: High carbon steels. Medium carbon steels
Material Properties: Alpha iron 共ferrite兲: Body-centered cubic, gamma iron

共austenite兲: Face-centered cubic, 7.85 g / cm3, 1528° C 共2782° F兲, HV 70 共ferrite兲.
Low carbon steel: ⬍0.2 % C, medium carbon steel: 0.2–0.5 % C, high carbon steel:
⬎0.5 % C 共weight %兲.
Comments on Material: The plain carbon steels are characterized by their
composition, having only carbon as the important alloying element. A typical
medium carbon steel 共SAE-AESI 1042兲 has the composition: 0.4–0.47 % carbon,
0.60–0.90 % manganese, maximum 0.040 % phosphorus, maximum 0.05 % sulfur.
The plain carbon steels and other steels are classified according to their
composition by the American Iron and Steel Institute 共AISI兲 and the Society of
Automotive Engineers 共SAE兲. ASTM also has a classification system built on the
steel product and its application. The ASTM standards are specifications for
specific products; a few examples are: A 1, A 3, A 36 共see Section 12.4.2兲. The
microstructure of plain carbon steels is a mixture of ferrite and pearlite, with an
increase in pearlite corresponding to the increase in carbon content. At 0.8 %
carbon, only pearlite is present and above 0.8 % carbon, cementite will develop.
Medium and high carbon steels are relatively easy to prepare. The problem is to
obtain a true ferrite without deformation. At higher carbon contents with small
amounts of ferrite, the preparation can be cut down to three or four steps for
routine examination 共see below兲. These materials are well suited for electrolytic
polishing.
Sectioning: The correct selection of the specimen is important, especially on

rolled material 共see Section 2.1兲. In wet abrasive cutting an Al2O3 cut-off wheel
should be used. Overheating should be avoided because martensite can be
developed. Cutting pressure should be moderate and cooling should be efficient on
both sides of the cut-off wheel. If shearing or band sawing is used, the increase in
deformation should be taken into consideration, prolonging the plane grinding
step, or possibly use of a rougher grinding paper before grit 220.
Mounting: For routine examination bakelite as powder or tablets is sufficient. In
the case of examination of coatings, other mounting materials should be used 共see
Material/Preparation Tables 08–15兲. For mounting for electrolytic polishing, see
Section 3.11.6.
Grinding: Grinding normally will give no problems with these materials. Care
should be taken that the deformations from plane grinding are effectively removed
before the polishing. If not, the deformed ferrite can be seen after etching, and the
process must be repeated from FG 1. In the case of water sensitive inclusions,
mineral spirits or kerosene can be used for grinding with SiC grinding paper 共see
also Material/Preparation Tables 36兲.
Polishing: The problem can be to obtain a perfect ferrite phase as mentioned
above. In the case of only small deformations, prolong the 3 ␮m step for 1 – 2 min.
For medium carbon steels the final step could be with diamond 共see below兲.
A common test on steels is nonmetallic inclusion identification; often SEM and
EDAX analysis is used. As Si may be contained in the indigenous inclusions, silica
共SiO2兲 should be avoided for the last polishing step. Therefore this step should be
changed to diamond 共see below兲.
Electrolytic polishing can be recommended.
Etching: A high number of etchants are available for steels. In most cases a
relative small selection will cover the need in a given laboratory 共see below兲.
Electrolytic etching is possible.

Case or coating B 487, E 1077 C-28
thickness/hardness
surface layers
Grain size, grain boundaries E 112, E 930, E 1181, E 1382 C-28, T-28,
El-01
Heat influenced zone E 1077 C-28
Heat treatment C-28, T-28,
El-01
Image analysis, rating E 45, E 562, E 768, E 1077, C-28
of inclusion content E 1245, E 1268, E 1382, E 2283
High planeness
Inclusions in steel E 45, E 768, E 1245 C-28, T-28
Microhardness, hardness E 10, E 18, E 92, E 103, E 110, C-28, T-28
E 140, E 384, E 448
Microstructure A 892, E 3, E 45, E 407, E 562, E C-28, T-28,

768, El-01
E 883, E 1077,
E 1181, E 1245, E 1268,
E 1351, E 1382, E 1558
Phase identification C-28, T-28,
El-01
Structure changes 共forging兲 C-28, T-28,
El-01
Sectioning
Cut-Off Wheel Al2O3, bakelite bond
Mounting
Hot Compression Resin Bakelite Cold Mounting Resin Acrylics

Mounting Time 8–9 Time 6 – 10 min
Grinding
T-28: In some cases, at high C content, FG 1 can be omitted.

Polishing
C-28 and T-28: In case of SEM and EDAX analysis of inclusions, the final
polishing step is changed to diamond 1 ␮m, see step P 2 in Method C-29. Also,
0.25 ␮m diamond can be used as a step after 1 ␮m diamond, using the same
cloth and same data.
C-28: P 1: The cloth can be changed to napless, hard, wov, silk.
C-28: P 2: This step can be changed to diamond 1 ␮m, see P 2 in C-29, and the
silica step will be P 3 or it may be omitted.
T-28: P 3: Often the alumina suspension can be diluted with water 1:1. In some
cases this step can be omitted.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, hard Cloth, Cloth,
fixed, res napless, napless,
hard, wov, soft, porous, syn
syn
Abrasive Type Diamond Dia, spr Dia, spr Silica
or susp or susp
Grit or Grain Size ␮m P220 9 3 0.02/ 0.05
Rotation 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Force per 30 共7兲 25 共5.5兲 20 共4.5兲 10 共2.2兲
Specimen N 共lb兲
Time Until plane 4–6 3 1–4
Minutes

Section 13.2.2.兲
Polishing
Disk/Cloth SiC SiC SiC Cloth, Cloth, Cloth,
paper paper paper napless, napless, napless,
hard, hard, porous,
wov, silk wov, syn syn
Abrasive SiC SiC SiC Dia, spr or Dia, spr or Alumina
Type susp susp
Grit or P220 P320 P500 6 3 0.02/ 0.05
Grain
Size ␮m
Lubricant Water Water Water Alco or wat Alco or
Type wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen N
共lb兲
Time Until 0.5–1 0.5–1 3 3 1–4

Minutes plane
Etchants
Fe+ C and 76, 74a, 77, 78, 79 General structure
Fe+ ⬍ 1 C 74a, 77, 31a, 223 Ferrite grain boundaries
+ ⬍ 4% additions 80, 81, 82 Prior austenitic grain boundaries in
martensitic and bainitic steels
78, 222a Untempered martensite
31b, 78 Carbides and phosphides 共matrix
darkened carbides and phosphides
remain bright兲
83 Cementite attacked rapidly, sustenite
less, ferrite and iron phosphide least
84 Overheating and burning stains
carbides
85 Stains carbides
86 Chemical polish-etch
210, 211 Colors ferrite
213, 214 Colors carbides
216 Color latch martensite in low carbon
222b high-alloy grades for dual phase steels;
reveals pearlite, darkens martensite
and outlines austenite
Material: Low carbon steels

Low carbon steel: ⬍0.2% C, medium carbon steel: 0.2– 0.5 % C, high carbon steel:
⬎0.5% C 共weight %兲
Comments on Material: Low carbon steels are relatively easy to prepare. The
problem is to obtain a true ferrite without deformation. This depends on the
carbon content and often, at higher carbon contents, a fine grinding step can be
omitted for routine examination 共see Material/Process Tables 28兲.

Case or coating B 487, E 1077 C-29
thickness/hardness
surface layers
Grain size, grain E 112, E 930, E 1181, E 1382 C-29, T-29,
boundaries El-02
Heat influenced E 1077 C-29
zone
Heat treatment C-29, T-29,
El-02
Image analysis, rating E 45, E 562, E 768, E 1077, C-29
High planeness
Microhardness, E 10, E 18, E 92, E 103, E 110, C-29, T-29
hardness E 140, E 384, E 448
Microstructure A 892, E 3, E 45, E 407, E 768, E 883, C-29, T-29,
E 1077, E 1181, E 1245, El-02
E 1268, E 1351, E 1382, E 1558
El-02
Structure changes C-29, T-29,
共forging兲 El-02
Sectioning
Mounting
Resin Bakelite Resin Acrylics

Cold Mounting Time 8–9 Time 8 – 10 min
Grinding
C-29: P 2: This step can be changed to SiC paper grit P220/320.

T-29: In some cases, at a relatively high carbon content, FG 1 can be omitted.
Polishing
C-29 and T-29: In case of SEM and EDAX analysis of inclusions, the final
polishing step is changed to diamond 1 ␮m, see step P 2 in Method C-29 and
step P 3 in T-29. Also 0.25 ␮m diamond can be used as a step after 1 ␮m
diamond, using the same cloth and same data.
C-29: P 2: For certain materials 共cast iron兲 this step can be omitted or P 3 can be
omitted.
C-29 and T-29: Silica can be used instead of alumina.
T-29: A fine polishing step, P 3, from C-29 can be added.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk RCD, soft Cloth, Cloth, Cloth, nap
fixed, res napless, med. nap, soft, less, soft,
hard, wov, syn porous, syn
syn
Abrasive Diamond Dia, Dia, spr Dia, spr Alumina
Type spr or or or
susp susp susp
Grit or Grain P220 9 3 1 0.02/ 0.05
Size ␮m
Lubricant Water Alco Alco Alco
Type or wat or wat or wat
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen N 共lb兲
Time Until plane 4–6 4–5 1 1
Minutes

Section 13.2.2.兲
Polishing
paper paper paper paper napless, napless, med
hard, hard, nap,
wov, silk wov, syn soft,
syn
Abrasive SiC SiC SiC SiC Dia, spr Dia, spr Dia, spr
Type or susp or susp or susp
Grit or P220 P320 P500 P1200 6 3 1
Grain Size
␮m
Lubricant Water Water Water Water Alco or Alco or Alco or
Type wat wat wat
Rotation 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp Comp Comp Comp Comp Comp
contra
Force per 40 共9兲 40 共9兲 40 共9兲 40 共9兲 40 共9兲 35 共8兲 35 共8兲
Specimen
N 共lb兲
Time Unit 0.5–1 0.5–1 0.5–1 3–4 3–4 1
Minutes plane
Etchants
See Material/Preparation Tables 28.
Material: Gray cast iron, lamellar. Malleable cast iron

Gray cast iron: Carbon 2.5–4.0 %, silicon: 0.5–3.5 %, manganese: 0.2–1.3 %,
phosphorus 0.002–1.0 %, sulfur: 0.2–0.15 % 共weight %兲.
Comments on Material: Gray cast iron is by far the most used cast iron. The
microstructure consists of ferrite or pearlite with graphite in flakes 共lamellar兲, or
both, or in other shapes. The name refers to the color of a fresh fractured surface,
which is grayish because of the graphite. Gray cast iron has a relatively high
silicon content because silicon promotes the formation of graphite during
solidifidation. The microstructure of lamellar cast iron contains 5–10 volume % of
graphite, and the lamellar size and distribution are important for the strength of
the cast iron, but in general lamellar cast iron has a relatively low strength
because of the graphite. The type, size, and distribution are standardized in the
ASTM Standard Test Method for Evaluating the Microstructure of Graphite in Iron
Castings 共A 247兲. Also, a number of other specifications are described in ASTM
standards; some examples covering gray cast iron and malleable cast iron are: A
47, A 48, A 126, A 159, A 197, A 220, A 338, and A 602 共see Sections 12.4.2兲.
Malleable cast iron, also called TG 共temper graphite兲 iron, is made by heat
treatment of white cast iron. During this treatment, up to 20 h, the carbides of the
white cast iron are changed into graphite which will be separated into irregularly
shaped nodules in a ferritic or ferritic/pearlitic matrix. This condition makes
malleable cast iron comparable to steel regarding strength, but the importance of
this material has been reduced because of the development of nodular cast iron
共ductile cast iron兲共see Material/Preparation Tables 31兲.
As the microstructure strongly influences the mechanical properties of cast iron,
metallographic/materialographic examination is important. The examination is
supported by standard reference comparison charts or image analysis techniques,
or both, to determine the morphology, size, and distribution of the graphite on an
unetched specimen.
During the metallographic/materialographic preparation, the retention of the free
graphite in a ferrite/pearlite matrix causes a problem. The difference in hardness
between the two phases and the relative brittleness of the graphite may cause
pull-outs of the graphite and development of a relief between the phases. To obtain
a correct result of a running analysis, it is important that the same high number of
graphite lamellars/nodules are satisfactorily present in the structure without
missing parts of the graphite. The pull-outs to a high degree take place during the
rougher steps of the grinding and therefore it is important that the graphite is
re-established during the fine grinding and polishing steps.
SiC paper may cause a pull-out of graphite even at the fine grain sizes. In that case
Method C-30 should be used.
In the case of a matrix containing much ferrite this may cause problems with
deformations 共see Material/Preparation Tables 28兲. For certain cast irons,
electrolytic polishing can be used.
Method C-29 and T-29 can also be used for cast iron.
Sectioning: These materials are normally sectioned with wet abrasive cutting
without problems using an Al2O3, bakelite bond cut-off wheel. If band sawing is
used, the increase in deformation should be taken into consideration, prolonging
the plane grinding step, or possibly use of a rougher grinding paper before grit
220. Standards test bars are to be preferred, reducing the amount of sectioning,
only it should be considered, whether the microstructures of the test bar truly
represent the structure of the casting.
Mounting: Normally a mounting is not needed except for establishing a suitable
shape for automatic preparation. Often the preparation and examination shall take
place as part of a production process and the time for preparation is very short. In
that case the shape of the test bar coming from the production should be so that it
fits into a specimen holder or specimen holder plate without mounting.
If graphite close to the edge shall be examined, mounting in a suitable mounting
material with a hardness corresponding to the cast iron is recommended.
Grinding: In Method T-30 the high number of grinding papers is due to the
development of the correct graphite at the finest papers. In case of problems with
retaining of graphite, the steps FG 3 and FG 4 may be used without water. Often
the number of steps can be reduced 共see also Method T-31兲. Always use fresh
paper, as worn down paper may create pull-out of the graphite.
Polishing: In case of routine examination without image analysis, polishing may
stop after the P 1 step for Method C-30 and after the P 2 step in Method T-30.
Electrolytic polishing cannot be recommended, but it may be used for routine
examination of certain materials.

thickness/hardness,
surface layers
Graphite in cast iron A 247 C-30, T-30
El-03
Heat treatment C-30, T-30
of inclusion
content
High planeness
Microhardness, hardness E 10, E 18, E 92, E 103, E 110, C-30
E 140, E 384, E 448
Microstructure A 247, E 3, E 407, E 562, E 883, C-30, T-30,
E 1245, E 1351, E 1382, E 1558 El-03
Sectioning
Mounting

Minutes Minutes/
Hours
Grinding
Polishing
C-30: A P 3 step from T-30 can be added.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper RCD, soft Cloth, Cloth, short
napless, nap,
hard, wov, syn soft, syn
Abrasive Type SiC Dia, spr or susp Dia, spr or Dia, spr or susp
susp
Grit or Grain P220 9 3 1
Size ␮m
Rotation 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen N 共lb兲
Minutes

Section 13.2.2.兲
Polishing
Cloth paper paper paper paper paper napless, napless, napless,
hard, hard, soft,
wov, wov, porous,
silk or syn syn
nonwov,
syn
Type spr spr
or or
susp susp
Grit or P220 P320 P500 P1200 P2400 6 1 0.04/
Grain 0.05
Size ␮m
Alco Alco
Type or or
wat wat
Rotation 300/150 100/150 300/150 300/150 300/150 150/150 150/150 150/150
Disk/
Holder
rpm/
rpm
Comp/ Comp or Comp Comp Comp Comp Comp Comp Contra
Contra contra
Force per 40 共9兲 30 共7兲 30 共7兲 30 共7兲 30 共7兲 30 共7兲 25 10 共2.2兲
Specimen 共5.7兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 4–5 2–3 1
Minutes plane
Etchants
Material: Nodular cast iron „ductile iron…

Nodular cast iron: Carbon 3.0–4.0 %, silicon: 1.8–2.8 %, manganese: 0.1–1.0 %,
phosphorus: 0.01–0.1 %, sulfur: 0.01–0.03 % 共weight %兲.
Comments on Material: Nodular cast iron, also called ductile iron and spheroidal
graphite 共SG兲 cast iron, is a cast iron with the graphite in the form of nodules or
spheres. Unlike malleable cast iron 共see Material/Preparation Tables 30兲, the
nodules are developed during the solidification due to small additions of
magnesium and cerium. The advantage of nodular cast iron is the considerable
increase in toughness, caused by the spheroidal graphite, which makes it
comparable to steel for many purposes. The type, size, and distribution are
standardized in the ASTM Standard Test Method for Evaluating the
Microstructure of Graphite in Iron Castings 共A 247兲. Also a number of other
specifications are described in ASTM standards; some examples are: A 377, A 439,
A 536, and A 439 共see Sections 12.4.2兲.
The metallographic/materialographic examination of the microstructure is as
described in the Material/Preparation Tables 30. Also Methods C-30 and T-30 can
be used for nodular cast iron.
Grinding: Fine grinding with the finer grades of SiC paper in Method T-31 is
important to re-establish the graphite after pull-outs with the coarser grades.
Polishing: At routine examinations, not using image analysis, the specimen
surface after the 3 ␮m polishing step might be satisfactory. Electrolytic polishing
cannot be recommended, but it may be used for routine examination of certain
materials.

thickness/hardness,
surface layers
Graphite in cast iron A 247 C-31, T-31
of inclusion
content
High planeness
E 140, E 384, E 448
Microstructure A 247, E 3, E 407, E 562, E 883, C-31,

E 1245, E 1351, E 1382, E 1558 T-31,
El-03

Sectioning
Mounting

Minutes Minutes/
Hours
Grinding
C-31: SiC grinding paper P220 can be used for PG.

When the difference is
more than 100– 150 ␮m between the center and the periphery, the disk is either
discarded or trued.
Polishing
C-31 and T-31 Both methods can be finished with a fine polishing step with
silica 共see Method T-30
step P 3兲.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, soft Cloth, napless, Cloth, nap-
fixed, res hard, less, hard, wov,
nonwov, syn syn
Abrasive Type Diamond Dia, spr Dia, spr Dia, spr

Size ␮m
Rotation 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen N 共lb兲
Minutes

Section 13.2.2.兲
Polishing
hard, hard, med
wov, silk wov, hard,
silk wov,
wool
Abrasive SiC SiC SiC SiC Dia, spr Dia, spr Dia,
Type or susp or susp spr
or
susp
Grit or Grain P220 P320 P500 P1000 6 3 1
Size ␮m
Lubricant Water Water Water Water Alco or Alco or Wat-oil
Type wat wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp or Comp or Comp Comp Comp Comp
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 5 3–4 3–4
Minutes plane
Etchants
Material: White cast iron

White cast iron: Carbon 1.8–3.6 %, silicon: 0.5–1.9 %, manganese: 0.25–0.8 %,
phosphorus: 0.006–0.2 %, sulfur: 0.06–0.2 % 共weight %兲.
Comments on Material: If the liquid iron-carbon is solidified relatively fast, the
carbide is not formed as graphite like in gray cast iron, but as cementite in a
network. This makes the white cast iron very hard and wear resistant, and the
cementite gives the fractured surface the white appearance. If white cast iron is
heated over a period of time, the cementite will break down to form graphite 共see
Material/Preparation Tables 30兲. White cast iron is often alloyed with nickel,
chromium, or molybdenum or combinations thereof, to improve the wear
resistance. The different types of white cast irons are standardized in the ASTM
Specification for Abrasion-Resistant Cast Irons 共A 532兲共see Sections 12.4.2兲.
Materialographic preparation of white cast iron is relatively easy because of the
very hard cementite.
Sectioning: Wet abrasive cut-off should be done with a soft Al2O3, bakelite bond
cut-off wheel. White cast iron may be difficult to cut because of internal stresses
and the feed speed should be low. For very hard materials a CBN wheel resin bond
may be needed 共see Section 2.4.2兲.
Mounting: Normally mounting is not needed except in the case of examination of
surface layers 共see Material/Preparation Tables 08–15兲, or in the case of obtaining a
shape of the specimen suited for automatic preparation. If possible, the specimen
should be sectioned so that it can be placed in a specimen holder without
mounting.
Grinding: Because of the high hardness, the SiC grinding papers will be worn very
fast, and especially at the PG step several sheets may be needed.
Polishing: The polishing step with silica may be omitted for routine examinations
共see below兲.
Etching: See below and Material/Preparation Tables 28, 33, and, 34.

thickness/hardness,
surface layers
of inclusion
content
High planeness

hardness E 140, E 384, E 448
E 1351, E 1382, E 1558
Sectioning
Cut-Off Wheel Al2O3, bakelite bond. For very hard materials 共⬎HV
500–700兲 a CBN wheel resin bond may be
needed 共see Section 2.4.2.兲.
Mounting
Hot Compression Resin Epoxy with Filler Cold Resin Acrylics

Mounting Mounting with Filler
Time 8–10 Time 6 – 15 min
Minutes Minutes/
Hours
Grinding
C-32 and T-32: The PG step may start with SiC grinding paper grit P120 or
P180, if a high material removal is needed.
Polishing
C-32: P 3. This step can often be omitted.

T-32: A step like P 2 in Method C-32 can be added.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk RCD, hard Cloth, Cloth, med Cloth,
fixed, res napless, nap, soft, napless,
hard, wov, syn soft,
silk porous,
syn
susp susp susp
Grit or Grain P220 9 3 1 0.04/ 0.05
Size ␮m

Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen N
共lb兲
Time Until 4 4 3 1
Minutes plane

Section 13.2.2.兲
Polishing
paper paper paper v. hard, napless, napless,
wov, syn hard hard,
nonwov, wov, syn
syn
Abrasive Type SiC SiC SiC Dia, spr or Dia, spr or Dia,
susp susp spr or
susp
Grit or Grain P220 P320 P500 9 6 3
Size ␮m
Lubricant Type Water Water Water Alco or Alco or Alco
wat wat or wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp or Comp or Comp Comp Comp
Force per 40 共9兲 40 共9兲 40 共9兲 40 共9兲 35 共8兲 30 共7兲
Specimen N 共lb兲
Time Until 0.5 0.5 4 4 3
Minutes plane
Etchants
White cast iron 210 General structure
See also Material/Preparation Tables 28, 33,
and 34
Material: High-alloy steels. Heat-treated, low-alloy steels. Heat-
treated, High-alloy steels. Other ferrous metals
共austenite兲 face-centered cubic, 7.85 g / cm3, 1528° C 共2782° F兲, HV 70 共ferrite兲.
High-alloy steels: ⬎8 % total alloying elements 共weight %兲.
Comments on Material: High-alloy steels have been developed to obtain special
characteristics like resistance to corrosion, heat, and wear. The corrosion resistant
steels, stainless steels, are described in Material/Preparation Tables 34. The heat
resistant steels can be low- or high-alloyed depending on the temperature range.
The high-alloyed steels may contain chromium, molybdenum, nickel, cobalt, and
titanium to obtain highest heat resistance. For iron-based super alloys, see
Material/Preparation Tables 35. The wear resistant high-alloy steels, tools steels,
may contain a high percentage of chromium and manganese, molybdenum, and
vanadium 共see Material/Preparation Tables 38兲.
High-alloy steels can be difficult to prepare because of the often relatively soft
matrix. It can be difficult to conserve all inclusions and carbides, especially if the
specimen should be examined by image analysis. Also hardened alloy steels can be
difficult to prepare; they often have different hardness within the microstructure
and contain a high amount of very hard and brittle carbides. For problems with
smearing, loss of inclusions, etc., see Section 13.6. Often electrolytic polishing can
be used.
Sectioning: Wet abrasive cutting with an alumina, bakelite bond cut-off wheel
with an effective cooling should be without problems. For very hard materials a
CBN wheel resin bond may be needed 共see Section 2.4.2兲. Cutting with a band saw
may give deformations and possible work hardening in steels with an austenitic
structure that should be removed at a prolonged plane grinding, or only used for
initial cutting followed by wet abrasive cutting.
Mounting: Normally mounting is not needed except in case of examination of
surface layers 共see Material/Preparation Tables 08–15兲 or in case of obtaining a
shape of the specimen suited for automatic preparation. If possible the specimen
mounting.
Grinding: In case of water-sensitive inclusions or carbides Method C-33 should be
preferred without the final polishing step.
Polishing: Electrolytic polishing can be recommended for steels not having a too
heterogenous microstructure.
Etching: For observation of certain phases, like carbides, in the microstructure, a
minimal relief can be developed during the last polishing step so that these can be
seen in the microscope without chemical etching 共see Section 9.6兲. A number of
etchants are stated below 共see also Material/Preparation Tables 34兲.

Case of coating thickness/ E 1077 C-33
hardness, surface layers
Grain size, grain E 112, E 930, E 1181, E 2283 C-33,

boundaries T–33,
El-04
Heat treatment C-33,
T-33
Image analysis, rating of E 45, E 562, E 768, E 1077, C-33
inclusion content E 1122, E 1245, E 1268, E 1382,
E 2283
High planeness
Inclusion in steel E 45, E 768, E 1122, E 1245 C-33,
T-33
Microhardness, hardness E 10, E 18, E 92, E 103, E 110, C-33,
E 140, E 384, E 448 T-33
E 768, E 883, E 1077, E 1181, T-33,
E 1245, E 1268, E 1351, El-04
E 1382, E 1558
T-33,
El-04
Structure changes 共forging兲 C-33,
T-33,
El-04
Sectioning
Cut-Off Wheel Al2O3, bakelite bond. For very hard materials 共⬎HV
500–700兲 a CBN wheel resin bond may be
needed 共see Section 2.4.2.兲.
Mounting

Mounting Time 8–10 Time 6–10
Minutes Minutes/
Hours
Grinding
C-33: PG: For low-alloyed steels SiC paper grit P220 should be used.
C-33: FG 1: For low-alloyed steels an RCD soft can be used.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, hard Cloth, Cloth, med.
fixed, res napless, nap, soft, syn
hard, wov,
silk
Abrasive Type Diamond Dia, spr or Dia, spr or Dia, spr or
susp susp susp
Grit/Grain Size ␮m P220 9 6 1
Lubricant Type Water Alco or wat Alco or Alco or wat
susp
rpm/rpm
contra
Specimen N 共lb兲
Minutes

Section 13.2.2.兲
Polishing
paper paper paper paper nap- nap- nap-
less, less, less,
hard, hard, soft,
wov, silk wov, syn porous,
syn
Abrasive Type SiC SiC SiC SiC Dia, spr Dia, spr Alumina
or susp or susp
Grit or P220 P320 P500 P1200 6 3 0.02/ 0.05
Grain
Size ␮m
Lubricant Type Water Water Water Water Alco or Alco or
wat wat
Rotation Disk/ 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Holder
rpm/
rpm
Contra or or or
Specimen
N 共lb兲
Time Until 0.5 0.5 0.5 3–4 3 1
Minutes plane
Etchants
Fe+ 4 − 12 Cr 80, 87, 88, 89, 90, 91, 79, 210 General structure
Fe+ 12− 30 Cr+ ⬍ 6Ni 80, 87, 88, 89, 34, 40, 92, 93, General structure
共400 Series兲 94, 95, 91, 226
96, 97, 98 Sigma phase
31c Carbides
86 Chemical polish etch
219 Grain boundary
220 Darkens delta ferrite
High temperature 89, 25, 105, 106, 97, 212, 221 General structure
107, 108, 213, 86 ␤ precipipate chemical
polish etch
Nonstainless maraging 109, 89, 99, 100, 221 General structure
steels
Nonstainless maraging 83b, 86 Grain boundaries,
steels chemical
polish etch
Material: Stainless steels. Pure iron

Austenitic stainless steels: 15–24 % chromium, 3–22 % nickel.
Ferritic stainless steels: 10.5–27 % chromium.
Martensitic stainless steels: 11.5–18 % chromium.
Duplex stainless steels: 23–28 % chromium, 2.5–5.0 % nickel, 1.0–2.0 %
molybdenum.
Precipitation-hardening stainless steels: 12.25–18 % chromium, 7.5–8.5 % nickel
共weight %兲.
Comments on Material: The stainless steels are corrosion resistant steels

classified according to the type of microstructure, austenitic, ferritic,
austenitic-ferritic, martensitic, duplex, and precipitation-hardening. The austenitic
stainless steels have a microstructure of austenite at room temperature because of
a high nickel content, and they are nonmagnetic. The steels are chromium-nickel
steels, and a typical alloy is the steel 18 % chromium, 8 % nickel. The ferritic
stainless steels are basically chromium steels without nickel, therefore, the ferritic
microstructure. Martensitic stainless steels are chromium steels with a higher
carbon content than other stainless steels making hardening possible. Duplex
stainless steels have a mixed microstructure of ferrite and austenite.
Precipitation-hardening stainless steels are alloyed with elements as copper and
aluminum to establish the precipitation hardening. They can have either a ferritic
or martensitic microstructure.
Pure iron 共Fe兲 has a ferritic microstructure.
Most stainless steels having an austenitic or ferritic microstructure give difficulties
in metallographic/materialographic preparation because these structures are
relatively soft and ductile. Austenite may work harden during cutting and grinding.
It can be difficult to remove all deformation and scratches and obtain a true
structure preserving all inclusions, often brittle carbides and oxides. The
martensitic microstructure is easier to prepare, but in case of brittle carbides,
these can easily be damaged. For advice on smearing, inclusions, etc., see Section
13.6.
The ferrite of pure iron may give problems with deformations 共see Material/
Preparation Tables 28兲.
Sectioning: Wet cut-off cutting with a correct Al2O3, bakelite bond cut-off wheel
will be without problems. Cutting with a band saw and shearing may give
deformations and cold work that should be removed at a prolonged plane
grinding. For deformation sensitive austenitic steels these methods should be
avoided.
Mounting: Normally mounting is not needed except in the case of examination of
surface layers 共see Material/Preparation Tables 08 to 15兲 or in case of obtaining a
shape of the specimen suited for automatic preparation. If possible, the specimen
mounting.
Grinding: Due to deep deformations and possible cold work in the austenite, it is
important that the fine grinding steps are carefully performed to secure that all
deformations and cold work from the sectioning and plane grinding are removed.
Using new SiC grinding paper there is a risk that retained austenite is transformed
into martensite due to mechanical deformation. Also very rough papers and high
grinding forces should be avoided, as deep deformation, introduced in the first
grinding steps may not be removed by the fine grinding.
Polishing: It can be a problem to obtain a perfect ferrite phase as mentioned
Often electrolytic polishing can give very good results 共see Section 13.3兲.
Etching: For stainless steels, observation of inclusions can normally be done

without etching. Chemical etching is relatively difficult, often electrolytic etching
gives good results. A much used electrolytic etching is with 10 g oxalic acid,
100 mL water, using 6 – 8 volts for 20– 30 s, in a stainless steel beaker, using the
beaker as cathode 共see Section 9.5兲. For etchants, see below and Material/
Etchants for pure iron, see Material/Preparation Tables 28.

Case or coating E 1077 C-34
thickness/hardness
surface layers
El-05
High planeness
E 140, E 384, E 448
E 768, E 883, E 1077, El-05
E 1181, E 1245, E 1268, E 1351,
E 1382, E 1558
El-05
Structure changes 共forging兲 C-34, T-34,
El-05
Sectioning
Mounting

Grinding
C-34: PG: Use SiC paper grit P320 for pure iron.
Polishing
T-34: P 1: This step can be changed to an FG 4 step with SiC paper grit P4000,
same data as FG 3.
C-34 and T-34: The final step can be done with alumina 0.02/ 0.05 ␮m.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper RCD, soft Cloth, Cloth,
napless, napless,
hard, wov, syn soft, porous, syn
Abrasive Type SiC Dia, spr or susp Dia, spr or Silica
susp
Grit/Grain P220 9 3 0.04/ 0.05
Size ␮m
Rotation 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Force per 25 共5.5兲 30 共7兲 25 共5.5兲 15 共3.3兲
Specimen N 共lb兲
Minutes
Traditional Method T-34 共For definitions of parameters and consumable see

Section 13.2.2.兲
Polishing
Cloth paper paper paper paper napless, napless, napless,
hard, med soft,
wov, silk hard, porous
wov,
wool
Grit or P220 P320 P500 P1200 6 3 0.04/ 0.05
Grain
Size ␮m
Lubricant Water Water Water Water
Alco or Alco or
Type wat wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/
rpm
Contra or or or
Force per 20 20 20 20 30 共7兲 25 共5.5兲 15 共3.4兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 4 3–5 1–2
Minutes plane
Etchants
Fe+ 12− 20 Cr+ 4 − 10 Ni+ ⬍ 7 % 80, 31c, 89, 99, 100, 91 General
other elements structure
共controlled
transformation,
precipitation
hardening,
stainless
maraging
alloys兲
31c Carbides
86 Chemical polish-
etch
220 Darkness delta
ferrite
Fe+ 15− 30 Cr+ 6 − 40 13b, 89, 87, 88, General structure
Ni+ ⬍ 5% 83a, 80, 94, 95,
other elements 共300 91, 101, 212, 221,
series兲 226
13 a, 102, 31 c, Carbides and
48 c, 213 sensitiza-
tion
Fe+ 16- 25 Cr+ 3 − 6 48, 96, 97, 98 Stains sigma phase
Ni+ 5 − 10
Mn 共200 series兲 103, 104, Delineates sigma

98 phase and welds
of dissimilar
metals
86 Chemical
polish-etch
219 Grain boundary
etch 共no
twins兲
220 Darkens delta
ferrite
Pure iron 74a Grain boundaries
75 Substruc-
ture
210 Colors ferrite
grains
Material: Super alloys, iron based

Super alloys 共Fe based兲: 26 to 55 % nickel, 13 to 23 % chromium, 1 to 2.5 %
titanium, 1 to 9 % molybdenum 共weight %兲.
Comments on Material: The Fe based super alloys are closely related to the high
alloy steels described in Material/Preparation Tables 33.
Etching: See below and Material/Preparation Tables 33 and 34.

thickness/hardness,
surface layers
Grain size. E 112, E 930, E 1382 C-35, T-35,
grain boundaries E1-06
Heat influences zone C-35
Image analysis, E 45, E 562, E 768, E 1245, E 1382, E 2283 C-35
rating of inclusion
content
High planeness

hardness E 140, E 384
E 448
E 768, E 883 E1-06
E 1245, E 1351, E 1382, E 1558
E1-06
Sectioning
Cut-off Wheel Al2O3, bakelite bond
Mounting

Grinding
C-35: PG: SiC paper grit P220 can be used.

C-35: FG 1: Very often this step can be omitted. In that case the step FG 2 共RCD,
soft兲 is prolonged to seven minutes.
When the difference is more than 100— 150 ␮m between the center and the
Polishing
C-35: P 2: Often this step can be omitted.

C-35: P 3: Alumina 共0.02/ 0.05兲 can be used.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, RCD, Cloth, Cloth, short Cloth,
fixed, res hard soft napless, nap, napless,
hard, soft, syn soft,
wov, porous,
silk syn
Abrasive Type Diamond Dia, spr Dia, spr Dia, spr Dia, spr Silica
or susp or susp or susp or susp
Grit/Grain size 220 9 9 6 1 0.04/ 0.05

␮m
Lubricant Water Alco or Alco or Alco or Alco or
Type wat wat wat wat
Rotation Disk/ 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Holder
rpm/rpm
contra
Specimen
N 共lb兲
Time Until 3 3 4 3 1–2
Minutes plane
Traditional Method T-35 共For definitions of parameters and consumable see

Section 13.2.2.兲
Polishing
paper paper paper paper napless, napless, med.
hard, hard, nap,
syn
Abrasive SiC SiC SiC SiC Dia, Dia, Dia,
Type spr spr spr
Size ␮m
Lubricant Water Water Water Water Alco or Alco or Alco or
Type wat wat wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Force per 30 共7兲 30 共7兲 30 共7兲 30 共7兲 30 共7兲 30 共7兲 20 共4.5兲
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 4–5 4 1–2
Minutes plane
Etchants
Super alloys 86, 87, 94, 221, 226 General etch
共Fe based兲
111 General structure

111 ␥⬘ depletion
Material: High strength low-alloy steels

High strength low-alloy steels: Low and medium carbon steels with small amounts
of alloying elements, vanadium, niobium, titanium.
Comments on Material: High strength low-alloy 共HSLA兲 steels are a group of low-
and medium-carbon steels with small amounts of alloying elements to improve the
yield strength. The steels are classified by SAE according to yield strength and by
ASTM according to composition, mechanical property requirements, and
application. Examples of the ASTM specifications are: A 242, A 572, and A 656 共see
Section 12.4.2兲.
The microstructure of HSLA steels is a mixture of ferrite, pearlite, bainite, and
martensite, and the problems regarding preparation are the same as with medium-
and low-carbon steels 共see Material/Preparation Methods 28 and 29兲. In some
cases, water sensitive inclusions should be examined; for this reason the polishing
steps in Methods C-36 and T-36 are stated with water-free lubricants.
Sectioning: At wet abrasive cutting with an Al2O3 cut-off wheel, overheating
should be avoided because martensite can be developed. Cutting pressure should
be moderate and cooling should be efficient on both sides of the cut-off wheel. If
shearing or band sawing is used, the plane grinding should be prolonged to
remove possible deformation or a rougher grinding paper should be used before
grit P220.
Mounting: For routine examination bakelite as powder or tablets is sufficient. In
the case of examination of coatings, other mounting materials should be used 共see
Material/Preparation Tables 08–15兲. For mounting for electrolytic polishing, see
Section 3.11.6.
Grinding: Grinding normally will give no problems with these materials. Care
should be taken that the deformations from plane grinding are effectively removed
before the polishing. If not, the deformed ferrite can be seen after etching and the
process must be repeated from FG 1.
Polishing: The problem can be to obtain a perfect ferrite phase as mentioned
Electrolytic polishing can be recommended for certain alloys.
Etching: A high number of etchants are available for steels. In most cases a
relative small selection will cover the need in a given laboratory 共see Material/
Preparation Tables 28 and 33兲.

Case or coating thickness/hardness, B 487, E 1077 C-36
surface layers Perfect edge retention
Grain size, grain boundaries E 112, E 930, E 1181, E-36,

E 1382 T-36
El-04
Heat treatment C-36,
T-36,
El-04
Image analysis, rating of inclusion E 45, E 562, E 768, C-36
content E 1077, E 1245,
High planeness E 1268, E 1382, E 2283
Inclusion in steel E 45, E 768, E 1245 C-36,
T-36
Microhardness, hardness E 10, E 18, E 92, E 103, E 110, C-36,
E 110, E 140, E 384, E 448 T-36
E 768, E 883, E 1077, E 1122, T-36,
E 1181, E 1245, E 1268, E 1351, El-04
E 1382, E 1558
T-36,
El-04
Structure changes 共forging兲 C-36,
T-36,
El-04
Sectioning
Cut-Off-Wheel Al2O3, bakelite bond
Mounting

Grinding
C-36: PG: SiC paper grit P220 can be used.

Polishing
C-36 and T-36: Steps P 1 and P 2 are stated with water-free diamond
suspensions. These can be changed to normal water-based suspensions.
C-36: P 2: This step can be followed by a final step with silica like step P 3 in
Method C-35.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, soft Cloth, napless, Cloth, med. nap,
fixed, res hard, wov, syn soft, syn
Abrasive Type Diamond Dia, spr or susp Dia, spr or Dia, spr or
susp, water-free susp, water-free
Size ␮m
Lubricant Type Water Alco or wat Alco or oil, Alco or oil,
water-free water-free
Rotation 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
pecimen N 共lb兲
Minutes
Traditional Method T-36 共For definitions parameters and consumables see

Section 13.2.2.兲
Polishing
Cloth paper paper paper paper napless, naplesss, napless,
hard, hard, soft,
wov, wov, porous,
silk syn syn
Abrasive SiC SiC SiC SiC Dia, Dia, Alumina
Type spr spr
or or
susp susp
Grit or P220 P320 P500 P1200 6 3 0.02/ 0.05
Grain
Size ␮m

Type oil, oil,
water- water-
free free
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/rpm
Contra or or or
Force per 35 共8兲 35 共8兲 35 共8兲 25 25 共5.7兲 25 共5.7兲 10 共2.2兲
Specimen 共5.7兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 3 3 1–2
Minutes plane
Etchants
See Material/Preparation Tables 28 and 33.
Material: Carbonitrided steels. Carburized steels. Nitrided steels.
Other surface treated steels

Comments on Material: Case hardening is a term that covers the process of
changing the surface layer of steel by absorption of carbon or nitrogen, or both.
The process can be done in different ways as carbonitriding, carburizing,
cyaniding, nitriding, and nitrocarburizing. With or without further heat treatment
a hard surface layer is created.
Mostly low carbon steels are used for carburization, often a case with a carbon
content of 0.7–1 %, and a hardness of approximately 60 HRC 共HV 700兲. The case
depth varies from 0.3 to 3 mm depending on processing time and temperature.
For nitriding low carbon steels and steels alloyed with Al, Cr, and V are used. The
hardness of the diffusion layer may be up to 70 HRC 共HV 1000兲 and the thickness
0.01– 0.5 mm depending on process time and temperature.
The metallographic/materialographic examination normally covers layer thickness,
diffusion zone, and defects in the layer. For this reason it is very important to
obtain the highest degree of edge retention 共see also the Material/Preparation
Tables 08–15兲.
Sectioning: Cutting, often of a test piece treated along with the work piece, should
be wet abrasive cutting with an Al2O3, bakelite bond cut-off wheel. It is important
that excessive heat and deformation is avoided. When cutting nitrided layers that
are very hard, a relatively soft wheel is used and cooling should be very effective.
If shearing or band sawing is used, the plane-grinding step should be prolonged to
remove possible deep deformation. It is important that the cutting takes place
perpendicular to the surface to be prepared. If the plane of the cross section is not
perpendicular to the plane of the surface layer, the measured thickness will be
greater than the true thickness. For example, an inclination of 10° will contribute
a 1.5 % error.
should be used, preferably epoxy. For very hard coatings hot mounting with epoxy
with a filler should be preferred. Also, a phenolic resin with carbon fibers can be
of advantage. For hot mounting a special application can be made to secure the
edge: Tightly wrap up the specimen in Al foil 共household type兲. This gives a good
separation between mounting material and surface layer. Also, a copper foil can be
used on nitrided and carburized layers giving an excellent edge definition and
contrast. Choose a mounting material with hardness as close as possible to the
hardness of the coating. As a less ideal alternative, cold mounting with epoxy or
an acrylic material with filler can be used.
Grinding: The preparation process should secure the highest possible edge
retention. This means that all grinding, either on SiC grinding paper, diamond
pads, or rigid composite disks 共RCDs兲, should be as short as possible.
In Method T-37 the grinding is suggested with diamond pads, considered for very
hard surface layers. In case of softer layers these pads can be changed to SiC
grinding paper, as stated in Method T-32 共see below兲.
It has been found that the use of fixed diamonds for plane grinding of certain
nitrided and carburized layers may introduce fine cracks in the hard layer,
therefore, SiC paper should be used 共see below兲.
Polishing: Also the polishing steps should be kept as short as possible.
Etching: See Material/Preparation Tables 28, 33, and 34.

thickness/hardness,
surface layers
Prefect edge retention
Image analysis, rating E 45, E 562, E 768, E 1077 C-37, T-37
of inclusion content E 1245, E 1268,
High planeness E 1382, E 2283
Microhardness, hardness E 10, E 18, E 92, E 103, C-37, T-37
E 140, E 684, E 448
Microstructure A 892, E 3, E 45, E 407, E 562, E

768,
E 883, E 1077, E 1245, E 1268,
E 1351, E 1382, E 1558
Sectioning
Mounting
Hot Compression Resin Expoxy Cold Mounting Resin Epoxy

Mounting with Filler with filler
Time 9 Time 6–8 h
Minutes Minutes/
Hours
Grinding
C-37 and T-37: PG: For certain nitrocarburized/nitrided layers, disks/pads with
fixed diamonds should be avoided 共see above兲. SiC paper grit P220 should be
used. Also FG 1 in Method T-37 shall be changed to SiC paper grit P320/P500
共see Method T-32兲.
C-37: Very often FG 1 can be changed to RCD, soft and FG 2 can be omitted.
T-37: In case of relatively soft surface layers, the diamond pads in PG and FG 1
can be changed to SiC grinding paper 共see Method T-32兲.
Polishing
T-37: To improve edge retention, the step P 2 can be changed to P 2 from

Method C-37.

Section 13.2.2.兲
Grinding PG FG 1 FG 2 P1 P2
Polishing
Disk/Cloth Dia, disk RCD, hard RCD, soft Cloth, Cloth, med
fixed, res napless, nap, soft, syn
hard, wov,
syn
Abrasive Diamond Dia, spr or Dia, spr or Dia, spr or Dia, spr or
Type susp susp susp susp
Grit or 220 9 3 3 1
Grain
Size ␮m
Lubricant Water Alco or wat Alco or wat Alco or wat Alco or wat
Type
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/ Comp or Comp Comp Comp Comp
Contra contra
Force per 35 共8兲 25 共5.5兲 25 共5.5兲 40 共9兲 25 共5.5兲
Specimen N
共lb兲
Time Until 5 4–5 4–5 1–2
Minutes plane

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, pad Dia, pad met Cloth nap- Cloth, Cloth,
met less, v. hard napless, napless,
nonwov or hard, soft,
wov, syn wov, syn porous, syn
Abrasive Type Diamond Diamond Dia, spr or Dia, spr or Silica
susp susp
Grit or Grain 125 40 9 3 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Alco or wat Alco or wat Alco or wat
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp or Comp Comp Contra
contra contra
Force per 35 共8兲 35 共8兲 40 共9兲 40 共9兲 15 共3.4兲
Specimen N 共lb兲
Time Until plane 2 4–5 4–6 1
Minutes
Etchants
See Material/Preparation Tables 28, 33, and 34.
Material: High-speed steels. Low-alloyed tool steels. Other tool
steels
Comments on Material: The tool steels cover a wide range from the highly
alloyed high-speed steels to low-alloy steels with small amounts of a few alloying
elements. Most tool steels contain molybdenum or tungsten, or both. Often other
elements like vanadium, cobalt, nickel, and chrome are added. The tool steels are
classified by the American Iron and Steel Institute 共AISI兲 using a letter to represent
each class of steel. Tool steels are metallographically/materialographically
examined for inclusion content, decarburization, degree of spheroidization, grain
size, hardness, etc., and they are often difficult to prepare because of the hardness
and the brittle carbides. For advice on artifacts developed during the preparation,
see Section 13.6.
Sectioning: In the case of nontempered tool steels, it is important that the
sectioning takes place without excessive heat because this will introduce localized
tempering effects. Cutting should take place as wet, abrasive cutting with an
efficient cooling, preferably using a thin cut-off wheel, or a relatively soft wheel, or
both. The feed speed should be low with a low force in the cut. For high-hardness,
high-alloy steels, precision cutting with a thin CBN cut-off wheel may be of
advantage, producing a cut surface with very little damage. Steels with a hardness
below 35 HRC may be cut using a band saw, but in this case, because of the
considerable deformation, the plane grinding should start with SiC grinding paper
rougher than grit 220. In case of as-quenched high-alloy steels, the specimen may
be sectioned by fracture.
Mounting: For routine examination bakelite as powder or tablets is sufficient if
heat degredation is not anticipated. In the case of examination of coatings, other
mounting materials should be used 共see Material/Preparation Table 08–15兲. For
mounting for electrolytic polishing, see Section 3.11.6.
Grinding: The often very hard material will wear out the SiC grinding papers in a
very short time, and often several sheets of each grain size should be used. In case
of pull-outs of carbides at high-alloy steels, Method C-38 should be preferred.
Polishing: For routine examination, the number of steps may be reduced 共see
below兲.
Etching: A number of etchants are stated below.

Case or coating B 748, C 664 C-38
thickness/hardness,
surface layers
Image analysis, E 45, E 562, E 768, E 1077 C-38, T-38

rating of inclusion E 1245, E 1268, E 1382, E 2283
content
High planeness
Inclusions in steel E 45, E 768, E 1245 C-38
hardness E 140, E 384, E 448
Microstructure A 892, E 3, E 45, E 407, E 562, E
768,
E 883, E 1077, E 1245, E 1268, E
1351, E 1382, E 1558
Sectioning
Mounting

Grinding
C-38: For certain tool steels, the step P 1 can be changed to an RCD, soft.
T-38: For routine examination the step FG 3 may be omitted.
Polishing
C-38: For certain tool steels, the step P 2 can be changed to P 3 from Method
T-38 or P 3 共Method T-38兲 can be added.
T-38: In case of routine examinations, the step P 2 can be changed to step P 1
from Method C-38, as the last step.

Section 13.2.2.兲
Grinding/ PG FG P1 P2
Polishing
Disk/Cloth Dia, disk, RCD, hard Cloth, Cloth, med.

fixed, res napless, nap,
hard, wov, soft, syn
syn
Abrasive Type Diamond Dia, spr or Dia, spr or Dia, spr or
susp susp susp
Grit or Grain Size P220 9 3 1
␮m
Rotation Disk/ 300/ 150 150/ 150 150/ 150 150/ 150
Holder
rpm/rpm
contra
Force per Specimen 35 共8兲 35 共8兲 35 共8兲 40 共9兲
N 共lb兲
Minutes

Section 13.2.2.兲
Polishing
paper paper paper paper napless, napless, napless
hard, hard, soft
wov, silk wov, porous,
syn syn
Abrasive Type SiC SiC SiC SiC Dia, spr Dia, spr Alumina
or susp or susp
Size ␮m
Type wat wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 5 4 1–2
Minutes plane
Etchants
Tool steels 74a, 80, 14 General structure
110 Grain boundaries in tempered tool steel
210, 211 Colors ferrite, lower alloy grades
214 Colors cementite
224, 225 Carbides attacked and colored
Material: Cement clinker. Concrete
Material Properties: Portland cement clinker, mineralogical composition: Alite

共C3S兲 35–75 %, Belite 共C2S兲 0–40 %, Aluminate 共C3A兲 1–10 %, Ferrite 共C4AF兲 2–15
%, Periclase 共MgO兲 0–3 %, Free lime 共CaO兲 0–5 %, Arcanite 共K2SO4兲 0–3 %,
Ca-Langbeinite 共2CaSO4兲 0–3 %.
Comments on Material: Portland cement clinker is a raw material for cement
production consisting of several mineral phases with different physical properties,
as mentioned above.
Hardened concrete consists of cement paste mixed with aggregates like sand and
stone.
Cement clinker and concrete can be examined in reflected light and in transmitted
light. The preparation of cross sections for reflected light is stated below. Thin
sections for transmitted light is described in Section 7.13.
Both cement clinker and concrete often are very sensitive to water used during the
preparation and, consequently, this should be avoided, especially during the last
steps of the preparation.
Sectioning: The material being brittle should be treated carefully to avoid
damage. Often it can be of advantage to impregnate the specimen before cutting
共see below兲. Cutting is preferably done with a precision cut-off machine with a
thin cut-off wheel, diamond, metal bond or SiC, bakelite bond and with a
water-free coolant.
Mounting: Very often the specimen is porous so that impregnation with epoxy is
needed to stabilize the material. Also, often the examination, especially at
concrete, is done to determine pores 共air voids兲 and microcracks, and therefore it
can be recommended to add fluorescent dye to the epoxy 共see Section 3.10兲.
Grinding: The traditional method, T-39, stated below is based on lapping on cast
iron disks, as known from preparation of mineralogical materials. Often the
lapping can be changed to the use of SiC grinding paper, as indicated under
Preparation Process 39 below.
Polishing: The two methods stated below have a 3 ␮m step as the last polishing
step. If needed, this step can be followed by finer steps, as indicated under
Preparation Process 39 below.
Etching: Normally these materials are not etched.

Case or coating Cement clinkers and concrete are covered C-39
thickness/hardness, by a number of ASTM standards. These are
surface layer not stated here, as it is considered outside
Perfect edge retention the scope of this book.
Grain size, grain C-39, T-39
boundaries
Image analysis, rating C-39
High planeness
Microhardness, C-39, T-39
hardness
Porosity C-39
Sectioning

共0.019 in兲 thickness
Mounting

Time Time 8 – 12 h
Grinding
C-39: PG, if material is very water sensitive use alcohol or glycerol instead of
water.
C-39: PG and FG: For clinker, lower force on specimens to 15 N.
C-39: In some cases 共clinker兲 FG 1 can be omitted.
T-39: In some cases the lapping on cast iron disks can be changed to SiC paper,
P220, P320, P500 and P1000 using glycerol as cooling fluid.
Polishing
C-39: P 1: For clinker, lower force per specimen to 10 N.

C-39 and T-39: If needed, P 1 can be followed with one or two steps, see
P 2 in Method C-38 with water-free lubricant, followed by P 2 in Method T-37.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, fixed, Dia, disk, fixed, RCD, soft Cloth, napless,
res res hard, wov, syn
Abrasive Type Diamond Diamond Dia, spr or susp, Dia, spr or
water-free susp,
water-free
Grit or Grain P220 P1200 9 3
Size ␮m
Lubricant Type Water/ Water/glycerol Alco, Alco, water-
glycerol water-free free
Rotation 300/ 150 300/ 150 300/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or contra Comp Comp Comp
Specimen N /lb
Time Until plane 5 5 5
Minutes

Section 13.2.2.兲
Polishing
Disk/Cloth Cast iron Cast iron Cast iron Cast iron
Cloth,
disk disk disk disk
napless,
hard,
wov, syn
Abrasive Type SiC powder SiC powder SiC powder SiC powder Dia, spr or
susp, water-
free
Grit or Grain P220 P400 P800 P1200 3
Size ␮m
Lubricant Type Glycerol Glycerol Glycerol Glyecerol Alco or oil,
water-free
Rotation 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Contra Contra Contra Contra Comp

Specimen N
共lb兲
Time 2–3 2–3 2–3 2–3 5
Minutes
Material: Minerals. Ores
Comments on Material: Minerals, ores, and rocks cover a wide field of materials
with a high variety of phases. Most often minerals are brittle and hard, but often
with a very different hardness of the different phases. This makes preparation of
minerals relatively difficult, both because of the risk of deformation, the
brittleness, pores, and cracks, creating the risk of pull-outs, and the tendency for
relief between the phases.
Minerals are prepared as polished sections for reflected light examination and as
thin sections for transmitted light examination. Below the preparation of polished
sections is described; thin sections are described in detail in Section 7.13 共see also
Material/Preparation Tables 39兲.
Sectioning: It is important that the often very hard and brittle material is not
damaged too much during the sectioning. Often the cutting of an intermediate
piece is cut with a large machine specially built for cutting of minerals, using a
diamond cut-off wheel, metal bond. For the actual specimen, wet abrasive cutting
is often done with a thin diamond, metal bond cut-off wheel on a precision cut-off
machine to ensure a good surface. In case of very brittle materials, with pores and
cracks, an impregnation before the cutting is recommended 共see below兲. For softer
minerals an SiC bakelite bond cut-off wheel can be used.
Mounting: Often the specimen, being brittle and with pores and cracks, should be
impregnated under vacuum with an epoxy 共see Section 3.10兲. To easily distinguish
pores and cracks, the epoxy resin can be added as a dye 共see Section 3.10兲. Also,
an impregnetion with a dye makes it possible to distinguish between original pores
and “pores,” pull-outs, caused by the preparation process 共see Section 13.6兲.
Grinding: The “traditional” grinding of minerals is made as a lapping with loose
grains 共see Section 6.7.7兲. This method is stated in Method T-39, however, below,
the two methods stated are with fixed grains considered the most useful for
polished sections. Some phases in minerals are very sensitive to deformation like
certain soft and ductile metals. For this reason the fine grinding step with 9 ␮m
diamond in Method C-40 and the steps with 9 ␮m and 6 ␮m in Method T-40 are
very important to create a deformation free surface, and these steps should be
prolonged if the deformation is not reduced to a satisfactory level that can be
removed by the 3 ␮m step.
Polishing: In the case of phases with very different hardness, the polishing time
should be kept as short as possible and the force as low as possible to reduce
relief.
Etching: Etching of minerals can be done for identification of the single phases in
a mineral based on the reaction of a specimen material to a standard set of
reagents. Another approach is to use the reagents for revealing the microstructural
details, as it is known from etching of metals. Both approaches are relatively
complicated and fall outside the scope of this book.

Case or coating ASTM standards covering C-40
thickness/hardness, minerals and ores are
surface layers Perfect edge not stated here, as it is
retention considered outside the
scope of this book.
Image analysis, rating of inclusion C-40
content
High planeness
Microhardness, hardness C-40, T-40
Porosity C-40
Sectioning

共0.019 in兲 thickness
Mounting

Mounting Time Time 8 – 12 h
Grinding
C-40: For soft/brittle materials, SiC paper grit P320 can be used.
C-40: FG: For hard materials a step like FG 1 in Method C-39 can be added.
Attention: In C-methods, when using RCD: the disk turns concave during use.
Polishing
C-40: P 1 and P 2: For hard materials a step like P 2 in Method C-38 can be used
between the steps P 1 and P 2.
T-40: P 1 can be followed by a P 2 step like in Method C-40

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk RCD, soft Cloth, Cloth
hard, soft,
wov, syn porous, syn
Abrasive Type Diamond Dia, spr, or susp Dia, spr or Silica
susp
Grit or Grain P220 9 3 0.04/ 0.05
Size ␮m
Rotation 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen N 共lb兲
Minutes

Section 13.2.2.兲
Grinding/ FG 3 P1
Disk/Cloth Dia, pad Cloth, Cloth, napless, Cloth, Cloth,
bak napless, v. hard napless, napless,
v. hard, nonwov/ v. hard hard,
nonwov/ wov nonwov/ wov, silk
wov wov
Abrasive Type Diamond Dia, spr Dia, spr Dia, spr Dia, spr
or susp or susp or susp or susp
Grit or Grain 30 9 6 3 1
Size ␮m
Lubricant Type Water Alco Alco Alco Alco
or wat or wat or wat or wat
Rotation 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp Comp Comp Comp Comp
Force per 25 共5.7兲 30 共7兲 30–40 共7–9兲 30–40 共7–9兲 10–30 共2.3–7兲
Specimen N 共lb兲
Time Until 5 5 5 2
Minutes plane
Material: Pure aluminum. Cast aluminum alloys
Material Properties: Aluminum: Face-centered cubic, 2.699 g / cm3, 660.2° C

共1220° F兲, HV 150.
Cast alloy: Aluminum-silicon: 12.5 % Si 共eutectic composition兲. Other cast alloys:
Aluminum-silicon-magnesium, aluminum-silicon copper, aluminum
silicon-copper-magnesium, aluminum-magnesium, aluminum-zinc-magnesium,
aluminum-copper-titanium-magnesium 共weight %兲.
Comments on Material: Commercially pure aluminum has an aluminum content
higher than 99 % for wrought alloys and 99.5 % for cast alloys. Cast alloys can be
alloyed with a number of elements as mentioned above. Aluminum and its alloys
are classified through a number of systems, the most important is the system
established by the Aluminum Association 共see below兲. Another important system
uses the chemical symbols of the most important alloying elements combined with
a number stating the content in weight %. AlMg3MnCr describes an alloy with 3 %
magnesium and amounts of manganese and chromium, normally 共but not always兲
below 1 % each. Less important alloying elements are not mentioned.
Aluminum Association has developed a system for wrought and cast alloys
consisting of four numbers followed by a — with a letter and a number. For
wrought alloys the four numbers are like: nnnn, at cast alloys the numbers have a
dot: nnn.n. For wrought alloys the first number expresses:
1nnn Commercially pure aluminum 共⬎99 % 兲
2nnn Copper as most important alloying element
3nnn Manganese
4nnn Silicon
5nnn Magnesium
6nnn Magnesium and silicon.
7nnn Zinc
8nnn Other alloying elements
9nnn Is not used
For cast alloys the first number expresses:
1nn.n Commercially pure aluminum 共⬎99.5% 兲
2nn.n Copper
3nn.n Silicon with copper or magnesium
4nn.n Silicon
5nn.n Magnesium
6nn.n Is not used
7nn.n Zinc
8nn.n Tin
9nn.n Other alloying elements
The letter following the — expresses heat treatment and the number will express
further specification of the alloy.
ASTM has specified a high number of aluminum alloys and a number of test
methods for aluminum.
Pure aluminum is a very soft and ductile metal that can be difficult to prepare
mechanically. It is important that deformations developed during sectioning and
grinding are removed through the polishing steps. Also, there is a risk of
embedded grains 共see Section 13.6.4兲. Electrolytic polishing can be done with a
perchloric acid electrolyte and often gives very good results. Cast aluminum alloys
and wrought alloys are easier to polish mechanically and they are normally not
suited for electropolishing.
Sectioning: Wet abrasive cutting with an SiC bakelite bond cut-off wheel should
be recommended. To avoid solid state transformation in certain materials, an
efficient cooling is important. If shearing or band sawing are used, it is important
that the induced heavy deformation is removed during the plane grinding step.
Mounting: Both hot and cold mounting materials can be used. In the case of
heat-sensitive alloys cold mounting is recommended. For examination of pores
共castings兲, vacuum impregnation may be of advantage 共see Section 3.10兲.
Preferably the mounting material should be a little harder than the hardest
constituent in the specimen material. In the case of examination of thin layers it
can be recommended that the specimen is tightly wrapped in thin metal foil 共e.g.,
household aluminum foil or nickel foil兲 and then hot mounted. In this way the
surface layer can be easily distinguished from the mounting material.
Grinding: It is important that the deformation from sectioning and the rough
grinding steps are removed. If the grinding steps give too high deformation, the
force per specimen should be reduced.
Polishing: The rough polishing steps with 6 and 3 ␮m are important. If strong
deformation can be seen after 3 ␮m, the process should be repeated from FG 1.
With only small deformation the time can be prolonged or the force increased, or
both. If relief develops between matrix and a second phase, Method C-41 should
be used.
Electrolytic polishing can be used for pure aluminum and for not too
heterogenous alloys.
Etching: It can be difficult to etch the surface of aluminum due to a thin oxide
film. Also, it is difficult to etch the matrix and several intermetallic phases and
precipitates with the same etchant, making the use of several ecthants necessary. It
is, however, possible to avoid this for a number of alloys by using a color etchant
based on potassium permanganate 共Weck, see Ref. 47, Part I兲: 100 mL distilled
water +4 g potassium permanganate, after dissolving: +1 g sodium hydroxide.
Immersion in 15 s at room temperature with a freshly prepared solution. The
drawback with this etchant is that the specimen surface must be absolutely free
from deformation. This can be obtained by pre-etching the surface with 100 mL
distilled water +2 g sodium hydroxide. Immersion in 30 to 60 s at room
temperature. For other etchants, see below, and Material/Preparation Tables 42/43.

Case or coating thickness/ B 487 C-41
hardness,
surface layers
Grain size, grain E 112, E 930, E 1181, E 1382 C-41, T-41
boundaries El-10 共pure
Al兲
Image analysis, E 562, E 1245, E 1382 C-41, T-41
rating of inclusion
content
High planeness
E 110, E 140, E 384,
E 448
E 1181, E 1245, E T-41,
1351, E 1382, E 1558 El-10 共pure
Al兲
Sectioning
Cut-Off Wheel SiC, bakelite bond
Mounting

Grinding
C-41: PG: If possible use SiC paper grit P320.

T-41: Very often FG 4 can be omitted.
Polishing
C-41: P 2: This step can often be omitted.

Pure Al: Electrolytic polishing will give good results.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper RCD, soft Cloth, Cloth, med Cloth,
napless, nap, soft, syn napless,
med hard, soft, porous,
wov, wool syn
Abrasive Type SiC Dia, spr or Dia, spr or Dia, spr or Silica
susp susp susp
Grit or Grain P220 9 3 1 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Wat-oil Wat-oil
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp Comp Comp Comp Contra
Force per 25 共5.7兲 30 共7兲 25 共5.7兲 20 共4.5兲 15 共3.3兲
Specimen N 共lb兲
Time Until plane 5 5 1–2 1–2
Minutes

Section 13.2.2.兲
Polishing
Disk/Cloth SiC SiC SiC SiC SiC Cloth, Cloth, Cloth,
paper paper paper paper paper nap- nap- nap-
less, less, less,
hard, med soft,
wov, hard, porous,
silk wov, syn
wool
Type spr spr
or or
susp susp
Grit or P220 P320 P500 P1200 P2400 6 3
0.04/
Grain 0.05
Size ␮m
Lubricant Water Water Water Water Water Alco or Wat-
Type wat oil
Rotation 300/150 300/150 300/150 300/150 150/150 150/150 150/150 150/150
Disk/
Holder
rpm/
rpm

Contra or or or or
contra contra contra contra
Force per 25 共5.7兲 25 共5.7兲 25 共5.7兲 25 共5.7兲 25 共5.7兲 25 共5.7兲 20 共4.5兲 15 共3.4兲
Specimen
N
共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 4 3–4 1–2
Minutes plane
Etchants
Material Etchants see 共Table 12.2兲 Uses
Pure aluminum 1a, 2, 3 General structure
Cast aluminum 共2000 series兲 3, 2, 1a General structure
8a, 6, 7 Phase identifications
Cast aluminum 共4000 series兲 3, 1a General structure
Material: Other aluminum alloys
Material Properties: Aluminum: Face-centered cubic, 2.699 g / cm3, 660.2 °C
共500° F兲, HV 150.
Etching: See Material/Preparation Tables 41/43 and below.

Case or coating thickness/hardness, B 487 C-42
surface layers
El-10
content
High planeness
E 110, E 140, E 384, E 448
Microstructure E 3, E 407, E 562, E 883, C-42, T-42,
E 1181, E 1245, E 1351, El-10
E 1382, E 1558
Sectioning
Mounting

Grinding

Polishing
C-42: P 1: For harder alloys this step can be changed to a napless, hard, wov, silk
cloth.
C-42: For softer alloys the step P 1 from Method T-42 can be added, between FG
1 and P 1.
T-42: P 3 can be followed by a step with silica, see C-42. Also at harder alloys the
step P 3 can be omitted.
Often electrolytic polishing can be recommended for the examination of the
microstructure.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper RCD, soft Cloth, Cloth, napless,
napless, med soft, porous, syn
hard, wov,
wool
Abrasive Type SiC Dia, spr or susp Dia, spr or Silica
susp
Grit or Grain P220 9 3 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Wat-oil
Rotation 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm

contra
Specimen N 共lb兲
Time Until 5 3 1–2
Minutes plane

Section 13.2.2.兲
Polishing
hard, hard, nap,
syn
Grit or P220 P320 P500 P1200 6 3 1
Grain
Size ␮m
Lubricant Water Water Water Water Alco or Alco or Wat-oil
Type wat wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 4 4 1
Minutes plane
Etchants
Al alloys 3, 1a, 2 General structure
共7000 series兲 4, 5 Grain structure under polarized light
3b, 6 Phase identification
Material: Wrought aluminum alloys
Material Properties: Aluminum: Face-centered cubic, 2.699 g / cm3, 660.2° C

共500° F兲, HV 150. Wrought aluminum alloys: Manganese. Magnesium.
Magnesium-manganese-chrome. Magnesium-silicon. Copper. Copper-manganese
and copper-silicon-manganese. Zinc-magnesium. Zinc-magnesium-copper.
Lithium-copper-magnesium.
Polishing: Alloys containing magnesium may be sensitive to water and should be
polished with water-free lubricants 共see also Material/Preparation Tables 41兲.
Etching: See Material/Preparation Tables 41/42 and below.

Case or coating B 487 C-43
thickness/hardness,
surface layers
El-10
Image analysis, rating E 562, E 1245, E 1382 C-43, T-43
High planeness
E 140, E 384, E 448
Microstructure E 3, E 407, E 562, E 883, E 1181, C-43, T-43,
E 1245, E 1351, E 1382, E 1558 El-10
Sectioning
Mounting

Grinding

C-43: FG 2: Very often this step can be omitted.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper RCD, soft RCD, soft Cloth, Cloth, nap-
napless, less, soft,
med hard, porous,
wov, wool syn
Abrasive Type SiC Dia, spr or Dia, spr or Dia, spr or Silica
susp susp susp
Grit or Grain P220 9 3 3 0.04/ 0.05
ize ␮m
Lubricant Type Water Alco or wat Alco or wat Wat-oil
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Specimen
N 共lb兲
Time Until plane 5–7 5 5 1
Minutes

Section 13.2.2.兲
Polishing
med soft,
hard, porous,
wov, syn
wool
Abrasive SiC SiC SiC SiC SiC Dia, spr Alumina
Type or susp
Grit or Grain P220 P320 P500 P1200 P2400 3 0.02/
Size ␮m 0.05
Lubricant Water Water Water Water Water Wat-oil

Type
Rotation 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
or or or or
contra contra contra contra
Force per 25 25 25 25 25 20 共4.5兲 15 共3, 4兲
Specimen 共5.7兲共5.7兲共5.7兲共5.7兲共5.7兲
N 共lb兲
Time Unit 0.5–1 0.5–1 0.5–1 0.05–1 3–4 1–2
Minutes plane
Etchants
1000 series 1a, 2, 3, General structure
4, 5 Grain structure under
polarized light
6, 7 Phase identifications
3000 series 3, 1a General structure
polarized light
8a, 6, 7 Phase identifications
5000 series 3, 1a, 2, 6, 8a General structure
polarized light
6000 series 3, 1a, 2, 6, 8a, 222 General structure
polarized light
1a, 2, 7, 6, 8a Phase identifications
Material: Pure antimony. Sb alloys, and Sb bearing alloys. Pure
bismuth. Bi alloys
Material Properties: Antimony: Hexagonal, 6.691 g / cm3, 630.5° C 共1167° F兲.

Bismuth: Hexagonal, 9.78 g / cm3, 271.3° C 共520° F兲, HB 70.
Comments on Material: Both antimony and bismuth are seldomly used as pure
metals, but mostly used as alloying elements. Antimony is used for bearing alloys.
Pure antimony is relatively hard and pure bismuth is soft. Both metals are very
brittle.
Sectioning: Care should be taken that the brittle materials are not damaged too
much during the cutting. At wet abrasive cutting, a thin SiC cut-off wheel bakelite
bond should be used. To avoid cracking during cutting it may be useful to mount
the specimen in epoxy before cutting.
Mounting: Both hot and cold mounting can be used. Be careful that the high
pressure during hot mounting doesn’t damage the brittle specimen.
Grinding: During grinding with SiC grinding paper, the paper may be loaded with
the material because this is not taken away by the water flow. A loaded paper
should not be used as it will give stronger damage to the specimen. The water flow
should be strong and the aggressiveness of the paper can be dampened by adding
a small amount of hard wax to the paper surface before use, or the new paper can
be “run-in” with a hard material in a few seconds.
Polishing: It is important that all deformations from the grinding are removed
after the rough polishing step P 1. For polishing of pure antimony and pure
bismuth, a solution of 3 % nitric acid in glycerol can be added to the silica used
for the last step. At polishing of Sb alloys containing lead, the last polishing step
can be with a 0.3 alumina suspension with added ammonium tartrate, 1 g per 1 L
distilled water. At polishing of Bi, the 6 ␮m step can be omitted 共see below兲.
Both pure antimony and bismuth are well suited for electrolytic polishing.
Etching: See below.

thickness/hardness,
surface layers
Grain size, grain E 112, E 930, E 1181, E 1382 C-44, T-44
boundaries El-10
High planeness
hardness E 140, E 384, E 448
E 1245, E 1351, E 1382, E 1558 El-10
Sectioning
Mounting
Hot Compression Resin Bakelite Cold Mounting Resin Acrylics/Epoxy

Mounting Time 8–9 Time 6 – 10 min/ 6 – 8 h
Minutes Minutes/
Hours
Grinding
T-44: For harder alloys, FG 4 can be omitted.

Polishing
C-44 and T-44: P 1: At polishing of bismuth and Bi alloys this step can be
omitted.
C-44: P 3: At polishing of bismuth and Bi alloys the time may be increased to
several minutes.
For the final step chemical mechanical polishing can be recommended 共see
above兲.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper SiC paper RCD, soft Cloth, Cloth, Cloth,
napless, napless, nap-
hard, med less,
wov, silk hard, soft,
wov, porous,
wool syn
Abrasive Type SiC SiC Dia, spr Dia, spr Dia, spr Silica
Grit or Grain P220 P320 9 6 3 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Water Alco or Wat-oil
wat
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/
rpm
Contra contra
Force per 25 共5.7兲 25 共5.7兲 30 共7兲 25 共5.5兲 25 共5.7兲 15 共3.3兲
Specimen
N 共lb兲
Time Until 0.5–1 5 4 3 1
Minutes plane

Section 13.2.2.兲
Polishing
Cloth paper paper paper paper paper nap- nap- nap-
less, less, less,
hard, med. soft,
wov, hard, por-
silk wov, ous,
wool syn
Abrasive SiC SiC SiC SiC SiC Dia, spr Dia, spr Silica
Grit or P220 P320 P500 P1200 P2400 6 3 0.04/
Grain 0.05
Size ␮m
Lubricant Water Water Water Water Water Wat-oil Wat-oil
Type
Rotation 300/150 300/150 300/150 150/150 150/150 150/150 150/150 150/150
Disk/
Holder
rpm/
rpm
Contra or or or
Force per 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 20 共4.5兲 15 共3.4兲 15 共3.4兲
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 4–5 3 1
Minutes plane
Etchants
Sb, lean, 935 General structure
Sb alloys
Sb 938 Grain contrast
Sb, Sb alloys 936, 937, 940 General structure
Sb-Pb alloys 938, 941 General structure
Bi, Bi alloys 937, 940 General structure
Bi-Sn alloys, Bi-Ca alloys 938 General structure
Material: Pure beryllium. Be alloys
Material Properties: Beryllium: Hexagonal close-packed, 1.8 g / cm3, 1350° C
共2462° F兲, HRB 80.
Comments on Material: Beryllium is a light metal which is mostly used as an
alloying element, improving the strength of the alloy. Pure beryllium is toxic to
inhale which means that the preparation process, when dust is developed, must
take place in a glove box or under an efficient fume hood, or both.
Pure beryllium resembles magnesium 共see Material/Preparation Tables 53兲 it
deforms and fractures easily and preparation must be done with great care.
Sectioning: For wet abrasive cutting a thin SiC bakelite bond cut-off wheel should
be used. For alloys based on copper, a medium hard wheel is recommended. For
nickel-based alloys a softer wheel should be used. The cooling should be efficient
to avoid thermal damage. When cutting pure beryllium and alloys with a high Be
content, it is important that the sludge, metal dust, and particles from the wheel
are correctly disposed of because of the toxicity.
Mounting: Both hot mounting and cold mounting can be used.
Grinding: When wet grinding pure beryllium and alloys with a high Be content
the dust is bound by the water, but care must be taken to have the correct disposal
of the sludge. For pure beryllium the force on the specimen should be reduced and
often it can be of advantage to make the grinding on a stationary paper in one
direction.
Polishing: For pure beryllium and certain alloys electrolytic polishing is
recommended. Also a chemical mechanical polishing can be used 共see below兲.
Etching: Pure beryllium can be examined in polarized light. For etchants, see
below.
Purpose ASTM Standard 共See Section 12.4.兲 Method

thickness/hardness,
surface layers
El-10
High planeness
E 110, E 140, E 384,
E 448
Microstructure E 3, E 407, E 562, E 883, E 1181, E 1245, C-45, T-45,
E 1351, E 1382, E 1558 El-10
Sectioning
Mounting

Grinding

T-45: Pure Be is relatively brittle and grinding should be performed with Method
T-45, but with lower force than indicated.
Polishing
C-45, T-45: For the last step with silica, one part of hydrogen peroxide 共30 %兲
can be added to five parts of silica suspension.

Section 13.2.2.兲
Grinding PG FG 1 P1 P2
Polishing
Disk/Cloth Dia, disk, RCD, soft Cloth, Cloth,
hard, soft,
wov, silk porous, syn
Abrasive Type Diamond Dia, spr Dia, spr or Silica
or susp susp
Grit or Grain P220 9 3 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Water
rpm/rpm
Comp/Contra Comp or contra Comp Comp Contra
Force per Specimen 20 共4.4兲 30 共6.6兲 25 共5.5兲 15 共3.4兲
N 共lb兲
Minutes
Traditional Method T-45 共For definitions of parameters and consumables

see Section 13.2.2.兲
Polishing
hard, hard, soft,
wov, wov, porous,
silk syn syn
Grit or P220 P320 P500 P1200 6 3 0.04/ 0.05
Grain
Size ␮m
Lubricant Water Water Water Water Alco-wat Wat-oil
Type
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/
rpm
Comp/ Comp or Comp or Comp or Comp Comp Comp Contra
Contra contra contra contra
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 4–5 3–4 1–2
Minutes plane
Etchants
Pure Be 9, 10 General structure via polarized light
Be alloys 11 General structure
Material: Pure chromium. Cr alloys
Material Properties: Chromium: Body-centred cubic, 7.17 g / cm3, 1875° C

共3407° F兲, HB 125.
Comments on Material: Chromium belongs to the refractory metals and pure
chromium is soft and ductile. The alloys, which are commercially available, often
used for plating, are hard and relatively brittle.
The machinability of chromium is low and cold working is easy which makes
chromium relatively difficult to prepare mechanically.
Sectioning: Wet abrasive cutting can be made with an SiC bakelite bond cut-off
wheel. Due to the poor machinability a relatively soft wheel, as thin as possible,
should be used.
Mounting: Both hot and cold mounting can be used.
Grinding: Because of the poor machinability the grinding papers should only be
used as long as they are cutting efficiently, if not, cold work and deformation will
develop.
Polishing: It is important that the deformations from grinding are removed during
the rough polishing step. It can be difficult to remove all deformation by
mechanical polishing and often chemical mechanical polishing can be an
advantage 共see below兲. Also electrolytic polishing can be recommended.
Etching: Chromium is difficult to etch, two etchants are stated below.
Purpose ASTM Standard Method

共See Section 12.4兲
thickness/hardness,
surface layers
boundaries El-11
High planeness
Microhardness, E 10, E 18, E 92, E 103, E 110, E 140, C-46, T-46,
hardness E 384, E 448 El-11
E 1351, E 1382, E 1558 El-11
Sectioning
Mounting

Grinding
T-46: Very often FG 3 can be omitted.

Polishing
C-46 and T-46: The last polishing step can be with alumina 共0.02– 0.05 ␮m兲 in
distilled water 共100 mL兲 with sodium hydroxide 共5 g兲, or alumina 共300 mL兲 with
hydrogen peroxide 共H2O2兲共20 mL兲共30 %兲.
C-46: If needed the step P 1 from T-46 can be used between FG 1 and P 1
expanding the method with one step.
C-46: P 2: This step can often be omitted.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, soft Cloth, Cloth, med. Cloth, nap-
fixed, res napless, nap, soft, syn less, soft,
silk
Abrasive Diamond Dia, spr or Dia, spr or Dia, spr or Silica
Type susp susp susp
Grit or Grain P220 9 3 1 0.04/ 0.05
Size ␮m
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/
rpm
Specimen
N 共lb兲
Minutes

Section 13.2.2.兲
Polishing
hard, med soft,
wov, silk hard, porous,
wov, syn
wool
Abrasive SiC SiC SiC SiC Dia, Dia, Alumina

Type spr spr
or or
susp susp
Grit or P220 P320 P500 P1200 6 3 0.02/ 0.05
Grain
Size ␮m
Lubricant Water Water Water Water Alco or Wat-oil
Type wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/
rpm
Contra
Force per 15 15 15 15 30 共7兲 20 共4.5兲 10 共2.3兲
N共lb兲
Time Until 0.5–1 0.5–1 0.5–1 4–5 3 1
Minutes plane
Etchants
Cr 12, 13c General structure
Material: Pure Cobalt. Co Alloys
Material Properties: Cobalt: Above 417° C 共783° F兲: Face-centred cubic. Below
417° C 共783° F兲: Hexagonal close packed, 8.8 g / cm3, 1495° C 共2723° F兲.
Comments on Material: Cobalt is a metal with characteristics close to iron and
nickel; it is tough and the machinability is relatively low. Cobalt is very magnetic
and used for magnets and for alloying element to improve strength. For super
alloys based on cobalt, see Material/Preparation Tables 48. For cobalt in cemented
carbides, see Material/Preparation Tables 67.
Pure cobalt being tough and with a tendency to cold work and deformation is
relatively difficult to prepare. Cobalt alloys are less difficult. Preparation is similar
to the refractory metals 共see Material/Preparation Tables 55兲.
Sectioning: Wet abrasive cutting is done with an SiC bakelite bond cut-off wheel.
A thin and relatively soft wheel is recommended to secure a cut with the lowest
deformation possible.
Mounting: Hot mounting and cold mounting can be used.
Grinding: Due to the toughness of cobalt the SiC grinding papers shall not be
used for too long of a time to avoid smeared layers.
Polishing: It is important that the rough polishing step has removed the
deformation from the grinding. If this cannot be obtained with the 3 ␮m step, a
6 ␮m step is used 共see below兲. Electrolytic polishing can be recommended.
Etching: See below.

Case or coating thickness/ B 487 C-47
hardness, surface layers
Grain size, E 112, E 930, E 1181, E 1382 C-47, T-47,
grain boundaries El-12
High planeness
Microhardness, E 10, E 18, E 92, E 103, C-47, T-47,
hardness E 110, E 140, E 384, El-12
E 448
E 1181, E 1245, E 1351, El-12
E 1382, E 1558
Sectioning
Mounting

Grinding
Polishing
C-47: The step P 1 from Method T-47 can be used between the FG 1 step and the
P 1 step 共see above兲.
C-47: P 2: Often this step can be omitted.
T-47: The method can be expanded with P 3 from C-47.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk RCD, hard Cloth, Cloth, med Cloth,
fixed, res napless, nap, soft, napless,
hard, syn soft,
wov, syn porous, syn
Abrasive Type Diamond Dia, spr Dia, spr Dia, spr Alumina
Grit or Grain P220 9 3 1 0.02/ 0.05
Size ␮m
Lubricant Water Alco or Alco or Alco or wat
Type wat wat
rpm/rpm
Force per 25 共5.7兲 30 共7兲 30 共7兲 30 共7兲 10 共2.2兲
Specimen N 共lb兲
Time Until 5–6 4 2
Minutes plane

Section 13.2.2.兲
Polishing
Disk/Cloth SiC SiC SiC SiC Cloth, Cloth, Cloth
hard, hard, nap,
wov, wov, soft,
silk silk syn
Size ␮m
Lubricant Water Water Water Water Alco Alco Alco
Type or or or
wat wat wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/
rpm
Comp/ Comp or Comp or Comp or Comp Comp Comp Comp
Contra contra contra contra
Force per 20 共4.5兲 20 共4.5兲 20 共4.5兲 15 共3.4兲 25 共5.7兲 30 共7兲 30 共7兲

Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 4–5 4 2
Minutes plane
Etchants
Pure Co 14, 15, 17 General structure
Hard-facing and tool metals 18, 19, 20 General structure
High temperature alloys 20, 18, 16, 21, 22b, 24, 25 General structure
19 Phase identification
Material: Cobalt-based super alloys
Material Properties: Cobalt: Above 417° C 共783° F兲: Face-centered cubic. Below
417° C 共783° F兲: Hexagonal close packed, 8.8 g / cm3, 1495° C 共2723° F兲.
Super alloys 共Co based兲: Heat-resistant casting alloys: 20–32 % chromium, 7–13 %
tungsten, 1–11 % nickel and molybdenum, niobium, zirconium, titanium,
aluminum, tantalum, boron, silicon and manganese.
Wrought heat-resistant alloys: 1–15 % iron, 3–35 % nickel, 20–30 % chrome, 7–10
% molybdenum, carbon, manganese, tungsten, niobium 共weight %兲.
Comments on Material: The cobalt-based super alloys are high-temperature
resistant materials. They are hard and tough, relatively easy to prepare. Stellite is a
special cobalt-based alloy with 45–65 % Co, 25–35 % Cr, and 5–20 % W. This alloy
is very wear resistant used only as casting alloy. It is hard and brittle. Cobalt is
also used in cemented carbides 共see Material/Preparation Tables 67兲.
Sectioning: Wet abrasive cutting is done with an SiC bakelite bond cut-off wheel.
Very often shearing or other more rough sectioning methods should be avoided, as
serious distortions and cold work could be introduced. Use only these methods for
sectioning of large pieces, later to be sectioned by wet cutting.
Mounting: Both hot mounting and cold mounting can be used. In case of edge
retention a hot mounting material like bakelite or epoxy with a filler should be
used.
Grinding: For the harder alloys, like stellite, Method C-48 should be preferred.
Polishing: For the final step with alumina, the pH should be lowered to around 4.
Electrolytic polishing is recommended.

thickness/hardness
surface layers
Grain size, E 112, E 930, E 1181, E 1382 C-48,

grain boundaries T-48
E-12
Image analysis, E 562, E 1245, E 1382 C-48,
rating of inclusion T-48
content
High planeness
Microhardness, E 10, E 18, E 92, E 103, E 110, C-48,
hardness E 140, E 384, E 448 T-48
El-12
Microstructure E 3, E 407, E 562, E 883, E 1181, C-48,
E 1245, E 1351, E 1382, E 1558 T-48
El-12
T-48
Sectioning
Mounting
Hot Compression Resin Bakelite/ Cold Mounting Resin Acrylics

Mounting Epoxy
Grinding
C-48: FG: Very often FG 1 can be changed to RCD, soft, and FG 2 and FG 3 can
be omitted.
Polishing
C-48 and T-48: The P 3 step: Use alumina with a pH around 4.

Contemporary Method C-48 共for definitions of parameters and consumables see

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk RCD, hard RCD, soft RCD, soft Cloth, nap- Cloth,
fixed, res less, hard, napless,
wov, syn soft,
porous,
syn
Abrashive Diamond Dia, spr Dia, spr Dia, spr Dia, spr Alumina
Type or susp or susp or susp or susp
Grit or Grain P220 9 6 3 3 0.02/ 0.05
Size ␮m
Lubricant Water Alco Alco Alco Alco
Type or wat or wat or wat or wat
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Contra contra
Force per 30 共7兲 30 共7兲 30 共7兲 25 共5.7兲 30 共7兲 15 共3.4兲
Specimen
N共lb兲
Time Until 4–5 4 5 2–4 1–2
Minutes plane
Traditional Method T-48 共For definitions parameters and consumables see

Section 13.2.2.兲
Polishing
Disk/Cloth SiC SiC SiC SiC Cloth Cloth Cloth
hard, hard, soft,
syn syn
Abrasive SiC SiC SiC SiC Dia, spr Dia, spr Alumina
Grit or Grain P220 P320 P500 P1200 6 3 0.02/
Size ␮m 0.05
Type wat wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm

Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 5 2–3 1
Minutes plane
Etchants
Material: Copper and copper alloys. Brass. Bronze. Other copper
alloys
Material Properties: Copper: Face-centered cubic, 8.93 g / cm3, 1083° C 共1981° F兲,
HRB 37.
␣-brass: Body-centered cubic, up to 38 % zinc.
␣-␤-brass: Body-centered cubic, 38 to 47 % zinc.
Bronze: Up to 30 % tin
Comments on Material: Copper makes alloys with a high number of other
metals. In alloys improving the characteristics of pure copper, small amounts of
alloying elements like silver, cadmium, sulfur, tellurium, chromium, beryllium, and
cobalt are used. The alloys with zinc, brasses, are numerous, often with lead as a
further alloying element. In special brasses further elements like aluminum, tin
共1–2 %兲 manganese nickel and iron are used. Brass can be obtained as wrought
and cast alloys. The alloys with tin, bronzes are supplied as wrought bronzes with
up to 6 % tin and cast bronzes with up to 30 % tin Often zinc is added up to 2 %
and other elements like phosphorous and lead. Aluminum bronze is a group of
bronzes with 5–11 % aluminum, up to 6 % nickel, 6 % iron, and 2 % manganese.
Manganese bronze contains 5–15 % manganese. Copper-nickel alloys have a nickel
content of 4.5–45 % nickel with small amounts of iron and manganese.
Copper and copper alloys are specified in a number of systems by a number of
organizations. The most important are:
UNS System, Standard Designations for Copper and Copper Alloys, by Copper
Development Association 共CDA兲.
AMS System, Aerospace Material Specifications, by Society of Automotive
Engineers 共SAE兲.
ASME System, by American Society of Mechanical Engineers 共ASME兲.
ASTM System by ASTM.
AWS System by American Welding Society 共AWS兲.
Ingot No System by Brass and Bronze Ingot Manufacturers.
Federal System and Military System.
SAE System by American Society of Mechanical Engineers 共ASME兲.
Metallographic examination is often used for the determination of grain size,
evaluation of the distribution of second phase, and control of heat treatment.
Copper alloys are soft and ductile, making them difficult to prepare without
deformation. Care should be taken to keep the deformation low at sectioning and
grinding and to remove deformation from previous steps. See also the Material/
Preparation Tables 50 covering the preparation of pure copper and copper bearing
alloys.
Sectioning: Wet abrasive cutting with an SiC bakelite bond cut-off wheel. Use an
efficient cooling to avoid recrystallization of cold-worked lean alloys. When using
shearing or band sawing, care should be taken that the strong deformation
developed is removed during the plane grinding.
Mounting: Hot and cold mounting can be used.
Grinding: Sectioning and the rough grinding steps introduce deep deformation so
it is important to remove this during the finer grinding steps.
Polishing: It can be very difficult to remove the last deformation and obtain a
scratch-free surface with mechanical polishing. Using chemical mechanical
polishing at the last polishing step is an efficient way to obtain a correct surface
共see below兲. Electrolytic polishing gives very good results with a number of brasses
and bronzes.
Etching: See below.

thickness/hardness,
surface layers
Grain size, E 112, E 930, C-49, T 49,
grain boundaries E 1181, E 1382 El-13
共Brass兲, El-
14 共Bronze兲
Image analysis, E 562, E 1245, C-49, T-49
rating of inclusion E 1382
content
High planeness
Microhardness, hardness E 10, E 18, E 92, E 103, E 110, E 140, C-49, T-49
E 384, E 448
E 1351, E 1382, E 1558 El-13
共Brass兲, El
14 共Bronze兲
Sectioning
Mounting

Grinding
Attention: In C-method, when using RCD: The disk turns concave during use.
Polishing
C-49 and T-49: For Cu and Cu-alloys a chemical mechanical polishing can be
obtained in the last polishing step by mixing 98 共96兲 mL colloidal silica with
1 mL 共2 mL兲 H2O2 共30 %兲 and 1 mL 共2 mL兲 ammonia solution 共25 %兲.
Electrolytic polishing: Brass: El-13. Bronze: El-14

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper RCD, soft Cloth, Cloth,
napless, napless,
hard, wov, soft,
syn porous,
syn
or susp or susp See note
Grit or Grain P220 9 3 0.04/ 0.05
Size ␮m
Lubricant Type Water Alco or wat Wat-oil
Rotation 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Contra Comp Comp Contra
Specimen N 共lb兲
Time Until plane 4 4 2–3

Minutes

Section 13.2.2.兲
Grinding/ PG FG 1 FG 2 FG 3 FG 4 FG 5 P1 P3
Polishing
Disk/ SiC SiC SiC SiC SiC SiC Cloth, Cloth
Cloth paper paper paper paper paper paper nap- nap-
less, less,
med soft,
hard, por-
wov, ous,
wool syn
Abrasive SiC SiC SiC SiC SiC SiC Dia, Silica
Type spr See
or note
susp
Grit or P220 P320 P500 P1200 P2400 P4000 3 0.04
Grain / 0.05
Size ␮m
Lubricant Water Water Water Water Water Water Wat-oil
Type
Rotation 300 300 300 150 150 150 150 150
Disk/ / 150 / 150 / 150 / 150 / 150 / 150 / 150 / 150
Holder
rpm/
rpm
Contra or or or
Force per 25 共5.7兲 25 共5.7兲 25 共5.7兲 25 共5.7兲 25 共5.7兲 20 共4.5兲 25 10 共2.2兲
Specimen 共55.7兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 0.5–1 3 1
Minutes plane
Etchants
Cu-Al 共aluminum, 44, 31d, 34 b, 35, 36, General structure
bronze兲 37, 38, 39, 40, 45, 215
Cu-Be 46, 41, 45 General structure
Cu-Cr 41 General structure
Cu-Mn 41 General structure
Cu-Ni 34, 47, 48, 40, 49, 50 General structure
Cu-Si 41 General structure
Cu-Sn 共tin 51, 52 General structure

bronze兲
Admirality metal 8b General structure
Gilding metal, 31d, 32, 33, 41, 42, 49 General structure
cartridge metal,
free
cutting brass,
nickel silver
Cu alloys 26, 27, 28, 29, 30, 44, General structure
41, 31d, 32,
33, 34b, 35, 36, 37, 38,
39, 210, 215
53, 43, 28, 49 Chemical polish
and etch
42, 49, 210 Darkens beta in
alpha-beta brass
54 Etching of cold
worked brass
Material: Pure copper. Copper-bearing alloys
Material Properties: Copper: Face-centered cubic, 8.93 g / cm3, 1083° C 共1981° F兲,
HRB 37.
Copper bearing alloys: 3.5–25 % lead, 3.5–11 % tin, 0.5–4 % zinc, small additions
of antimony, nickel and iron 共weight %兲.
Comments on Material: Commercially pure copper, 99.9–99.99 %, can be
obtained as oxygen-free electronic copper and as tough pitch copper containing
very small amounts of oxide. Copper bearing alloys have high contents of lead and
tin, as mentioned above.
Pure copper is very ductile and soft making the preparation difficult. Copper
bearing materials, having the very soft phases of lead and tin is difficult to prepare
without smearing of these phases. The methods described in Material/Preparation
Tables 49 can also be used for pure copper. For further information see Material/
Sectioning: Wet abrasive cutting with an SiC bakelite bond cut-off wheel. When
using shearing or band sawing, care should be taken that the strong deformation
developed is removed during the plane grinding.
Grinding: Sectioning and the rough grinding steps introduce deep deformation so
it is important to remove this during the finer grinding steps.
Polishing: It is important that the deformation developed during the grinding is

removed after the step with 9 ␮m or 6 ␮m. For pure copper it can be very difficult
to remove the last deformation and obtain a scratch- free surface with mechanical
polishing. Using chemical mechanical polishing at the last polishing step is an
efficient way to obtain a correct surface 共see below兲. Electrolytic polishing gives
good results with pure copper using Method El-13. Electrolytic polishing of
bearing alloys can be done with Method El-14 if the amount of phases is not too
high.
Etching: Etching can take place between preparation steps to remove deformation
共see below兲. See etchants below.

thickness/hardness,
surface layers
Perfect edge
retention
Grain size, E 112, E 930, C-50, T-50,
grain boundaries E 1181, E 1382 El-13 共Pure
copper兲, El-14
共Bearing
alloys兲
rating of inclusion
content
High planeness
E 140, E 384, E 448
E 1245, E 1351, E 1382, E 1558 El-13 共Pure
copper兲, El-14
共Bearing
alloys兲
Sectioning

Mounting

Grinding
T-50: FG 4: This step can often be omitted.

Polishing
C-50 and T-50: To remove deformation after the last FG step etch with 100 mL
water mixed with 100 mL ethanol and 10 g iron 共III兲 nitrate before the P 1 step.
C-50 and T-50: For Cu and Cu alloys a chemical mechanical polishing can be
obtained in the last polishing step by mixing 98 共96兲 mL colloidal silica with
1 mL 共2 mL兲 H2O2 共30 %兲 and 1 mL 共2 mL兲 ammonia solution 共25 %兲. An
alternative is adding a few drops of the nitrate etchant mentioned above to the
colloidal silica during the polishing.
Electrolytic polishing: Pure copper: El-13. Copper bearing alloys: El-14.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper SiC paper RCD, soft Cloth, Cloth, nap-
napless, less, soft,
med hard, porous,
wov, wool syn
susp susp See note
Grit or Grain P220 P320 9 3 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Alco or wat Wat-oil
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Force per Specimen 20 共4.4兲 20 共4.4兲 30 共7兲 2.5 共5.7兲 15 共3.3兲
N 共lb兲
Time Until plane 0.5–1 3–4 5 1–2
Minutes
Traditional Method T-50 共For definitions of parameters and consumables 共see

Section 13.2.2.兲
Polishing
Cloth paper paper paper paper paper nap- nap- nap-
less, less, less,
hard, med soft,
wov, hard, por-
silk wov, ous,
wool syn
Abrasive SiC SiC SiC SiC SiC Dia, spr Dia, spr Silica
Type or susp or susp See
note
Grit or P220 P320 P500 P1200 P2400 6 3 0.04/
Grain 0.05
Size ␮m
Type
Rotation 300/150 300/150 300/150 150/150 150/150 150/150 150/150 150/150
Disk/
Holder
rpm/
rpm
Contra or or or
Force per 20 20 20 20 20 25 25 15
Specimen 共4.5兲共4.5兲共4.5兲共4.5兲共4.5兲共5.7兲共5.7兲共3.3兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 3–4 3–4 1
Minutes plane
Etchants
Material Etchants Uses
共see Table 12.2兲
Pure Cu 26, 27, 28, 29, General structure
30, 31d, 32, 33,
34b, 35, 36, 37,
38, 39, 40, 41,
42, 8b, 210, 215
43, 28 Chemical polish and etch
Material: Pure gold. Au alloys
Material Properties: Body-centered cubic, 19.3 g / cm3, 1063° C 共1945° F兲

Comments on Material: Gold belongs to the precious metals which include the
platinum-group metals 共see Material/Preparation Tables 57兲, gold and silver, Pure
gold, 99.99 % is seldomly used, most often gold is alloyed with silver, copper,
nickel, or the platin-metals. Gold is the most ductile metal; it can be rolled to a
thickness of 1 / 12 000 mm. Gold is used for jewelry and has a number of industrial
applications. Often gold is used as a coating on other materials, and for electronic
parts gold is used as coatings for certain components 共see Section 7.10.3 and
Material/Preparation Tables 22 and 26兲. Pure gold, being very soft and ductile, is
very difficult to prepare; deformation and smearing are difficult to avoid. Also,
there is a risk of embedded abrasive grains in the specimen surface. Some alloys
are harder and therefore easier to prepare.
Sectioning: Because of the high price of gold, the wet abrasive cutting should be
with a thin cut-off wheel to reduce the kerf loss. Cutting is best done on a
precision cut-off machine using SiC bakelite bond cut-off wheels 0.5 mm 共0.02 in兲
thick and with an efficient cooling. In the case of examinations of coatings, the
cutting should be done correctly 共see Material/Preparation Tables 08–10兲. Also, it
can be of advantage to mount the specimen in epoxy before cutting to stabilize the
coating 共see below兲. If using shearing, the strong deformation of the edge should
be taken care of when plane grinding the specimen.
Mounting: Hot and cold mounting can be used. Very often coatings should be
examined and the correct hot mounting material, with a filler, should be used.
Also, cold mounting with epoxy may be satisfactory 共see Sections 3.1.3 and 3.11兲.
Grinding: If following a proper cutting, grit P220 grinding paper should be
avoided, starting with grit P320. To reduce the induction of deformation in the
material, the grinding paper can be covered with a thin layer of wax, or the paper
can be “worn-in” with a hard specimen for a few seconds. It is important that all
deformation from the previous step is removed. In the case of embedded SiC
grains in the specimen surface, use Method C-51. To avoid embedded abrasive
grains 共see Section 13.6.4兲, a softer grinding/polishing surface should be used. In
the case of embedded grains the FG 2 step of Method C-51 can be changed to a
hard, nonwoven, synthetic cloth. Also diamond paste, fixing the grains in the cloth,
can be used. As an alternative to C-51, Method C-58 for silver can be used. For the
softest materials, Method C-51 should be used.
Polishing: For pure gold and alloys with a high gold content chemical mechanical
polishing can be used for the last polishing step 共see below兲.
Etching: See etchants below.

Case or coating B 487 C51
thickness/hardness,
surface layers
Grain size, grain E 112, E 930, E 1181, E 1382 C-51,

boundaries T-51
Image analysis, E 562, E 1245, E 1382 C-51,
rating of inclusion T-51
content
High planeness
Microhardness, E 10, E 18, E 92, E 103, E 110, C-51,
hardness E 140, E 384, E 448 T-51
Microstructure E 3, E 407, E 562, E 883, E 1181, C-51,
E 1245, E 1351, E 1382, E 1558 T-51
T-51
Sectioning
Cut-Off Wheel SiC, bakelite bond, 0.5 mm 共0.02 in兲 thick
Mounting
Hot Compression Resin Bakelite/Bakelite Cold Resin Acrylics/

Mounting with a Filler Mounting Epoxy
Time 8–9 Time 6 – 10 min/
Minutes Minutes/ 6–8 h
Hours
Grinding
C-51: The step FG 2 can be changed to a hard, nonwoven, synthetic cloth if

embedded abrasive grains are a problem using the RCD.
Polishing
C-51 and T-51: Both methods can be finished with chemical mechanical
polishing: Step P 3 in C-51 with alumina 共0.05 ␮m兲 added a few drops of etchant
62: 1 – 5 g CrO3, 100 mL HCl 共see Etchants below兲.
C-51: For certain alloys the step P 1 can be changed to 3 ␮m diamond, followed
by P 2 from Method T- 51 for 2 – 8 min so that P 2 and P 3 are omitted.
T-51: Can be finished with P 3 from C-51.
T-51: Steps FG 3 and FG 4 can be changed to P 1 from C-51. In some cases P 1
can be omitted, and P 2 changed to 1 ␮m diamond.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper SiC paper RCD, Cloth, Cloth, nap- Cloth,
soft napless, less, med napless,
hard, soft, soft,
wov, silk wov, wool porous,
syn
Abrasive SiC SiC Dia, Dia, Dia, Alumina
Type spr or spr or spr or 共see note兲
susp susp susp
Grit or Grain P220 P320 9 6 3 0.02/ 0.05
Size ␮m
Lubricant Water Water Alco or Wat-oil Wat-oil
Type wat
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Specimen
N 共lb兲
Time Until 0.5–1 5 5 3 1
Minutes plane

Section 13.2.2.兲
Polishing
paper paper paper paper paper napless, med
med nap,
hard, soft,
wov, syn
wool
Abrasive SiC SiC SiC SiC SiC Dia, Dia,
Type spr spr
or or
susp susp
Grit or Grain 320 500 1000 2400 4000 3 0.25
Size ␮m
Lubricant Water Water Water Water Water Wat- Wat-
Type oil oil
Rotation 300/ 150 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
or
contra
Force per 20 20 20 20 20 20 共4.5兲 15
Specimen 共4.5兲共4.5兲共4.5兲共4.5兲共4.5兲共3.4兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 1 4 2–8
Minutes plane
Etchants
Pure Au 61, 62 General structure
63 Chemical polish and etch
Au alloys 64b, 62 General structure
⬎90 % noble metals 61 General structure
⬍90 % noble metals 65 General structure
Material: Pure lead. Pb alloys. Pb bearing alloys
Material Properties: Lead: Face-centered cubic, 11.34 g / cm3, 327° C 共621° F兲, HV
25–40.
Lead bearing alloys: 0.9–11.0 % tin, 3–16 % antimony, 0.1–0.7 % copper, arsenic,
bismuth, zinc, aluminum, cadmium 共weight %兲.
Comments on Material: Lead is a very soft and ductile metal with a low melting
point and a recrystallization temperature around 20° C 共68° F兲. Lead and most lead
alloys are toxic both when inhaled and ingested. Pure lead is difficult to prepare,
whereas bearing alloys are less difficult. After cold working lead rapidly
recrystallizes. The cold work developed during sectioning and grinding should be
kept at a minimum to avoid development of a pseudostructure through
recrystallization. Also, abrasive grains are easily embedded in the specimen
surface.
No “contemporary” 共C兲-method for lead is available. C-52 describes a method
based on etching between steps. T-52 is a “normal” “traditional” method. Method
C-52 with etching between steps is recommended for pure lead.
Sectioning: Abrasive wet cutting of pure lead and lead alloys can be done with a
thin SiC bakelite cut-off wheel, preferably on a precision cutting machine. Also, a
toothed cut-off wheel can be used. Pure lead also can be cut by using a sharp knife
or a band saw or hand saw with fine teeth. If a microtome is available, very good
surfaces can be obtained so that grinding is not needed 共see Section 2.7.6兲. In the
case of examination of corrosion products 共batteries兲, the specimen should be
impregnated before sectioning 共see Section 3.10兲.
Mounting: As a rule pure lead and lead alloys should not be hot compression
mounted, both because of the low recrystallization temperature and because of
voids and pores in the alloys that possibly may collapse under the high pressure of
hot mounting. To obtain the lowest possible temperature during cold mounting,
epoxy should be used 共see Section 3.8.3兲.
Grinding: To minimize the risk of embedded SiC grains in the specimen surface,
the grinding paper can be treated with wax and a low pressure is used. Also
paraffin can be used instead of water. In both cases an abundant flow of liquid
should be used to secure the removal of loose grains. In Method C-52 the
specimen is etched after the last grinding step 共FG 2兲 to remove deformation from
grinding 共see below兲.
Polishing: It is important that the deformation from the grinding is removed
during the rough polishing step. For pure lead chemical mechanical polishing is
recommended for the last polishing step 共see Method C-52 below兲. Lead and some
lead alloys are suited for electrolytical polishing.
Etching: See below.

Case or coating B 487 C-52, T-52
thickness/hardness,
surface layers
Grain size, grain boundaries E 112, E 930, E 1181, E 1382 C-52, T-52, El-15
rating of inclusion
content
High planeness
hardness E 140, E 384, E 448
E 1245, E 1351, E 1382, E 1558 El-15
Sectioning
Cut-Off Wheel SiC bakelite bond cut-off wheel, 0.5 mm 共0.02 in兲
thick, low speed, very careful, see also above.
Mounting
Hot Compression Resin Cold Mounting Resin Acrylics/epoxy w.

Mounting lowest possible
peak temp.
Time Time 6 – 8 min/ 12– 24 h
Grinding
T-52: PG, FG 1 and FG 2: Charge SiC papers with wax or use paraffin instead of
water.
C-52: Instead of water, paraffin is used for SiC steps.
C-52: After FG 2 the specimen is etched in Solution 1: 15 mL acetic acid, 15 mL
nitric acid 共65 %兲, 60 mL glycerol. Do not store, use fresh solution at 80° C
共176° F兲. The solution is etchant 113 below.
See also alternative below.
C-52: As an alternative to Solution 1, Solution 2 can be used: 100 mL hydrogen
peroxide 共30 %兲 mixed with 139 mL ammonia 共25 %兲.
Polishing
C-52 and T-52: For pure lead use chemical mechanical polishing with last step,
P 3: Solution 3: 84 mL glycerol, 8 mL acetic acid 共96 %兲, 8 mL ammonia 共25 %兲.
10 mL of Solution 3 is added to 90 mL colloidal silica. Also a mixture of 90 mL
silica and 10 mL hydrogen peroxide 共30 %兲 can be used. A third possibility is
adding a few drops of ammonium tartrate to the silica.
T-52: P 2: This step can often be omitted.

Section 13.2.2.兲
Polishing
paper paper paper paper napless, med. napless,
med nap, soft,
hard, soft, porous,
wov, syn syn
wool
Abrasive Type SiC SiC SiC SiC Dia, spr Dia, spr Silica,
or susp or susp see note
Size ␮m
Lubricant Paraffin Paraffin Paraffin Paraffin Wat-oil Wat-oil

Type
Rotation 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Force per 15 15 15 15 20 共4.5兲 15 共3.4兲 10 共2.2兲
N共lb兲
Time 0.5–1 0.5–1 0.5–1 0.5–1 3–4 3 1–2
Minutes

Section 13.2.2.兲
Polishing
paper paper paper napless, napless, napless,
hard, med hard, soft,
wov, silk wov, wool porous,
syn
Abrasive Type SiC SiC SiC Dia, Dia, Silica
spr or spr or
susp susp
Grit or Grain 320 500 1200 9 3 0.04/ 0.05
Size ␮m
Lubricant Water Water Water Alco or wat Wat-oil
Type
Rotation 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Force per 10–20 10–20 10–20 15–20 15–20 10
Specimen 共2.2–4.5兲共2.2–4.5兲共2.2–4.5兲共3.4–4.5兲共3.4–4.5兲共2.2兲
N 共lb兲
Time Until 0.5–1 0.5–1 4–5 3 2
Minutes plane
Etchants
Pure Pb 57, 112 General structure
Pure Pb, Pb+ ⬍ 2Sb, Pb+ ⬎ 2Sb, 113 For alternate polishing
Pb+ Ca and etching
Pb+ ⬍ 2Sb 114, 115, 57, 74b General structure
Pb+ ⬎ 2Sb 114, 57, 74b General structure
Pb+ Ca 112 General structure

Pb alloys 116, 117b General structure
Babbitt 74b General structure
Material: Pure magnesium and Mg alloys
Material Properties: Magnesium: Hexagonal close-packed, 1.74 g / cm3, 650° C

共1202° F兲, HB共B兲 35.
Magnesium alloys: 1.2–10 % aluminum, 0.15–1.5 % manganese, 0.2–3.0 % rare
earths, 1.8–3.0 % thorium, 0.5–5.7 % zinc, 0.6–0.7 % zirconium 共weight %兲.
Comments on Material: Magnesium is the light metal with the lowest specific
gravity in practical use. Pure magnesium is rarely used because of the low
strength, but in form of alloys based on the five alloying elements mentioned
above. Magnesium alloys are normally available as low-pressure casting alloys,
high-pressure casting alloys, and wrought alloys. Magnesium alloys are not
universally classified, but in ASTM “Practice for Temper Designation of
Magnesium Alloys, Cast and Wrought” 共B 296兲 a designation is stated.
Magnesium is soft and will easily cold-work making it difficult to prepare. As the
dust from grinding may ignite, all sectioning and grinding should be with a
cooling fluid. Pure magnesium and many alloys are sensitive to water.
The preparation of Mg cast and wrought alloys vary considerably, and therefore a
number of suggestions are stated below. For harder alloys use Method C-53.
Sectioning: At examination of die castings it should be recognized that the
microstructure varies strongly through the casting. This should be considered
when selecting the sample. Wet abrasive cutting with an SiC cut-off wheel. Care
should be taken to avoid excessive deformation of the cut surface and the fixing of
the work piece should be as gentle as possible. As mentioned above the
magnesium swarf/dust may ignite and even development of hydrogen may take
place at the contact with water, and special precautions should be made. If cutting
with a shear or a band saw, at least 1 mm of the cut surface should be removed
during the plane-grinding step.
Mounting: The pressure that is needed for hot mounting may cause cold-work in
the specimen, and cold mounting should be preferred. In case of heat-sensitive
alloys only epoxy should be used for cold mounting, keeping the peak temperature
low 共see Section 3.8.3兲.
Grinding: The plane grinding should be performed with the finest possible grit. If
the sectioned surface is not very rough, the first grinding step can be with grit
P320 or P500 as deep deformations are very difficult to remove at the later steps.
For water-sensitive materials use a mixture of glycerol and ethanol, 1:3, instead of
water, or pure ethanol for the finer grits. In case of embedded SiC particles in the
specimen surface, charge the surface of the grinding paper with wax.
Polishing: For most materials water should be totally avoided for polishing.
Ultrasonic cleaning in ethanol between polishing steps is recommended. During
the polishing a relief may develop between the matrix and hard particles; to avoid
this use Method C-53. Also this method should give the smallest amount of
embedded abrasive grains in the specimen surface. By the final cleaning, water
should be avoided for most alloys. Use soap and ethanol, and avoid using cotton
after the last polishing step because new scratches may be introduced.
Pure magnesium and most alloys can be electrolytically polished.
Etching: Magnesium having a hexagonal close-packed crystal structure can be
examined in polarized light. For enchants, see below.

thickness/hardness,
surface layers
rating of inclusion content
High planeness
E 140, E 384, E 448
E 1351, E 1382, E 1558 El-16
Sectioning
Mounting
Hot Compression Resin Cold Mounting Resin Acrylics

Mounting Time Time 6 / 10 min
Grinding
C-53 and T-53: If the material is very water sensitive use ethanol or a mixture
1:3 of glycerol and ethanol instead of water.
C-53: FG 1: For water-sensitive materials use water-free lubricant.
Polishing
Cleaning: For most alloys cleaning between polishing steps should be done
without water.
C-53 and T-53: If the specimen material is sensitive to water use water-free
polishing media and lubricants.
C-53 and T-53: The final cleaning can be done on a rotating polishing cloth, med
nap, soft, syn, only with ethanol.
C-53: P 3: This step can be changed to step P 2 in Method T-53, only with 1 ␮m
diamond in 2 min.
C-53: Polishing step, P 3: Mix silica 1:1 with ethanol.
T-53: P 1: This step can be changed to a step like FG 3 with SiC paper grit 2400.
T-53: P 2: The cloth can be changed to napless, med hard, wov, wool.
T-53: P 3: For pure Mg: Use same data as P 2 except grain size: 1 ␮m.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC RCD, Cloth, Cloth, Cloth,
paper soft napless, napless, napless, soft,
hard, wov, med hard, porous, syn
silk wov, wool
Abrasive SiC Dia, spr or Dia, spr or Dia, spr or Silica, see
Type susp susp susp above
Grit or Grain P500 9 6 3 0.04/ 0.05
Size ␮m
Lubricant Water Alco or wat Alco or wat Wat-oil
Type
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Force per 20–30 共4.5–7兲 20–30 30 共7兲 15 共3.3兲 10 共2.2兲
Specimen 共4.5– 7兲
N 共lb兲
Time Until plane 5–8 4 3–5 1–2
Minutes

Section 13.2.2.兲
Polishing
paper paper paper paper napless, med. napless,
hard, nap soft,
wov, silk soft, syn porous,
syn
or susp or susp
Grit or 220 320 500 1200 15 3 0.04/ 0.05
Grain Size
Type oil oil
Rotation 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Force per 20–30 20–30 20–30 10–20 30 共7兲 25 共5.7兲 15 共3.4兲
Specimen 共4.5–7兲共4.5–7兲共4.5–7兲共2.3–4.5兲
N 共lb兲
Time Until 0.5–1 0.5–1 1–2 3–4 3–4 0.5–1
Minutes plane
Etchants
Pure Mg 118, 119, 74a, General structure
120, 121, 122
123 Stainfree polish-etch
Mg-Mn 119, 74a, 124, 122 General structure
Mg-Al, Mg-Al-Zn 118, 119, 74a, 125, General structure
共Al+ Zn⬍ 5 % 兲 124, 123, 122
120, 125, 126, 127 Phase identification
124, 126, 127 Grain structure
Mg-Al, Mg-Al-Zn 118, 119, 74a, 125, General structure
共Al+ Zn⬎ 5 % 兲 124, 121, 122
120, 125, 126, 127 Phase identification
Mg-Zn-Zr and Mg-Zn-Th-Zr 118, 119, 74a, 1d, 128, General structure
124, 126, 127, 121, 122
120, 121 Phase identification
Mg-Th-Zr 118, 119, 74a, 1d, 124, General structure
127, 121, 122
Mg-rare earth-Zr 120, 121 Phase identification
Material: Pure manganese. Mn alloys
Material Properties: Manganese: Body-centered cubic or body-centered
tetragonal, 7.2 g / cm3, 1260° C 共2300° F兲, HRC 35.
Comments on Material: Manganese is a metal resembling iron, but it is harder
and very brittle. It is primarily used as an alloying element, examples are with
steel, where 0.2–2 % manganese is used, brass with up to 3 % and bronze with
5 – 15 % Mn.
Pure manganese and alloys with high manganese content are not difficult to
prepare. In the case of most alloys, the Material/Preparation Tables covering the
base metal should be followed.
Sectioning: Wet abrasive cutting with an Al2O3 bakelite bond cut-off wheel.
Grinding: No special precautions are needed.
Polishing: Pure manganese and some alloys can be electrolytically polished.
Etching: See below.

thickness/hardness,
surface layers
rating of inclusion
content
High planeness
hardness E 140, E 384, E 448
E 1181, E 1245, E 1351, El-01
1382, E 1558
Sectioning

Mounting

Grinding
C-54: PG: For pure Mn use SiC paper grit P220.


Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, hard Cloth, napless, Cloth, napless,
fixed, res hard, wov, syn soft, porous, syn
Abrasive Type Diamond Dia, spr or susp Dia, spr or Alumina
susp
Grit or Grain P220 6 3 0.02/ 0.05
Size ␮m
Rotation 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or contra Comp Comp Contra
Specimen
N 共lb兲
Time Until plane 4 4 2
Minutes

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper SiC paper SiC paper SiC paper Cloth, Cloth,
napless, napless,
hard, soft,
wov, syn porous,
syn
Abrasive Type SiC SiC SiC SiC Dia, spr or Alumina
susp
Grit or Grain P220 P320 P500 P1200 3 0.02/ 0.05
Size ␮m
Lubricant Type Water Water Water Water Alco or wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp or Comp or Comp Comp Contra
Specimen
N共lb兲
Time Until 0.5–1 0.5–1 0.5–1 4 1–2
Minutes plane
Etchants
Mn-Fe, Mn-Ni, 74 General structure
Mn Cu, Mn alloys
Pure Mn, Mn-Cu, 942 General structure
and small additions
of Ni, Cu, Fe, Ge
Material: Pure molybdenum. Mo alloys. Pure
niobium„Columbium…. Nb „Cb… alloys. Pure rhenium. Re alloys.
Pure tantalum. Ta alloys. Pure tungsten. W alloys. Pure
vanadium. V alloys
Material Properties: Molybdenum: Body-centered cubic, 10.2 g / cm3, 2620° C

共4748° F兲, HV 200.
Niobium 共Columbium兲: Rhombohedral, 8.4 g / cm3, 1950° C 共3542° F兲.
Rhenium: Hexagonal close packed, 20.53 g / cm3, 3000 °C 共5432° F兲, HK 200.
Tantalum: Body-centered cubic, 16.6 g / cm3, 2996° C 共5425° F兲, HV 110.
Tungsten: Body-centered cubic, 19.3 g / cm3, 3410° C 共6170° F兲, HV 350.
Vanadium: Body-centered cubic, 5.96 g / cm3, 1710 °C 共3110° F兲, HB 72.
Comments on Material: Molybdenum, niobium, rhenium, tantalum, tungsten,
and vanadium all having high melting points belong to the refractory metals. They
are seldomly used pure but mostly as alloying elements. Pure niobium, rhenium,
tantalum, and vanadium are soft and ductile, difficult to prepare. Pure
molybdenum and tungsten are harder and more brittle. All metals have a low
machinability and this combined with development of deformation and cold-work
makes it difficult to obtain a true microstructure by mechanical polishing; often it
must be combined with chemical mechanical polishing.
Sectioning: Wet abrasive cutting can be made with a SiC bakelite bond cut-off
wheel. Due to the poor machinability and to minimize the deformation, a
relatively soft wheel, as thin as possible, should be used.
Mounting: Both hot and cold mounting can be used. In case of examination of
porosity, a vacuum impregnation with epoxy may be useful 共see Section 3.10兲. For
mounting of wires, see Section 3.12. Foils and wire samples should preferably be
cold mounted to avoid induction of deformation at hot compression mounting.
Grinding: Because of the poor machinability the SiC grinding papers should only
be used as long they are cutting efficiently; if not, cold work and deformation will
develop. In case of alloys with hard nonmetallic precipitates, it may be of
advantage to use Method C-55 to avoid relief and pull-outs. Variation regarding
specific materials, see below.
Polishing: It is important that the deformations from grinding are removed during
the rough polishing step, and if needed this step must be prolonged. It can be
difficult to remove all deformation by mechanical polishing and often chemical
mechanical polishing can be an advantage 共see below兲. Also electrolytic polishing
can be recommended 共see below for methods covering the different metals兲.
Etching: See etchants below. Molybdenum may be electrolytically etched 共see
Method El-01兲.

thickness/hardness,
surface layers
Grain size, E 112, E 930, C-55, T-55,
grain boundaries E 1181, E 1382 El-
methods,
see below
Image analysis, rating E 562, E 1245, C-55, T-55
of inclusion E 1382
content
High planeness
E 110, E 140, E 384,
E 448
E 1181, E 1245, E 1351, El-
E 1382, E 1558 methods,
see below
Sectioning
Cut-Off Wheel SiC, bakelite bond, a thin wheel
Mounting

Grinding
Niobium: T-55: An extra step with P4000 SiC paper can be added after FG 4.
Rhenium: Method C-55 can be recommended.
Tantalum and other very soft metals: C-55: A grinding step with P320 SiC
paper can be used between PG and FG 1 steps.
Polishing
Tungsten: C-55, T-55: The polishing step P 1 may be prolonged.

Molybdenum: C-55 and T-55: To remove deformed layers, the P 2 step can be
used with 0.05 ␮m alumina dispersed in a small amount of a 30 % K3Fe 共CN兲6
aqueous solution.
Molybdenum, niobium, tantalum, tungsten: C-55, T-55: To remove deformed
layers, the P 2 step can be used with colloidal silica 共95 mL兲 added 5 mL of a 20
% aqueous solution of chromium 共VI兲 oxide 共20 g CrO3 in 100 mL distilled
water兲.
Molybdenum: C-55 and T-55: For last step mix 96 mL of colloidal silica with
2 mL of ammonia 共25 %兲 and 2 mL of hydrogen peroxide 共30 %兲.
Niobium, pure vanadium: C-55, T-55: The last polishing step can be done as
chemical mechanical polishing: Mix 80 mL of colloidal silica with 20 mL of
hydrogen peroxide 共30 %兲.
Tungsten, vanadium: C-55 and T-55: For last step mix 95 mL of colloidal silica
with 5 mL of hydrogen peroxide 共30 %兲.
Rhenium: C-55, T-55: The last polishing step can be done as chemical
mechanical polishing: 15 g potassium ferricyanide 共K3Fe共CN兲6, 2 g sodium
hydroxide 共NaOH兲, 100 mL distilled water and equal part of silica.
Electropolishing: Molybdenum: El-01, Vanadium: El-22, Tungsten: El-21

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, soft Cloth, Cloth, nap-
fixed, res napless, less, soft,
silk
Abrasive Type Diamond Dia, spr Dia, spr Silica,
or susp or susp see above
Grit or Grain P220 9 3 0.04/ 0.05
Size ␮m
Rotation 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Contra
Force per 20–30 20–30 30 共7兲 10–15
Specimen 共4.5–7兲共4.5–7兲共2.3–3.4兲
N 共lb兲
Minutes

Section 13.2.2.兲
Polishing
hard, soft,
wov, syn porous,
syn
Abrasive SiC SiC SiC SiC SiC Dia, spr Silica,
Type or susp see
above
Grit or Grain P220 P320 P500 P1200 P2400 3 0.04/ 0.05
Size ␮m
Lubricant Water Water Water Water Water Alco or
Type wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/contra Comp or Comp or Comp or Comp Comp Comp Contra
Force per 20–30 20–30 20–30 20–30 20–30 20 共4.5兲 20 共4.5兲
Specimen 共4.5–7兲共4.5–7兲共4.5–7兲共4.5–7兲共4.5–7兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 3–5 2–5
Minutes plane
Etchants
Mo base 98c, 129, 130, 131 General structure
As cast 132 a Chemical polish prior to etching
Nb and Nb 129, 66, 158, 159, 160, 161, General structure
alloys 162, 163
164, 129, 160 Grain boundaries
Re base 13b, 98c, 132b, 170a General structure
Pure Ta 177 General structure
Ta alloys 159, 66, 178, 163, 161, 179 General structure
164 Grain boundaries and inclusions
158 Grain boundaries—retains carbide
precipitate
Pure W 98c, 131 General structure
As cast 132a Chemical polish prior to etching
W-Th 209 General structure
Pure V 170b, 165b General structure
197, 198 Grain boundaries
V alloys 199, 198 General structure
Material: Pure nickel. Ni alloys. Ni Based super-alloys
Material Properties: Nickel: Face-centered cubic, 8.89 g / cm3, 1452° C 共2646° F兲.
Nickel-copper alloys: 28–34 % copper, 1 % manganese, 1 % iron, carbon,
aluminum.
Nickel-iron alloys: 0.1 % carbon, 0.2 % manganese, 0.2 % iron.
Super alloys 共nickel based兲: Heat resistant casting alloys: 8–15 % chromium, 2–28
% molybdenum 0.5–2 % niobium, 0.8–4.7 % titanium, 0.5–6 % aluminum, 1–18.5
% iron, 0.1–10 % tungsten, 0.3–1 % tantalum, 2.5–18.5 % cobalt, carbon,
zirconium, boron.
Wrought heat resistant alloys: 1–8 % iron, 2–19 % cobalt, 5–50 % chromium, 0.4–5
% titanium, 3–25 % molybdenum, carbon, tungsten, niobium, aluminum,
zirconium, boron, tantalum 共weight %兲.
Comments on Material: Pure nickel and nickel-copper alloys are mostly used for
the good resistance to corrosion, also for this purpose nickel is used for coatings.
Nickel being somewhat magnetic, it makes special magnetic alloys with iron. The
superalloys are very heat resistant.
Nickel is a metal with characteristics close to iron and cobalt; it is tough and the
machinability is relatively low. Pure nickel being tough and with a tendency to
cold-work and deformation is relatively difficult to prepare. Nickel alloys are less
difficult.
Sectioning: Wet abrasive cutting is done with an SiC bakelite bond cut-off wheel
with an efficient cooling. A thin and relatively soft wheel is recommended to
secure a cut with the lowest deformation possible. Very often shearing or other
more rough sectioning methods should be avoided, as serious distortions and
cold-work could be introduced. Use only these methods for sectioning of large
pieces later to be sectioned by wet cutting.
Mounting: Hot mounting and cold mounting can be used. In the case of
examination of nickel coatings, see Material/Preparation Tables 08–10.
Grinding: Due to the toughness of nickel the SiC grinding papers shall not be
used for a too long time, to avoid smeared layers.
Polishing: It is important that the rough polishing step has removed the
deformation from the grinding. In case of pure nickel and soft alloys, it may be
necessary to add a silica step to the methods 共see below兲. Electrolytic polishing can
be recommended. Often a very short electrolytic polishing after mechanical
polishing will remove smeared material 共see Method El-17兲.
Etching: Nickel is relatively difficult to attack, strong solutions are needed 共see
etchants below兲.

Case of coating B 487 C-56
thickness/hardness,
surface layers

rating of inclusion
content
High planeness
Microhardness, E 10, E 18, E 92, E 103, E 110, C-56, T-56,
hardness E 140, E 384, E 448 El-17
E 1181, E 1245, E 1351, E 1382, El-17
E 1558
Sectioning
Mounting

Grinding
C-56: PG: For pure nickel and the most ductile alloys SiC paper grit P220/ 320
should be used.
Polishing
Pure Ni and Ni-Cu alloys: T-56: P 3 can be followed by or replaced by a step

with silica, see P 2 in Method C-56.
C-56: P 2: Alumina 0.02/ 0.05 ␮m can be used instead of silica.
T-56: In some cases FG 3 can be omitted.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, soft Cloth, Cloth,
fixed, res napless, napless, soft,
hard, wov, porous,
syn syn
Abrasive Type Diamond Dia, spr or Dia, spr or Silica

susp susp
Grit or Grain P220 9 3 0.04/ 0.05
Size ␮m
Rotation 300/ 300 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen
N共lb兲
Minutes

Section 13.2.2.兲
Grinding/ PG FG1 FG 2 FG 3 FG 4 P1 P2 P3
Polishing
Cloth paper paper paper paper paper nap- nap- med
less, less, nap,
hard, hard, soft,
wov, wov, syn
silk silk
Abrasive SiC SiC SiC SiC SiC Dia, Dia, Dia,
Type spr or spr or spr
susp susp or
susp
Grit or P220 P320 P500 P1000 P1200 6 3 1
Grain
Size ␮m
Alco Alco Alco
Type or wat or wat or wat
Rotation 300/150 300/150 300/150 150/150 150/150 150/150 150/150 150/150
Disk/
Holder
rpm/
rpm
Comp/ Comp Comp Comp Comp Comp Comp Comp Comp
Contra
Force per 25 共5.7兲 25 共5.7兲 25 共5.7兲 25 共5.7兲 25 共5.7兲 30 共7兲 30 共7兲 20 共4.5兲
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 4 3 1–2
Minutes plane
Etchants
Pure Ni and 133, 134, 47, 135, 136, 25, 108, 31c General structure
high Ni alloys
137 Grain boundary sulfidation
Ni-Ag 38, 138, 50, 139 General structure
Ni-Al 50, 140, 141, 142, 89, 143 General structure
Ni-Cr 144, 50, 83, 134, 145, General structure
98, 146, 147, 13a
Ni-Cu 38, 138, 50, 133, 140, 25, General structure
134, 47, 48b, 94, 108, 34
Ni-Fe 50, 140, 141, 83, 134, 148, 40, General structure
107, 149
74e, 25, 150 Orientation pitting
Ni-Mn 74e General structure
Ni-Mo 143 General structure
Ni-Ti 143, 151, 50, 133 General structure
Ni-Zn 152 General structure
Superalloys 94, 105, 138, 153, 12, 87, 89, 212, General structure
226, 25, 94 Grain size
107, 111, 13a Reveals microstructural
inhomogneity
133 Grain boundary sulfidation
154 Fine precipitation structure
19b, 155, 156 Differential matrix and
nonmetallic staining
22a For passive alloys 共for
example, UNS Alloy N06625兲
157 Specific for UNS Alloys
N10004
107 Submicroscopic structure in
aged super alloys particularly
for electron microscopy
Stains the matrix when ␥⬘
precipitates are present
154 ␥⬘ banding
18 Pre-etch activation for passive
specimens 共electrolytic etchant兲
213 Colors carbide and ␥⬘
Material: Pure palladium. Pd alloys. Pure platinum. Pt alloys.
Pure iridium. Ir alloys. Pure osmium. Os alloys. Pure rhodium. Rh
alloys. Pure ruthenium. Ru alloys
Material Properties: Palladium: Face-centered cubic, 12.16 g / cm3, 1553° C

共2827° F兲.
Platinum: Face-centered cubic, 21.37 g / cm3, 1773.5° C 共3224° F兲.
Iridium: Face-centered cubic, 22.42 g / cm3, 2350° C 共4262° F兲, HV 220.
Osmium: Hexagonal, 22.48 g / cm3; 2700° C 共4892° F兲.
Rhodium: Face-centered cubic, 12.5 g / cm3, 1985° C 共3605 °F兲, HV 122.
Ruthenium: Hexagonal, 12.2 g / cm3, 2450° C 共4442° F兲.
Comments on Material: The above-mentioned metals belong to the so-called
platinum metals that belong to the precious metals with gold and silver. Platinum
is used as base metal in a number of alloys used for jewelry and technical
purposes. The other metals are to a high degree used as pure or as alloying
elements in materials for the electronics, medical, and other industries.
Palladium and platinum are soft ductile metals, difficult to prepare because of
deformation and smearing. Iridium and rhodium, and especially the hexagonal
close-packed ruthenium and osmium are harder and less difficult to prepare.
Because of the high ductility, embedded abrasive grains in the specimen surface is
a risk 共see below兲.
No “contemporary” method is available for these metals, and C-57 is a variation of
T-57. In case of harder alloys the C-methods, C-51 共se also Grinding below兲 and
C-58 may be used.
Sectioning: Because of the high price of the platinum metals, the wet abrasive
cutting should be with a thin cut-off wheel to reduce the kerf loss. Cutting is best
done on a precision cut-off machine using SiC bakelite bond cut-off wheels
0.5 mm 共0.02 in兲 thick with efficient cooling. In the case of examinations of
coatings, the cutting should be done correctly 共see Material/Preparation Tables
08–10兲. Also, it can be of advantage to mount the specimen in epoxy before cutting
to stabilize the coating 共see below兲. If using shearing, the strong deformation of
the edge should be taken care of when plane grinding the specimen.
Mounting: Hot and cold mounting can be used. If coatings should be examined
the correct hot mounting material, with a filler, should be used. Also cold
mounting with epoxy may be satisfactory 共see Sections 3.1.3 and 3.11兲.
avoided, starting with grit P320. It is important that all deformation from the
previous step is removed. Wax can be used to reduce the aggressiveness of the SiC
paper, or the paper can be “dulled” by grinding a hard material in 1 – 5 s before
use. In the case of embedded SiC grains in the specimen surface, use Method C-51
or C-58 to reduce the use of SiC grinding paper. To avoid embedded abrasive
grains 共see Section 13.6.4兲, a softer grinding/polishing surface should be used. In
the case of embedded grains the FG 2 step of Method C-51 or the FG 3 step of
C-58 can be changed to a hard, nonwoven, synthetic cloth. Also diamond paste can
be used to improve the fixation of the diamond grains.
Polishing: Methods C-57 and T-57 both use diamond for the last polishing step.
For use of silica for the last step see Methods C-51 and C-58.
For chemical mechanical polishing 共etch-polishing兲 of ruthenium and osmium
alloys see Etchants below.
Etching: See below.

thickness/hardness,
surface layers
Grain size, E 112, E 930, E 1181, E 1382 C-57, T-57
grain boundaries
rating of inclusion
content
High planeness
hardness E 140, E 384, E 448
E 1245, E 1351, E 1382, E 1558
Sectioning
Mounting
Hot Compression Resin Bakelite Cold Resin Acrylics/epoxy

Mounting Time 8–9 Mounting Time 6 – 10 min/ 6 – 8 h
Grinding
See above.
Polishing
C-57: For pure metals use wat-oil lubricant in P 1 and P 2.

T-57: P 2: This step can be changed to P 3 in C-57.

Section 13.2.2.兲
Polishing
Cloth paper paper paper paper paper nap- nap- med
less, less, nap,
hard, hard, soft,
wov, wov, syn
silk silk
Abrasive SiC SiC SiC SiC SiC Dia, Dia, Dia,
Type spr spr spr
or or or
susp susp susp
Grit or P220 P320 P500 P1200 P2400 6 1 0.25
Grain
Size ␮m
Lubricant Water Water Water Water Water Alco or Alco or Wat-oil
Type wat wat
Rotation 300/ 300/ 300/ 150/ 150/ 150/ 150/ 150/
Disk/ 150 150 150 150 150 150 150 150
Holder
rpm/rpm
Comp/ Comp Conmp Comp Comp Comp Comp Comp Contra
Contra or or
contra contra
Force per 15–20 15–20 15–20 15–20 15–20 15–20 15 共3.4– 10–15
Specimen 共3.4–4.5兲共3.4–4.5兲共3.4–4.5兲共3.4– 共3.4– 共3.4–4.5兲 4.5兲共2.3–
N 共lb兲 4.5兲 4.5兲 3.4兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 4 2 1–2
Minutes plane

Section 13.2.2.兲
Polishing
paper paper paper paper paper napless, med
med hard, nap,
wov, soft, syn
wool
Abrasive Type SiC SiC SiC SiC SiC Dia, spr Dia, spr
or susp or susp
Grit or Grain P320 P500 P1000 P2400 P4000 3 1
Size ␮m
Lubricant Type Water Water Water Water Water Wat-oil Wat-oil
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
or
contra
Force per 15–20 15–20 15–20 15–20 15–20 15–20 10–15
Specimen 共3.4– 共3.4– 共3.4– 共3.4– 共3.4– 共3.4–4.5兲共2.3–3.4兲
N 共lb兲 4.5兲 4.5兲 4.5兲 4.5兲 4.5兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 4 2
Minutes plane
Etchants
Pure Pd 61, 166, 62, 165a General structure
Pd alloys 166, 64a, 62, 165a General structure
⬎90% noble metals 61 General structure
Pure Pt 64a, 73a General structure
167 Electrolytic polish and etch
Pt alloys 64b, 73a General structure
⬎90 % noble metals 61 General structure
Pt-10 % Rh 168 General structure
Os base 165a General structure
165a Etch-polish for viewing grains
for polarized light
Rh base 171 General structure
Ru base 73b General structure
73b Etch-polish for viewing grains
for polarized light
Material: Silver. Ag alloys
Material Properties: Silver: Face-centered cubic, 10.5 g / cm3, 961° C 共1762° F兲, HV
25.
Comments on Material: Silver is used for jewelry and in the electronics and
chemical industries. Pure silver, like the other precious metals 共see Material/
Preparation Tables 51 and 52兲, is soft and ductile and therefore has a strong
tendency to deformation and smearing during the preparation. Also, abrasive
grains can be embedded in the specimen surface 共see Section 13.6.4兲. Silver alloys,
like Ag-Cu, Ag-Pd, and Ag solders are harder and therefore easier to prepare. Often
silver is used as a coating and if this coating should be examined the methods
stated in Material/Preparation Tables 08–10 may be used.
Sectioning: Because of the relatively high price of silver, the wet abrasive cutting
should be with a thin cut-off wheel to reduce the kerf loss. Cutting is best done on
a precision cut-off machine using SiC bakelite bond cut-off wheels 0.5 mm
共0.02 in兲 thick with an effective cooling. In the case of examination of coatings, the
cutting should be done correctly 共see Material/Preparation Tables 08–10兲. Also, it
can be of advantage to mount the specimen in epoxy before cutting to stabilize the
coating 共see below兲. If using shearing, the strong deformation of the edge should
be taken care of when plane grinding the specimen.
Mounting: Hot and cold mounting can be used. If coatings should be examined,
the correct hot mounting material,with a filler, should be used. Also, cold
mounting with epoxy may be satisfactory 共see Sections 3.1.3 and 3.11兲.
avoided, starting with grit P320. Wax can be used to reduce the aggressiveness of
the SiC paper, or the paper can be “dulled” by grinding a hard material in 1–5 s
before use. It is important that all deformation from the previous step is removed.
In the case of embedded SiC grains in the specimen surface, use Method C-58. To
avoid embedded abrasive grains 共see Section 13.6.4兲, a softer grinding/
polishing-surface should be used. For this reason the FG 3 step of Method C-58
can be changed to a hard, nonwoven, synthetic cloth and possibly the FG 2 step
can be omitted. Also diamond paste, fixing the grains in the cloth, can be used. As
an alternative to C-58, Method C-51 for gold can be used.
Polishing: For pure silver and alloys with a high content of silver, chemical
mechanical polishing can be used for the last polishing step 共see below兲.
Electrolytic polishing can be used for pure silver and certain alloys.

thickness/hardness,
surface layers
boundaries El-18
of inclusion
content
High planeness
hardness E 140, E 384, E 448
E 1181, E 1245, E 1351, E 1382, E 1558 El-18
El-18
Sectioning
Mounting
Hot Compression Resin Bakelite or Cold Resin Acrylics/

Mounting bakelite w. filler Mounting Epoxy
Time 8–9 Time 6 – 10 min/
Minutes Minutes/ 6–8 h
Hours
Grinding
See above.
Polishing
C-58: P 2: Chemical mechanical polishing of silver alloys can be done by adding

a solution of 25 mL distilled water, 25 mL ammonia solution 共32 %兲 and
10– 20 mL hydrogen peroxide 共30 %兲 to 1000 mL of colloidal silica.
C-58: P 2: This step can be changed to P 2 from Method T-58.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC SiC SiC RCD, Cloth, Cloth,

paper paper paper soft napless, napless,
hard, wov, soft,
silk porous, syn
Abrasive Type SiC SiC SiC Dia, spr Dia, spr Silica, see
or susp or susp note above
Grit/Grain P220 P320 P500 9 3 0.04/ 0.05
Size ␮m
Lubricant Type Water Water WaterAlco or Wat-oil
wat
Rotation Disk/Holder 300/ 150 300/ 150 150/150 150/150 150/150 150/150
rpm/
rpm
Comp/ Comp Comp Comp Comp Comp Contra

Contra or
contra
Specimen N 共lb兲
Time Until 0.5–1 0.5–1 5 5 1
Minutes plane

Section 13.2.2.兲
Polishing
Disk/Cloth SiC SiC SiC paper SiC SiC Cloth, Cloth,
paper paper paper paper napless, med
med hard, nap,
wov, soft,
wool syn
Abrasive SiC SiC SiC SiC SiC Dia, spr Dia,
Type or susp spr
or
susp
Grit or 320 500 1000 2400 4000 3 0.25
Grain
Size ␮m
Lubricant Water Water Water Water Water Wat-oil Wat-
Type oil
Rotation 300/ 150 300/ 150 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/
rpm
Comp/ Comp Comp Comp Comp Comp Comp Comp
Contra or
contra
Force per 15–20 15–20 15–20 15–20 15–20 15–20 10–15
Specimen 共3.4–4.5兲共3.4–4.5兲共3.4–4.5兲共3.4–4.5兲共3.4–4.5兲共3.4–4.5兲共2.3–3.4兲
N 共lb兲
Time Until 0.5 0.5 0.5 1 4 2
Minutes plane
Etchants
Pure Ag 172 173, 62 General structure
Ag alloys 65, 61, 174, 175, 62 General structure
Ag-Cu alloys 130 General structure
Ag-Pd alloys 173 General structure
Ag solders 173, 176 General structure
Material: Tin, Sn bearing alloys and other Sn alloys
Material Properties: Body-centered tetragonal 共⬎13.2° C 共56° F兲兲, 7.29 g / cm3,

232° C 共450° F兲, ⬍HV 25.
Tin bearing alloys: 7 to 8 % antimony, 0.5 % lead, 3 to 4 % copper, iron, arsenic,
bismuth, zinc, aluminum.
Other tin alloys: Tin-lead, tin-copper, tin-zinc 共weight %兲.
Comments on Material: Pure tin is a soft metal, with a recrystallization
temperature close to room temperature. Pure tin is often used for coating to
obtain a reduced corrosion 共tinned steel plate兲 and on electric parts to make
soldering easier. Tin-lead alloys are used for solders and tin-antimony alloys for
bearing materials.
Tin and tin alloys being soft and having a low recrystallization temperature makes
the preparation very difficult, and all steps in the preparation process must be
performed with great care. For the softest alloys use Method T-59.
Sectioning: Abrasive wet cutting of pure tin and tin alloys can be done with a thin
SiC bakelite cut-off wheel, preferably on a precision cutting machine with an
efficient cooling. Pure tin also can be cut by using a sharp knife or with a band
saw or hand saw with fine teeth. In the case of sawing the very deformed zone
must be carefully removed during grinding. For cutting of tinned steel plate, see
Material/Preparation Tables 08.
Mounting: As a rule pure tin and tin alloys should not be hot mounted, both
because of the low recrystallization temperature and because of voids and pores in
the alloys which possibly may collapse under the high pressure of hot mounting.
To obtain the lowest possible temperature during cold mounting, epoxy with a low
peak temperature should be used 共see Section 3.8.3兲. In the case of examination of
thin coatings see Material/Preparation Tables 08–10.
Grinding: To minimize the risk of embedded SiC grains in the specimen surface,
the grinding paper can be treated with wax and a low pressure is used. For water
sensitive alloys paraffin 共kerosene兲 can be used instead of water.
Polishing: It is important that the deformation from the grinding is removed
during the rough polishing step. Chemical mechanical polishing can be used at the
last step 共see below兲. For pure tin and certain alloys, the specimen surface can be
“cleaned” by electrolytic “shock-polishing,” using Method El-19 in only 1 – 2 s. Tin
and some tin alloys are suited for electrolytical polishing.
Water sensitive alloys: use water-free lubricants and clean between steps without
water 共see below兲.

Case or coating thickness/hardness, B 487 C-59
surface layers
rating of inclusion
content
High planeness
hardness E 140, E 384, E 448
E 1245, E 1351, E 1382, E 1558 El-19
El-19
Sectioning
Cut-Off Wheel SiC bakelite bond cut-off wheel, 0.5 mm 共0.02 in兲
thick, low speed, very careful 共see also above兲
Mounting
Hot Compression Resin Cold Mounting Resin Epoxy, lowest

Mounting possible peak
temp.
Grinding
T-59: The cutting action of SiC papers P1000 and P1200 can be reduced by using
wax before grinding, or making the paper “dull” by first grinding a hard material
in 10 s.
Polishing
C-59 and T-59: P 3: Mix 96 mL of colloidal silica with 2 mL ammonia 共25 %兲

and 2 mL of hydrogen peroxide 共30 %兲.
T-59: P 1: This step can be changed to a step like FG 4, only with SiC paper grit
P4000.
C-59 and T-59: To remove deformed layers and scratches, electrolytic polishing
in a short time, 1 – 2 s 共shock-polishing兲, can be recommended to follow the P 3
step 共see Method El-19兲.
Water sensitive alloys: C-59: The step P 1 can be omitted and the step P 3 is
changed to a diamond step like P 2 in Method T-57 using a water-free lubricant.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC RCD, Cloth, Cloth, nap- Cloth, napless,
paper soft napless, less, med soft, porous,
hard, wov, hard, wov, syn
silk wool
Abrasive SiC Dia, spr Dia, spr Dia, spr Silica
Grit or Grain 320 9 6 3 0.04/ 0.05
Size ␮m
Lubricant Water Alco or wat Alco or Wat-oil
Type wat
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Force per 20 共4.5兲 25 共5.5兲 25 共5.5兲 25 共5.5兲 10–15
N 共lb兲
Minutes

Section 13.2.2.兲
Polishing
Disk/Cloth SiC SiC SiC SiC SiC Cloth, Cloth, Cloth,
paper paper paper paper paper nap- nap- nap-
less, less, less,
hard, med soft,
wov, hard, porous,
silk wov, syn
wool
Type spr spr
or or
susp susp
Grit or P220 P320 P500 P1000 P1200 6 3 0.04/

Grain 0.05
Size ␮m
Lubricant Water Water Water Water Water Alco Wat-oil
Type or
wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/
rpm
Contra
Force per 20 20 20 20 20 20 25 15–20
Specimen 共4.5兲共4.5兲共4.5兲共4.5兲共4.5兲共4.5兲共5.5兲共3.3–
N 共lb兲 4.4兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 5 5 1–2
Minutes plane
Etchants
Pure Sn 74d, 180, 151 General structure
181 Grain boundaries
Sn-Cd 74d General structure
Sn-Fe 74d, 177a General structure
Sn-Pb 182, 183, 74b General structure
116 Darkens Pb in Sn Pb
eutectic
Sn coatings on steel 183 General structure
Babbitts 184 General structure
Sn-Sb-Cu 74b General structure
Material: Titanium and Ti alloys
Titanium: 共allotropic: more than one crystallographic form兲: ␣-titanium:
Close-packed hexagonal, ␤-titanium: Body-centered cubic, 4.5 g / cm3, 1670° C
共3038° F兲, HB 70.
Titanium alloys: ␣ alloys: Alloying elements: Aluminum, gallium, germanium,
carbon, oxygen, and nitrogen. ␤ alloys: Alloying elements: 共Isomorphous group兲:
Molybdenum, vanadium, tantalum, and niobium. 共Group forming eutectoid
systems兲: Manganese, iron, chromium, cobalt, nickel, copper, and silicon.
Comments on Material: Titanium is a relatively new metal that is expensive to

produce, but nevertheless is gaining ground for applications in the aerospace
chemical, and medico-technical industries. Titanium has a high strength to weight
ratio, and it has a self-healing oxide layer that provides an effective barrier against
incipient corrosion. Commercial titanium grades and alloys are divided into four
groups: 1兲 commercially pure titanium, 2兲 ␣ and near ␣ alloys such as
Ti-6Al-2Sn-4Zr-2Mo, 3兲 ␣-␤ alloys like Ti-6Al-4V, and 4兲 ␤ alloys that have a high
content of vanadium, chromium, and molybdenum.
Commercially pure titanium and most of the alloys are soft and ductile with a low
machinability, difficult to prepare because of development of a deformed layer.
Also, titanium can be sensitive to hydrogen and high temperatures during the
preparation. Heat-treated alloys are harder and consequently easier to prepare.
Sectioning: Due to the high ductility and toughness of titanium it has low
machinability. Consequently it can be very difficult to cut with wet abrasive cutting
using the standard cut-off wheels because the edge will clog-up with abraded
material.
Titanium should be cut with a special SiC, bakelite bond wheel with a strong flow
of cooling fluid to obtain a cool and burr-free cut. Sectioning with a shear or with
a band saw cannot be recommended, but if they are used, care should be taken
with prolonged plane grinding to remove the heavy deformation 共cold work兲
developed during cutting.
Mounting: Generally hot and cold mounting can be used. Because of the low
machinability of titanium a mounting material with a high wear resistance should
be used 共see Section 3.1.3兲. Still it can be experienced that the mounting material
is removed at a much higher rate than the sample. This can be dampened by
placing two or more samples in the same mount, not only one in the center of the
mount.
If the specimen should be etched with a strong etchant, a mounting material with
a high chemical resistance should be used. In the case of examination of surface
layers, special mounting materials should be used 共see Material/Preparation Tables
08–10兲. If the examination involves the hydride phase, it may be of advantage to
leave the specimen unmounted or use an epoxy which cures slowly at a
temperature not much above room temperature.
Grinding: As rough SiC papers will leave deep deformation in the specimen, the
plane grinding should be performed with the finest grinding paper possible. Plenty
of water should be used. In the two methods below grit 220 is stated for plane
grinding, but if the sectioned surface is not very rough, grit 320 should be
preferred. New papers should be used. Often the paper can only be used in
20– 25 s to avoid smearing and development of cold work.
Polishing: Using finer and finer diamond grades as is normally done develops
deformed layers in titanium, very difficult to remove. Therefore, the deformation
from the grinding is removed by chemical mechanical polishing 共see below兲.
Both pure titanium and a number of alloys can be electrolytically polished.
Etching: A microstructure of titanium can be examined in polarized light without
etching. For Etchants, see below.

thickness/hardness,
surface layers
Image analysis, E 562, E 1245, E 1382 C-60
rating of inclusion
content
High planeness
hardness E 140, E 384, E 448
E 1245, E 1351, E 1382, E 1558 El-20
El-20
Sectioning
Cut-Off Wheel SiC, bakelite bond, specially developed for titanium
Mounting
Hot Compression Resin Bakelite/Epoxy Cold Resin Epoxy

Mounting with Filler Mounting
Time 8–9 Time 8 – 24 h
Grinding
C-60 and T-60: Use a grit 320 grinding paper for the PG step if possible, for pure
titanium and soft alloys.
Polishing
C-60: For the step P 1 use one of the following solutions: 90 mL silica with
10 mL hydrogen peroxide 共30 %兲 or 96 mL silica, 2 mL hydrogen peroxide 共30 %兲
and 2 mL ammonia solution 共25 %兲.
T-60: For the steps P 1, P 2, and P 3 use the solution: 260 mL silica, 40 mL
hydrogen peroxide 共30 %兲, 1 mL nitric acid 共65 %兲 and 0.5 mL hydrofluoric acid
共40 %兲.

Section 13.2.2.兲
Grinding/ PG FG 1 P1
Polishing
Disk/Cloth SiC paper RCD, soft Cloth, napless,
soft,
porous,
syn
Abrasive Type SiC Dia, spr or susp Silica,
see note above
Grit or Grain 220 9 0.04/ 0.05
Size ␮m
Lubricant Type Water Alco or wat
Rotation 300/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Contra Comp Contra
Force per 25 共5.7兲 30 共7兲 20–30 共5.7–6.6兲
Specimen
N 共lb兲
Time Until plane 5 8–10
Minutes

Section 13.2.2.兲
Polishing
soft, soft, soft,
porous, porous, porous,
syn syn syn
Abrasive SiC SiC SiC SiC Silica, Silica, Silica,
Type see see see
note note note
above above above
Grit or Grain P220 P320 P500 P1200 0.04/ 0.05 0.04/ 0.05 0.04/
Size ␮m 0.05
Lubricant Water Water Water Water
Type
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp Comp Comp Comp Contra Contra Contra
or or or
Force per 20 20 20 20 35 共8兲 20 共4.5兲 10 共2.2兲
N 共lb兲
Time Until 0.25–1 0.25–1 0.25–1 10 2 2
Minutes plane
Etchants
Pure Ti 186, 187, 67, 68, 69, 217 General structure
188 Removes stain
Ti-5Al-2.5Sn 189 Reveals hydrides
Ti-6Al-6V-2Sn 190 Stains alpha and transformed
beta, retained beta remains
white
Ti-Al-Zr 191 General structure
Ti-8Mn 192 General structure
Ti-13V-11Cr-3Al 共aged兲 192 General structure
Ti Si 193 General structure
Ti alloys 186, 187, 192, 194, 158, General structure
132b, 1c, 67, 68, 69, 3a, 218
11, 1c Reveals alpha case
72, 192, 178 Chemical polish and etch
170a Outlines and darkens hydrides
in some alloys
188 Removes stain
Material: Zinc and Zn alloys
Material Properties: Zinc: Close-packed hexagonal, 7.14 g / cm3, 419° C 共786° F兲.
Zinc alloys: Zn is mainly alloyed with aluminum, 1 to 15 % and copper up to 4 %.
Other alloying elements are lead, cadmium, iron, titanium, magnesium, and tin
共weight %兲.
Comments on Material: Zinc is to a high degree used for die-casting and for
coating of steel sheet 共see Material/Preparation Tables 08–10兲.
Zinc is very difficult to prepare because of the tendency to form layers of plastic
deformation with smearing and twins when being ground and polished. Also,
embedding of abrasive grains during grinding and polishing is a risk.
Sectioning: Abrasive wet cutting of pure zinc and zinc alloys can be done with a
thin SiC bakelite cut-off wheel, preferably on a precision cutting machine with an
efficient cooling. Zinc also can be cut by shearing or with a band saw or hand saw
with fine teeth. In the case of shearing and sawing the very deformed zone must
be carefully removed during grinding. For cutting of zinc coated steel sheet, see
Material/Preparation Tables 08–10.
Mounting: Cold mounting should be preferred because hot compression mounting
may cause deformation and recrystallization in the material. In the case of
mounting of zinc coated steel sheet, see Material/Preparation Tables 08–10.
Grinding: If the sectioned surface is not very rough, plane grinding should be
done with grit 320 SiC grinding paper. To minimize the risk of embedded SiC
grains in the specimen surface, the grinding paper can be treated with wax and a
low pressure is used. Also, paraffin can be used instead of water. For pure zinc it
can be of advantage to extend the time for the last FG steps to ensure that
deformation from earlier steps is removed.
Polishing: Only use a polishing cloth for zinc, do not mix with copper or lead. It
is important that the deformation from the grinding is removed during the P 1
polishing step. Pure zinc and some zinc alloys are suited for electrolytic polishing.
Cleaning: Avoid water for cleaning between the polishing steps; use alcohol for
cleaning and finish the polishing with a very brief polish with pure alcohol
followed by rinsing and drying.
Etching: A microstructure of zinc can be examined in polarized light without
etching. For Etchants, see below.

thickness/hardness,
surface layers
El-23
Image analysis, rating of E 562, E 1245, E 1382 C-61
inclusion content
High planeness
E 110, E 140, E 384,
E 448
E 1183, E 1245, E El-23
1351, E 1382, E 1558
El-23
Sectioning
Cut-Off Wheel SiC bakelite bond, thin wheel
Mounting

Grinding
T-61: Cutting action of SiC papers can be dampened with wax. If possible, use
grit P320 for the PG step.
Polishing
C-61: In some cases P 2 can be omitted. Also, the cloth in P 2 can be changed to
a medium nap, soft, synthetic.
T-61: A step like P 2 in Method T-57 can be added between steps P 1 and P 2.
Cleaning: Avoid water for cleaning between polishing steps, use alcohol for
cleaning and finish the polishing with a very brief polish with pure alcohol
followed by rinsing and drying.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC RCD, Cloth, Cloth, Cloth,
paper soft napless, napless, napless,
hard, hard, soft,
wov, wov, silk porous,
syn syn
Abrasive Type SiC Dia, spr or Dia, spr Dia, spr Silica
susp or susp or susp
Grit/Grain P320 9 3 1 0.04/ 0.05
Size ␮m
Lubricant Type Water Alco or wat Wat-oil Alco or wat
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Force per 25 共5.7兲 30 共7兲 25 共5.7兲 20 共4.5兲 10–15

N 共lb兲
Time Until 4 4–6 3–5 1–2
Minutes plane

Section 13.2.2.兲
Polishing

med soft,
hard, porous,
wov, wool syn
Abrasive Type SiC SiC SiC SiC Dia, spr Silica
or susp
Grit or Grain P220 P320 P500 P1200 3 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Water Water Wat-oil
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp or Comp or Comp Comp Contra
Specimen
N 共lb兲
Time Until 0.5–1 1–2 1–2 4–6 1–2
Minutes plane
Etchants
Pure Zn 200a General structure
Zn-Co 177 General structure
Zn-Cu 201 General structure
203 Distinguishes gamma 共␥兲
and epsilon 共␧兲
Zn-Fe 74a Structure of galvanized sheet
Die castings 202 General structure
Material: Zirconium. Zr alloys. Zircalloy. Hafnium. Hf alloys
Material Properties: Zirconium: Close-packed hexagonal, 7.14 g / cm3, 1490° C

共2714° F兲.
Hafnium: Close-packed hexagonal, 13.3 g / cm3, 1700° C 共3092° F兲. Zircalloy:
Zirconium with tin, oxide, iron, chromium, and nickel.
Comments on Material: Pure zirconium and zircalloy are mainly used for
cladding of uranium fuel elements for nuclear power plants. Hafnium also is used
in the nuclear reactors. Both pure zirconium and hafnium are soft and ductile,
difficult to prepare, they deform easily and mechanical twinning may develop. Also
the machineability is low.
Sectioning: Sectioning should take place with great care to avoid excessive
deformation. Wet abrasive cutting can be done with an SiC bakelite bond cut-off
wheel. Preferably the cutting should take place with a precision cut-off machine
using a thin wheel 共0.5 mm 共0.02 in兲兲. It is important that the cooling is very
efficient so that over-heating is avoided. If shearing or band sawing is used, plane
grinding should be extended to remove the strong deformation caused by these
cutting methods.
Mounting: Hot mounting and cold mounting can be used. If the specimen is to be
studied for hydrogen content, or in the case of a risk for mechanical twinning by
the pressure at hot mounting, cold mounting should be preferred. As the specimen
may be attacked by rather strong acids for chemical mechanical polishing and
etching, a mounting material with good chemical resistance, like epoxy, should be
used 共see Sections 3.6.1 and 3.13.1兲.
Grinding: To avoid excessive deformation, the plane grinding should preferably be
done with a grit P320 grinding paper. The grinding should always be wet because
Zr and Hf dust may generate fire. The cutting action of the finer grinding papers
may be dampened with wax.
Polishing: To obtain a surface free from deformation, the final mechanical
polishing step can be turned into chemical mechanical polishing. The chemical
solutions contain strong acids and precautions should be taken to avoid attack of
the grinding/polishing disk and the machine 共see below兲. In the case of hard
particles in the specimen surface, use Method C-62 to avoid relief. For pure metals
use Method T-62 because SiC paper has a better cutting action than diamond.
Etching: Both zirconium and hafnium can be examined in polarized light. For
Etchants, see below.

thickness/hardness,
surface layers
Grain size, E 112, E 930, C-62, T-62,
grain E 1181, E 1382 El-24
boundaries 共Zirconium兲,
El-11
共Hafnium兲
Heat C-62, T-62
treatment
Image analysis, E 562, E 1245, C-62
rating of inclusion E 1382
content
High
planeness
Micro- E 10, E 18, E 92, E 103, C-62, T-62
hardness, E 110, E 140, E 384, E 448
hardness
Micro- E 3, E 407, C-62, T-62,
structure E 562, E 883, El-24
E 1181, E 1245, E 1351, 共Zirconium兲,
E 1382, E 1558 El-11
共Hafnium兲
Phase C-62, T-62,
identification El-24
共Zirconium兲
El-11
共Hafnium兲
Preparation Process
Sectioning
Cut-Off Wheel SiC bakelite bond, a thin wheel
Mounting
Hot Compression Resin Bakelite/Epoxy Cold Resin Acrylics/

Mounting Mounting Epoxy
Minutes Minutes/Hours /6–8 h
Grinding
C-62 and T-62: Avoid grit P220 if possible for PG.

T-62: The cutting action of the SiC papers can be damped with wax.
Polishing
C-62 and T-62: The step P 2: A chemical mechanical polishing can be obtained
by using 96 mL colloidal silica with 2 mL hydrogen peroxide 共30 %兲 and 2 mL
ammonia solution 共25 %兲 or 95 mL colloidal silica with 5 mL chromium trioxide
solution 共20 g CrO3 to 100 mL distilled water兲. Another solution is 75 mL
distilled water, 10 g oxalic acid, 5 mL acetic acid 共glacial兲, 6 mL nitric acid 共70
%兲 and 2 mL hydrofluoric acid 共48–52 %兲共Caution!兲. One part of the solution is
mixed with four parts of silica for the purer zirconium materials and 1 to 1 for
zircalloys and hafnium materials.
Also, a mixture of 90 mL colloidal silica and 10 mL of hydrogen peroxide 共30 %兲
can be used. Zirconium can be electropolished with Method El-24 and hafnium
with El-11.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper RCD, Cloth, napless, Cloth, napless
soft hard, wov, syn soft, porous, syn
Abrasive SiC Dia, spr or susp Dia, spr or Silica, see note
Type susp above
Grit/Grain P320 9 3 0.04/ 0.05
Size ␮m
Rotation 300/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/rpm
Comp/ Comp or contra Comp Comp Contra
Contra
Specimen
N 共lb兲
Minutes

Section 13.2.2.兲
Polishing
Disk/ SiC SiC SiC SiC SiC paper Cloth, Cloth,
Cloth paper paper paper paper napless, napless,
hard, soft,
wov, silk porous,
syn
Abrasive SiC SiC SiC SiC SiC Dia, spr Silica
Type or susp see note
above
Grit or P320 P500 P1200 P2400 P4000 3 0.04/ 0.05
Grain
Size ␮m
Type
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/ Comp or Comp Comp Comp Comp Comp Contra
Contra contra
Specimen
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 4–6 3–10
Minutes plane
Etchants
Zr base 66, 67, 204, 68, 69, 205 General structure
206 Electrolytic polish and etch
71 Grain structure under polarized light
Material: Bones. Carbon. Coal. Graphite. Paper. Teeth. Tissue.
Wood. Other organic materials
Comments on Material: Common to the preparation of organic materials is the
grinding steps on SiC grinding paper to the finest grit. For this reason no
“contemporary” method is developed, and both Methods C-63 and T-63 stated
below are “ traditional” methods. Often organic materials, having pores, cracks,
and voids should be impregnated to obtain a surface that can be satisfactorily
prepared 共see below兲.
Sectioning: Many organic materials like paper and wood can be cut with a scissor
or a fine toothed saw. Other materials like teeth, bones, and coal should be cut on
a precision cut-off machine with a thin cut-off wheel, either with SiC bakelite
bond, diamond in a metal bond, or with fine teeth. In some cases the material
should be impregnated before cutting 共see below兲. For some materials like coal,
the selected sample is crushed and the particles are mounted in a transparent
mounting material 共see Section 3.11.4兲.
Mounting: Often the material contains pores, cracks, and cavities, or it is very
brittle. In this case a vacuum impregnation with epoxy should be done 共see
Section 3.10兲. An example of an organic material, difficult to prepare without
impregnation is paper. It is important that the paper fibers are totally wetted. This
is done with an epoxy with a low viscosity, which, to obtain the best wetting, is
thinned with acetone or another thinner. A method is to briefly soak the paper
specimen in acetone to wet it, soak the specimen in a 50 % acetone/epoxy mixture
for several minutes with abundant stirring. Then transfer the specimen to a 10 %
acetone/90 % epoxy mixture for several minutes, followed by transfer to a bath
with 100 % epoxy for several minutes and finally transfer to a second bath of 100
% epoxy in the mounting cup in which the specimen should be hardened. Several
specimens can be mounted in the same mounting cup, using clips to keep the
specimens upright and separated.
Grinding: In the two methods stated below grinding to P4000 is stated. For some
materials the steps FG 3 and FG 4 can be omitted.
Polishing: Diamond polishing generally is not suited for organic materials;
therefore, diamond is only used for one polishing step in Method T-63. The
polishing step, with silica in Method C-63 can vary considerably in time,
depending on the material being prepared.
Etching: Normally no etching is done.

thickness/hardness,
surface layers
Grain size, C-63, T-63
grain boundaries
Image analysis, rating of C-63, T-63
inclusion content
High planeness
Microstructure E 883 C-63, T-63
Sectioning
Cut-Off Wheel Thin wheel, SiC bakelite bond or diamond with metal
bond or with fine teeth
Mounting
Hot Compression Resin Cold Mounting Resin Epoxy/Acrylics

Mounting Time Time 6 – 12 h / 6 – 10 min
Grinding
C-63, T-63: Carbon and similar materials: Step FG 3 and FG 4 can be omitted,
when followed by a step with 3 ␮m diamond 共see below兲.
periphery, the disk is either discarded trued.
Polishing
Carbon and similar materials and paper: C-63 and T-63: Establish a P 1 step
with a napless, hard cloth with 3 ␮m diamond, see step P 1 in Method C-62,
followed by P 1 in C-63 or T-63. To improve planeness a napless, hard, wov, silk
cloth can be used in P 1 of T-63, possibly followed by P 1 in C-63.
Bones and teeth: T-63: The step P 1 from Method C-64 can be added as final
step.
Paper: C-63: The step FG 4 can be changed to the step P 1 in Method C-62 using
wat-oil lubricant.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC SiC SiC SiC SiC Cloth,
paper paper paper paper paper napless,
soft,
porous,
syn
Abrasive Type SiC SiC SiC SiC SiC Silica
Grit or Grain P320 P500 P1200 P2400 P4000 0.04/ 0.05
Size ␮m
Lubricant Type Water Water Water Water Water
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen
N 共lb兲
Time Until 2 2 2 1–2 1–10
Minutes plane

Section 13.2.2.兲
Polishing
Disk/Cloth SiC paper SiC paper SiC paper SiC paper SiC paper Cloth,
med nap,
soft, syn
Abrasive Type SiC SiC SiC SiC SiC Dia, spr
or susp
Grit or Grain P320 P500 P1200 P2400 P4000 1
Size ␮m
Lubricant Type Water Water Water Water Water Wat-oil
Rotational 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp Comp Comp Comp Comp
contra
Specimen
N 共lb兲
Time Until 2 2 2 1–2 1–6
Minutes plane
Material: EPDM polymers. Silicone. Other elastomers.
Polypropylene „PP…. Polystyrene „PS…. Polyvinylchloride „PVC….
Other thermoplastics
Comments on Material: Plastics and polymers cover a very wide range of

materials with different characteristics, rigid, semi-rigid, and nonrigid. The plastics
and polymers are classified in ASTM Classification System for Specifying Plastic
Materials 共D 4000兲.
A basic reason for making materialographic examinations of plastics and polymers

is to gain a more complete understanding of the relationships between the
manufacturing processes, the microstructure and texture of the material, and the
product’s performance. The microstructures of plastics and polymers visible in the
light microscope are affected to a considerably greater extent by their chemical
composition and method of production than is the case with metals.
Plastics and polymers can be examined in different ways, as cross sections
共polished兲 in reflected light, or as thin sections and microtome sections in
transmitted light 共see Section 7.13兲. The cross sections can be prepared by
grinding and polishing and by ultramilling; only the preparation by grinding and
polishing is described below.
Plastics and polymers are normally soft and very often the material is sensitive to
heat and possibly also to the type of cooling fluid used during the preparation. It is
important that the correct fluid is used in sufficient amounts both at sectioning,
grinding, and polishing to avoid thermal damage. Heat developed may cause a
softening of the material resulting in embedding of abrasive grains in the
specimen surface. It can be advised to test the cooling fluids 共water, alcohol, etc.兲
and mounting material 共acrylics, etc.兲 on the specimen material before the
preparation to check the resistance of the material.
The preparation of plastics and polymers is described in the ASTM Standard
Guide for Preparation of Plastics and Polymeric Specimens for Microstructural
Examination 共E 2015兲.
No “contemporary method” is developed for these materials, so Method C-64
below is a variant of the “traditional method,” T-64 by Trempler, Ref. 40, 共Part I兲.
Also, Methods C-65 and T-65 can be used for these materials. For further
information on preparation of plastics and polymers see Refs. 40 and 41, 共Part I兲.
Sectioning: Selection: The selection of the test specimen is extremely important
and dependent upon the purpose of the examination, the material, and the
microscopical technique to be used. It should be decided whether the specimen
should be taken as a cross section, longitudinal, or inclined. The selection criteria
must include the following considerations: The size and scale of homogeneity/
heterogeneity of all structures, textures, and other features within the work piece
being studied, the size or scale and distribution of the structures to be studied,
and the need for control/reference specimens. In general, sectioning should
produce a flat, relatively damage-free surface near to the region of interest.
Depending on the type of material, the sectioning can be made by cutting with a
sharp knife, a pair of scissors or a scalpel. This technique will introduce a strain
共typically dominated by ductile deformation兲 in the region near the cut face. The
width of the strain region can be minimized by properly securing the specimen
during cutting, using a sharp instrument, making the cut with uniform speed and
force, and making the cut at the appropriate temperature 共often below room
temperature兲. The cut face from a 共cryogenically兲 microtomed specimen is often
ready for microstructural examination with minimal final polishing or without
additional preparation. Sawing either manually or by precision cut-off machine
can be done with a sharp, fine short-toothed saw blade with an efficient cooling.
The surface after sawing is rather rough and the region with nonuniform strain
must be removed by the following grinding and polishing. Also, wet abrasive
cutting with a precision cut-off machine using a wheel with electroplated
diamonds or an abrasive wheel with SiC in a bakelite bond may be used. Abrasive
wheels tend to clog when cutting certain materials and a diamond wheel should be
preferred, using a low feed rate. The cutting should take place with an efficient
cooling using a cooling fluid which is nonreactive with the specimen material.
Often small specimens or parts, or both, with the plane of interest not parallel to a
flat surface may require mounting prior to sectioning to facilitate sectioning of the
specimen parallel to the desired plane to be polished. Also, laminated, friable, or
very ductile materials may be mounted prior to sectioning to minimize damage
during the process.
Mounting: The specimen can be clamped between plates of the same or similar
type of material as the specimen. Also, the specimen can be cold mounted using a
mounting material that does not react with the specimen material, and generally
with a peak temperature sufficiently below the softening temperature of the
specimen material. The softening temperature being in the range from
70 to 125° C 共158 to 257° F兲 for most plastics and polymers limits the use of cold
mounting materials to acrylics having a peak temperature of 90° C 共194° F兲 and
slow curing epoxy with a peak temperature of 30 to 60° C 共86 to 140° F兲. It can be
recommended to work with a temperature not above 40° C 共104° F兲. This limits the
cold mounting material to a slow curing epoxy that also can be used for vacuum
impregnation in case of porous or cracked specimen materials 共see Section 3.10兲.
To discriminate between the mounting material and the specimen material, the
epoxy should be added to a dye. To slow down the curing to keep the temperature
low, the smallest amount of mounting material should be used, and curing can
take place in a refrigerator. Also, cooling can be obtained by placing metal heat
sinks into or around the mount. In the case of the mounting of small parts,
powder or particles, see Section 3.11. In the case of a very sensitive specimen
material, the specimen can be sputter coated with a 20 to 60 nm thick metal film
of gold or gold/palladium to form a barrier towards the mounting material. Also, a
⬎100 nm film will make a good contrast between the specimen-mounting material.
In the case of examination of materials with hard fibers an acrylic mounting
material with a filler should be used.
Hot mounting cannot be recommended for plastics and polymers because of the
high temperatures and high pressure.
Grinding: In Methods C-64 and T-64 four grinding steps are indicated, but often
the step FG 4 and in fewer cases both FG 3 and FG 4 can be omitted. The force on
the specimens should be low and the rotational speed of the grinding/polishing
wheel should not be higher than indicated in the methods. The specimen surface
should be inspected after every 15 to 30 s of grinding to ensure that material
removal does not go beyond the area of interest; this is especially important at
mounted and impregnated specimens. Water is normally used as cooling fluid and
the cooling must be effective. In case the specimen material reacts with water,
another fluid must be chosen.
Perfluorinated liquids, such as those used as diffusion pump oil or as cooling
liquids for active electronic circuits, are often appropriate for use with
water-soluble plastics and polymers. In the case of embedded SiC grains, use more
cooling fluid, lower the force on the specimen and briefly move a blind specimen
across the new grinding paper before it is used for the specimens.
Polishing: When using the grinding papers grit P2400 and P4000 as indicated in
Methods C-64 and T-64, the rough polishing, step P 1, can be done with 3 ␮m
diamond. It is important to ensure a good cooling during the polishing. Use water,
or in special cases glycerol, as lubricant. Care must be taken not to embed the
abrasive in the specimen which can easily occur with softer plastics and polymers.
The use of a lubricant that contains a surfactant or wetting agent can minimize
the embedding of the abrasive. Also, a polish only with distilled water in a few
minutes may remove embedded grains. If after the step P 1, only a few fine
scratches are visible, then proceeding to the final polish, as indicated in Method
T-64, is appropriate. If numerous scratches are visible, then repeat the step P 1 or
follow Method C-64, going to a step with 1 ␮m diamond.
Cleaning: Cleaning is very important when preparing plastics and polymers. The
specimen should be cleaned between each step in an aqueous solution of dish soap
if the material is not water sensitive. The use of ultrasonic baths cleaning is
usually an acceptable practice. However, materials such as partially cured resins
may be damaged by excessive cavitation in ultrasonic cleaning. When drying,
avoid hot air.
Etching: Relief polishing may be sufficient to establish a good examination of the
specimen in dark field illumination 共DF兲 or in differential interference contrast
共DIC兲共see Section 9.2兲. For Etchants, see below.

thickness/hardness,
surface layers
Image analysis, C-64, T64
rating of inclusion content
High planeness
Microhardness, hardness D 785, D 1415, D 2240, E 384 C-64, T-64
Sectioning
Cut-Off Wheel SiC bakelite bond, thin, a thin electroplated diamond

wheel or a fine toothed saw blade
Mounting

Mounting Time Time 6 – 15 min/ 12– 24 h
Grinding
C-64, T-64: For some materials the steps FG 4 and even FG 3 can be omitted.
Polishing
C-64, T-64: Check that the specimen material is not damaged by the lubricant.
For water sensitive materials use glycerol. Clean in distilled water.
C-64 and T-64: Colloidal silica can be used instead of alumina.

Section 13.2.2.兲
Polishing
Cloth paper paper paper paper paper nap- med nap-
less, nap, less,
med soft, soft,
hard, syn porous,
wov, syn
wool
Abrasive SiC SiC SiC SiC SiC Dia, Dia, Alumina
Type spr spr
or or
susp susp
Grit or P320 P500 P1200 P2400 P4000 3 10.02/
Grain 0.05
Size ␮m
Type
Rotation 150/150 150/150 150/150 150/150 150/150 150/150 150/150 150/150
Disk/
Holder
rpm/
rpm

Contra
Force per 10–20 10–20 10–20 10–15 10–15 20 共4.5兲 20 共4.5兲 10 共2.2兲
Specimen 共2.2– 共2.2– 共2.2– 共2.2– 共2.2–
N 共lb兲 4.5兲 4.5兲 4.5兲 3.4兲 3.4兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 4–5 3 Up to
Minutes plane 10

Section 13.2.2.兲
Polishing
hard, soft,
wov, syn porous,
syn
Abrasive Type SiC SiC SiC SiC SiC Dia, Alumina
spr or
susp
Grain or P320 P500 P1200 P2400 P4000 3 0.02/ 0.05
Grain
Size ␮m
Type
Rotation 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Force per 10–20 10–20 10–20 10–15 10–15 20 共4.5兲 10 共2.2兲
Specimen 共2.2–4.5兲共2.2–4.5兲共2.2–4.5兲共2.2–3.4兲共2.2–3.4兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 0.5–1 5 Up to 10
Minutes plane
Etchants
Polypropylene 共PP兲 943, 942, 945, 946 General structure
Polyethylene 共PE兲 945 Reveals lamellar structure
946 Reveals spherolites
Polyamid 共PA兲 946, 947 General structure
Material: Acrylics. Acrylonitrile butadiene styrene „ABS….
Polyamid „PA…. Polycarbonate „PC…. Polyethylene „PE….
Polymethyl methacrylate „PMMA…. Polyester „saturated….
Polyoxymethylene „POM…. Epoxy „EP…. Phenolics. Polyester „un
saturated…. Polyurethane „PUR…. Other thermosetting plastics
Comments on Material: See Material/Preparation Tables 64. Also Methods C-64
and T-64 can be used for these materials.
Mounting: ASTM E 2015 recommends: For polyurethanes 共PUR兲: Sputter coat
with 40 nm of gold, and encapsulate in a moderately soft epoxy 共70 to 75 Shore D
hardness兲 under vacuum and cure at room temperature for 24 h. For
polycarbonates: Sputter as for PUR and encapsulate in acrylic or hard epoxy 共80
Shore D hardness or greater兲 under vacuum; cure acrylic at less than room
temperature; cure epoxy at room temperature for 24 h. For polymethyl
methacrylate 共PMMA兲 the same procedure as for polycarbonates is recommended
only a hard setting epoxy resin should be used since PMMA may react with acrylic
mounting resin For polyester thick films and sheets: Sputter as for PUR and
encapsulate in moderately hard 共75 to 80 Shore D hardness兲 epoxy under vacuum
共for contrast兲, and cure epoxy at room temperature for 24 h.
Grinding: ASTM E 2015 recommends: For grinding of PMMA and polycarbonates:
The FG 3 step in Methods C-65 and T-65 are changed to a rough polishing step
with 6 ␮m diamond or to 9 ␮m diamond for polyester thick films and sheets 共see
below兲.
For preparation of soft and ductile materials, use T-65.
Polishing: ASTM E 2015 recommends: For final polishing of urethanes, PMMA
and polycarbonates: The P 3 step in Methods C-65 and T-65 are changed to
0.05 ␮m gamma alumina 共see below兲.
Etching: See etchants below and Material/Preparation Tables 64.

Case or coating B 487 C-65, T-65
thickness/hardness,
surface layers
Image analysis, rating of C-65, T-65

inclusion content
High planeness
Microhardness, hardness D 785, D 1415, D 2240, E 384 C-65, T-65
Microstructure E 3, E 2015 C-65, T-65
Phase identification C-65, T65
Sectioning
Cut-Off Wheel SiC bakelite bond, thin wheel or wheel with fine teeth
or a thin electroplated diamond wheel
Mounting

Mounting Time Time 6 – 15 min/ 12– 24 h
Grinding
C-65 and T-65: For PMMA and polycarbonates: Change the step FG 3 to a rough
polishing step with a soft napless nonwoven synthetic cloth, 6 ␮m diamond,
lapping oil, 150/ 150 r / min, Comp, 18–27 共4–6兲 N 共lb兲, 30 s, repeat as needed. For
polyester thick film and sheets: Change the step FG 3 to a rough polishing step
with a perforated hard nonwoven chemitextile pad, 9 ␮m diamond, distilled
water, 120/ 120 r / min, Comp, 13 共3兲 N 共lb兲, 30 s, repeat as needed.
C-65: Often a step with SiC paper grit P2400 should be added between FG 2 and
FG 3.
Polishing
C-65 and T-65: For urethanes, PMMA and polycarbonates: Use 0.05 ␮m alumina
for final polishing, step P 3, instead of the stated silica. For polyester thick film
and sheets: Use 0.05 ␮m alumina mixed with colloidal silica in high pH aqueous
suspension for step P 3.
C-65: Often the steps P 1 and P 2 can be omitted.

Section 13.2.2.兲
Polishing
paper paper paper paper napless, med nap, napless,
hard, soft, syn soft,
wov, silk porous,
syn
Abrasive Type SiC SiC SiC SiC Dia, Dia, Silica
spr spr
or or
susp susp
Grit or P320 P500 P1200 P4000 3 1 0.04/ 0.05
Grian
Size ␮m
Lubricant Water Water Water Water Wat-oil Wat-oil
Type
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
or
Contra
Force per 20–30 20–30 20–30 20–30 30 共7兲 20–30 10–20
Specimen 共4.5–7兲共4.5–7兲共4.5–7兲共4.5–7兲共4.5–7兲共2.2–4.5兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 3–4 2–3 0.5–1
Minutes plane

Section 13.2.2.兲
Polishing
paper paper paper paper napless, med napless,
med nap, soft,
hard, soft, porous,
wov, syn syn
wool
or susp or susp
Grit or P320 P500 P1200 P2400 3 1 0.04/ 0.05
Grain
Size ␮m
Lubricant Type Water Water Water Water Wat-oil Wat-oil
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
or
contra
Force per 20–30 20–30 20–30 20–30 30 共7兲 20–30 10–20
Specimen 共4.5– 共4.5– 共4.5– 共4.5– 共4.5–7兲共2.2–4.5兲
N 共lb兲 7兲 7兲 7兲 7兲
Time Until 0.5–1 0.5–1 0.5–1 3–4 2–3 0.5–1
Minutes plane
Etchants
Polyoxymethylene 共POM兲 945 Reveals spherolite spherolite
cores and growth direction
948 General structure
Polycarbonate of styrene 947 General structure
Material: Powder Metals. Ferrous. Nonferrous
Material Properties: Iron-graphite mixtures: Up to 0.8 % carbon. Iron-copper: 2

to 20 % copper. Iron- copper-carbon: 2.0 to 5.0 % copper, 0.8 % carbon.
Iron-phosphorous: Phosphorous less than 1 %. Iron- nickel: 2 to 4 % nickel, 0.4 to
0.8 % carbon, up to 2.0 % copper.
Stainless steels: Compositions that approximate AISI designations 303, 304, 316,
for austenitic stainless steels and 410 for martensitic stainless steels.
Copper-base: Bronzes with 10.0 % tin Brasses with 10, 20, and 30 % zinc. Nickel
silver with 18 % zinc and 18 % nickel. Some alloys may contain 2.0 % lead.
Titanium-based: 6.0 % aluminum, 4.0 % vanadium.
Aluminum-based: 0.25 to 4.4 % copper, 0.6 to 0.8 % silicon, 0.4 to 1.0 %
magnesium 共weight %兲.
Comments on Material: Powder metal is one of the four major methods of
forming metals 共casting, machining, and plastic forming兲. It is the process of
producing metal shapes from metallic powders. The metal powder is blended,
pressed 共compacted兲 into shape, and sintered to temperatures just below the
melting point. The process offers a wide variety of alloys and material properties.
The main production of powder metal parts is small to medium sized parts for the
auto and manufacturing industry. The advantage is that the parts have a good
surface finish with close dimensional tolerances so that machining is reduced or
avoided. Other alloys are made for cutting tools with tungsten carbide and other
carbides 共see Material/Preparation Tables 67兲. Powder metals are classified with a
prefix and a code, an example is: CNZ—1816–13, where C means copper 共base
element兲, N means nickel 共minor element #1兲, Z means zinc 共minor element #2兲, 18
means percentage of minor element #1, 16 means percentage of minor element #2,
and 13 means minimum yield strength.
During the sintering, recrystallization and grain growth occur between the
particles in a contact area, and a grain and lattice structure such as known from
solid metals is developed. Voids and pores between the particles are still present,
depending on the amount of compression and the time of sintering. When doing
metallographic/materialographic examination, the major difference between solid
metals and powder metals is the amount of porosity. Sintered materials generally
exhibit 0 to 50 % porosity which affects mechanical properties and strongly
interferes with the preparation and interpretation of the microstructure. Careful
preparation is important because the shape of the porosity is as important as the
amount in judging sintered strength and the degree of sintering. The main
problem during the preparation is the smearing of the pores during grinding and
rough polishing that may occur even when the pores are filled with a resin 共see
below兲.
For mounting of uncompacted powder, see Section 3.12.4. Preparation of mounted
specimens with uncompacted powder is in principle done as for the base material,
but often the preparation times should be reduced to avoid over-polishing of the
powder particles embedded in the epoxy.
Sectioning: Selection: As the density and other features can vary considerably, it
is important that the specimens are selected from the surface and interior of the
part and from top and bottom. Wet abrasive cutting with an SiC or Al2O3 bakelite
bond cut-off wheel, depending on the base material of the powder metal.
Preferably a precision cut-off machine with an effective cooling and a thin wheel
共0.5 mm 共0.02 in兲兲 should be used to reduce material damage.
In the case of band sawing, the relatively large deformed layer of the cut surface
should be removed through a careful plane grinding.
Mounting: Before mounting it may be necessary to remove fluids absorbed in the
pores of the material during the manufacture and cutting. If the specimen can be
heated, the fluids 共water and oil兲 can be removed by heating the specimen in a
short time on a hot plate under a fume hood. If the specimen material cannot be
heated an extractor-condenser like the Soxhlet apparatus may be used. The
apparatus consists of a flask, a siphon cup, and a condensing-coil unit that fits on
the top of the flask. A solvent, such as toluene or acetone, is placed in the flask,
and the specimen to be cleaned is placed in the siphon cup. Six cycles, requiring a
total of 1 h, will usually ensure removal of the oil. The method is described in
ASTM Standard Test Method for Density, Oil Content, and Interconnected Porosity
of Sintered Metal Structure Parts and Oil-Impregnated Bearings 共B 328兲. Also,
ultrasonic cleaning under a fume hood for one h in 1-1-1 trichloroethane and a
hot ultrasonic bath has been recommended. The residual entrapped solvent should
be evaporated from the specimen.
Mounting of specimens, which should be examined for porosity, should be done
with a low viscosity epoxy, ensuring an effective vacuum impregnation 共see Section
3.10兲. If edge retention is important, the epoxy should be mixed with a filler 共see
Section 3.11.2兲. Other specimens can be hot mounted or cold mounted with
acrylics.
Grinding: For materials with high porosity and which are relatively soft and
ductile it may be of advantage to extend Method T-66 with a step using grit 2400
grinding paper 共see below兲.
Polishing: It is important that the porosity is “clean,” all pores must be opened,
after the 3 ␮m diamond step. If this is not the case, the step should be prolonged.
For the final polishing step a chemical mechanical polishing may be of advantage
共see under the Material/Preparation Tables covering the base material兲.
Etching: Often the specimen is examined in unetched condition to evaluate the
number and distribution of the particle boundaries.
Etchants used for the base metal may be used; these can be found under the
relevant Material/Preparation Tables.

thickness/hardness,
surface layers
grain boundaries
rating of inclusion
content
High planeness
Microhardness, hardness B 931, B 932, B 933, C-66, T-66
E 10, E 18, E 92, E 103, E 110,
E 140, E 384, E 448
Microstructure B 328, E 3, E 407, E 562, E 883, E 1181, C-66, T-66
E 1245, E 1382, E 1558
Sectioning
Cut-Off Wheel SiC or Al2O3, bakelite bond, thin wheel
Mounting
Hot Compression Resin Bakelite Cold Resin Epoxy/Acrylics

Mounting Time 8–10 Mounting Time 6 – 12 h / 6 – 10 min
Grinding
T-66: In case of soft, ductile materials a grinding step, FG 4, with grit P2400
grinding paper can be added.
Polishing
C-66 and T-66: For final polishing chemical mechanical polishing may be used
共see the relevant Material/Preparation Tables for the base material兲.
C-66: Often the step P 2 can be omitted.

Section 13.2.2.兲
Polishing
Disk/Cloth SiC SiC RCD, Cloth, Cloth, Cloth,
paper paper soft napless, med napless,
hard, nap, soft,
wov, soft, porous,
syn syn syn
Abrasive SiC SiC Dia, Dia, Dia, Alumina
Type spr spr spr
or or or
susp susp susp
Grit/Grain P220 P500 9 3 1 0.02/ 0.05
Size ␮m
Lubricant Water Water Alco or wat Alco or wat Alco or wat
Type
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/
rpm
Contra contra
Force per 20–30 20–30 20–30 20–30 20–30 10–15
Specimen 共4.5–7兲共4.5–7兲共4.5–7兲共4.5–7兲共4.5–7兲共2.2–3.4兲
N 共lb兲
Time Until plane 1 5 4 3 1
Minutes

Section 13.2.2.兲
Polishing
hard, hard, soft,
silk syn
Size ␮m
Type wat wat
Rotation 300/ 150 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
Force per 20–30 20–30 20–30 20–30 20–30 20–30 10–15
Specimen 共4.5–7兲共4.5–7兲共4.5–7兲共4.5–7兲共4.5–7兲共4.5–7兲共2.2–3.4兲
N 共lb兲
Time Until 0.5–1 0.5–1 0.5–1 4 3 1–2
Minutes plane
Etchants
See under the relevant Material/Preparation Tables covering the base material of
the powder metal.
Material: Sintered „cemented… tungsten carbides. Hard metals.
Other coated sintered carbides
Comments on Material: Cemented carbides 共sintered carbides, hard metals兲 are

sintered materials consisting of tungsten carbide or a mixture of tungsten carbide,
titanium, or tantalum carbide in powder form, sintered in a matrix of cobalt or
nickel. Cemented carbides, being very hard and tough with a high wear resistance,
are suited for cutting tools, metal forming tools, rock drilling, and other purposes
where a high wear resistance is needed. To improve the wear resistance of the
cutting tool, often the cemented carbide insert is coated by chemical vapor
deposition 共CVD兲 with one or more hard materials like titanium carbide, titanium
nitride, titanium carbonitride, and aluminum oxide, the coating being
0.2 to 10 ␮m thick.
Cemented carbides are covered by a number of ASTM standards regarding

specimen preparation 共B 665兲, determination of microstructure 共B 657兲, apparent
grain size 共B 390兲, and apparent porosity 共B 276兲共see below and Section 12.4兲.
The high hardness of cemented carbides makes only metallographic/
materialographic preparation with diamond possible. The relatively soft cobalt can
be smeared over the carbides and lack of adequate pressure on the specimen
during polishing may result in pull-outs 共material being torn from the surface of
the specimen兲. This condition may erroneously be interpreted as porosity 共see
Section 13.6.4兲.
Sectioning: The carbides, being very hard, the wet abrasive cutting should be
done with a diamond metal bond cut-off wheel preferably on a precision cut-off
machine so that a thin wheel can be used, reducing the damage to the cut surface.
The cutting, with an efficient cooling, should be performed with a suitable low
feed speed to avoid fracturing of the relatively brittle material, especially at the
end of the cut.
Mounting: Due to the high hardness, cemented carbides should always be
mounted in a mounting material with a filler. For hot mounting, epoxy with a filler
is recommended and for cold mounting acrylics with a filler or epoxy with an
in-mixed filler may be used 共see Sections 3.1.3 and 3.11.2兲. In the case of
examination of coatings, an epoxy mounting material should be used 共see also
Material/Preparation Tables 08–15兲.
Grinding: If the sectioning has been without excessive deformation, the PG step in
Method T-67 can be omitted.
Polishing: It is important that all deformation from the previous steps are
removed after the 3 ␮m diamond step, P 1 in Method C-67 and P 2 in T-67. Often
the surface after this step is satisfactory for routine examination. Alumina should
not be used for cemented carbides with cobalt matrix because the surface may
corrode. Also, the cleaning should be with alcohol only because water may corrode
the cobalt matrix.
Etching: See etchants below. A physical etching by relief polishing can be made if
a napped cloth is used for the final polishing step, a relief between carbides and
matrix will develop 共see below兲 Also, vapor deposition of interference layers may
give good results 共see Section 9.6兲.

Case of coating thickness/ B 487 C-67
hardness, surface
layers
Grain size, grain boundaries B 390, E 1382 C-67, T-67
Image analysis, rating E 562, E 1245 C-67, T-67
High planeness
Microhardness, hardness E 10, E 18, E 92, E 140, E 384 C-67, T-67
Microstructure B 657, B 665, E 3, E 562, C-67, T-67
E 1245
Porosity B 276 C-67, T-67
Sectioning
Mounting
Hot Compression Resin Epoxy Cold Resin Epoxy with Filler/

Mounting with Filler Mounting Acrylics with Filler
Time Time 6 – 12 h / 6 – 10 min
Minutes Minutes/
Hours
Grinding
C-67: Very often the FG 2 step can be omitted.

T-67: Very often the PG step can be omitted.
Polishing
C-67: In case of pull-outs developed during the grinding, the time of step P 1
should be prolonged.
T-67: In case of pull-outs developed during the grinding, the time of step P 2
should be prolonged.
C-67 and T-67: The final polishing step can be changed to 1 ␮m diamond on a
medium napped cloth
共see Method T-65, step P 2兲.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, hard RCD, Cloth, Cloth,
hard, wov, soft, porous,
syn syn
susp susp susp
Grit or Grain P120 9 3 3 0.04/ 0.05
Size ␮m

Type
Rotation 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Specimen N
共lb兲
Time Until 5 5–10 5–8 1–2
Minutes plane

Section 13.2.2.兲
Polishing
Disk/Cloth Dia Dia pad, Cloth, Cloth, Cloth, Cloth,
pad, met bak napless, napless, napless, napless,
v. hard hard, hard, soft,
wov, syn nonwov, porous,
wov, syn syn syn
Abrasive Type Diamond Diamond Dia, spr or Dia, spr or Dia, spr or Silica
susp susp susp
Grit or Grain 125 30 15 6 3 0.04/ 0.05
Size ␮m
Lubricant Water Water Alco or Alco or wat Alco or
Type wat wat
Rotation 300/ 150 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra contra
Specimen N
共lb兲
Time Until 3–5 6 5 5 2
Minutes plane
Etchants
Cemented tungsten 951 Identification
carbides according to of ␩ phase
ASTM Standard B 657
共Etching Technique 1兲
Cemented tungsten 949 in combination with Identification

carbides according to 950 of ␥ phase
ASTM Standard B 657
Cemented tungsten 951 Identification
carbides according to of ␣ phase
ASTM Standard B 657
Material: Uranium and Uranium dioxide. Americium. Cadmium.
Indium. Mercury and amalgams. Neptunium. Plutonium. Rare
earth metals. Selenium. Tellurium. Thallium. Thorium
Material Properties: Uranium: Body-centered cubic, 238.07 g / cm3, 1689° C

共3010° F兲, HV 190. For all other materials mentioned above, see below.
Comments on Uranium: Uranium 共U兲 belongs to the rare earth metals radioactive
group. It is the most important of the rare earth metals 共see below兲 because it has
been used as a metallic fuel in producing atomic energy. The metallic fuels have
been superceded by oxide fuels, and the information below covers preparation of
uranium dioxide 共UO2兲. Uranium dioxide is normally used in the form of pellets
that are made through a process where the raw material in powder form is
sintered at a high temperature. In this state the uranium dioxide can be
considered a ceramic material of cubic crystal structure with a very high melting
point.
U and UO2 are radioactive materials and a health hazard so that all handling shall
take place in hot cells or glove boxes through manipulators so that human contact
with the radioactive material is avoided.
The metallographic/materialographic preparation process follows the same lines as
normal preparation, only as mentioned in a shielded environment and with special
precautions regarding the disposal of the used consumables. The preparation
process stated below is for uranium dioxide, and two methods, a “C-method” and
a “T-method” are indicated.
Comments on Other Materials:
Americium 共Am兲, neptunium 共Np兲, plutonium 共Pu兲, and thorium 共Th兲 are
radioactive metals and will not be discussed further.
Cadmium 共Cd兲, indium 共In兲, and thallium 共Tl兲 are very soft metals that are seldom
used. Cd and Tl are toxic. These metals will not be discussed further.
Mercury 共Hg兲 and amalgams: Amalgams are mercury alloys consisting of Hg
mixed with powders of silver, tin, copper, and zinc. Only amalgams can be
metallographically prepared, and these alloys will not be discussed further.
Rare earth metals: This group of 15 metals are very rarely prepared and will not
be discussed further. For yttrium 共Y兲 see Material/Preparation Table 20.
Selenium 共Se兲 and tellurium 共Te兲 are semiconductors and very toxic and will not
be discussed further. For preparation of the semiconductors silicon and
germanium see Material/Preparation Tables 21.
Sectioning: The uranium dioxide, in pellet form, is normally encapsulated in

epoxy 共mounted兲 prior to cutting. This is to minimize fragmentation of the
material and thereby reduce the waste and contamination issues. The cutting is
done on a special cutting machine made for the special conditions in a hot
cell/glove box, using a diamond wheel with resin or metal bond. A wheel with
electroplated diamonds may also be used, especially when cutting encapsulated
material. When working with radioactive material the volume of liquid in any hot
cell/glove box is strictly controlled to a minimum. Consequently, cutting is carried
out with a low rotational wheel speed, controllable feed rate, and wheel cooling by
dip transfer of the coolant to the wheel so that splashing is avoided and the
consumption of coolant is kept very low.
Mounting: Cold mounting with epoxy is used. Vacuum impregnation is used on
some applications 共see Section 3.10兲.
Grinding: Grinding and polishing are carried out on special semiautomatic
machines, often with modifications of standard machines so that all handling can
take place through manipulators.
When using SiC grinding paper, as indicated in Method T-68 below, a large
amount of low level contaminated waste is generated which involves costly
disposal.
Polishing: For the final step both alumina and colloidal silica can be used, often
with addition of hydrogen peroxide 共see below兲.
Etching: See below.

thickness/hardness,
surface layers
grain boundaries
High planeness
Microhardness, C 730, C 849, C 1326, C 1327, C-68, T-68
hardness E 384
E 1268, E 1382
Porosity C-68
Sectioning
Cut-Off Wheel Diamond, metal/resin or electroplated,

see above.
Mounting

Mounting Time Time 6–8 h
Grinding
C-68 and T-68: When using water for cooling this shall be only as drops to
reduce contaminated waste 共see above兲.
Polishing
C-68 and T-68: P 3: Mix 90 mL of alumina or colloidal silica with 10 mL of

hydrogen peroxide 共30 %兲.

Section 13.2.2.兲
Polishing
Disk/Cloth Dia, disk, RCD, Cloth, Cloth, Cloth,
fixed, res hard napless, napless, napless,
hard, hard, wov, soft,
nonwov, syn porous,
syn syn
Abrasive Diamond Dia, Dia, Dia, Silica
Type spr or spr or spr or 共see
susp susp susp note兲
Grit/Grain P220 6 6 3 0.04/ 0.05
Size ␮m
Lubricant Water Wat Wat Alco
Type 共drip兲共drip兲共drip兲 or wat
Rotation 300/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/Holder
rpm/rpm
contra
Force per Specimen N 共lb兲 30 共6.6兲 30 共6.6兲 35 共8兲 30 共6.6兲 30 共6.6兲
Time 2 5 5 4 1.5
Minutes

Section 13.2.2.兲
Polishing
Cloth paper paper paper paper napless, med. napless,
hard, nap, soft,
nonwov, soft, porous,
syn syn syn
Type or susp or susp 共see
note兲
Grit or P220 P320 P500 P1000 6 3 0.02/ 0.05
Grain
Size ␮m
Type 共drip兲共drip兲共drip兲共drip兲
Rotation 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150 150/ 150
Disk/
Holder
rpm/
rpm
Contra
Specimen
N 共lb兲
Time 3 ⫻ 1 min 4 ⫻ 1 min 6 ⫻ 1 min 10⫻ 1 min 8 6 5
Minutes
Etchants
UO2 924 General
structure
13.2.4 Manual Preparation

The methods stated in Section 13.2.3 are based on semiautomatic preparation. It is
possible, however, to use the data stated in the Method Tables for manual 共hand兲 prepa-
ration also.
The T-methods are most suited for preparation by hand, both the methods based
on SiC grinding paper, and the methods based on diamond disks/pads, but also the
C-methods, often using resin bonded diamond disks and rigid composite disks 共RCDs兲
for grinding, can in some cases be transferred to manual 共hand兲 preparation 共see be-
low兲.
As manual 共hand兲 preparation is less uniform, to a high degree depending on the
operator, the times indicated in the Method Tables should only be taken as guidelines
共see below兲.
Manual grinding/polishing should preferably be done on two machines, a grinder

with one or two disks especially designed for SiC paper 共see below兲, rotating with
300 rpm, and a polisher 共150 and 300 rpm兲 with one or two interchangeable disks for
mounting of several polishing cloths or one magnetic disk 共see Section 6.7.1兲. For
manual grinding and polishing, disks for 230 mm 共9 in兲 grinding paper and for
200 mm 共8 in兲 polishing cloths should be preferred. Separating the grinding and pol-
ishing on two machines reduces the risk of contamination, but both processes can also
be done on the same machine.
Before starting on manual preparation, it is recommended to read relevant sec-
tions in Chapters 6 and 7.
Grinding
SiC Grinding Paper
In the Method Tables, P220 grit is usually stated as the first step. If the original surface
of the specimen is very rough it might be necessary to start with P120 or P180 grit be-
fore grinding with a P220 grit. In general, paper with plain back should be used, the
paper being fixed by a thin layer of water between the paper and the disk. For this pur-
pose the disk has a raised edge, allowing water to stay on the disk when not rotating,
and water is added to the disk before the sheet of paper is placed. A ring is often used to
keep down the edge of the paper, but this ring is not fixing the paper, the fixation takes
place through the suction between disk surface and sheet, because most of the water is
slung away by the centrifugal force when the disk starts rotating. The paper should not
be stored in water between uses because this weakens the bond of the paper. Paper with
adhesive back can also be used, but generally the force on the paper at manual grinding
is so low that a plain backed paper can be used. Also, paper with adhesive back is con-
siderably more expensive than plain backed paper. As a “middle solution” a double ad-
hesive foil can be placed between disk and paper and the foil can be used for many
sheets. Water should be supplied in a constant flow to the center of the rotating disk
securing that all debris is washed away.
When grinding, hold the specimen in a firm grip, with a relatively strong pressure,
both hands can be used, and move it from periphery to center of the paper surface and
back in a slow movement. Be careful that the specimen is held so that the scratches are
in the same direction on a given paper. Also, be careful that the specimen is not tilting,
making facets on the surface. When going to next finer grit paper, turn the specimen 90°
so that the new scratch pattern can be seen perpendicular to the scratches from the
previous step. Continue grinding until all scratches from the previous step are re-
moved, and as a rule go on for at least the same period of time to remove possible defor-
mation. This rule covers harder materials with limited deformations introduced, but
for softer, more sensitive materials grinding shall go on for a longer period of time. In
some cases it might be necessary to use several sheets of the same grit. Do not use the
paper for too long, depending on the hardness of the material, the paper is worn after
20– 120 s. If the paper is worn out it is not removing material but creating deformation
in the specimen surface 共see Chapter 6兲. The specimen surface ground correctly is dull
with parallel scratches. If the surface is bright, the paper has been worn and new paper
should be used.
All grinding steps can be done without cleaning in between, but after the last 共fin-
est兲 step the specimen should be cleaned and dried 共see below兲.
Diamond Disks—Diamond Pads

Diamond disks with fixed diamond grains are in the form of diamond in a metal/
bakelite bond on a solid disk, as diamond pads or as resin 共epoxy兲 bonded diamonds,
both on a thin backing, to be fixed by adhesion or magnetically to a grinding/polishing
disk. They are all used with a flow of water and in the same way as SiC paper.
Rigid Composite Disks „RCD…

A disposable RCD is placed on a disk magnetically as described for polishing cloths
below, or a solid disk is used 共see Section 6.7.7兲. Also, the diamond is charged as stated
below, only spray and suspension can be used. The disk shall rotate with 150 rpm.
It can be difficult to use an RCD for hand preparation because the RCD normally
works with relatively little lubrication to avoid “aqua planing.” This process drags
strongly in the specimen and it might be difficult to hold it by hand. The effect is not
very strong on less aggressive 共soft兲 RCDs, and hand preparation can easily be per-
formed. The specimen is rotated around the disk, as described below under polishing;
take care that the whole surface of the disk is used to avoid an unplane surface.
A firm pressure is applied during grinding with RCD; both hands are often used,
like for SiC paper.
The disk should be cleaned regularly to avoid swarf closing the openings between
the segments on the surface.
Diamond Polishing
If using polishing cloths with adhesive back, take care that a number of disks, corre-
sponding to the number of polishing steps, including the step with silica or alumina, is
available. In this way, the cloths charged with different grain sizes can easily be
changed during the process and should only be removed from the disk when worn out,
securing the highest degree of cleanliness and avoiding contamination from disk to
disk. If cloths with magnetic backing are used, the cloth can be removed easily from the
magnetic disk which can stay in the machine, and only one disk is needed.
In the case of a new cloth, charge the cloth with a reasonable amount of diamond,
at paste, use approximately 1 g for a 200 mm disk and recharge regularly with 0.5 g. At
diamond spray, spray one round on the cloth for a start and respray every 2 – 3 min
during the process. At suspension, charge the new cloth with a reasonable amount and
recharge during the process every 2 – 3 min from a spray bottle. If a product with “dia-
mond and lubricant in one” is used, it is added as stated below for lubricant. According
to Samuels Ref. 7, 共Part I兲, diamond paste should give the highest removal rate at
manual polishing.
In the case of a used cloth, take care that the cloth can be used for the material in
question. Normally a cloth should only be used for the same group of materials; this
gives three sets of disks with cloths in an all-round laboratory: for ferrous metals, non-
ferrous metals, and for ceramics.
Starting with a dry cloth, the cloth is wetted with a reasonable amount of lubricant
so that the total surface is moist, but not “swimming,” 共see below兲. It is preferable to use
a water-based lubricant because alcohol- and oil-based lubricants may be dangerous to
health.
The polishing disk should rotate with 150 r / min and the specimen is rotated
slowly in a circle against the direction of the disk. The specimen is moved slowly from
the periphery to the center of the disk and back to secure a uniform wear of the polish-
ing cloth. By rotating the specimen, all phases in the specimen surface are uniformly
treated, ensuring a minimum of artifacts in the surface. Charge the cloth 共RCD兲 with
small amounts of lubricant at the center of the disk in short intervals so that the surface
is just “moist” when touched with a fingertip, not “wet.”
The pressure during polishing is firm at the rough steps and lower at the final steps.
Also, at all steps, the pressure is reduced during the last approximately 30 s.
Important: The times indicated in the Method Tables are based on semiautomatic
preparation, therefore the times for manual preparation could be longer. Until experi-
ence with a given material is developed, take care that deformations and scratches
from the previous step are removed by looking at the specimen surface in the micro-
scope 共see the “Metallographer’s Rule of Thumb” and Trouble Shooting 共Section 13.5兲兲.
Silica and Alumina Polishing

Be careful, especially with silica 共SiO2兲 polishing, that the cloth is absolutely clean be-
fore starting the process, not having dried-in particles from previous polishing; these
particles might scratch the specimen surface. Circulate the specimen as described
above, adding the polishing medium to the center of the cloth from a spray bottle in
small amounts at short intervals.
When finished, clean the specimen and the cloth by further “polishing” in approxi-
mately 10 s with plenty of water added to the center of the cloth. Silica can be especially
difficult to remove and at certain, not too sensitive materials, the specimen surface can
be rubbed with a wad of cotton. To clean a porous cloth use the edge of a piece of plastic
as a scraper on the rotating cloth to remove remaining polishing media to avoid par-
ticles that will later dry-in on the cloth.
Cleanliness and Cleaning

It is important that a step is not contaminated with abrasive grains from the previous
step. The specimen should be washed and cleaned with cotton in lukewarm water and
finally rinsed with ethanol and dried in a stream of warm air or cleaned 共dry兲 com-
pressed air 共see also Chapter 5兲. The hands of the operator should also be washed.
13.3 Electrolytic Polishing and Etching

In electrolytic polishing, or electropolishing, the specimen is placed as an anode in an
electrolytic cell. Material is removed from the specimen surface through the electroly-
sis, and because of this, the prepared surface often has a number of artifacts 共see Chap-
ter 8兲. If the specimen has two or more phases, with different potential, like cast iron
and contains nonmetallic 共nonconductive兲 inclusions, or both, the prepared surface
will not usually show a true or acceptable microstructure.
Electropolishing has, however, a number of advantages. The surface created is
usually scratch-free and without deformation, an advantage for soft metals, difficult to
polish mechanically. Also electropolishing is very effective for routine polishing, the
polishing time is very short, and often the etching can take place as part of the process.
In certain cases like in stainless steel, the etching cannot be done with the electro-
lyte used for polishing, and “external etching” can take place using a low voltage and a
special electrolyte 共see Section 9.5兲.
Trial and Error: To develop a new method, start with a relatively low voltage and
increase with 5 V for each trial until the correct voltage 共current density兲 is found.
Grind with relatively fine SiC paper between trials to remove traces from the previous
electropolishing. Newer electropolishers 共see below兲 have a built-in scan function that
indicates the correct voltage/current level for a given material.
Trouble Shooting: See Section 13.6.5.
Electrolytic polishing is described in the ASTM Guide for Electrolytic Polishing of
Metallographic Specimens 共E 1558兲共see Section 12.4兲.
13.3.1 Electropolishers
The methods stated in this book are based on the use of an apparatus in which the
specimen is placed as an anode on top of a polishing chamber with a mask defining a
specific area to be polished, the chamber containing a cathode and a flow of electrolyte.
The area is usually from 0.5– 5 cm2 共0.08– 0.8 in2兲. A number of parameters, voltage,
polishing/etching current 共amperage兲, flow rate of electrolyte, polishing/etching time,
and electrolyte temperature, are controlled by the apparatus 共see Chapter 8兲.
13.3.2 Electrolytes—Methods for Electropolishing—Table 13.2

A number of electrolytes have been developed for most metals, mainly based on per-
chloric, perchloric/acetic, phosphoric, and sulfuric acids. The composition of a num-
ber of electrolytes covering most materials is stated in Table 13.2. To obtain the formu-
las of a very high number of electrolytes, see Table 2 in the ASTM Standard E 1558 共see
Section 12.4兲.
To find the correct electrolyte for a specific material, go to Table 11.1 and find the
Electropolishing Method 共El-Method兲 number. These methods are stated in Section
13.3.5. The El-Method numbers are also stated in the Material/Preparation Table, Sec-
tion 13.2.3. In the El-Method, the Electrolyte number is stated. This number is taken to
Table 13.2, and the composition is found.
When mixed, the electrolytes often have a relatively short shelf life, around two
months for the most used perchloric acid type. Life also depends on the number of pol-
ishings performed. Often an electrolyte only works best after a few polishings when a
number of metal ions are established.
Attention: Perchloric acid is very dangerous 共explosion兲 when in contact with or-
ganic material at high concentrations. For this reason, only “authorized” electrolytes
containing perchloric acid should be used, and care should be taken that the concen-
tration of perchloric acid is not increased by evaporation of other ingredients in the
electrolyte, like ethanol.
General Safety Precautions: Work with acids and other chemicals is potentially
dangerous. Before using or mixing any chemicals, all product labels and pertinent Ma-
terial Safety Data Sheets 共MSDS兲 should be read and understood. All general precau-
tions should be taken regarding protection of persons. For specific information on han-
dling electrolytes, see Chapter 26.
13.3.3 Table 13.2—Electrolytes for Electropolishing/Etching

Comments to Table 13.2:
The electrolytes are split into five groups. The group number is the first digit in the Elec-
trolyte Number.
Group 1: Perchloric Acid and Alcohol With and Without Organic Additions
Group 2: Perchloric Acid and Glacial Acetic Acid in Varying Proportions
Group 3: Phosphoric Acid in Water or Organic Solvent
Group 4: Mixed Acids or Salts in Water or Organic Solvent
Group 5: Alkaline Solutions
TABLE 13.2—Electrolytes for Electropolishing/Etching.

Electrolyte
Number Use Formula Remarks
1-1 Steel, cast iron, Al, Al Ethanol (95 %) 700 mL One of the best formulas for
alloys, Ni, Sn, Ag, Be, 2-butoxy ethanol 100 mL universal use.
Ti, Zr, U, heat resisting Perchloric acid (30 %) 200 mL Add the perchloric acid to the
alloys mixture of the other two
components.
1–2 Iron and steel in Ethanol (95 %) 730 mL Universal use.
general, stainless steel, Distilled water 90 mL Add the perchloric acid to the
Al, Al alloys, Ni, Sn, Butylcellosolve 100 mL mixture of the other three
Ag, Mo, Ti, Zr, Pb, Pb- Perchloric acid (60 %) 78 mL components. Shelf life around
Sa, Zn, Zn-Al-Cn, Mg two months.
and high Mg alloys
1–3 Carbon, steels, alloyed Methanol (100 %) 600 mL Vogel’s Sparbeize is an inhibitor
steels, stainless, steels, Perchloric acid (60 %) 60 mL used in industrial electrolytic
martensite, high temp. Butylcellosolve 360 mL polishing. The electrolyte can
alloys, Pb, Al-Cu Vogel’s Sparbeize 2 mL be used without this.
alloys, Mn, Mo, Sn, Ti, Attention: Methanol is a poison,
Ti-alloys, Zr, V use fume hood.
1–4 Cast iron, low alloyed Ethanol (95 %) 800 mL Mix in the following way:
C-steels, stainless Propanol (100 %) 100 mL Propanol and ethanol are mixed
steels, Be, Mg, Ni Perchloric acid (60 %) 15 mL and hydroxychinolin is dissolved.
Sodium thiocyanate dihydrate After dissolution the sodium
60 g thiocyanate is added and after
Citric acid 75 g dissolution the citric acid. When
Hydroxychinolin ortho 10 g the citric acid is added, the liquid
turns muddy, but turns clear when
all is dissolved and the perchloric
acid is added.
2-1 Austenitic steels, Cr, Acetic acid (glacial) 950 mL Alternative to Group 1 electrolytes
Hf, Ni, Pb, Th, Ti Perchloric acid (60 %) 50 mL for certain materials.
3-1 Alpha, alpha+beta Distilled water Alternative to electrolyte No. 3-2
brass, Cu-Fe, Cu-Co, 600 mL for Cu alloys.
Co, Cd Ortho phosphoric acid (84 %)
400 mL
3-2 Cu, brass, Au Distilled water Vogel’s Sparbeize is an inhibitor
Ethanol (95 %) 250 mL used in industrial electrolytic
Propanol (100 %) 50 mL baths; this or another similar
Ortho phosphoric acid (84 %) inhibitor improves the electrolyte,
250 mL but can be omitted.
Urea 5 g
Vogel’s Sparbeize 2 mL
4-1 Cd, Mg, Zn, Pb Ethanol (95 %) 800 mL The sodium thiocyanate is
Butylcellosolve 80 mL dissolved in the mixture of water
Distilled water 20 mL and ethanol. When in solution the
Sodium thiocyanate dihydrate butylcellosolve is added.
160 g
4-2 Bronzes, brasses, Methanol (100 %) 900 mL Methanol and propanol are
examination of Propanol (10 %) 140 mL mixed and tartaric acid is
inclusions, materials Butylcellosolve 200 mL dissolved in the mixture, then
with strongly varying Acetic acid (glacial) 120 mL the cobalt nitrate, the iron nitrate
structural elements, Cobalt nitrate (II) 400 g and the urea is dissolved. At
steels with inclusions Iron (III) nitrate 40 g last the acetic acid and butylcellosolve
Tartaric acid 140 g are added.
Urea 4 g Attention Methanol is a poison,
use fume hood.
5-1 W Distilled water 1000 mL The NaOH content can be
Sodium hydroxide 20 g increased to 100 g
13.3.4 Mechanical Preparation for Electropolishing

To shorten the polishing time and thereby improve the quality of the electropolished
surface, the specimen is normally ground on a number of SiC grinding papers before
polishing. In the Method Tables 共Section 13.3.6兲 only three grinding steps are stated. If
only fine grinding 共FG兲 is indicated, often a plane-grinding step should be performed
before the FG steps. If the polishing time should be reduced, it is recommended to use
finer grits of SiC paper, a rigid composite disk, or a hard polishing cloth both with dia-
mond for fine grinding and rough polishing 共see the Method Tables for the given mate-
rial in Section 13.2.3兲.
Short Time „Shock… Polishing

In case of materials difficult to electropolish, the polishing time can be reduced to
1 – 2 s, in some cases repeated two to three times, when a mechanical preparation, in-
cluding the 3 ␮m and even 1 ␮m diamond steps are performed. In this way only an
electrolytical “cleaning” of the surface takes place.
13.3.5 Electropolishing—Method Tables

In Section 13.3.6 a number of Method Tables are stated, containing the parameters for
electropolishing of a number of metals. The methods are called El-01 to El-25.
The user will find the method for a specific material by using Table 11.1. The meth-
ods are also stated in the Material/Preparation Tables 共Section 13.2.3兲.
Parameters
Preparation before the electrolytic polishing is stated with a number of parameters 共ab-
breviations兲 similar to the Method Tables of mechanical preparation 共see Section
13.2.2兲.
The electrolytic polishing and etching is stated with the following parameters:
Electrolyte. An “electrolyte number” will be stated. This number is taken to Table 13.2,
which indicates the formula of the electrolyte.
Area. The polished area in cm2, always 1 cm2 共0.16 in2兲. The current stated corre-
sponds to this area.
Temp. The electrolyte temperature during the process in °C 共°F兲. The temperature
should not increase more than 10° C above room temperature during the polishing
process. If polishing large areas or many specimens with short intervals, the electrolyte
must be cooled 共see Chapter 8兲.
Voltage. Voltage between specimen 共anode兲 and cathode in V 共see Area above兲. Two
values are indicated: polishing and etching.
Current. Current 共amperage兲 in A passing between the cathode and the specimen. The
process depends on the correct “current density,” A per cm2共in2兲.
Flow Rate. The flow of electrolyte through the polishing chamber. The rate is indicated
as low, medium, and high.
Time. Polishing and etching time in seconds, indicating the period of time the voltage
is on.
13.3.6 Electropolishing—Methods El-01 To El-25

This section contains 25 Method Tables for electrolytic preparation. The tables include
the data regarding preparation before the electropolishing, and the data for electropol-
ishing and etching.
The data for electropolishing are based on the use of a commercial available elec-
tropolisher 共see Section 8.6兲 that is able to control the stated data. The values indicated
refer to an area of 1 cm2 共0.16 in2兲. In the case of mounted specimens, the mounting
resin in the surface of the mount should not be conductive 共see Section 3.11.6兲.
Attention: A mixed electrolyte will often have a limited shelf life, the most used per-
chloric acid based electrolyte 共No. 1–2兲 only approximately two months.
Trouble Shooting: See Section 13.6.5.
Method Table—Electrolytic Polishing Method El-01

Material: High carbon steels. Medium carbon steels. Manganese
and Mn alloys. Molybdenum and Mo alloys
Method El-01
Grinding/ FG 1 FG 2 FG 3
Electropolishing/ Electrolytic Electrolytic
Polishing Etching Polishing Etching
Disk/Cloth SiC SiC SiC Electrolyte No. 1–3 1–3
paper paper paper 共Table 13.2兲
Abrasive SiC SiC SiC Area cm2 1 1
Type
Grit/Grain P220 P320 P500
Temperature 20–30 20–30
Size ␮m °C 共°F兲共68–86兲共68–86兲
Lubricant Water Water Water Voltage V 40 2–3
Type
Rotation 300/ 150 300/ 300/ Current A 1.8–2 0.2–0.3
Disk/Holder 150 150
rpm/rpm
Comp/ Comp or Comp Comp
Contra contra
Force per 30 共7兲 30 共7兲 30 共7兲 Flow Rate Medium Medium/
Specimen high
N 共Ib兲
Time Minutes 0.5–1 0.5–1 0.5–1 Time s 6–8 2–5
Comments
Electrolytes: 1–2 or 1–1 can be used as alternatives. In case of inclusions, use elec-
trolyte 4–2.

Matherial: Low carbon steels
Method El-02
Grinding/ FG 1 FG 2 FG 3 Electropolishing/ Electrolytic Electrolytic

Type
Gri/Grain P220 P320 P500 Temperature 20–30 20–30
Lubricant Water Water Water Voltage V 35–40 1,5
Type
Rotation 300/ 300/ 300/ Current A 1.8–2 0.2–0.3
Disk/ 150 150 150
Holder
rpm/rpm
Comp/ Comp Comp Comp
Contra or
contra
Force per 30 30 30 Flow Rate Medium Medium/
Specimen 共7兲共7兲共7兲 high
N 共Ib兲
Time 0.5–1 0.5–1 0.5–1 Time s 8 5
Minutes
Comments
Steels with very low carbon content could be fine ground with P1000 SiC paper.
Electrolyte: In case of inclusions, use 4-2.

Material: Gray cast iron. Malleable cast iron. Nodular cast iron
Method El-03
Grinding/ FG 1 FG 2 FG 3 Electro- Electrolytic Electro-
Polishing polishing/ Polishing lytic
Etching Etching
Disk/Cloth SiC SiC Cloth, Electrolyte No. 1–4
paper paper napless, 共Table 4.4兲
hard,
wov, silk
Abrasive SiC SiC Dia, Area cm2 1
Type spr or
susp
Grit/Grain P500 P1200 6 Temperature 20–30
Size ␮m °C 共°F兲共68–86兲
Lubricant Water Water Alco or Voltage V 80
Type wat
Rotation 300/ 150 150/ 150/ Current A 1.8–2
Disk/Holder 150 150
rpm/rpm
Contra contra
Force per 30 共7兲 20 共4.5兲 30 共7兲 Flow Rate Low/medium
Specimen
N 共lb兲
Time Minutes 0.5–1 0.5–1 4–5 Time s 4–6
Comments
In general, cast iron is not suited for electrolytic polishing.
If performed, the process should be short and etching should be chemical with
etchant No. 74 共Nital兲共Table 12.2兲.
The result can be improved by introducing a polishing step before the electropol-
ish, see step P 2 in Method T-30, and cut down the electrolytic polishing to 3 – 4 s.

Material: Heat treated steels
Method El-04
Grinding/ FG 1 FG 2 FG 3 Electro- Electro- Electro-
Polishing polishing/ lytic lytic
Etching Polishing Etching
Disk/Cloth SiC SiC SiC Electrolyte 1–3 1–3
paper paper paper No.
共Table 13.2兲
Abrasive Type SiC SiC SiC Area cm2 1 1
Grit/Grain P220 P320 P500 Temperature 20–30 20–30

Size °C 共°F兲共68–86兲共68–86兲
␮m
Lubricant 300/ 300/ Alco Voltage V 80
Type 150 150 or
water
Rotation 300/ 150 150/ 150 150/ 150 Current A 2 0.2–0.3
Disk/Holder
rpm/rpm
Contra or or
contra Contra
Force per 30 30 30 共7兲 Flow Rate Medium Medium
Specimen 共7兲共7兲
N 共lb兲
Time Minutes 0.5–1 0.5–1 0.5–1 Time s 10 2–10
Comments
Electrolyte: 1-2 or 1-1 can be used as alternatives.
Steels with a high Cr–Ni content might not be electrolytically etched as part of the
process 共see Method El-05兲.

Material: Stainless steels. High alloy steels
Method El-05
Disk/Cloth SiC SiC SiC Electrolyte 1–2 1–2,
paper paper paper No. 共Table 13.2兲 see below
Abrasive SiC SiC SiC Area cm2 1
Type
Size␮m °C 共°F兲共68–86兲共68–86兲
Lubricant Water Water Water Voltage V 40–50 15–20
Type
Rotation 300/ 150 300/ 150 300/ 150 Current A 1.9 0.2–0.3
Disk/Holder
rpm/rpm
Contra contra
Force per 30 共7兲 30 共7兲 30 共7兲 Flow Rate Low/medium High
Specimen
N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 12 up to 120

Minutes
Comments
Etching: For stainless steels external electrolytic etching in oxalic acid 共10 %兲 at
6 V in 10– 15 s, can be recommended.
Electrolytes: 1–3 can be used as an alternative. 2-1 is suited for austenitic steels.
In some cases FG can be reduced to grit P500 SiC paper.

Material: Super alloys, Fe based
Method El-06
Grinding/ FG 1 FG 2 FG 3 Electro- Electrolytic Electrolytic
Polishing polishing/ Polishing Etching
Etching
paper aper paper 共Table 13.2兲
Type
Lubricant Water Water Water Voltage V 40–50
Type
Roation 300/ 150 300/ 150 300/ 150 Current A 1.5–2 0.2–0.3
Disk/Holder
rpm/rpm
Contra contra
Force per 30 共7兲 30 共7兲 30 共7兲 Flow Medium High
Specimen Rate
N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 10–12 5–10
Minutes
Comments
Electrolyte: 1–2 and 1–3 can be used as alternatives.

Material: Iron, pure
Method El-07
paper paper paper No. 共Table 13.2兲
Type
Size °C 共°F兲共68–86兲共68–86兲
Lubricant Water Water Water Voltage V 30–35 1.5
Type
Rotation 300/ 300 150/ 300 150/ 150 Current A 1.5–2 0.2
Disk/Holder
rpm/rpm
Comp/ Comp or Comp or Comp
Force per 30 共7兲 30 共7兲 20 共4.5兲 Flow Rate Medium Medium/
Specimen high
N 共lb兲
Time Minutes 0.5–1 0.5–1 0.5–1 Time s 8–10 5
Comments
Electrolyte: 1–2 and 1–3 can be used as alternatives. In case of inclusions, use 4-2.

Material: High-speed steels
Method El-08
Disk/ SiC paper SiC paper SiC Electro- 1–2 See
Cloth paper lyte No. below
共Table. 13.2兲
Type
Grit/Grain P220 P320 P500 Temper- 20–30
Size ␮m ature 共68–86兲
°C 共°F兲
Type
Rotation 300/ 150 300/ 150 150/ 150 Current A 2

Disk/
Holder
rpm/rpm
Force per 30 共7兲 30 共7兲 30 共7兲 Flow Rate Medium
Specimen
N 共lb兲
Times 0.5–1 0.5–1 0.5–1 Time s 6–10
inutes
Comments
Etching: External electrolytic etching with oxalic acid 共10 %兲 at 5 – 10 V in 10– 15 s.
Electrolytes: 1-1 and 1–3 can be used as alternatives.

Material: Low-alloyed tool steels
Method El-09
Abrasive Type SiC SiC SiC Area cm2 1 1
Lubricant Water Water Water Voltage V 30–40 3
Type
Rotation 300/ 150 300/ 150 300/ 150 Current A 1.8–2 0.3
Disk/ Holder
rpm/rpm
Force per 30 共7兲 30 共7兲 30 共7兲 Flow Rate Medium Medium/
Specimen high
N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 6–10 5–10
Minutes
Comments
Electrolytes: 1-1 and 1–3 can be used as alternatives.

Material: Aluminum and Al alloys. Antimony and Sb alloys.
Beryllium and Be aloys. Bismuth and Bi alloys
Method El-10
Type
Grit/Grain P500 P1200 P2400 Tempera- 20–30 20–30
Size ␮m ture 共68–86兲共68–86兲
°C 共°F兲
Type
Rotation 300/ 150 150/ 150 150/ 150 Current A 1.5–2 0.2–0.4
Disk/Holder
rpm/rpm
Contra contra
Force per 20 共4.5兲 20 共4.5兲 20 共4.5兲 Flow Rate Low/medium High
Specimen
N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 5–15 10–20
Minutes
Comments
Cast Al with Si is not suited for electrolytic polishing. Al alloys with a low Si con-
tent can often be polished as Al alloys.
Electrolytes: 1–1 and 1–3 can be used as alternatives.
Al-Cu alloy should be polished with the electrolyte 1–3.
Etching: Often electrolytic etching is not satisfactory, chemical etching is recom-
mended 共see the Material/Preparation Tables, Section 13.2.3兲.
Fine grinding: By introducing grit P4000 SiC paper before electropolishing the
polishing time can be shortened and a possible relief reduced.
Antimony: The electrolyte 2–1 can be an alternative.
Beryllium: The electrolytes 1–1 and 1–4 can be alternatives.

Material: Chromium and Cr alloys
Method El-11
Disk/ SiC SiC SiC Electrolyte 2–1

Cloth paper paper paper No.
共Table.
13.2兲
Type
Grit/ P500 P1200 P2400 Temperature 20–30
Grain °C 共°F兲共68–86兲
Size
␮m
Type
Rotation 300/ 150 150/ 150 150/ 150 Current 1.8–2.2
Disk/ A
Holder
rpm/rpm
Comp/ Comp Comp
Contra or
contra
Force 20 20 20 Flow Medium
per 共4.5兲共4.5兲共4.5兲 Rate
Specimen
N 共lb兲
Time 0.5– 0.5– 0.5–1 Time s 10–15 5–10
Minutes 1 1
Comments
Etching: Chemical etching is recommended 共see Material/Preparation Tables 46兲.
Fine grinding: By introducing grit 4000 SiC paper and a rough polishing step 共see
Method T-46, step P 1兲, the polishing time can be shortened or deformations in the elec-
tropolished surface can be avoided.

Material: Cobalt and Co alloys
Method El-12
paper paper paper 共Table. 13.2兲
Type
Lubricant Water Water Water Voltage V 15–30 3–4
Type
Rotation 150/ 150 150/ 150 150/ 150 Current A 1.8–2.5 0.1–0.2
Disk/
Holder
rpm/rpm
Contra
Force per 15 15 15 共3.4兲 Flow Rate Medium Medium/
Specimen 共3.4兲共3.4兲 high
N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 10–15 5–10
Minutes
Comments
Electrolyte: As an alternative use phosphoric acid 共85 %兲.

Material: Brass. Copper alloys. Pure Cu
Method El-13
Type
Grit/Grain P500 P1200 P2400
Temperature 20–30 20–30
Lubricant Type Water Water Water Voltage V 15–30 3–4
Rotation 300/ 150 150/ 150 150/ 150 Current A 1.8–2.5 0.1–0.2
Disk/Holder
rpm/rpm
Contra or
contra
Force per 20 共4.5兲 20 共4.5兲 20 Flow Rate Medium Medium/
Specimen 共4.5兲 high
N 共lb兲
Time Minutes 0.5–1 0.5–1 0.5–1 Time s 10–5 5–10
Comments
␤ brass: Having more than one phase, further fine grinding with SiC paper grit
4000 is recommended to shorten the electropolishing time. Also a mechanical polish-
ing step with 3 ␮m diamond can be recommended 共see Method T-49兲.
Copper alloys: See also El-14.
Copper with oxides: See ␤ brass above.

Material: Bronze. Copper bearing alloys
Method El-14
Type
Type
Rotational 300/ 150 150/ 150 150/ 150 Current A 1.5–2 0.1–0.2
Disk/Holder
rpm/rpm
Comp/Contra Comp or Comp Comp
contra
Force per 20 共4.5兲 20 共4.5兲 20 共4.5兲 Flow Rate Medium High
Specimen N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 10–15 10–15
Minutes
Comments
Bronze and other alloys with several phases see Method El-13 regarding prepara-
tion before electropolishing.
Method Table–Electrolytic Polishing Method El-15

Material: Lead and Pb alloys
Methods: El-15
Grinding/ FG 1 FG 2 FG 3 Electro- Electrolytic Electroytic
Polishing polishing Polishing Etching
Etching
Disk/Cloth SiC SiC Cloth, Electrolyte No. 1–1
paper paper napless, 共Table 13.2兲
hard
wov,
sil
Abrasive SiC SiC Dia spr Area cm2 1
Type or
susp
Grit/Grain P500 P1200 6 Temperature 20–30
Lubricant Water Water Wat-oil Voltage V 40–60

Type
Rotation 150/ 150 150/ 150 150/ 150 Current A 1.5–2
Disk/
Holder
rpm/rpm
Contra
Force per 20 20 20 Flow Rate Low
N 共lb兲
Time 0.5–1 0.5–1 5 Time s 3–5
inutes
Comments
Etching: Chemical etching 共see Material/Preparation Tables 52兲.
Electrolytes: 1–2, 2–1, and 4–1 can be used as alternatives.
Electrolytic polishing of Pb should only be last step in a mechanical preparation
process 共see Method T-52兲.
Method Table–Electrolytic Polishing Method El-16

Material: Magnesium and Mg alloys
Method El-16
Disk/Cloth SiC SiC SiC Electrolyte No. 4–1
Type
Grit/Grain P500 P1200 P2400 Temperature 20–30
Type
Disk/
Holder
rpm/rpm
Contra
Force per 20 共4.5兲 20 共4.5兲 20 共4.5兲 Flow Rate Low
Specimen
N 共lb兲
Time 0.5–1 0.5–1 5 Time s 10–15
Minutes
Comments
Etching: Often the surface is etched by the electrolyte. Chemical etching is recom-
mended 共see Material/Preparation Table 53兲.
Electrolytes: 1–2 and 1–4 can be used as an alternative.

Material: Nickel and Ni alloys. Ni-based super alloys
Method El-17
Type
Type
Rotation 150/ 150 150/ 150 150/ 150 Current A 2–2.5
Disk/
Holder
rpm/
rpm
Contra
Force per 20 共4.5兲 20 共4.5兲 20 共4.5兲 Flow Rate Low
Specimen
N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 10
Minutes
Comments
Electrolyte: 2–1 can be used as an alternative.
Preparation before electropolishing: See Method El-13 and T-56.
Short time 共shock兲 polishing: Often a specimen, prepared according to M/PT 56
can be “cleaned” by electrolytic polishing in 1 – 2 s.

Material: Silver and Ag alloys
Method El-18
Grinding/ FG 1 FG 2 FG3 Electropolishing Electrolytic Electrolytic

Type
Lubricant Water Water Water Voltage V 20 15
Type
Rotation 300/ 150/ 150/150 Current A 1.7
Disk/ 150 150
Holder
rpm/rpm
Contra or
contra
Force per 10 10 10 Flow Rate Medium Medium
N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 10 5–10
Minutes
Comments
Electrolyte: 1–1 can be used an alternative.

Material: Tin and Sn alloys
Method El-19
Etching
Type
Grit/ P500 P1000 P1200 Temperature 20–30
Grain °C 共°F兲共68–86兲
Size ␮m
Lubricant Water Water Water Voltage V 60
Type
Disk/Holder
rpm/rpm
Contra contra
Force per 20 共4.5兲 20 共4.5兲 20 共4.5兲 Flow Rate Medium
Specimen
N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 10

Minutes
Comments
Etching: Use chemical etching 共see Material/Preparation Tables 59兲.
Preparation before electropolishing: To avoid deformation, a rough polishing step
can be performed before electropolishing 共see Method T-59兲.
See also Method El-10 for antimony alloys.

Material: Titanium and Ti alloys
Method El-20
Etching
Type
Type
Rotation 300/ 150 150/ 150 150/ 150 Current A 2
Disk/Holder
rpm/
rpm
Contra or
contra
Force per 25 共5.7兲 25 共5.7兲 25 Flow Rate Medium
Specimen 共5.7兲
N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 20–30
Minutes
Comments
Electrolytes: 1-1, 1–2, and 2–1 can be used as alternatives.

Material: Tungsten and W alloys
Method El-21
Etching
Disk/Cloth SiC SiC SiC Area cm2 1
paper paper paper
Abrassive SiC SiC SiC
Type
Lubricant Water Water Water Voltage V 50
Type
Rotation 150/ 150 150/ 150 150/ 150 Current A 2–2.5
Disk/Holder
rpm/rpm
Contra
Force per 20 20 20 Flow Rate Low
N 共lb兲
Time Minutes 0.5–1 0.5–1 0.5–1 Time s 15–20
Comments

Material: Vanadium and V Alloys
Method El-22
paper paper paper 共Tables 13.2兲
Type
Type
Rotation 150/150 150/150 150/150 Current A 2–2.5
Disk/Holder
rpm/rpm

Contra
Specimen
N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 10
Minutes
Comments
Fine grinding: See Method El-11.

Material: Zinc and Zn alloys
Method El-23
Etching
Type
Type
Rotation 150/150 150/150 150/150 Current A 2–2.5
Disk/Holder
rpm/rpm
Contra
Specimen
N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 20–25
minutes
Comments
Etching: Chemical etching can be recommended 共see Material/Preparation Tables
61兲.
Preparation before electropolishing: A rough polishing step can be performed to
avoid deformation 共see Method T-61兲.
Electrolytes: 1–2 can be used as alternative.

Material: Zirconium and Zr alloys
Method El-24
Etching
Type
Type
Rotation 150/ 150 150/ 150 150/ 150 Current A
Disk/Holder
rpm/rpm
Contra
Specimen
N 共lb兲
Time 0.5–1 0.5–1 0.5–1 Time s 10
Minutes
Comments
For preparation before electropolishing: See Method T-62.

Material: Hard metals. Sintered carbides
Method El-25
Grinding/ FG 1 FG 2 FG 3
Electropolishing/ Electrolytic Electrolytic
Disk/Cloth See See See Electrolyte No. 5–1
below below below 共Table 13.2兲
Abrasive Type Area cm2 1
Grit/Grain Temperature 20–30
Lubricant Type Voltage V 15–24
Rotation
Disk/Holder
rpm/rpm
Comp/
Contra
Force per Flow Rate Medium
Specimen
N 共lb兲
Time Minutes Time s 1
Comments
Electropolishing can only be done as a shock polishing. The specimen is prepared
according to Material/Preparation Tables 67 except for the last step, which is done as
electropolishing, shown above.

Preparation
Nondestructive preparation is used for metallographic/materialographic examination
in the field on steam pipes, boilers, etc., and for inspection of large structures like drop
forgings, weldings, etc. The preparation of the surface is along the same lines as for a
normal specimen; both mechanical and electrolytic preparation can be used. Portable
apparatus are available for mechanical grinding/polishing and electropolishing, either
cable- or battery-driven. A portable microscope is needed to check the prepared sur-
face before, in most cases, a replica is made so that the microstructure can be examined
in the laboratory. The process, apparatus, and consumables are described in Part I.
13.4.1 Mechanical Preparation

The same grinding and polishing media are used as stated in the T-methods 共see Sec-
tion 13.2.3兲. A surface of approximately 25 mm 共1 in兲 diameter is prepared to be sure
that a replica of 12 by 18 mm 共0.5 by 0.75 in兲 can be made. The prepared surface is
normally chemically etched before the replica is made. The preparation should be
done very carefully and the prepared area cleaned between polishing steps and before
replication 共see also Manual Preparation, Section 13.2.4兲.
Trouble Shooting: See Section 13.5/6.
13.4.2 Electrolytic Polishing

Normally grinding before electropolishing is made mechanically by hand or with a por-
table grinder. Often also a rough mechanical polishing is performed to shorten down
the electropolishing time and thereby improving the result. For electropolishing, the
data stated in Section 13.3.6 are used only the polished area and corresponding
voltage/current should be calculated. Etching can often be done electrolytically as part
of the polishing process.
Trouble Shooting: See Sections 13.5.4 and 13.6.5.
13.4.3 Replication
The prepared surface is controlled with a portable microscope to ensure that the sur-
face expresses a microstructure that can be accepted for further examination.
The replica can be made either with a piece of plastic 共acetate兲 film or with an
amount of silicon rubber-based material positioned on the prepared spot 共see Section
7.11.2兲.
Fig. 13.1—Part after torching, heavy thermal damage.
Plastic Film
The plastic film, 12 by 18 mm 共0.5 by 0.75 in兲, normally made of methyl acetate, can be
used in two ways. It can be wetted on one side with a suitable solvent such as mono
methyl acetate and after a moment 共5 – 10 s兲 to dissolve the surface, pressed against the
prepared spot, or the spot can be wetted with the solvent, and the film pressed against
the spot. It should be held against the work piece with stable, high pressure with a fin-
ger, and it should be placed very carefully to avoid a movement parallel to the work
piece surface. It is important that the film adheres to the work piece before it is re-
moved; usually a time of 10– 20 s is needed.
In case the plastic film is transparent, it may be difficult to distinguish the details of
the microstructure. This can be improved by coating the backside with black paint or
tape. Another more complicated, but better type of enhancement is to place the replica
in a sputtering device producing an interference layer on the replica 共see Section 9.6.5兲.
Silicone Rubber
The silicone rubber material is dispensed with a hand-operated dispensing gun di-
rectly on the prepared spot. The material will cure in 5 – 15 min and can be used at tem-
peratures from −10° C 共15° F兲 to 180° C 共350° F兲.
When the replica is made it is placed on a glass slide with double adhesive tape to
improve the handling both for microscopy and for filing together with the report.
See also Section 7.11 and ASTM Practice for Production and Evaluation of Field
Metallographic Replicas 共E 1351兲 in Section 12.4.
13.5 Trouble Shooting—How to Improve Preparation Results

The goal of metallographic/materialographic specimen preparation is to produce a
specimen that gives a true picture of the microstructure, reflecting the influence of the
previous manufacturing process or any other process intended to influence or change
the properties of the material.
If the material has in any way been treated with an influence on the microstructure
as a result, either thermally, mechanically, or chemically, this change has to be visible
so it may be classified or graded. In many cases the purpose of the metallographic/
Fig. 13.2—Part after sawing, heavy mechanical damage.
materialographic examination is the validation of the quality of the involved process.

Therefore, it is of utmost importance that the finished specimen, after metallographic/
materialographic preparation, displays the changes introduced during the manufac-
turing, no more and no less.
The preparation must in no way change the structure which means it must not add
any characteristics that have not been there before and, as important, it must not re-
move any of the characteristics that have been introduced during manufacturing. Oth-
erwise the metallographer may misinterpret the result shown in the microscope that
might result in either faulty parts being classified as being satisfactory, or good parts as
being scrap.
To illustrate the above here are a couple of examples: If a specimen is coated with a
thin layer of a soft material this coating can be smeared over the base material, indicat-
ing a thicker layer than actually exists. Thus the layer can be measured and accepted
even if the actual layer thickness is insufficient.
More often it will happen that correctly manufactured parts are rejected because
of incorrect specimen preparation. If hardened materials are cut using insufficient
cooling the reached temperature might anneal the material, resulting in a lower hard-
ness. Thus, a complete batch of correctly treated parts might be scrapped only because
of faulty specimen preparation.
The first case, accepting faulty parts as correct ones, might be the most critical, but
the other, scrapping good parts, can also be very costly.
Therefore it is essential that the prepared specimen shows what can be described
as the “True Structure.”
As shown previously, the entire preparation process can be divided into a series of
preparation steps, from cutting over mounting to grinding and polishing. All these
steps can introduce preparation artifacts if they are not carried out correctly.
In the following the individual preparation steps are listed and possible failures
that can occur during these steps are explained. Afterwards these preparation artifacts
and how to avoid or overcome them are discussed in detail.
13.5.1 Sectioning
There are several possible reasons for sectioning:
• To reduce the size of the work piece and turn it into a manageable sample.
• To be able to measure or examine layers, coatings, hardened zones, or welds.

• To be able to examine a part in different orientations or angles.
In all cases it is important to ensure that a representative part of the work piece is
taken out for further examination. Especially important when sectioning a part with a
surface treatment or some sort of layer is the correct angle of the cut. If the cut is not
carried out in an angle of 90° to the surface, the layer, coating, or hardened zone will be
enlarged, and the result is a kind of taper section, something used quite often on pur-
pose when mounting samples for easier measurement of layer thickness 共see Section
3.11.1兲.
Apart from that, the most important consideration to take when sectioning is to
avoid any mechanical or thermal influence that could alter the structure. As previously
described, wet abrasive cutting is the most appropriate way of sectioning when also
time and economy are considered.
Most of the other sectioning techniques introduce either heavy thermal damage
such as after torching as shown in Fig. 13.1, or mechanical damage as is the case after
hacksawing to be seen in Fig. 13.2. In case of bandsawing, however, an acceptable re-
sult often can be obtained when the correct machine, saw blade, speed, pressure, and
cutting fluid are used.
For this reason the following examples are concentrating on wet abrasive cutting
and bandsawing. However, also with these two methods, thermal or mechanical, dam-
age can occur if care is not taken.
Thermal Damage
Thermal damage is a result of excessive heat generated in the cut. Either because of
insufficient cooling due to an insufficient amount of cutting fluid in the actual cut or
because the feed speed is too high and thus too much heat is introduced 共see Section
2.3兲. Thermal damage can change the structure of the material to be examined which
especially is critical with heat treated parts where these structural changes can result in
wrong readings in the following microhardness tests. To avoid thermal damage make
sure that there always is plenty of cooling fluid in the cut and that the feed speed is set
correctly, i.e., not too high 共see Figs. 13.7 and 13.8兲.
In wet abrasive cutting, also the selection of cut-off wheels is important. Wheels
with a hard bond release abrasive grains slower. That makes them more economical
but also less suited for cutting of harder materials, as blunt abrasive particles will not
cut properly, but instead introduce heat and result in thermal damage 共see also Section
2.3.5兲. At bandsawing, the type of saw blade is important 共see Section 2.7.4兲.
Mechanical Damage
Wet Abrasive Cutting

Mechanical damage mostly occurs when cutting brittle materials or materials with
brittle or fragile coatings. In many cases damage first occurs when the cut-off wheel is
exiting the part to be sectioned. If the force or the selected feed speed is too high, the
sample fractures easily. If it is not possible to use a low pre-set constant feed-speed and
thus avoid the damage, it usually helps to support the sample with some similar mate-
rial or bond it onto another material using wax.
When cutting coated materials it is very important to cut through the layer or coat-
ing into the base material as this then acts as a support. Otherwise the layer might be
pushed away from the base material resulting in cracks or delamination. During the
final examination in the microscope it can be impossible to tell if this kind of fault is a
real fault from production or if it has been introduced during cutting. Cylindrical,
coated samples can, if possible, be rotated during cutting, thus securing support of the
coating over the entire circumference.
Bandsawing
Bandsawing, as a rule, always leaves more mechanical damage than wet abrasive cut-
ting. For most materials this damage, if all sawing parameters are correct, can be re-
moved through an effective plane grinding, but in case of a too low band velocity or a
too coarse pitch of the band, or both, an unacceptable mechanical damage can be de-
veloped. Also, feed speed that is too high or a cutting fluid that is not enough or is wrong
may give a very rough surface with deep mechanical damage.
13.5.2 Mounting
There are several reasons for mounting samples. The most common reason is simply to
get specimens with uniform size and shape to facilitate future preparation. In this case,
requirements to the mounting techniques are limited. However, a few matters should
be considered.
If the sample to be mounted is sensitive to heat, cold mounting should be preferred
to hot mounting, because the temperature during hot mounting can get as high as
180– 200° C 共350– 400° F兲. Cold mounting is not really “cold” but temperatures seldom
exceed 100° C 共210° F兲 for a normal-sized mount of 30 mm 共1.25 in兲 diameter.
If the temperature is really critical then only slow curing epoxy resins can be used.
To keep temperatures as low as possible epoxy resins can sometimes even be cured in a
refrigerator. That takes a longer time but the temperature of the mount does not exceed
room temperature.
Some materials and fragile samples are sensitive to pressure. In this case, hot
mounting cannot be used and cold mounting must be utilized instead.
Impregnation
Porous materials are usually impregnated under vacuum and here epoxy resins are
used; most of the other resins will start boiling when exposed to a pressure below the
atmospheric pressure. Vacuum impregnation has several advantages:
• Vacuum impregnation acts as a reinforcement of the sample because the resin
works as a bonding agent in the pores. This facilitates the following specimen
preparation as pull-out of material is eliminated or at least reduced. Pull-out of par-
ticles during the final polishing steps is very often the cause of deep scratches re-
sulting in lengthy reruns of the preparation method.
• Colored dyes can be added to the epoxy resin to help distinguish between porosity
and pull-out. Very often fluorescent dyes are used as these show up more brightly
than normal colors. This dye is added to the epoxy resin before impregnation. Dur-
ing impregnation all pores connected to the surface are filled with the dyed epoxy
resin and after the preparation is finished all the filled pores can be identified easily.
Areas that are not filled can then be either unfilled pores or pull-outs. The trained
metallographer can often determine pull-outs from pores by looking at the circum-
ference of the “hole.” Pull-outs leave a more jagged edge than real pores 共see also
Section 3.10兲.
Fig. 13.3—Deformation after grinding on SiC grinding stone, grit 150.
Shrinkage
A general rule when cold mounting is that the faster a resin cures or the higher the
caring temperature gets, the higher the shrinkage. Shrinkage of the resin can result in a
variety of preparation artifacts 共see also Section 3.1兲.
Staining
Water, cleaning agents, alcohol, and etchants are trapped in the gap between specimen
and resin Cleaning is almost impossible and the different liquids will continue seeping
out of the gap and staining the specimen. This can produce problems both when exam-
ining the specimen, but also when etching the specimen, as some other liquid might
cover part of the surface, which then will not be attacked correctly 共see Fig. 3.1兲. When
hydrofluoric acid is used for etching, this can even ruin the objective of the microscope
because the acid seeping out of the gap during examination of the specimen might etch
the glass.
Fig. 13.4—Deformation after grinding on ZrO2 / Al2O3 paper, grit 120.

Fig. 13.5—Deformation after grinding on SiC paper, grit P1000.
Scratching
If the gap is large enough, coarse abrasive grains from an earlier preparation step can
be transferred to one of the final steps, ruining the preparation result and contaminat-
ing the polishing cloth.
Edge Rounding
Gaps can also result in edge rounding of the sample, as the resin cannot support the
edge of the sample. However, when using modern preparation methods, this risk is
quite limited since the consumables used today provide very good edge retention.
Delamination
When resins with relatively high shrinkage are used for mounting of samples with po-
rous coatings, the coating can be pulled away from the substrate during the polymer-
ization of the resin This is quite rare and not explained in the section: How to Overcome
Preparation Artifacts.
Fig. 13.6—Deformation after grinding on rigid composite disk 共RCD兲 using 6 ␮m diamonds.

As cutting or mounting, or both, not always are necessary operations the “real” speci-
men preparation process usually is defined as grinding and polishing.
Preparation time should be kept as short as possible. In production control, time is
important and the faster the specimens are finished the earlier production can con-
tinue. The second important point is that shorter preparation times usually also reduce
costs for consumables and labor.
The first preparation step is grinding.
Grinding
There are two considerations when the grinding process is started.
• How is the surface finish from the previous cutting?
• Are the specimens prepared as single specimens or are they clamped in a specimen
holder?
If cutting has been carried out correctly the surface finish is in many cases suffi-
cient for immediate fine grinding. However, if the specimens are clamped together in a
holder, plane grinding has to be carried out first to level all specimens in the specimen
holder at the same height.
In this case the correct grit/grain size of abrasive has to be selected to have a re-
moval rate high enough to achieve short grinding times, but on the other hand, not too
coarse to avoid unnecessary deformation which then must be removed in the following
steps. Figures 13.3 and 13.4 show the deformation after plane grinding with a grinding
stone, 150 grit and a ZrO2 / Al2O3 grinding paper, grit 120, respectively, and the heavy
deformation is evident. Figures 13.5 and 13.6 show the much smaller deformation at
SiC grinding paper grit P1000 and a rigid composite disk 共RCD兲 using 6 ␮m diamonds.
Especially with soft materials, very coarse grit sizes should be avoided. The defor-
mation introduced can be very deep and might take a very long time to be removed in
the following steps. It can even happen that fractured abrasive grains become embed-
ded into the soft material during the preparation and may disturb future preparation.
Like with cutting, sufficient cooling is required to avoid thermal damage of the
specimens. Water is in most cases sufficient but for water-sensitive materials other flu-
ids like water-free oil can be used to avoid attack of the sensitive phases. Recirculation
cooling systems are advantageous in these cases because the fluid is reused continu-
ously. However, in many cases even water-sensitive materials can be ground using wa-
ter as a lubricant during the first step since plenty of material still is removed after-
wards and material is removed beyond the damaged area.
Polishing
After grinding to a sufficiently fine finish the preparation is continued with polishing.
During polishing the last deformation is removed and a reflective surface is produced.
A reflective surface is necessary for examination in an optical microscope. Addition-
ally, the surface should be plane without height differences between different phases or
rounded edges. Otherwise a correct evaluation of the specimen might be difficult or
even impossible. Especially when working with very thin coatings, edge rounding can-
not be tolerated.
There are several ways to avoid edge rounding and unplaneness. Using the correct
mounting technique was already mentioned, but also the choice of polishing cloths is
very important for the result. Soft cloths usually give a better reflectivity but can easily
generate unplane samples and rounded edges.
During polishing, a lubricant must be used to avoid any thermal damage. Espe-
cially during the final stages of the preparation, water-free products must be used if the
material to be prepared is water sensitive. Otherwise certain phases might be attacked
or even dissolved and a correct assessment is no longer possible.
13.5.4 Electrolytic Polishing

As described in Section 8.3, electrolytic polishing is well suited for the preparation of
homogeneous materials whereas it is difficult, in most cases impossible, to get accept-
able results with heterogeneous materials. The most common artifacts are relief, miss-
ing inclusions 共see Fig. 8.6兲 and edge rounding 共see Fig. 8.8兲.
In any case, like with mechanical preparation, it is important that the consum-
ables used are in perfect condition. Take care that the correct electrolyte for the given
material is available 共see Section 13.3兲. The electrolyte must not be too old since impu-
rities in the electrolyte may cause phenomena that might lead to a wrong interpreta-
tion of the prepared specimen. Used electrolytes may be heavily loaded with metal ions
from the specimens. These ions can act as catalysts and reduce the lifetime of the elec-
trolyte which in turn will have a negative influence on the following preparation.
Therefore the electrolytes must be discarded in due time.
13.5.5 General Rules—“The Metallographer’s Rule of Thumb”

Before the actual preparation process is started it is important to define the purpose of
the specimen preparation: “Why am I going to prepare this specimen; what do I want to
evaluate?”
If you are working with the inspection of incoming materials and have to check a
certain type of steel for a certain heat treatment, e.g., normalized, a short preparation
of an unmounted sample will in most cases be sufficient. A slight rounding of the edge
or a few scratches will not influence the examination. In this case it is important to get a
result in a very short time and in many cases also at low cost. Therefore a short prepara-
tion method with few steps is selected.
However, specimens with very specific characteristics, such as a very thin coating
that has to be measured accurately, must be treated in a completely different way. Al-
ready during cutting great care has to be taken to avoid damage of the coating. The
sample should be mounted in a resin with low shrinkage to prevent any edge rounding
and also the preparation method has to be selected carefully with regards to planeness
and edge retention. The entire preparation process will take longer, as in the previous
example, and the cost will be higher, but it is the only way to ensure that the correct
result is obtained.
When the purpose is established, use the “Metallographer’s Rule of Thumb,” when
a new preparation procedure shall be developed:
Put Up a Goal for Each Preparation Step

When following this rule, the result of every step is checked in the microscope. This is
to avoid that one of the early steps are not correctly made, a fact that often is not real-
ized before the final polishing step, causing a repetition of the whole process.
The above also means that you request as much information as possible if you are
asked to prepare a new material or a different kind of sample. Without having sufficient
information about the type of material, mechanical, chemical, or thermal treatment,
service history and request to the final examination, it is very difficult to choose the
correct preparation method and to put up acceptable goals for the preparation process.
13.6 Trouble Shooting—How to Overcome Preparation Artifacts

In the following sections the most important preparation artifacts are described in
some detail and solutions on how to avoid or overcome them are presented.
• Whenever a new method is established for a specific material, the specimens
should be checked under the microscope after every step to ensure that the
scratches, deformation, and other possible damage from the previous step have
been removed before continuing with the next step.
• The preparation times should be kept as short as possible without sacrificing the
quality of the preparation. This usually results in specimens with better planeness
and edge retention and saves time and consumables.
• When utilizing “fresh” consumables like RCDs or polishing cloths where abrasive
has to be added, they have to be used for a while before they reach maximum per-
formance. Allow for a slightly longer preparation time in the beginning.
The first part of the preparation process, sectioning, does by and large not cause
very high requirements to the equipment used. But generally it can be said that at wet
abrasive cutting the more automatic cut-off machines can produce better or at least
more repeatable results than manual equipment.
Mounting depends much more on the correct choice of consumables than on the
equipment used, especially with cold mounting where no equipment except maybe a
vacuum chamber for the impregnation is employed.
With the grinding and polishing procedures it is a completely different situation.
To be able to achieve the best possible preparation results and to use the guidelines
stated in the following sections, the specimen preparation has to be carried out on ei-
ther semiautomatic or automatic equipment. Otherwise it is not possible to control
force, time, dosing levels, polishing dynamics and other preparation parameters and
consistent results can only be accomplished with great difficulty.
13.6.1 Preparation Artifacts—Flow Charts

The following artifacts are described both in words and pictures, and a flow chart is
used to show ways to improve the quality of the prepared specimen and avoid the
artifacts.
Sectioning
Thermal damage
Mechanical damage
Cracks
Delamination
Mounting
Staining
Scratching
Edge rounding
Grinding and Polishing

Scratching
Lapping tracks
Deformation
Smearing
Pull-outs—False porosity
Embedded abrasive
Destroyed inclusions—Pull-outs
Edge rounding and relief
Comet tails
Flow Chart Symbols

The symbols used in the flow chart indicate the following:
13.6.2 Sectioning—General Problems—Flow Charts
Wet Abrasive Cutting
General Problems
As an introduction to the flow charts for the specific artifacts connected to wet abrasive
cutting, a number of general problems with suggested solutions are indicated in the
table below.
Problem Cause Solution

Wheel does not cut Incorrect wheel, the Use a softer wheel,
or stops cutting abrasive has or in case of
after some time become blunt, or the very hard material
rim of the wheel use diamond or
has been clogged CBN as abrasive
Arc of contact too large Increase the force,
if possible
Use oscillating cutting
Wheel wears very fast Wheel is too soft Use a harder wheel
Wheel wobbles or Wheel is not straight Change wheel
vibrates
Wheel is not clamped Clamp the wheel
correctly correctly
Wheel is too hard Use a softer wheel
or reduce the
speed of the wheel
Bearings of machine are defect Have machine repaired
Wheel breaks Feed speed too high Reduce the feed speed

Work piece has moved Clamp the work piece
correctly
Wheel bends while cutting Did the wheel attack a
tilting surface? Take care
that a notch is made
before the cutting starts
Check fixation of work
piece
“Disk brake effect,” Internal stress in work
the wheel is piece, lower feed speed
pinched in cut or preferable use
oscillating/step cutting,
clamp sample downwards on both sides
Wheel does not Wheel bond varies Change wheel
cut straight
Work piece not clamped Realign and clamp work
correctly piece
Attack of wheel not Change position of work
perpendicular piece or
take care that the wheel
makes a notch before the
cutting starts
Feed speed too high Reduce feed speed
Signs of overheating Wheel is too hard or Use a softer wheel or
of specimen surface too thick a thinner wheel
Feed speed too low Increase feed speed
Wheel is clogged Used a softer wheel
Feed speed too high Reduce feed speed
Arc of contact too large Change position of
work piece or
use a softer wheel
Cooling not efficient Check the cooling system, the
level of the cooling liquid and the
positioning of the nozzles
Foam and smell from the Additive to cooling Check that the cooling liquid has
cooling liquid, or both liquid is not active, the correct additive content or
bacteria might have clean system using bacterial killer, or both.
developed
Wet Abrasive Cutting—Flow Charts
Thermal Damage
There can be different reasons for thermal damage of the sample during cutting.
Mostly thermal damage is directly visible as discoloration on the cut surface, as shown
in Fig. 13.7. A cross section through the discolored area shows how deep the thermal
damage extends, see Fig. 13.8. A correctly cut sample does not display any discolora-
tion and is free from any thermal damage, as shown in Fig. 13.9. The most common
reason is the lack of cooling fluid during cutting. A relatively large amount of cooling
fluid is needed to remove the heat generated during cutting. Therefore the
Fig. 13.7—Thermal damage after cutting with insufficient cooling.
recirculation-cooling unit has to be monitored and the level of cooling liquid checked
regularly and refilled if necessary.
Another reason might be the wrong selection of the cut-off wheel. As described in
Section 2.6.1, different cut-off wheels are available for different materials. If a wheel is
used which is too “hard” for the material to be cut, “free cutting” cannot be obtained,
the specific pressure in the cut rises and overheating will take place. To avoid overheat-
Fig. 13.8—Cross section of part shown in Fig. 13.7, deep thermal damage can be seen.
Fig. 13.9—No thermal damage after cutting.
ing a softer wheel must be used. A softer wheel will break down faster, releasing more
abrasive grains and consequently cut more efficiently through hard materials.
The same behavior can be achieved by reducing the speed of the cut-off wheel. If it
is possible to adjust the spindle speed on the cut-off machine the “hardness” of the
wheel can be modified. Lower speed makes the wheel act softer and higher speed pro-
duces harder wheels 共see Section 2.3.8兲. Instead of changing wheels when different ma-
terials have to be cut, an adjustment of the wheel speed can simply compensate for the
variation in hardness of the different materials.
The third reason for thermal damage is very often a too high feed speed. Material
from the sample cannot be removed as fast as the wheel is moved into the cut. “Free
cutting” is not achieved and overheating is taking place 共see Sections 2.3.5 and 2.3.8兲.
Often the reason for using high feed speed is to save time. This is usually not a good
idea, since the time saved during cutting has to be used again in the grinding process to
remove the thermal damage. In many cases more time has to be spent than was saved
in the first place. Therefore it cannot be recommended to go too fast during cutting; it
usually prolongs the total preparation time instead of reducing it.
Thermal damage during cutting can usually be avoided if these three guidelines
are followed:
• Check and maintain the correct cooling fluid in the recirculation-cooling unit. Di-
rect the cooling fluid into the cut.
• Select the correct cut-off wheel for the material to be cut. If a variable wheel speed
is available it can be used instead of changing the cut-off wheel.
• Adjust the feed speed depending on sample material and size.
Abrasive Wet Cutting, Thermal Damage
Fig. 13.10—Plasma sprayed coating with crack.
Mechanical Damage
When cutting correctly, the total amount of applied energy can be transformed into
removal of material. If the feed speed is too high more energy is applied than can be
transformed. The excess energy has to be consumed somehow, and where it often is
transformed into heat resulting in thermal damage with metallic materials, it can re-
sult in the initiation of cracks in brittle materials as shown in Figs. 13.10 and 13.11.
Fig. 13.11—Prior to grinding and polishing, the sample was vacuum impregnated using an
epoxy resin with a fluorescent dye 共showing up green when examined using fluorescent light兲.
As the crack is completely filled with resin it was there before the grinding and polishing were
started. Whether it was there before cutting or created during cutting cannot be said.
With solid materials we very often get cracks extending from the surface into the mate-
rial whereas we often see delamination, the separation of layers, with coated materials.
Therefore special care has to be taken with ceramics and other brittle materials and
with coated materials. In Fig. 13.12 a delamination is seen; the coating is not in contact
with the base material.
In many cases thermal damage is restricted to the area around the cut, whereas
cracks propagate deep into the material.
Often materials are examined to see whether cracks or delamination have been
introduced during the manufacturing process. This means that cracks or delamination
that have been introduced during cutting might cause the entire series to be scrapped
or at least lead to a lot of extra work, because the production process will be suspected
to be faulty. This can be avoided by impregnation of the specimen before cutting using
an epoxy with a fluorescent dye. In Fig. 13.11 a specimen is shown that has been
vacuum impregnated before grinding and polishing so when examined in the micro-
Fig. 13.12—Delamination between coating and base material.

scope it can be seen whether a crack existed before the preparation. The same type of
impregnation can be done before cutting.
To reduce the risk of introducing cracks during cutting a few simple rules should
be followed.
• Always use moderate feed speed.
• Use the correct cut-off wheel for the material to be cut. In the case of coatings the
cut-off wheel should be selected to suit the majority of the material, e.g., a thin ce-
ramic coating on a steel bar should be cut using an abrasive Al2O3 wheel suitable
for the steel bar instead of using a diamond cut-off wheel that would suit the ce-
ramic coating only.
• Thin cut-off wheels should be preferred to thicker wheels because they remove less
material and thus introduce less energy.
• With very brittle and fragile materials, vacuum impregnation prior to the cut can
reinforce the samples and prevent cracking.
• With coatings: always cut through the coating into the base material. Thus the
coating is supported all the time and the risk of cracking is reduced.
Abrasive Wet Cutting, Mechanical Damage
Bandsawing
General Problems
When working with a vertical bandsaw a number of problems can be experienced, and
below the most important of these are listed with suggested solutions 共see also Section
2.7.4兲.
Problem Solution
Premature dulling of teeth Decrease band velocity.
Use band with finer pitch.
Apply proper cutting fluid when cutting ferrous
and nonferrous materials.
Keep teeth engaged. Do not allow the teeth to
idle through cut.
Increase feeding pressure.
Apply cutting fluid at point of cut, saturating the
teeth evenly when cutting ferrous and
nonferrous alloys.
Be sure that band is running with teeth pointing
down.
Band vibrating in the cut Increase or decrease band velocity.
Increase band tension.
Use band with finer pitch.
Hold work piece firmly.
Band teeth ripping out Use fine-pitch bands on thin work piece
sections.
Eliminate vibration by holding work piece
firmly while it is fed into the band.
Use cutting fluid on ductile materials.
If gullets are loading, use heavier duty cutting
fluid.
Reduce feed pressure.
Surface of finished cut too Increase band velocity.
rough Use band with finer pitch.
Use slower feeding rate.
Apply correct amount of proper cutting fluid.
Premature band breakage Change to band with gage that is not too heavy
for diameter of wheels and speed of the
machine.
Decrease band velocity.
Check periphery of wheels for defects.
Cracking at weld. Try longer annealing period,
decrease unit load by using finer pitch.
Decrease feeding pressure.
Decrease band tension.
Properly adjust band tool guides.
Apply cutting fluid.
Band making belly-shaped cut Increase band tension.
Adjust guides close to work piece.
Use band with coarser pitch.
Decrease feeding pressure.
Gullets loading Use band with coarser pitch.

Lower band velocity.
Band not running true against If clicking against saw guide backup bearing,
saw guide backup bearing remove burr on back of band where joined.
If hunting back and forth against saw guide
backup bearing, re-weld with back of band in
true alignment.
Check alignment of band carrier wheels.
Check saw guide backup bearing, if worn or
unbalanced, replace same.
Negative camber developing in Band riding too heavy on saw guide backup
band bearing. Adjust band for alignment on top and
bottom wheels.
Cutting rate too slow Increase band velocity.
Use band with coarser pitch.
Band leading in cut Unbalanced set or partial dullness caused by
striking hard inclusion in material being cut.
Saw guides out of adjustment. Carefully readjust
guide inserts or rollers. If worn, replace same.
In the case of brush-equipped cut-off machines,
make sure brushes are properly adjusted, if
worn, replace with new.
Reduce feeding pressure.
Premature loss of set Band too wide for radii being cut.
Decrease band velocity.
Positive camber developing in Reduce feeding pressure.
band Use band with coarser pitch to permit greater
tooth penetration.
Saw guides too far apart, adjust closer to work
piece.
Band developing twist Band binding in cut, decrease feeding pressure.
Side inserts or rollers of saw guides adjusted too
close to band.
Wrong width of band for radii.
Decrease band tension.
13.6.3 Mounting—General Problems—Artifacts

General Problems—Hot Mounting
In the following overview some of the general problems that can arise during hot
mounting are shown and both cause and the possible solution are described 共see also
Section 3.6兲.
General Problems—Cold Mounting

In the subsequent overview some of the problems that can arise during cold mounting
are shown and both cause and the possible solution are described 共see also Section
3.13兲.
Problem Cause/Solution
The surface of the mount is The components are not mixed in the correct
sticky after normal curing time. quantities, the mixing has not been correct or
the room temperature has been too low.
Mix carefully with the exact portions of each
component and check that the room
temperature is approx. 20–22° C 共68– 72° F兲.
Also cover the mounting cup so as to prevent
any reaction between the surface of the mount
and the air.
The mount is brown after The temperature during curing has been too
curing, too rapid curing. high.
Mix carefully with the exact portions of each
component and check that the room
temperature is approx. 20–22° C 共68– 72° F兲.
When using large amounts of resin make sure
that the mount is cooled during curing. Use
either a stream of cool air, a water bath or a
refrigerator.
It is very difficult to remove the The mounting resin 共epoxy兲 has very little
mount from the mounting mold. shrinkage and good adhesion to all materials.
Use a more flexible mounting mold or coat the
inner surface with a thin layer of silicone mold
release agent.
The mount is soft after curing, The components are not mixed in the correct
not cured completely. quantities or one of the components is too old.
Check the expiry date of the components and
make sure to measure the correct quantities of
each component. The mount can maybe be
saved by placing it in an oven at 40–50° C
共100– 120° F兲.
Specimen moves, turns, falls or The specimen is very light.
floats in the mounting mold. Coat the bottom of the mounting mold with
spray lacquer and position the specimen before
the lacquer is dry or use double adhesive tape
to secure the specimen.
Staining
Staining is the discoloration of the specimen surface through residues of liquids used
during preparation, cleaning, or etching of the specimen.
Sometimes staining is used to purposely contrast the specimen surface in order to
identify different phases, but here we are only talking about unintended discoloration.
Staining usually occurs when the sample is not mounted correctly and there is a
gap between the sample and the mounting material. This gap is often filled with lubri-
cant that is accumulated there during polishing or with cleaning liquid or etchant that
has been used during the preparation process. Very often the gap is rather narrow, but
the capillary action fills the gap easily with liquid. Figure 3.1 共Section 3.1.2兲 shows a
specimen surface with staining caused by a gap, and in Fig. 3.2共b兲 a correct mount is
seen without gap and consequently without staining.
To avoid staining the subsequent rules can be followed:
• Always clean and degrease the samples prior to mounting; this will provide a better
adhesion of the resin to the sample.
• Select a resin with very low shrinkage; these usually are hot mounting resins con-
taining a filler material or epoxy resins for cold mounting. The epoxy resins provide
the best result, especially with vacuum impregnation; however, the long curing
time often prohibits their use.
• Clean the specimen carefully after each step, possibly using ultrasonic cleaning.
• Dry the specimen very thoroughly to avoid bleeding out of liquids during examina-
tion with the microscope.
• Use a piece of soft tissue together with a hair dryer to make sure that all liquid is
removed from the gap. 共Be careful with soft materials that the tissue does not
scratch the material.兲
• After etching the specimen make sure that all etchant is removed from the speci-
men or the gap in the specimen, otherwise the specimen might start “bleeding” on
the microscope. This can destroy the specimen, or, if hydrofluoric acid was used,
even the objective of the microscope.
Scratching
Scratching is usually not related to mounting; however, under certain circumstances a
poor quality of the mount might result in scratching of the specimen surface.
As with the previous example, incorrect mounting can result in a gap between the
sample and the mounting material. During preparation some of the abrasive particles
can be trapped in the gap and carried on to the following preparation stage, as shown in
Fig. 13.13. If the particles are falling out of the gap and stay on the polishing cloth they
will result in few but distinct scratches.
To avoid scratching because of poor mounting quality, follow these rules:
Fig. 13.13—Abrasive grains in the gap between sample and mounting resin When these fall
out during preparation they will result in scratching.
• Always clean and degrease the samples prior to mounting; this will provide a better
adhesion of the resin to the sample.
• Select a resin with very low shrinkage; these usually are hot mounting resins con-
taining a filler material or epoxy resins for cold mounting. The epoxy resins provide
the best result, especially with vacuum impregnation; however, the long curing
time often prohibits their use.
• Clean the specimen carefully after each step, possibly using ultrasonic cleaning.
If abrasive particles are carried from one preparation step to a following step, it
will not only damage the specimen and require at least part of the preparation method
to be repeated, it will also require the contaminated polishing cloth to be exchanged.
The result is both longer preparation time and increased cost 共see also Section 13.6.4兲.
Edge Rounding
Mounting is often carried out to protect the edges of the sample, especially when the
sample is coated with very thin layers of another material. To be able to measure the
thickness of these layers accurately it is crucial that they are absolutely plane without
any rounding. The same is valid when microhardness testing has to be carried out very
close to the edge; also here perfect planeness of the sample is required.
Today’s selection of consumables for grinding and polishing has made the prepa-
ration easier and faster as previously stated. Still, when the maximum edge retention is
required it is usually not possible to avoid mounting the samples. The correct mount-
ing resin has to be selected carefully to avoid a gap between sample and mounting ma-
terial, and usually there are not so many choices. The best option when mounting
samples with porous or fragile coatings is epoxy resin because this can be used under
vacuum and will provide both a reinforcement of the coating and a mount without any
gap. For mounting of samples with very hard coatings or the mounting of surface hard-
ened materials it can be advantageous to use hot mounting. In this case resins with
different filler materials are available. This makes it possible to select a mounting resin
that has similar wear characteristics as the material to be prepared. Thus a uniform
removal of material across the entire specimen surface is obtained and perfect plane-
ness and edge retention will be the result 共see Section 3.1.3.兲 Figure 3.2共a兲 shows a
mount with a mounting material not in contact with the sample, causing edge round-
ing. In Fig. 3.2共b兲 the correct mounting material adhering to the sample is used.
13.6.4 Grinding and Mechanical Polishing—Flow Charts
Scratching
The mechanical removal of material from the surface is carried out step-by-step using
continuously finer grain sizes of abrasive. The abrasive particles act as machining
tools, removing small chips of material. As a result, the surface is covered with unidi-
rectional grinding scratches getting smaller after every step of the preparation, disap-
pearing totally at the end, or at least being so small that they are no longer visible in an
optical microscope. The unidirectional pattern is achieved when the specimen is pre-
pared using some kind of automatic or semiautomatic preparation equipment as de-
scribed in Section 7.9. To avoid scratches on the finished sample, the specimen has to
be examined after every preparation step to ensure that all scratches from the previous
step have been removed completely before continuing to the following step. Otherwise
steps from one of the early grinding steps might still be visible after final polishing. It is
crucial that the specimen is checked carefully after every step because the removal rate
Fig. 13.14—Scratched and deformed surface after plane grinding.
of smaller abrasives is much less than that of larger abrasives causing the polishing
times needed to be extremely long if a final polishing step should remove scratches
from an initial grinding step. Figure 13.14 shows the very rough scratch pattern with
heavy deformations after plane grinding, in contrast to the pattern developed during
the fine grinding shown in Fig. 13.15.
It is also very important to clean the specimens carefully after every step as con-
tamination of a polishing cloth quite easily can occur. 共Scratching because of mounting
gaps has been described in Section 13.6.3.兲
Fig. 13.15—Uniform scratching after fine grinding.

Scratching
Lapping Tracks
During mechanical preparation the abrasive particles should act as small cutting tools,
machining chips from the surface of the specimen. This requires the abrasive grain to
be held firmly on the polishing cloth while the specimen is passing over it as the abra-
sive grain otherwise will start rolling.
Since we use loose abrasives that are added during preparation, this presents a
challenge to the polishing cloth used. The polishing cloth must be selected carefully
depending on the grain size of abrasive it is going to be used with and especially in
relation to the hardness of the material to be prepared. If the polishing cloth is too soft
the abrasive will disappear into the fabric and will not remove any material. If the pol-
Fig. 13.16—Specimen with lapping tracks, BF.
ishing cloth is too hard the abrasive cannot be pressed deep enough into the cloth and
the abrasive may start rolling, resulting in lapping tracks. If the cloth is even harder, or
a rigid fine grinding disk with too high of a hardness is used, the abrasive might even be
pressed into the sample material and become firmly embedded 共see the section below
on embedded abrasives兲.
Lapping on softer materials does not remove any material, it only introduces deep
deformation. The lapping tracks are easy to identify, they follow a straight line, like a
grinding scratch; however, it is interrupted as the abrasive grain is tumbling across the
surface, as shown in Figs. 13.16 and 13.17 in bright field 共BF兲 and differential interfer-
ence contrast 共DIC兲, respectively.
For information on polishing cloths see Section 7.4.
Fig. 13.17—Specimen with lapping tracks, DIC.

Lapping Tracks
Deformation
The entire mechanical preparation process is based on the removal of material through
grinding and polishing as described earlier. Any mechanical treatment will result in a
certain amount of plastic deformation of the surface of the specimen. It is the purpose
of metallographic/materialographic specimen preparation to remove the deformation
from the surface to allow for the examination of the true structure. Therefore,
metallographic/materialographic specimen preparation is carried out in steps to
gradually remove the deformation from the previous steps; see Fig. 13.18 that shows
the preparation process schematically from the surface left after cutting through plane
grinding, fine grinding, and polishing to a surface to be examined on the microscope
共see also Section 7.7兲. However, very often some residual deformation is left after the
preparation is finished and that can lead to wrong conclusions; see Fig. 13.19 that
shows the remaining deformation from an earlier grinding step. Therefore, it is
Fig. 13.18—The preparation process. Deformation is removed step-by-step.
Fig. 13.19—Remaining deformation from preparation, following early grinding scratches.

Fig. 13.20—Color etched specimen, remaining deformation can clearly be seen.
important to follow certain preparation routines and to check the specimens fre-
quently during preparation.
Generally each step has to remove the material deformed during the previous step,
while at the same time only introducing a limited amount of new deformation. With
today’s modern consumables the preparation of most materials can be reduced to
about four steps resulting in a deformation free sample surface. If these steps are not
carried out correctly deformation may be visible after preparation. Very often the de-
formation is first visible after etching. Especially color etching will reveal even the
smallest amount of remaining deformation as shown in Fig. 13.20.
Fig. 13.21—Smearing on a soft type of steel.

Deformation
Smearing
Smearing is not as common as many of the other artifacts; however, it is important to
be aware of the possibility and the influence smearing can have on the final result.
Smearing usually happens with very soft materials, as shown in Fig. 13.21, and often
when soft materials are contained in layers. Instead of being cut cleanly the material is
pushed across the surface. Especially when the thickness of layers has to be measured,
e.g., copper and solder layers on a PCB, the correct thickness must be obtained, other-
wise the part might be not acceptable. As can be seen in Fig. 13.22 the soft solder mate-
rial has been deformed and dragged across the copper layer following a coarse grind-
ing scratch. The exact measurement of the different layers in this case is not possible.
Therefore, smearing is not acceptable and has to be avoided. Also, smeared material
may hide the pores in the surface 共see Pull-Outs—False Porosity, below兲.
Mostly the occurrence of smearing is due to one of the following reasons:
• Wrong type of abrasive used. Abrasives that are too blunt cannot cut properly and
may result in smearing. Therefore diamond is the best choice of abrasive for the
first, relatively coarse polishing steps. Diamond is the hardest known abrasive and
consequently will produce a clean cut over a long period of time. Polycrystalline
diamonds are superior for specimen preparation.
Fig. 13.22—Smearing on a PCB. The solder material is smeared over the copper layer, following
a grinding scratch.
• Insufficient lubricant level during polishing. When the amount of lubricant added
to the polishing cloth is too low, the lubricant film between specimen and cloth can
be imperfect and thus smearing can occur. The lubricant level should be main-
tained on a stable level throughout the entire preparation step in a way that the
polishing cloth is moist but not wet.
• Polishing cloths that are too soft. With soft polishing cloths the abrasive can be
pressed too deep into the textile and thus not create any cutting action. Change to a
harder polishing cloth or increase the abrasive grain size 共see below兲.
• Abrasive grain size that is too small. This is similar to the above reason; small abra-
sive grains can also be pressed so deep into the fabric of the cloth that their cutting
action is nonexistent. Either increase the size of the abrasive used or change to a
harder polishing cloth to avoid the condition that the abrasive is pressed too deep
into the fabric.
Smearing
Pull-Outs—False Porosity
As stated earlier, the goal of metallographic/materialographic preparation is to show
the true structure. For most solid materials that is a relatively easy task, but porous
materials quite often produce a challenge, even to experienced metallographers. De-
pending on the type of material, the preparation process can produce either a too high
porosity level or a too low level.
Porous, brittle materials usually display a higher porosity level than what is actu-
ally in the material due to fracturing of the material during cutting and plane grinding.
This fracturing creates pull-outs, cavities in the surface, and cracks 共see Section 6.3.2,
see also pull-outs in connection with inclusions in the following section兲.
Ductile materials often display a too low porosity since the softer metallic material
can be smeared into the pores during plane grinding, covering these up.
The following examples are taken from the same type of application, thermal
spray coatings, using two different types of materials where the above can be seen very
clearly. To reach the correct result, displaying the accurate porosity level with the same
routine can be used with both types of material. When preparing such a specimen for
the first time it is important to monitor the porosity level throughout the entire prepa-
ration and first continue to the following preparation step when the porosity level stays
constant. With brittle materials it will get smaller and smaller until it reaches the cor-
rect level as shown in Figs. 13.23–13.26. At ductile materials the porosity level will in-
crease with finer and finer preparation steps until the final, correct level is reached, as
shown in Figs. 13.27–13.32.
In both sections on false porosity the use of an RCD is recommended. Experience
shows that the constant supply of abrasive during preparation on an RCD gives the
most constant removal of material and thus is best suited for fine grinding of both soft
and hard porous materials when the correct porosity level has to be obtained. If the use
of an RCD is not possible the correct type of abrasive for the material in question
should be selected.
On hard, brittle materials diamond grinding disks or diamond pads in successively
finer grain sizes should be used to remove the damage from plane grinding.
For soft materials fine grained SiC paper can be selected; however, it is important
to change the paper frequently to allow fresh, still sharp grains to remove material and
thus avoid smearing.
Fig. 13.23—Ceramic plasma sprayed coating after plane grinding, the porosity level is very high
due to many pull-outs.
Fig. 13.24—Same specimen as in Fig. 13.23 after fine grinding, pull-outs are reduced.
Fig. 13.25—Same specimen as in Fig. 13.23 after diamond polishing, pull-outs are further
reduced.
Fig. 13.26—Same specimen as in Fig. 13.23 after final polishing, correct porosity level.
Fig. 13.27—WC/Co plasma sprayed coating after plane grinding. The surface is completely
smeared and the pores are not visible.
Fig. 13.28—Same specimen as Fig. 13.27 after fine grinding. Most of the pores are still smeared
over.
Fig. 13.29—Same specimen as Fig. 13.27 after 6 ␮m polishing. Pores start to open up.
Fig. 13.30—Same specimen as Fig. 13.27 after 3 ␮m polishing. More pores are opening up.
Fig. 13.31—Same specimen as Fig. 13.27 after 1 ␮m polishing.
Fig. 13.32—Same specimen as Fig. 13.27 after final polishing on colloidal silica. Correct porosity
level.
Pull-Outs, False Porosity, Hard, Brittle Materials

False Porosity, Soft, Ductile Materials
Destroyed Inclusions
Many materials contain different types of nonmetallic inclusions. They are naturally
contained in the material or added to improve machinability. These inclusions have
different mechanical behavior than the base material; they can be harder or softer and
often they have other thermal expansion values resulting in relatively bad adhesion of
the inclusions to the base material.
During metallographic/materialographic preparation these inclusions can be
crushed if they are very brittle 共see Fig. 13.33兲, or removed by a long napped polishing
cloth if they are soft, but the result is the same, partly or completely missing inclusions
in the base material. Apart from misleading results in the following microscopic ex-
amination, these inclusion particles, pulled out during the preparation can also result
in other preparation artifacts such as scratching.
There is, however, another important group of inclusions, the water-sensitive in-
clusions. If not treated correctly, the result after preparation will be the same with these
inclusions as with those described above; they will simply be missing when examining
the specimen 共see Fig. 13.34兲. This takes place if the polishing consumables used, espe-
cially during the last steps of the preparation, contain water.
Fig. 13.33—Brittle inclusion, removed during polishing.
Fig. 13.34—Missing water-sensitive inclusions.

Destroyed Inclusions
Embedded Abrasives
Contrary to pull-outs, no material is removed from the specimen, but during prepara-
tion, abrasive grains are embedded into the specimen surface. Also, this is unwanted
because the foreign matter will make interpretation much more difficult or even im-
possible. Embedded abrasives are only seen with relatively soft materials, and mostly
because they are prepared on preparation disks that are quite hard; this can be rigid
composite disks 共RCDs兲 or hard polishing cloths, but even from SiC grinding paper
grains can be embedded in the specimen material.
This can pose a problem with certain composite materials. If they consist of both
hard and soft phases, RCDs and hard polishing cloths are recommended to keep the
specimens plane and avoid edge rounding. Therefore, a way has to be found to fulfill
both requirements at the same time, plane specimens without embedded abrasive
grains. Figure 13.35 shows embedded abrasive particles after 3 ␮m diamond polishing
in a PbSn solder, and Fig. 13.36 shows the same specimen in SEM.
To resolve the problem with embedded abrasive it is essential to know when the
abrasive particles became embedded. Therefore, the specimens have to be checked af-
ter every preparation step to be certain
Fig. 13.35—Embedded abrasive 共3 ␮m diamonds兲 in PbSn solder.
Fig. 13.36—Same specimen as Fig. 13.35, SEM image of diamonds in the solder phase.
Embedded Abrasive
Edge Rounding and Relief

The goal of specimen preparation is to produce specimens showing the true structure.
This usually requires perfect edge retention and absolutely plane specimens. With
composite materials containing phases of very different hardness or materials with
thin, sometimes multiple coatings, this can present a serious challenge to the metallog-
rapher. Figures 13.37 and 13.38 show a composite material with relief and without re-
lief, respectively. Figures 13.39 and 13.40 show a coated material with rounded edge
and with perfect edge retention, respectively.
Fig. 13.37—Composite material with relief between fibers and matrix.
Fig. 13.38—Same specimen as Fig. 13.37 after correct preparation, perfect planeness.
Fig. 13.39—Coated material with rounded edge.

Fig. 13.40—Same specimen as Fig. 13.39 after correct preparation, perfect edge retention.
Edge rounding has already been touched upon in connection with mounting in
Section 3.1.3; however, it is not always possible to mount the sample and in the follow-
ing some tips are provided to get good edge retention without mounting. Basically the
same rules are valid to avoid relief between the different phases in the specimen.
• Use rigid composite disks 共RCDs兲 for fine grinding and relatively hard cloths for
polishing to keep the specimen flat.
• Use diamond as the abrasive because it can cut equally through all phases.
• Use polishing times as short as possible.
• Use as few polishing steps as necessary, e.g., go directly from 6 to 1 ␮m polishing,
omit the 3 ␮m step.
• Use a lubricant with higher viscosity for the finer polishing steps.
Fig. 13.41—Specimen after unidirectional polishing with comet tails around the inclusions.
Edge Rounding and Relief
Comet Tails
Comet tails owe their name to their characteristic shape. They are found adjacent to
inclusions or pores and are the result of unidirectional polishing 共see Fig. 13.41兲. By
adjusting the polishing dynamics, comet tails can be avoided easily 共see Section 7.9.2兲.
As with the other artifacts we also assume here that the preparation process is car-
ried out on some kind of semiautomatic or automatic equipment. To achieve an accept-
able polishing result it is necessary that the specimen is moved across the entire surface
of the polishing disk and that the specimen holder at the same time is rotated around its
center. This is difficult to carry out manually, but most modern machines are designed
to utilize the entire preparation surface and to rotate the specimens at the same time.
One reason to move the specimen across the entire preparation surface is to wear
the polishing cloth symmetrically, thus increase the lifetime and as result reduce the
cost of specimen preparation. But more important is that the specimen is subjected to
a unidirectional influence from the polishing cloth. This is important as different
phases or constituents in the specimen react differently to metallographic/material-
ographic specimen preparation. If we are polishing a material with hard inclusions,
the inclusions will be polished slower than the rest of the material, and after a while the
inclusions will stick slightly out of the base material. As a result, less of the base mate-
rial will be removed in the “shadow” of the inclusion. When examined in the micro-
scope this characteristic feature will look like a comet tail. Apart from disturbing the
examination it will also make, for instance, correct automatic inclusion rating using
image analysis impossible, since the inclusions will seem larger than they actually are.
To avoid comet tails it is important that the speed of the polishing disk and the
speed of the specimen holder or specimen mover disk in which the specimens are lo-
cated are almost the same. They must not be identical because the specimens other-
wise would run in exactly the same track over and over again, but they should be simi-
lar. As a rule of thumb the speed of the specimen holder should not differ more than
±5 – 10 % from the speed of the preparation disk.
This is only relevant during polishing where the removal rate is limited and the
relative softness of the cloths contributes to uneven removal between softer and harder
phases. Grinding is carried out on hard supporting disks and the removal rate is much
higher. Here comet tails will not occur and therefore the speed of the grinding disk can
be much higher than the speed of the specimen holder to achieve a higher removal rate
and thus a shorter preparation time.
13.6.5 Electropolishing—General Problems—Artifacts

In the following overview some of the problems and artifacts that can be observed dur-
ing electrolytic preparation are indicated and both cause and the possible solution are
displayed.
General Problems and Artifacts

Surface not polished Current density insufficient Adjust the voltage
or only partly Electrolyte too old Renew electrolyte
polished Insufficient quantity Add electrolyte
of electrolyte Reduce the flow rate
Spots that have not Gas bubbles Adjust flow rate
been polished Check the electrolyte
temperature
Decrease the voltage
Etching of the Chemical attack of Remove the specimen
polished surface grain boundaries immediately when the
after switching off current is switched off
the current Choose a less corrosive
electrolyte
Phases in relief Polishing film is Increase the voltage
inadequate Improve the mechanical
preparation
of the specimen
Polishing time too long Reduce the polishing time
Pitting Polishing time too long Improve the mechanical
preparation
Decrease the time
Voltage too high Lower the voltage
Insufficient anodic layer Reduce flow rate
Use a different electrolyte
Attack at the edge Film too viscous or too thin Decrease the voltage
of the specimen Increase flow rate
The center of the Polishing film did not form Increase the voltage
specimen is in the center of the Reduce the flow rate
deeply attacked or not specimen Add more electrolyte
polished at all
Deposits on the Insoluble reaction products Renew electrolyte or try a
surface different one
Increase the voltage
Wavy surface or Polishing time too short Increase the time
residual Flow rate too high or too Change the flow rate
deformation low Improve the preparation
Rough surface after prior to electrolytic
grinding polishing
Electrolyte too old Renew electrolyte
Selective polishing because Other electrolyte with
of potential differences in other polishing data or use
surface mechanical
共heterogeneous material兲 preparation instead
Part III: Light Microscopy
14
Introduction
METALLOGRAPHY/MATERIALOGRAPHY COMPRISES THE OPTICAL EXAMI-
nation of a material for the purpose of giving a qualitative and quantitative description
of that material’s structure. The structure is characterized by size, shape, distribution,
density, orientation, and type of phases, as well as microstructural defects 共see Fig. 1.2兲.
In this context, the light microscope is an important tool. In the following chapter,
the basic physical principles of reflected light microscopy and the most important
methods of microscopic examination will be described in more detail. In Chapter 16 a
short introduction to electron-microscopy and scanning probe microscopy is given.
The optical effect of enlargement that occurs when one looks through the rounded
glass of a convex lens 共magnifying lens or loupe兲 was known to the ancient Egyptians,
Greeks, and Romans. Today, a convex lens still serves as a magnifying glass for observ-
ing small objects, the useful magnification is limited to 10– 15⫻.
The first microscope, consisting of two lenses, was probably built by either Hans
and Zacharias Jansen in about 1590 in the Netherlands or by Cornelius Drebbel around
1600. In connection with the growing significance of the natural sciences in the 19th
century, microscopic observations in the fields of medicine, biology, and geology be-
came ever more important.
H. C. Sorby in England 共1864兲 and A. Martens in Germany 共1878兲 were the first to
prepare metallographic polished sections of steel and cast iron, examine them by mi-
croscope, and sketch or photograph their visible structure.
Microscopes used today are still built according to the old principle of a system of
lenses placed together. Their essential elements are source of light, lens, eyepiece 共or
ocular兲, prism, mirror, and shutter and filtering systems.
14.1 Visible Light–Table 14.1–Table 14.2

Light that can be seen by the human eye is an electromagnetic light wave with wave-
lengths of between 350 and 780 nm. Depending on the wavelength, the human eye sees
different colors 共see Table 14.1兲.
White light consists of a mixture of all the colors in the spectrum. Light of an even
wavelength is monochromatic.
When wavelengths of a particular range are missing from a beam of polychro-
matic light, we see a mixed color 共Table 14.2兲.
TABLE 14.1—Range of Wavelength of Visible Light and Color.

Range of Wavelength, nm Color
360–440 violet
440–495 blue
495–580 green
580–640 yellow/orange
640–780 red
525
TABLE 14.2—Spectral Color Filtered Out and Visible Mixed Color.

Spectral Color Filtered Out Mixed Color
Violet Green-yellow
Ice blue Orange
Yellow Ultramarine blue
Red Blue-green
14.2 The Human Eye

The construction of the human eye is similar to that of a camera 共Fig. 14.1兲. Thanks to
the muscles in our eyes, the focal distance of their flexible lenses 共1兲 can be varied to
enable us to focus on any object at a distance between approximately 20 cm and infin-
ity. The inner diameter of the iris 共3兲 can be varied to change the amount of light falling
into it. This variation produces a sharp image on the retina 共2兲, the gray values of which
are received by receptor-rods, and the color values of which are received by the cones
and transformed into electrical impulses. These impulses are in turn transmitted via
the optical nerve 共4兲 to the brain where they are then processed.
For example, let us look at a 160 m 共⬃490 ft兲 high tower from a distance of about
300 m 共⬃915 ft兲. If we imagine two lines that extend from the middle of our eye, one to
the foot of the tower and one to the top, we get what is called the visual angle. In this
example, the visual angle ␦ is about 30 degrees. We are not able to recognize the faces of
people on the tower because the visual angle is too small for our eye to process. But if
we go closer to the tower, then we can better recognize the details of the building and
the people. This means that the closer we bring an object to our eye, however, thereby
increasing the visual angle, the more details we are able to discern.
Normally, we are able to read the text on a page of a book from a distance of 25 cm
共⬃10 in兲. This distance is called the conventional visual range, or visual range of refer-
ence. It enables us to compare the magnification data of different optical systems.
To make out the details of the individual letters on that page of text, we must de-
crease the visual angle. If we bring the text closer to our eyes, in order to increase the
Fig. 14.1—Light path of the human eye, with lens, cornea 共1兲, retina 共2兲, iris 共3兲, optical nerve
共4兲.1
visual angle further, the text begins to blur because the ability of our lenses to adjust to
the visual angle is limited.
14.3 Magnifying Lens and Microscope

Magnifying glasses and microscopes are optical devices that enable us to increase the
visual angle between the eye and objects that are small and near so that details that
cannot be seen with the unaided eye now become visible.
If we place a convex lens 共magnifying glass兲 between our eyes and the page of text,
the visual angle is increased and the details of individual letters as well as the surface
structure of the paper become visible.
A magnifying glass produces an enlargement by means of a single imaging step.
The object lies in the center of focus and the eye is accommodated ad infinitum. The
smaller the focal point of the magnifying lens, the greater the magnification. Practi-
cally speaking, a magnification of the object of 10 up to a maximum of 15 times its
actual size remains in the useful range.
By using several lenses arranged one after the other, the magnification effect can
be increased considerably.
The construction of the classical microscope consists of a two-lens system. The
magnification takes place in two image-forming steps. First, an enlarged image of the
object is projected by the objective in the intermediate image plane. This image is then
magnified by the ocular, or eyepiece.
14.4 Magnification
Magnification, M, as the function of an optical instrument is defined as:
Visual angle with optical instrument ␦1

M= 共1兲
Visual angle without optical instrument ␦2
or
M = tan ␦1/tan ␦2 共2兲
Magnification by a compound microscope results as a product of the magnification of the

objective and the magnification of the eyepiece
M = Mobjective ⫻ Meyepiece 共3兲

15
The Optical Reflected Light
Microscope
15.1 The Path of Light Rays
FIGURE 15.1 SHOWS THE COURSE OF LIGHT RAYS IN A MODERN THREE-
lens transmitted light microscope with “infinity optics” 共the ICS principle, which
means “Infinity Color-corrected System”兲. Let us follow the light rays that emanate
from an object 共1兲. From these rays the objective 共2兲 projects an image to infinity. The
intermediate lens 共3兲 that also intervenes in the progress of the light rays creates a mag-
nified intermediate image 共4兲 from the rays that are now running parallel. This inter-
mediate image is further magnified by the eyepiece 共5兲. As the illustration shows, the
visual angle ␦1 that results when this optical system is used is considerably greater than
it is when the object is viewed by the naked eye at the same distance of 25 cm 共⬃10 in兲,
visual angle ␦2.
15.2 The Objective

The objective consists of a combination of lenses, both converging and diverging, that
are precisely adjusted to one another. This makes a correction of any part of the image-
forming process possible whereby something has been lost, e.g., missing color, and a
flat intermediate image is projected.
The angle of opening 2␣, the aperture of the objective lens system, is crucial for the
quality of a microscopic system 共Fig. 15.2兲. An effective aperture is one that is as large
as possible so that as many diffraction spectrum maxima as possible of the rays re-
flected by the object can be captured and an image rich in detail consequently ren-
dered.
If, with regard to the illumination, one uses a condenser lens system 共Fig. 15.2兲 that
concentrates the initially parallel rays into a cone, the objective can then catch rays that
are even more diffracted. This means a greater optical resolving power and, conse-
quently, more detail.
For technical reasons, the angle at which a ray of light can enter into the objective
is maximally ␣ = 72°.
15.2.1 Numerical Aperture—Resolution-Magnification–Table 15.1–Table

15.2
The numerical aperture, by means of which a comparison can be made between two
objectives, is defined as follows:
NA = n ⫻ sin ␣ 共1兲
In this equation, ␣ is half of the aperture angle of the objective.
If air is present between the objective and the object, the refractive index, n ⬃ 1 共see
Table 15.1兲.
528
Chapter 15 The Optical Reflected 529
Fig. 15.1—Optical path A in a three-lens transmitted light microscope with infinity optics with
the visual angle ␦1 compared to the visual angle ␦2, when the object is viewed by the naked
eye in beam path B. With object A and B 共1兲, objective 共2兲, tube lens 共3兲, magnified
intermediate image 共4兲, eyepiece 共5兲, eye 共6兲.1
Under comparable conditions, maximum achievable image brightness is propor-

tional to NA2.
The greater the aperture of the objective and the shorter the light wavelength 共␭兲
the better one can distinguish two adjacent image points from one another. The short-
est distance 共do兲 is a measure of the resolving power of the microscope. This is shown
schematically in Fig. 15.3.
According to the laws of wave optics, one has achieved this distance 共do兲 when a
maximum degree of refraction is emitted from each of two image points that are sepa-
rated from one another by a minimum of refraction.
Ernst Abbe has defined this relationship mathematically with the following equa-
tion:
Fig. 15.2—Optical path of a condenser lens system with object in transmitted light 共1兲, light
beam 共2兲, objective 共3兲, condenser 共4兲.1
TABLE 15.1—Immersions Agents, Their Refractive Index, and the Possible Numerical Aperture.
Medium Refractive Index (n) Numerical Aperture NA
Air 1 to 0.95
Water 1.333
Immersion oil 1.515 to 1.4
Monobromonaphtalene 1.66
Methylene iodide 1.740
␭ ␭
do = ⬇ 共2兲
NAObjective + NACondensor 2NA
Example: If we assume that the aperture of the objective and the condenser is 1.25
and a wavelength 共␭兲 in the middle range of 0.5 ␮m, respectively, we receive, as the
smallest distance possible between two object points that can just be distinguished, a
do value of 0.2 ␮m.
Fig. 15.3—The shortest distance 共d0兲 between two adjacent image points. The shortest distance
is a measure of the resolving power of the microscope.
The resolving power can be improved by using light of shorter wavelength and a
larger aperture in the objective. With the use of white light, if one takes a medium wave-
length ␭ of 0 , 56 ␮m and an immersion objective with an aperture of 1.4 and with k
= 0.61, a resolving power of 0.25 ␮m results. For blue light with a wavelength of ␭
= 0 , 49 ␮m, one gets a resolving power, under otherwise identical conditions, of about
0.2 ␮m. Table 15.2 shows some values of resolutions that are theoretically possible for
various objectives and for a wavelength of 0 , 55 ␮m. Here, do is the distance between
two points on the object and Do is the point distance on the intermediate image.
In actual practice, the attainable resolution is usually less than the theoretical val-
ues stated in Table 15.2. It is dependent on the quality of the objective, the optimal set-
ting of the aperture diaphragm, use of the right immersion oil and, naturally, the speci-
men. One gets the best results with dust-free microscope systems and clean objectives
and well prepared specimens.
The overall magnification of a microscope is the product of the scale magnification
of the objective multiplied by the ocular magnification.
The magnification number indicates how many times larger the intermediate im-
age produced by the objective is than the object itself.
M = Mobjective ⫻ Meyepiece 共3兲

With a 50⫻ objective and a 10⫻ eyepiece the overall magnification of the micro-
scope is 500⫻.
Commonly used are 5⫻, 10⫻, 20⫻, 50⫻, and 100⫻-objectives.
Additional magnifications gained through the use of between-lenses or zoom-
devices are to be borne in mind.
M = Mobjective ⫻ Meyepiece ⫻ Mbetween-lens or zoom-device 共4兲

TABLE 15.2—Values of Resolutions that are Possible for Various Objectives and for a Wavelength of 0 , 55 µm.
Objective NA do / µm Do / µm
5⫻ 0.15 2.2 11.2
10⫻ 0.30 1.1 11.2
40⫻ 0.75 0.45 17.9
40⫻ 1.3 oil 0.26 10.3
63⫻ 1.4 oil 0.24 15.1
100⫻ 1.3 oil 0.26 25.8
The magnifications achieved individually by the objective, the intermediate lens,

and the eyepiece must be attuned to one another. One obtains optimal image quality
with an objective of a high scale number in combination with an eyepiece of low mag-
nification. For example, the combination 50⫻-objective and 5⫻-eyepiece is preferable
to the combination 10⫻-objective with 25⫻-eyepiece.
The total magnification of a microscope should be from 500 to a maximum of 1000
times the aperture of the objective. This is the maximum useful magnification that al-
lows the objective to reproduce tiny details in which the intermediate image can then
be magnified further by the eyepiece.
The numerical aperture of an objective increases with the objective magnification,
while the depth of field decreases. It is possible to increase the depth of focus, within
limits, by lowering the aperture diaphragm. But this is done at the cost of resolution.
Setting the aperture diaphragm too low results in empty enlargements and blurred im-
ages inasmuch as one thereby leaves the range of useful magnification.
In the case of dry objectives, there is air between the front lens and the object. A
maximum aperture of 0.95 is possible. In the case of immersion objectives, use of cer-
tain immersion agents with a higher refraction index between the front lens and the
object makes possible an increase of the numerical aperture to 1.7. This is shown in
Fig. 15.4.
Table 15.1 shows some values of immersions agents, their refractive index and the
possible numerical aperture.
The numerical aperture 共NA兲 is of essential significance for:
• Maximum image brightness
• Resolving power
• Useful total magnification
• Depth of focus
15.2.2 Aberrations in Image-Formation

Geometric and chromatic aberrations in image-formation are possible with uncor-
rected optical systems.
Geometric aberrations in the imaging process can occur even with monochro-
matic light. These include:
Aperture errors: With light beams on a plane parallel to the axis, the convergence
on the image side occurs not in the ideal image plane but rather either in front of it 共in
the case of converging lens兲 or behind it 共in the case of dispersing lens兲.
Coma: Off-axis point objects appear as asymmetrical areas with a comet-like tail.
Astigmatism: Point objects appear not as point images but rather as line images.
Curvature of field: The image points of a larger object do not lie on a plane but
Fig. 15.4—Improved resolution by use of an immersion liquid 共6兲 between object, over slip 共5兲
and objective 共3兲.1
instead on a curved surface. With uncorrected optical systems one can therefore focus
sharply either on the center of the image or else on peripheral zones.
Distortion: The image scale is dependent on the distance of the image point from
the optical axis. Increasing that scale leads to a pillow-shaped distortion. Decreasing
the scale results in barrel-shaped distortions.
With the polychromatic light used in microscopy, chromatic aberration can also
occur.
Since the refractive index decreases with an increase in wavelength, the focal
length of a lens for these light rays increases. The image of an object point, produced by
short-wave light 共violet兲 lies in front of the image produced with long-wave light 共red兲.
Undesirable color fringes are the result.
The chromatic difference of spherical aberration manifests itself in blue and yel-
low fringes.
With an appropriate combination of converging and dispersing lenses made of op-
tical glass with varying dispersive and refractory properties, these aberrations can be
corrected and objectives with varying optical properties can be produced.
15.2.3 Available Objectives

Depending on the purpose for which they are used and the quality that is required of
the microscopic image, various corrected objective lens systems are available for selec-
tion.
The objectives most often used are achromats. They are inexpensive because they
consist of relatively few lenses. Spherically they are corrected for one wavelength and
chromatically for only two wavelengths, usually red and green. This may lead to red
and blue color fringes around the object, but this can be avoided to a large extent
through the use of a green filter. Because the flatness of field is limited, they are appro-
priate for visual fields of up to approximately 18 mm in diameter. These objectives can
be used for routine tasks, including those as in polarized light. They are less useful for
microscopy in darkfield and for color photography, especially when there is a high de-
gree of magnification.
With fluorite or semiapochromatic objectives, spherical and chromatic aberration
is more strongly corrected. Flatness of field is also improved. For these reasons such
objectives can be used for fields of vision of up to 23 mm in diameter and are appropri-
ate for color microphotography in reflected light and transmitted light as well as for
dark field and DIC.
With apochromats, spherical aberration is corrected for two colors and chromatic
aberration for three colors. Because of their even further improved flatness of field,
these objectives can be used for fields of vision of up to 25 mm in diameter. And be-
cause color fringes hardly ever occur, these high-quality objectives are well suited for
color photography and for microscoping in dark field. Because of the better image cor-
rection, higher numerical apertures are possible and consequently a better resolution.
These objectives are therefore appropriate for the upper range of magnification to dif-
ferentiate the finest details 共precipitations, grain boundaries兲 and capture them in their
true colors. This means, however, less depth of field and a smaller working distance
between objective and object in comparison with achromats.
Plan apochromats and epiplan apochromats exhibit an outstanding flatness of
field and can therefore be used for large fields of view. Furthermore, since they possess
color correction for four wavelengths, the color rendering is optimal. The high numeri-
cal aperture makes a maximum of resolution power possible. These objectives in the
upper price range satisfy the highest demands in research and technology.
Objectives are usually marked with color rings corresponding to their magnifica-
tions: red-5⫻, yellow-10⫻, green-20⫻, blue-50⫻, white-100⫻.
The most important technical data are also inscribed on the barrel of the objective.
For example,
Epiplan-Neofluar
10⫻ / 0 , 30 HD DIC
⬁/0
provides the following information:
“Epiplan” means that this is an objective for a reflected light microscope that ren-
ders a flattened intermediate image. “Fluar” refers to the fluorite glass with which the
objective has been constructed.
The indicated scale number “10⫻” means that the intermediate image is 10 times
larger than the object.
“0.30” is the numerical aperture of the objective.
Using a light with an assumed wavelength of ␭ = 500 nm, a resolving power of
1 ␮m can be calculated.
“HD DIC” means that this objective can be used for bright-field 共BF兲 illumination,
dark-field illumination 共DF兲, and differential interference contrast 共DIC兲 illumination.
On most microscopes, objectives of varying scale number are exchangeable with
the rotatory nosepiece. To keep the focus essentially unchanged, the distance between
the screw-on surface of the objective and the eyepiece head is an important mechanical
dimension. It is called the mechanical tube length and is engraved on the objective.
If “⬁” is indicated there, this means that the object is imaged to infinity by the ob-
jective and that an additional tube lens produces a real intermediate image.
With a transmitted light microscope, objects are placed on a glass stage and pro-
tected by a cover glass. Consequently, transmitted light objectives are calculated and
corrected for a cover glass thickness of 0.17 mm.
Fig. 15.5—Schematic cross section of an eyepiece, with the position of the intermediate image
plane 共1兲, the boundaries of the visible field of vision 共2兲, the eyepiece optical system 共3兲, the
pupil of the observer’s eye 共4兲 and the focusing ring for the diopter adjustment 共5兲.1
In our example we are looking at an objective for reflected light microscopy. Be-
cause one usually examines uncovered specimens, the cover glass thickness is repre-
sented as a “ 0.”
15.3 Eyepieces
The simplest eyepieces consist of a convergent lens that acts as a magnifying glass.
Good eyepieces are equipped with a corrected lens system including an eye lens 共above兲
and a field lens 共below兲. Figure 15.5 shows a schematic cross section of an eyepiece
with the position of the intermediate image plane 共1兲, the boundaries of the visible field
of vision 共2兲, the eyepiece optical system 共3兲, the pupil of the observer’s eye 共4兲, and the
focusing ring for the diopter adjustment 共5兲.
Although eyepieces magnify the intermediate image that is produced by the objec-
tive, they do not bring about any further improvement in resolving power. But since the
angle of vision is now larger, the human eye is able to discern more detail.
If aberrations are still present in the intermediate image, they can be corrected
with the appropriate eyepieces.
Many eyepieces are designed for people who wear eyeglasses. They are usually
equipped with eyecups. The eyecups can be attached or they can be folded up to get the
right visual distance if the individual wants to use the microscope without eyeglasses.
The area of the intermediate image that can be examined, the field of view, is re-
stricted by the field lens and the aperture diaphragm. The value S is the measure of the
field of vision and is indicated on every eyepiece.
The diameter of the field of vision can be calculated from the field of vision value of
the objective together with the objective’s scale number:
Field of vision value S/M 共objective兲
An example: If M 共objective兲 = 40 and S 共eyepiece兲 = 18 mm, the result is a viewing
field of 0.45-mm diameter.
Wide-field eyepieces should be used only in combination with corrected plane ob-
jectives that produce a well flattened intermediate image.
Micrometer eyepieces have a glass plate with a scale situated on the plane surface
of the diaphragm. After the system has been calibrated, linear measurements as well as
measurement of angles 共goniometric eyepiece兲 can be made. The corresponding stan-

dard guides for calibrating are cited.
A tip: The eyepiece can also be used as a magnifying glass. Simply turn the eye-
piece, train the eye lens on the object, and look through the field 共condensing兲 lens.
15.4 Illumination
Illumination source and light path are important elements of a microscope.
Halogen lamps are often used, as are xenon high-pressure lamps.
Halogen lamps of between 25 and 100 watts emit light with a color temperature of
about 3000 K. This must be kept in mind when colored photographs are being taken
and conversion filters must be used for correction.
Xenon high-pressure lamps that produce between 100 and 500 watts are available,
and they produce a light that is more like natural light. Spectral response of the radi-
ated light and color temperature are about 5000 K.
A microscope’s illumination should
• Be adapted to the illuminated object field.
• Illuminate completely and evenly the object field to be observed.
• Be such that the illuminated object field is adapted to the field of vision of the mi-
croscope.
• Be adjustable according to the aperture angle.
15.4.1 Koehler’s Illumination System

The illumination system proposed by August Koehler in 1893 is still used today with
many optical systems using transmitted- and reflected-light microscopy.
The Koehler’s illumination method produces images that are illuminated with
evenly distributed light using three lenses placed between the light source 共1兲 in Fig.
15.6 and the reflector 共2兲. This type of illumination also contributes to the enhance-
ment of the resolution power. On reflected-light microscopes used for metallography/
materialography the Koehler illumination system is adjusted by the microscope fac-
tory and should not be changed by the user, for transmitted light, the system shall be
adjusted regularly. The three lenses of the Koehler system are part of the illumination
elements 共A兲 in Fig. 15.6. As the first lens in front of the light source 共1兲, the collector
lens forms an image of the light source at the second lens, the first condenser lens. The
third lens, the second condenser lens, reproduces the image of the light source in the
back focal plane of the objective 共3兲 after passing the reflector 共2兲. In this way the sur-
face of the specimen is uniformly illuminated.
In the path of the illuminating light rays there are two important diaphragms.
The centering radiant field diaphragm makes it possible to adjust the illuminated
object field to the microscope’s actual field of view. This diaphragm is correctly set
when the image of the edges of the diaphragm disappear behind the border of the field
of vision. Stray light is avoided and contrast is heightened. With reflected-light micro-
scopes a one-time setting of the field diaphragm is sufficient; it does not have to be read-
justed each time the objective is changed.
By means of the aperture diaphragm, the cone of light is adjusted to the aperture of
the objective. It has an optimal setting when that part of the light rays that is not dia-
phragmed out covers about two-thirds of the objective’s entrance pupil. This dia-
phragm must be reset whenever the objective is changed to meet the requirements of
Fig. 15.6—Bright field 共BF兲 illumination in reflected light and components in the optical path
for establishing contrast: Light source 共1兲, beamsplitter, color neutral 共2兲, objective 共3兲, object
共4兲, lens 共5兲 and contrast components on the side of the lamp 共A兲, on the side of the eyepiece
共B兲 and components for both light paths 共C兲.1
the desired image. This means that a compromise must be made between resolution,
contrast, and depth of focal field.
15.5 Microscope Options

The optical elements of a microscope, i.e., the objective, tube lens, eyepiece or projec-
tive, illuminators with light source, aperture and light field diaphragm—are assembled
in a mechanical device, the microscope body.
Depending on the expandability and capability of the built-in optical and me-
chanical assembly parts, one differentiates between student microscopes, laboratory
microscopes, and research microscopes.
Student microscopes are the most simply built and therefore the most limited in
their uses. The interchangeability of the individual optical elements is limited. Because
of their ease of use these microscopes are appropriate for the beginner or are used for
the preselection of specimens.
Laboratory 共or working兲 microscopes are equipped in such a way that they can be
used without problem for many routine tasks. The stage can be rotated or can be ad-
justed in an x-y-direction, or both, and the focusing of the objective occurs through a
coarse and fine focusing mechanism.
As an illumination source, a halogen bulb is mostly used. Koehler illumination as
well as interchangeable objectives and filters make it possible to perform all the usual
examination procedures. Attachment possibilities for further fixtures, as for example
analogue or digital cameras, are present.
Research microscopes belong to the top class of instruments. With these micro-
scopes all the essential parts, such as lamp-housing, condenser turret, object holding
stage, objective rotator, and tubes are interchangeable and can be adapted to special
tasks. Specimens can be viewed in either reflected or transmitted light. All known
methods of microscopic examination are possible.
The motorized variants are especially convenient because they make it possible for
change of objective, focusing, and movement of the mechanical stage to occur auto-
matically. Moreover, with the appropriate software all the important data such as ob-
jective, illumination, magnification, coordinates of the object, and the digital photo-
graphing of the image can be saved and later retrieved.
In a metallographic/materialographic laboratory, reflected-light microscopes of
either the upright or inverted type are used. If other materials are also examined, for
example, ceramic, stone, glass, or synthetics, a microscope with reflected-light as well
as transmitted-light beam projection is necessary.
15.6 The Reflected-Light Microscope

In metallography/materialography, ground and polished surfaces of materials are the
main objects that are examined with reflected 共incident兲 light.
The essential parts of a reflected-light microscope are: light source, condenser,
aperture- and radiant-field diaphragm, filter holder, reflector, rotating nosepiece with
reflected-light objective, stage, intermediate optic, body tube, and eyepiece.
15.6.1 Upright Type of Reflected-Light Microscope

With the reflected-light microscope of the upright type that is customarily used in ma-
terials research, the top surface of the specimen is illuminated from above through the
objective. Here the light rays are reflected or scattered. These rays are collected by the
objective. The tube lens projects an enlarged intermediate image that is caught by the
eyepiece and further magnified.
Figure 15.7 shows a modern upright type, reflected-light microscope, for routine
purposes.
The specimen lies on a movable stage. Direct observation of the fully lit position is
possible.
For the area being examined to be positioned absolutely perpendicular to the opti-
cal axis, the specimen must be correspondingly orientated with a leveling device. The
thickness of the specimen is limited by the working distance between objective and
stage.
15.6.2 Inverted Type of Reflected-Light Microscope

In the field of metallography/materialography, reflected light microscopes of the in-
verted type are also used often. Following the suggestion of Le Chatellier, the specimen
Fig. 15.7—Upright type reflected-light microscope.2
is placed on a movable specimen stage with a hole above the microscope column and
the objective.
Figure 15.8 shows a modern research microscope, inverted type, reflected-light.
The inverted type has the following advantages: 共1兲 The specimen is simply placed
with the prepared surface facing down on the stage and over the hole; 共2兲 There is no
need for cumbersome manipulation of a leveling device in order to get the prepared
surface of the specimen perpendicular to the light path; 共3兲 Larger, irregularly shaped
specimens can be easily examined microscopically as well, inasmuch as the working
distance object-objective is not affected by the size of the specimen. One disadvantage
is that the prepared surface can become scratched when it is placed on the stage. Fur-
thermore, one may not be able to see the illuminated area very clearly.
The objective of a reflected-light microscope differs from that of a transmitted-
light microscope. Optical calculations must take into account the fact that surfaces like
polished specimens are examined without a cover glass. In addition, reflected-light ob-
jectives are especially well dereflected so that no disruptive “false flashes” are superim-
posed on the image of the specimen.
With both systems, all the necessary construction elements are integrated in the
microscope. With a rotating nosepiece, different objectives can be inserted into the
beam path and the magnification thereby changed. Exchangeable slide-in components
permit quick and simple change to other types of illumination or filters.
Fig. 15.8—Inverted type reflected-light microscope for research.3
A camera connection makes documentation of the magnified image of the object

possible.
15.7 Optical Examination Methods

The prepared specimen normally has a plane surface. The ground and polished metal-
lic surface reflects light very well, therefore, usually shine brightly. The surface is either
silver or slightly colored, depending on the composition of the material. However, we
can differentiate individual portions of structural constituents only when they show
different contrast. If the reflection difference between two structural constituents is
greater than 10 %, they can be distinguished from each other. If that difference is less
than 10 %, contrast must be heightened using methods suited to that purpose.
Before contrasting, either by chemical or physical means, can be undertaken on a
ground and polished specimen, the specimen should first be observed in a polished
condition. To this end it is advisable to begin with the lowest degree of magnification
and then proceed to greater magnification. This enables one to check the quality of the
specimen preparation. Moreover, fissures, shrinkage and pores, inclusions, impurities,
corroded areas, thin oxide films, peripheral layers, and their adhesion to the base mate-
rial can already be detected. If the contrast between individual structural constituents
is sufficiently high, they can be distinguished as well.
With most metallographically/materialographically prepared specimens, how-
ever, the reflection differences between the individual structural constituents or phases
are so small that the contrast must be heightened by using carefully selected methods.
One process used to effect a change in the specimen surface, and which is con-
nected with contrast-heightening, is the electrochemical etching method. This process
includes the classical chemical as well as electrolytic etching.
In addition, physical contrasting methods, including thermal etching, ionic etch-
ing, and the application of interference coating are used to bring about a change in the
surface of the specimen 共see Figs. 9.1 and 9.2兲. These methods are described in more
detail in Chapter 9.
Our task here is to consider in greater detail various optical methods of producing
contrast that do not cause any change in the specimen surface.
The four main optical contrast methods used for the purpose of examining the tex-
tures and structures of metallographically/materialographically prepared specimens
with a microscope are the following: bright-field illumination, dark-field illumination,
polarization contrast, and differential interference contrast.
15.7.1 Bright-Field „BF… Illumination
Reflected light bright-field illumination is the most important method used in
reflected-light microscopy. In this process, the light that is reflected into the light path
of the microscope passes through the objective directly onto the specimen surface. Fig-
ure 15.6 shows the light path when bright-field illumination is used. An integrated ver-
tical illuminator 共1兲 emits a light that travels through the reflected-light aperture dia-
phragm and the radiant-field diaphragm. The light beam is then reflected by a color
neutral beam splitter 共2兲, which is set at 45° to the optic axis, and through the objective
共3兲 the beam strikes the surface of the specimen 共4兲. There, the reflected or scattered
beams again pass through the objective 共3兲 and traverse the beam splitter 共2兲. The tube
lens 共5兲 then projects the intermediate image. The image is further enlarged by the eye-
piece. Half-translucent mirrors may be used as beam splitters, but a higher light yield is
obtained by using prism illuminators.
Figure 15.6 also shows the location of all possible contrasting components ar-
ranged in a small area above the objective with
A: Contrasting element of the illumination side,
B: Contrasting element of the observation side, and
C: Space for components for both light paths.
The reflecting capacity of the individual structural constituents depends on their
refraction number n. More important, however, is the varying absorption power of in-
dividual phases and diffuse reflections. Differences in absorption of individual phases
and the presence of diffuse reflections create contrasts. If this contrast is sufficient, the
differences can be visible to the eye.
Accordingly, the polished specimen of a single-phase gold alloy, as well as those of
many multiphase metal alloys, show hardly any contrasts. If the material has constitu-
ent parts of widely varying reflection power, e.g., cast iron with laminated graphite,
steel with slag inclusion or sulfides, those individual constituent parts are already mi-
croscopically detectable immediately after the material has been polished.
Diffuse reflection occurs when there are rough surfaces, grain boundaries, and
scratches. But the presence of these things may also give some indication, in individual
cases, of the material’s structure.
For microstructures in bright field 共BF兲, see Figs. 7.15 and 15.10共a兲.
In other methods of achieving optical contrast, the light rays emanating from the
light source are diverted or else altered. Various reflectors that are built into the reflec-
tor slide of the microscope are used for this purpose. To gain a particular kind of micro-
scopic illumination or to observe the specimen in a particular way, one simply inserts
the reflector in the corresponding position.
15.7.2 Dark-Field „DF… Illumination
In the case of reflected-light dark-field illumination 共Fig. 15.9兲, the light that is emitted
by the reflected-light illuminator 共1兲 does not fall directly on the specimen surface. By
Fig. 15.9—Dark field 共DF兲 illumination in reflected light, with light source 共1兲, mirror step
assembly 共2兲, mirror with an oval hole 共3兲, light, directed in a second housing case towards the
objective 共4兲, sample surface 共5兲.1
means of a reflector “staircase” 共2 and 3兲, the light is conducted around the actual ob-
jective and into a second housing case 共4兲 where it strikes a ring-shaped concave reflec-
tor. This device reflects the rays at a very flat angle of illumination onto the specimen
surface 共5兲. Only scattered light returns for observation in the microscopic beam path.
For this reason, the flat surface of a well-polished specimen appears dark.
Reflected-light dark-field illumination is well suited to show the quality of a pol-
ished surface inasmuch as the oblique light rays allow lapping tracks, scratches, and
fine cracks to show up bright. Unevenness and rough surfaces are easily detected as
well. Hard phases that stand out, deeper-lying soft phases, as well as contraction cavi-
ties and pores display bright edge seams 共relief兲. Half-opaque phases may show their
inherent color.
Figure 15.10 shows a carbon steel in bright field 共a兲 and dark-field 共b兲. The struc-
ture and texture as well as surface details can be clearly seen with dark-field
illumination.
15.7.3 Polarization Contrasting „POL…

When contrast is achieved using polarization, a polarizer 共P兲 is inserted into the illumi-
nation beam pathway and an analyzer 共A兲 into the observation beam pathway 共Fig.
Fig. 15.10—Microstructure of carbon steel in bright field 共a兲 and dark field 共b兲.
15.11兲. The direction of transmission of the analyzer 共6, A兲 is at a right angle to the po-
larizer 共2, P兲. Only the depolarized portions of the rays can reach the tube lens 共7兲. In
this polarized light a lambda plate 共6a, ␭兲 changes the gray contrast into color contrast.
Interference reflection can be prevented by using a rotating ␭ / 4-plate 共antiflex-
plate兲 between the object and the objective.
In the case of substances that are optically isotropic, e.g., cubic or amorphous, the
specimen always appears dark because reflection from these materials does not lead to
a change in the state of polarization. The polarized light is, consequently, not let
through by the analyzer.
Structural constituents that are optically anisotropic, as for example zinc, tita-
nium, spheroidal graphite, some nonmetallic inclusions or minerals on the other hand,
do change the polarization state of a ray of light when reflected. Then the depolarized
portions of the light can penetrate the analyzer.
Fig. 15.11—Polarization contrast 共POL兲 in reflected light, with polarizer 共2 P兲, analyzer 共6 A兲,
lambda plate 共6a ␭兲.1
Observation of a metallographic/materialographic polished specimen in polarized

light is therefore useful for differentiating between isotropic 共cubic兲 and anisotropic
共noncubic兲 phases. Ferromagnetic phases can be identified as well inasmuch as the
plane of polarization, affected by the magnetization, is turned. For this reason, the do-
main boundaries of the magnetic zones appear in varying degrees of brightness.
The gray contrasts that occur in anisotropic phases can be transformed into color
contrasts through the use of a lambda plate 共6a兲 in the observation beam pathway. Iso-
tropic phases can likewise be contrasted in polarized light by applying an optically an-
isotropic layer. For example, an oxide layer applied by anodization to aluminum pro-
duces color contrasts. With slag, minerals, ceramic, and glass that show half-opaque
behavior, the use of polarized light results in less scattered light. This makes a better
contrast possible and the structural constituents can be delineated better one from an-
other.
The microstructure in Fig. 15.12 shows titanium with deformed areas made vis-
ible with polarization contrast 共POL兲.
15.7.4 Differential Interference Contrasting „DIC…

When Nomarski’s differential interference contrast method is used, the polarized ray
of light is split into two beams of different oscillation directions 共Fig. 15.13兲 by a doubly
Fig. 15.12—Microstructure of titanium in polarized light. Cold work is visible.
refracting prism 共4兲. These two rays are out of phase with each other when they strike
the specimen 共6兲. If the specimen surface is not completely flat, path differences are the
result. In a reverse direction, the reflected or scattered beams, or both, now traverse the
DIC-prism 共4兲 and the analyzer 共7兲, thereby acquiring the same oscillation direction
and now capable of interfering with the intermediate image. The path differences that
are caused by the specimen surface are converted to gray values. Unevenness becomes
visible as relief. With a lambda plate, color contrasts can be obtained.
Figure 15.14 shows a microstructure of a soldering in bright field 共BF兲共a兲 and in
differential interference contrast 共DIC兲共b兲. In BF the solder can only be seen as a gray
phase in the lighter matrix, but in DIC the solder can be clearly discriminated from the
matrix.
15.7.5 Fluorescence in Reflected Light

Specific areas of a microstructure can be marked with a fluorescence dye 共see Section
3.10.1兲. These areas will absorb light of a specific wavelength in a short period of time,
and then emit the light. The wavelength of the emitted light is always around
20– 50 nm longer than the incoming light. If blue light is absorbed, green light is emit-
ted, from UV-light visible light is emitted.
Especially at the examination of medical and biological samples, fluorescence is
often used, as specific dyes are suited for specific phases in the sample. In this way an
exact microscopic examination can be performed.
In metallography/materialography the use of a dye can give important informa-
tion on size and distribution of pores, cracks, gaps between basic material and surface
layers, etc. 共see Section 3.10.1兲.
At the reflected fluorescence microscopy 共Fig. 15.15兲 a short pass filter 共A兲 is placed
in the light path, only allowing light of a narrow wavelength to pass to the specimen. In
between is placed a beam splitter 共B兲, which reflects the short waved reflected light and
only let through the long waved emitted light. The reflected light that is not absorbed by
the specimen surface is stopped by a long pass filter 共C兲; this filter only lets the long
waved fluorescence light pass.
Lamps with a high degree of red or infrared light are less suited for fluorescence
Fig. 15.13—Differential interference contrast 共DIC兲 in reflected light, with doubly refracting
prism 共4兲, objective 共5兲, specimen 共6兲 and analyzer 共7兲.1
microscopy; mercury vapor lamps with a line type spectrum are to be preferred.
For a microstructure impregnated with a dye and examined with fluorescence see
Fig. 3.14.
15.8 Practical Use of the Microscope

15.8.1 Setting up the Microscope
If possible, the microscope should be set up in a room of its own on a stable worktable.
There should be sufficient space to the right and to the left of the apparatus for the
depositing of specimens and supplemental equipment. If no separate room is available
for microscopic or measurement work, the instrument should be located in a place re-
moved from all sectioning, grinding, and polishing equipment to avoid any transfer-
ence of vibrations or abrasion particles. Moisture, especially alkaline and acid vapors
from electrolytic polishing or chemical etching, can also damage important parts of
the microscope after just a short time. Such chemical procedures should be performed
under a fume hood in a separate room.
Fig. 15.14—Microstructure of a soldering in bright field 共BF兲共a兲 and differential interference
contrast 共DIC兲共b兲.
15.8.2 Working with the Microscope

In this section and the following two sections, a number of points are stated that should
be followed when working with the microscope.
• Adjust the height of your chair in such a way that you are sitting erect but comfort-
ably as you look into the eyepiece and can reach all the operating parts of the in-
strument effortlessly.
• Turn on the source of light.
• Place a specimen on the microscope stage 共focus plane兲.
• Look into the distance, then, without changing the focus of your eyes, look into the
eyepiece.
• Adjust the distance between the eyepieces according to the distance between your
eyes.
• If you do not wear glasses, put rubber eyecups on the eyepieces to get the right eye
distance to the eyepiece.
Fig. 15.15—Fluorescence: Short pass filter 共A兲, beamsplitter 共B兲 and long pass filter 共C兲.1
If you do wear glasses, check to see whether the eyepieces are designed accord-
ingly. If you have done everything right you will have a clear view of everything in the
whole field of vision.
15.8.3 Correct Adjustment of the Microscope

• Begin by using an objective of a low scale number and bring the specimen into fo-
cus.
• Open the field diaphragm and center this and the condenser in such a way that the
viewing field is illuminated evenly.
• Close the field diaphragm and, through centering, bring the little fuzzy fleck of light
that is still present into the middle of the viewing field.
• This fleck of light can be brought into sharp focus by vertically adjusting the con-
denser.
• Open the centered field diaphragm in such a way that the diaphragm leaves extend
out over the field of vision.
• Open the aperture diaphragm and close it again carefully until the image has be-
come dark enough to show sufficient contrast.
With transmitted-light microscopes, a change of objective requires each time a re-
adjustment to accommodate the settings of the field and aperture diaphragms. Such
readjustments are not necessary with reflected-light microscopes. With the latter it is
sufficient to adjust the aperture diaphragm to the object and the objective.
15.8.4 Focusing and Practical Use

• The task of getting a sharp focus on shiny polished specimens of metal can be facili-
tated by partially closing the radiant-field diaphragm. After that, focus sharply on
the image of the radiant-field diaphragm. Because this diaphragm is imaged in the
object plane, it is easy to find the image of the specimen surface.

• As an alternative move the field of view to the edge of the sample. The contrast be-
tween the sample and the mounting material or air allows for a simple focus.
• In focusing the microscope, use at first an objective of weak magnification and look
for the area of interest. Then change to objectives with a higher magnification, as
necessary.
With unfamiliar specimens it is advisable to experiment with all the different illu-
mination possibilities 共optical contrasting methods兲. Often structural details can be
identified better in this way and distinguished from one another.
If an oil immersion objective is used on an upright type microscope, the area of the
object that is of interest is first of all located with an objective of a low magnification 共10
⫻ 兲. Then one focuses with the oil immersion objective 共e.g., 100⫻兲. After that, using the
objective revolver, this objective is turned to the side and the one with the lower magni-
fication is again swung into position. Now one applies a drop of immersion oil to the
illuminated area on the object, trains the objective with the higher magnification on
the specimen, and refocuses with fine focusing. Proceeding in this way can avoid
dampening other objectives with oil. In case of an inverted microscope, first focus with
the oil immersion objective without oil. The specimen is removed then from the micro-
scope, and a very small drop of immersion oil is placed on the center of the objective.
Now the specimen is replaced and a fine focusing is done.
After work with the microscope is finished, the oil on the objective and on the
specimen is removed immediately and carefully with fine tissue paper and then
cleaned with ethanol.
15.8.5 Measurements of Length

The microscopic image can be measured with eyepiece crosses on which there are
scales, squared grids, or reference samples. This can be in the form of a reticle, which is
a system of lines, circles, dots, cross hairs, or wires, or some other pattern, placed in the
eyepiece or at an intermediate plane on the optic axis which is used as a measuring
reference, focusing target, or to define a camera field of view. Also a graticule, which is a
scale on glass or other transparent material placed in the eyepiece or at an intermediate
plane on the optic axis can be used. The scale of the reticle or the graticule serves as a
reference gage. The distance between gradation marks on this scale is very precise, e.g.,
0.1 mm.
Let us suppose that we want to measure the length of an integral part of a micro-
structure that we are examining with an objective with a scale number of 100. If its
apparent length amounts to 1.2 mm in the intermediate image of the eyepiece, its true
length can be determined by dividing by the scale number on the objective. The length
is 1.2 mm divided by 100, i.e., 12 ␮m. It is not necessary to take the magnification of the
eyepiece into consideration.
A calculated magnification, using the manufacturer’s supplied ratings, as men-
tioned earlier, is only an approximation of the true magnification, since individual opti-
cal components may vary from their marked magnification. For a precise determina-
tion of the magnification 共calibration兲 observed through an eyepiece, a stage micro-
metre is used. This is a graduated scale, placed like a specimen on the stage of a micro-
scope and used for calibration.
It is very important that the measuring devices used are precise, and it is recom-
mended that these should be traceable to the National Institute of Standards and Tech-
nology 共NIST兲 or a similar organization.
Measurements should be performed according to ASTM Standard Guide for Cali-

brating Reticles and Light Microscope Magnifications 共E 1951兲. This guide covers
methods for calculating and calibrating microscope magnifications, photographic
magnifications, video monitor magnifications, grain size comparison reticles, and
other measuring reticles.
15.8.6 Measurements of Height Differences

Occasionally it is of interest to measure height differences of layers of differing hard-
ness or the depth of scratches. To do this, an objective of a high numerical aperture is
used because its depth of focus is very slight. One narrows the field diaphragm to a
small circle and focuses on the highest plane. On the fine-focusing knob scale a value
can be read. Then one focuses on the deepest place and again reads off the appropriate
value. If one knows the level difference 共obtained from the instruction manual兲 that
corresponds to the distance between two scale-marks on the fine focus mechanism,
one can easily calculate the measurement. Use of a dial gage that is connected to the
microscope stage or of an electric position encoder is more convenient.
15.8.7 Maintenance of the Microscope

Microscopes are precision instruments that should serve their purpose for many years.
For this reason they should be handled with care.
Dust particles or smoke are especially a problem. Always cover your microscope
with a protective dust cover after you have finished working and turned it off. The front
lenses of the objective are especially sensitive. Avoid letting the objective come into
contact with the specimen or the stage when you are focusing. The most minute
scratches that can occur when these touch one another can cause blurred areas in the
image.
Etched specimens should be thoroughly cleaned and dried before they are used in
the microscope. Acids and residual moisture can not only leave flecks on the specimen
but also have an adverse effect chemically on the front lenses of the objective, as for
example can happen with hydrofluoric acid.
If you must remove dust from the objective, eyepiece, or filter, blow them off with a
rubber dust blower. Fingerprints, traces of grease, and residues of immersion oil can be
removed with a cotton ball dipped in grease-free benzene if necessary.
It is a good idea to have the service department of the manufacturer check the de-
vice at least once a year and make any adjustments or calibrations that may be neces-
sary. Leave repair work to the service department of the manufacturer also.
15.9 Documentation
The documentation of microscopic images can be done in different ways. In the early
days of microscopy, the viewer sketched the image details that interested him.
Today either reflex cameras for photos in various formats or video or digital cam-
eras, or both, are used.
Modern microscopes are equipped accordingly. They have their own photograph/
television connection. One can change over to this connection from the ordinary bin-
ocular tube via a beam splitter.
Figure 15.16 shows the light path. Through a photo-ocular 共3兲, the intermediate
image 共2兲, coming from the tube lens 共1兲, is magnified and projected to infinity. The
Fig. 15.16—Optical path for photomicrography, with tube lens 共1兲, intermediate image 共2兲,
photo eyepiece 共3兲, central shutter 共4兲, camera lens 共5兲 and image in the film plane 共6兲.1
photo-objective produces from this an intermediate image on the film plane in the
camera 共6兲 if the central shutter 共4兲 is opened for exposure. The size of this intermediate
image must be adjusted to the format of the film. With microphotography film, for ex-
ample, a magnification with the factor 2.5⫻ must be effected when the original inter-
mediate image has a diameter of 20 mm. This means that the entire image cannot be
captured on film of microphotography format.
The housing of a reflex camera can be joined to the photo/TV connection by means
of an adapter with a built-in objective. The reflex camera should be equipped with an
electric motor for film transport and a remote control switch. One disadvantage is that
the flipping up of the mirror at the moment of exposure may cause both the microscope
and the camera to vibrate, resulting in blurred images.
For professional documentation, microscope cameras are to be preferred. All the
important camera settings can be regulated electronically from a control desk. The
camera itself works with a vibration-free shutter. Depending on the model, the film cas-
sette may be exchangeable.
For several years now, video cameras and digital cameras have been increasingly
used for image documentation. Because semiconductor sensors can be used with the
modern CCD-cameras that have very small active surface areas, the enlarged interme-
diate image in the microscope must be reduced again. For this purpose, TV-adapters
with special optics and a fixed reduction factor are necessary. With a TV-zoom-adapter,
the reduction factor and consequently the area of image detail can be changed. In this
way, the size of the image can be made to fit the format of the camera or video printer.
This can be of advantage in connection with the required standard magnifications.

Such linear standard magnifications are 25, 50, 75, 100, 200, 250, 400, 500, 750, 800,
and 1000⫻.
The picture taken by the camera can be shown on a monitor, printed out by a video
printer, or processed and stored in digitalized form on a PC.
In this process, the overall magnification, Mtotal, can be calculated from the optical
magnification, Moptical, and the electronic magnification Melectronic.
Moptical = Mobjective ⫻ Madapter 共5兲

where Mobjective is the magnification of the objective, and Madapter is the magnification of
the adapter.
Melectronic = Dmonitor/Dsensor 共6兲

where Dmonitor is the diagonal length of the image of the monitor and Dsensor is the diago-
nal of the active surface of the picture sensor.
So the overall magnification is
Mtotal = Moptical ⫻ Melectronic 共7兲

In addition to the conventional CCD-cameras that shoot from 25–30 images per
minute, “Slow-Scan” CCD-cameras are also being used in even greater numbers. These
cameras take fewer images per second but with higher resolution and with less noise.
In combination with a PC, digitalized images can be processed and archived.
Thanks to the many highly efficient software programs, they can also be qualitatively
improved, marked, and labeled. Program modules that analyze structure make pos-
sible the quantitative measurement of the structural parameters and a description of
the measurement results in the appropriate form, the numerical values in the form of
tables or clarifying diagrams 共see Part IV of this book兲.
15.10 The Confocal Laser Scan Microscope

Depth of focal field is a fundamental problem in light microscopy. It is also the reason
why we produce surfaces that are as plane possible when preparing metallographic/
materialographic specimens and why we arrange them perpendicularly to the micro-
scope’s light ray. This is the only way to achieve a sharp image over a larger area.
The greater a microscope’s magnification, the smaller the field of view, and the
shallower the depth of focal field.
This system-determined limitation on the light microscope can be circumvented,
and the possibilities for its use significantly broadened with the help of modern laser
and computer technologies. The specimen surface can be scanned in a line-by-line
manner with a focused laser ray. Confocal reproduction conditions, the recording,
storage, and processing of the signals in a PC, make a three-dimensional representa-
tion of the specimen surface possible. The laser scan microscope 共LSM兲 thus combines
the advantages of the light microscope with those of the scanning microscope and the
profilometer.
15.10.1 Function of Confocal Laser Scan Microscope

Figure 15.17 shows the path of light rays and the operational mechanism for the de-
vice. The laser ray is focused onto the specimen through the objective lens. Light that is
Fig. 15.17—Path of light rays and the operational mechanism for a confocal laser scan
microscope.1
reflected there is focused onto a variable pinhole aperture by an additional lens. Only
light coming from the objective’s focal plane can reach the detector unimpeded. Light
coming from other optical planes is suppressed by the confocal spatial filter that con-
sists of lens and aperture. The specimen surface, with the light ray falling onto it, can be
scanned point-by-point, line by line, by means of the dichroic mirror. The light signals
received by the detector are converted into electronic impulses and digitally processed.
We, therefore, obtain a reproduction of the level specimen surface on a monitor.
Because of the low depth of focal field, we obtain an “optical section” in x, y coordinates
when the surface is irregular.
By successively changing the arrangement of the object along a series of defined
steps in direction z, we can record several sections and compile these images into a
three-dimensional stacked image, process them digitally and draw qualitative as well
as quantitative conclusions about the topography of the specimen surface.
Lasers with varying excitation wavelengths in the ultraviolet through infrared
spectral range are used. As lasers of wavelengths 488 and 514 nm 共25 mW兲 and HeNe
lasers of wavelengths 543 nm 共1 mW兲 and 633 nm 共5 mW兲 are usually used in
metallography/materialography.
At 0.2, the laser scan microscope’s lateral resolution capability is somewhat better
than that of the conventional light microscope.
Depth resolution depends on the wavelength of the laser light, the numerical aper-
ture 共NA兲 of the objective and the diameter of the aperture, which is a determining fac-
tor for the quality of the confocal spatial filter.
Assuming that the aperture’s diameter in front of the detector approaches zero, the
following holds true for reflective surfaces:
Fig. 15.18—Confocal laser scan microscope.1
dz = n ⫻ 0.89 ⫻ ␭/共NA兲2 共8兲

where dz is the axial half-width of an intensity curve of light reflected by the object, deter-
mined by the height of the object stage; ␭ is the laser's wavelength and n is the refraction
index.
In practice, values between 20 and 50 nm turn out to correlate with a useful depth
of focal field, depending on objective type and the medium that is between the objective
and the object.
15.10.2 Applications of Confocal Laser Scan Microscope

Possible types of lighting for LSM are bright-field, differential interference contrast,
and fluorescence. If lasers that emit polarized light are used, polarization microscopy
can also be used. Figure 15.18 shows a confocal laser scan research microscope set up
with a motorized fine focusing stage and monitor.
In the area of material research and testing, confocal light microscopy is suitable
for the investigation of the surfaces of metallic materials, ceramics, plastics, and repli-
cas as well as of semitransparent and transparent layers such as glass, polymer foils,
coatings, or varnishes.
In addition to the representation of compounds, surface profiles can be recorded
and the microroughness of very small areas such as tears, pores, and hollow spaces can
Fig. 15.19—Confocal image of a fractured steel plate.4
be three-dimensionally ascertained. The arrangement and thickness of single and mul-

tiple layers can also be represented and quantitatively analyzed.
Figure 15.19 shows a fractured steel plate, the single grains can be seen three-
dimensionally.
15.11 Stereo Microscopy

For the purpose of a three-dimensional evaluation of fractured surfaces, the size and
shape of those fractures, as well as the three-dimensional shape and configuration of
constituent elements, it is advantageous to use a stereomicroscope. With a stereomi-
croscope the same spot on a specimen can be viewed from two places at a short dis-
tance from one another, similar to the distance between the two eyes of a human being.
Modern stereomicroscopes may use two different principles for the light ray
paths.
Following the Greenough principle, two light ray systems are directed onto the
specimen through two identical objectives that are tilted toward one another at the ste-
reo angle. This yields two images that produce a single three-dimensional image when
observed through the two eyepieces.
Following the telescope principle, two parallel but not axially aligned light beams
are directed through an objective. The beams are deflected by the objective and strike
the specimen at the stereo angle. With this method of operation, an expansion of the
operational possibilities becomes relatively easy because supplementary optical mod-
ules can be installed either above or below the body of the microscope.
For stereomicroscopes, a number of exchangeable objectives are obtained with
the magnifications from 5⫻ to 100⫻ and eyepieces from 5⫻ to 20⫻.
Fig. 15.20—Stereo microscope with digital camera.3
Apochromatic objectives are well suited for three-dimensional observations. For

flat objects like prepared specimens, wafers and foils, plan achromats are better suited.
For the finest structures with very low contrast, the apochromats can be used with ad-
vantage.
The magnification can be changed by zoom when a special system of lenses is
used. According to design and manufacturer the variation in magnification may be be-
tween 3:1 or 12:1.
The observation of details depends to a high degree on the illumination that shall
be adapted to the object and the purpose of examination. Therefore, different illumina-
tion systems can be obtained like halogen-incandescent lamp for incident light or co-
axial illumination, optical fiber for vertical illumination, and other light sources
for highest light intensity and for homogeneous illumination. Metallographic/
materialographic specimens or other flat, strongly reflecting objects like LCDs, wafers,
and integrated circuits may be examined most effectively with coaxial illumination.
Three-dimensional objects may be illuminated from two sides or with ring-
illumination. Using illumination under an angle will give an improved observation of
high differences in the surface. Vertical illumination is best suited for exposing of cavi-
tations and open pores. Fluorescence modules make examination of fluorescence sub-
stances possible.
The advantages of stereomicroscope systems are: Ample working distances, large
object fields, and the three-dimensional viewing of nonreversal images.
Stereomicroscopes can produce meaningful overall magnifications of up to about
250 times the original.
Figure 15.20 shows a modern stereomicroscope.
16
Electron Microscopy—Scanning
Probe Microscopy
AN IN-DEPTH DESCRIPTION OF ELECTRON MICROSCOPY AND SCANNING
probe microscopy falls outside the scope of this book, but in this chapter a short intro-
duction is given to the transmission electron microscope 共TEM兲, the scanning electron
microscope 共SEM兲, the focused ion beam techniques 共FIB兲, and a number of scanning
probe microscopes 共SPM兲.
16.1 The Transmission Electron Microscope „TEM…

Electron beams penetrate thin layers and, in doing so, are diffracted at the crystal lat-
tice and interferences arise. One can make these visible, after amplification with elec-
tromagnetic lenses and electronic processing, as bright-dark effects. With an accelera-
tion voltage of up to 1 million volts, magnifications of up to 106 with a resolution below
1 nm can be attained. Disruptions in the crystal lattice, such as dislocations, elimina-
tions, grain boundaries, and other lattice defects, are detectable; they appear mostly
dark.
Specimens for the TEM examinations must be thin enough for the electrons to
pass through and thick enough for their structural features to remain verifiable. Vari-
ous methods can be used for the preparation.
With metallic materials and ceramic basic materials, thinning procedures are pre-
ferred. Using this method, the specimen 共diameter 3 mm兲 is made sufficiently thin,
through either ion bombardment 共see Section 16.3兲 or electrolytically, that a hole is
produced in the middle. Areas next to the hole are sufficiently thin to be suitable for
TEM examination 共see Section 8.5兲.
For purposes of imaging the surfaces, carbon or lacquer is used to take a replica of
the specimen. The peeled-off layer of lacquer is then vapor-coated in a vacuum cham-
ber with carbon or metal 共Au, Pt兲 to bring out the contrast. After the layer of lacquer has
been removed, the metal foil or carbon foil can be transluminated.
Fine powder, dust, or smoke particles are applied directly to a backing film 共car-
bon, lacquer兲. With extraction replicas, individual particles of a specimen, their size,
and distribution can be identified.
With the use of ultramicrotomes one can produce thin sections from embedded
powders or synthetics. Synthetic materials that tend to smudge must be worked with at
low temperatures 共cryomicrotomy兲.
16.1.1 The Scanning Transmission Electron Microscope „STEM…
This microscope is a combination of a TEM and a SEM 共see below兲 and gives the advan-
tages of both microscope types. A STEM is a very high cost investment and primarily
used for research.
16.2 The Scanning Electron Microscope „SEM…

In the scanning electron microscope, the surface of the specimen is linearly scanned
with the electron beam 共ca. 0.01 ␮m兲. Secondary electrons are emitted and captured by
558
Chapter 16 Electron Microscopy 559
an electron detector. The spatial distribution of these secondary electrons can be made
visible, after electronic amplification, on a monitor. Depending on the acceleration
voltage of the primary electrons, magnifications of up to 200 000⫻ are possible. With
magnification of 1000⫻ the depth of field is about 35 ␮m; the resolution power
amounts up to 0.01 ␮m. Differences in levels on the surface of the specimen result in
differences in contrast. Moreover, shadow formations can arise as a result of the slant
with which the electron beams fall on the specimen. As a result, an image of high reso-
lution and great depth of field is obtained.
The SEM is used preferably for the examination of rough surfaces and investiga-
tions of damage or loss, e.g., fractured surfaces.
Preparation of the specimen for SEM examinations is simple: the specimen must
be free of volatile elements like water, oil, or grease. Loose particles must also be re-
moved. If the specimen does not consist of electricity-conducting material, the surface
must be coated with a layer of electro-conductive material 共C, Pt, Au兲 to prevent charg-
ing.
In case of mounting, care should be taken that metal powder, like copper, con-
tained in the mounting material, is not contaminating the specimen.
16.2.1 Energy Dispersive Spectroscopy „EDS…

An SEM can be equipped with additional equipment like EDS and EBSD 共see below兲.
Besides the electrons emitted from the specimen mentioned above, also X-rays are
emitted. As high-energy electrons produced with an SEM interact with the atoms
within the top few micrometres of a specimen surface, X-rays are generated with an
energy characteristic of the atom that produced them. The intensity of these X-rays is
proportional to the mass fraction of that element in the specimen. In EDS, X-rays from
the specimen are detected by a solid-state spectrometer that converts them to electrical
pulses proportional to the characteristic X-ray-energies. If the X-ray intensity of each
element is compared to that of a standard of known composition and suitably cor-
rected for the effects of other elements present, then the mass fraction of each element
can be calculated.
16.2.2 Electron Backscatter Diffraction „EBSD…

Electron Backscatter Diffraction 共EBSD兲 has become popular among materials scien-
tists since the first commercial automatic systems were available in 1994. The main
advantage of this method is the possibility to link morphology 共grain size and shape兲
with crystallographic features 共phase, orientation, disorientation兲 on the microscopic
scale, but still in a representative specimen area. During the examination, an electronic
backscatter pattern 共EBSP兲 is produced, an image consisting of relatively intense
bands 共Kikuchi bands兲 intersecting one another and overlying the normal distribution
of backscattered electrons, as a result of Bragg diffraction of electrons by atomic
planes in the crystal lattice. The results can be compared to TEM, but the specimen
preparation is much simpler than the preparation of thin foils. The specimens, how-
ever, are considerably more difficult to prepare than for normal imaging in SEM, be-
cause of the very low information depth of the EBSD signal based on channeling ef-
fects. This means that the very thin deformed layer, often left on the specimen after
mechanical preparation, cannot be tolerated to obtain a good pattern quality, and
therefore the specimen preparation shall be improved. In general, classic etching is not
needed for EBSD because the contrast is defined through the orientation differences.
Etching should even be avoided, as the induced surface roughening is disturbing due to
the high specimen tilt 共70°兲 during the examination process. The specimen preparation
for EBSD is discussed in Section 7.10.4.
16.2.3 The Electron Probe Microanalyzer „EPMA…

This instrument, also called the microprobe is closely related to the SEM, only the
X-ray detectors are not analyzing only the energy as in EDS mentioned above, but the
wavelength of the X-rays generated from the interaction of the primary and backscat-
tered electrons and the specimen. This is called wavelength dispersive spectroscopy
共WDS兲 and compared to EDS, WDS gives much more accurate quantitative data for the
single components in the specimen surface.
16.3 Focused Ion Beam „FIB…

A focused ion beam system 共FIB兲 is in principle built like an SEM. In the SEM an elec-
tron beam is used for scanning, but in the FIB a beam from a liquid metal ion source
共mostly gallium, Ga+兲 is used. This beam is focused so that it can be scanned like an
electron beam. This allows for sputtering material from the sample or for depositing
material on the sample if gases are used 共see Section 9.6.5兲. Also, imaging is possible by
ion-induced secondary electrons, as it is known from the SEM. As the FIB can remove
material with a very high precision, it is used for preparation of samples for TEM. This
covers both samples of electronic devices and samples for material research.
The TEM samples can be made either by using a pre-prepared sample in the form
of a thin strip of material, which then is further thinned by the FIB, or by the newer
lift-out technique. With this technique no mechanical preparation is needed, the ion
beam cuts into the base material and the sample is lifted out using a special manipula-
tor.
The great advantage of using FIB for preparation of samples for TEM is the shorter
times compared to conventional methods 共see Section 8.6兲, and the very high rate of
success.
16.4 Scanning Probe Microscopes „SPM…

In addition to the methods of optical metallography/materialography already men-
tioned 共LM, TEM, SEM兲, we will briefly discuss scanning probe microscopy. In the past
few years it has gained increasingly greater significance in the area of metallography/
materialography.
All scanning probe microscopes work according to the following principle: the sur-
face of the specimen is scanned with the sharp tip of a needle that is mounted on a
flexible cantilever. The interactive force that is present between the tip and the surface
serves as a measurement signal and can be evaluated. Through the use of piezoelectri-
cal actuators, movements of the measuring tip in the magnitude of atomic diameters
can be initiated, with a resolution of less than 1 nm. Scanning probe microscopes are
used in biology, physics, and materials science to characterize surfaces.
The first device of this kind, the Scanning Tunneling Microscope 共STM兲, was devel-
oped by Binnig and Rohrer and used for the first time in 1981. It makes use of the
quantum-mechanical tunneling effect for measurement of distance. For this purpose,
voltage is applied between the tip and the specimen. If one brings the tip closer to the
surface without actually touching it 共noncontact mode兲, a current begins to flow. Inas-
Chapter 16 Electron Microscopy 561
much as the amplitude of this current depends exponentially on the distance it can be
used to regulate the distance. With STM the surface topographies of conductive
samples and images in the atomic range can be shown.
With the Atomic Force Microscope 共AFM兲, the tip is positioned at the free end of a
cantilever. The interaction between tip and surface, e.g., a repulsive force, is registered
through the vibration of the cantilever. Its detection occurs in accordance with the light
conducting principle: a laser beam focused on the backside of the flexible cantilever is
reflected and registered by a photo diode. The measured values in the nanometre range
can be used to guide piezoelectric actuators in the x-, y-, z-direction of the tip. In this
manner one can obtain a three-dimensional image of the surface on the computer.
AFM is suited for electrical-conductive and nonconductive materials such as met-
als, ceramics, glasses, and synthetics. Samples, either unprocessed or processed, can
be examined in air, in a gaseous environment, or in liquids.
The field to which ATM is applied is constantly growing and now this technique is
also used for measuring of nano hardness and elastic modulus 共Young’s modulus兲共see
Section 21.6.1兲.
If the specimen is to be prepared metallographically/materialographically, one
must take care that it has been polished with as little resulting deformation as possible
共electrolytic polishing may be an advantage兲, and that through chemical etching only a
minimal level contrast in the nanometre range arises between the individual phases.
Very small structural elements, e.g., the very finest precipitates, can then be identified
that can no longer be seen with a light microscope because of its limited resolution
power. Nevertheless, other local interactive forces can be detected with the AFM proce-
dure.
With magnetic force microscopy 共MFM兲, the surface of the sample is scanned with
a nickel or iron tip in noncontact mode. One obtains an image of the local magnetic
characteristics with a resolution in the nanometre range.
Adhesion force microscopy conveys perceptions with regard to the local structure-
specific adhesive force between measuring tip and specimen surface.
With friction force microscopy, the local frictional forces can be measured and im-
aged. This is performed in contact mode by letting the tip move across the surface of
the specimen and measuring the deflection of the cantilever. Good contrasts can be ob-
tained especially with synthetics.
References „Part III…

关1兴 Courtesy of Carl Zeiss, Germany.
关2兴 Courtesy of Olympus, Germany.
关3兴 Courtesy of Leica Microsystems, Germany.
关4兴 Courtesy of E. Bischoff, Max-Planck-Institut für Metallforschung, Stuttgart, Germany.
Part IV: Quantitative
Metallography/Materialography—
Automatic Image Analysis
17
Quantitative Metallography/
Materialography—An Introduction
WHEN MAKING A QUALITATIVE EXAMINATION OF A MICROSTRUCTURE,
the interpretation of the structure is to a high degree based on the knowledge and expe-
rience of the observer. In quantitative metallography/materialography the constituents
in the microstructure are measured to provide more reliable data for materials engi-
neering and quality control purposes. Typical microstructural measurements include
the length, width, and area of features or the relative amount of a structure or phase.
The application of stereological principles enables two-dimensional measurement
data extracted from metallographic/materialographic specimens to provide accurate
information about three-dimensional structures increasing the usefulness and impor-
tance of quantitative microstructural analysis. It can be tedious to implement quanti-
tative methods. Digital image analysis equipment and software have been developed as
tools to automate the collection and reporting of quantitative data.
In this chapter, the most important uses of quantitative metallography/material-
ography and corresponding ASTM standards are discussed briefly. Automatic image
analysis is described in Chapter 18. Both chapters should be considered as introduc-
tions to quantitative metallography/materialography and image analysis 共see the Ref-
erences and Literature List for further study of these subjects兲.
17.1 Quantitative Metallography/Materialography

In short, quantitative metallography/materialography can be defined as the measure-
ment of microstructural parameters. This may be linear measurements when examin-
ing layer thickness, case depth, etc., or measurements of area, when analysis of volume
fraction or grain size is required.
Both manual quantitative methods, including measurements using point count-
ing screens or templates, and automatic image analysis are defined in a number of
standards.
17.1.1 Stereology–Table 17.1

Stereological methods are procedures used to characterize three-dimensional micro-
structural features based on measurements made on two-dimensional sectioning
planes.1
For the stereological calculations, the International Society for Stereology recom-
mends a number of symbols and notations. The most important are stated in Table
17.1.1,2
Basic Measurements
A number of the above-mentioned parameters are simple counting measurements that
are relatively easy to measure and are used in a number of equations 共see below兲.
565
TABLE 17.1—Principal Symbol and Combined Notations for Quantitative Metallography/Materialography.

Symbol Units Description Common Name
P ¯ Number of point elements or test points ¯
PP ¯ Point fraction (number of point elements per total number Point Count
of test points).
L mm Length of linear elements or test line length ¯
PL mm−1 Number of point intersections per unit length of test line ¯
LL mm/mm Sum of linear intercept lengths divided by total test line Lineal fraction
length
A mm2 Planar area of intercepted features or test area ¯
S mm2 Surface area or interface area, generally reserved for ¯
curved surfaces
V mm3 Volume of three-dimensional structure elements or test ¯
volume
AA mm2/ Sum of areas of intercepted features divided by total test Area fraction
mm2 area
SV mm2/ Surface or interface area divided by total test volume ¯
mm3 (surface-to-volume ratio)
VV mm3/ Sum of volumes of structural features divided by total test Volume fraction
mm3 volume
N ¯ Number of features ¯
NL mm−1 Number of interceptions of features divided by total test Lineal density
line length
PA mm−2 Number of point features divided by total test area ¯
LA mm/ Sum of lengths of linear features divided by total test area Perimeter (total)
mm2
NA mm−2 Number of interceptions of features divided by total test Area density
area
PV mm−3 Number of points per test volume ¯
LV mm/ Length of feature per test volume ¯
mm3
NV mm−3 Number of features per test volume Volumetric
density
L mm Mean linear interception distance, LL/NL ¯
A mm2 Mean area intercept, AA/NA ¯
S mm2 Mean particle surface area, SV/NV ¯
V mm3 Mean particle volume, VV/NV ¯
PP is the ratio P␣ / PT, where P␣ is the number of points that fall in the ␣-phase and
PT is the total number of test points 共see also below兲.
PL is the number of points of intersections generated per unit length of test line. An
intersection count is the number of boundaries between the matrix phase and the
phase or constituent of interest that are crossed by the lines of a test grid. For isolated
particles in a matrix, the number of feature intersections will equal twice the number
of feature interceptions. The total length of the test line is determined in advance to
facilitate calculations.
NL is the number of interceptions of features divided by total test line length. The
part of the test line superimposed on the feature constitutes the intercept. The number
of interceptions equals the number of particles 共or clusters of particles兲 of a phase or
Chapter 17 Quantitative 567
constituent of interest that are crossed by the lines of a test grid. For all microstructures
with more than a single phase, PL = 2 NL and for a single phase, PL = NL.
PA is the number of point features, such as grain boundary junctions, inside a given
area, divided by this area.
NA is the number of interceptions of features, such as grains or graphite nodules,
inside a given area, divided by this area.
See also ASTM Standard Terminology Relating to Metallography 共E 7兲 for stan-
dard stereological terminology definitions.
To obtain a true measurement, the instrument used must be calibrated 共see Sec-
tion 17.1.3兲.
Basic Equations
Based on the measurements mentioned above, a number of equations are developed
for covering the calculation of points, lines, areas, and volumes used for metall-
ographic/materialographic analysis. The most important measurements such as vol-
ume fraction, inclusion rating, etc., with the covering ASTM standards are described in
short below, and the relevant equations will be stated there.
Use of Comparison Charts and Grids

Comparison charts were developed for the evaluation of a given microstructure. An
example is the so-called JK charts 共developed by the Swedish Jernkontoret兲 depicting a
series of typical inclusion configurations 共size, type, and number兲 to be used for direct
comparison with the microscopical field in view. Comparison charts can be used also
for determination of volume fraction and grain sizes, but a grid is used normally 共see
the relevant standards below兲.
17.1.2 Specimen Preparation
Selection of Specimens
The selection of specimens, sampling, for quantitative analysis is very important be-
cause if the measured results are to be of value, the specimens must be representative
of the material that is being analyzed.
The number of specimens and the selection depends on the type of examination to
be performed. As described in ASTM Standard Practice for Calculating Sample Size to
Estimate, with a Specified Tolerable Error, the Average for Characteristic of a Lot or
Process 共E 122兲共see Section 12.4兲, random sampling should be performed.
As an example, the sampling procedure for the ASTM Test Method for Determin-
ing the Inclusion Content of Steel 共E 45兲, should be described in short: To obtain a rea-
sonable estimate of inclusion variations within a lot, at least six locations, chosen to be
as representative of the lot as possible, should be examined. For cases in which a defi-
nite location within a heat, ingot, or other unit lot is unknown, statistical random sam-
pling with a greater number of specimens should be employed. Very often the geometry
of the work piece plays a role; in examination of inclusions, the polished surface must
be parallel to the longitudinal axis of the product. In case of rolled or other hot worked
material, the microstructure to be measured will vary strongly according to the plane
of the prepared surface 共see also Section 2.1兲.
Reproducibility
It is very important that the specimen surfaces examined in quantitative metallo-
graphy/materialography are prepared with the highest degree of reproducibility; only
then can the measured results be compared. In case of manual image analysis, the op-
erator might be able to compensate for minor artifacts in the prepared microstructure,
but when using digital imaging equipment to delineate structures with image segmen-
tation, artifacts may be included in the measurements producing inaccurate results
共see below兲.
Preparation of the Specimen Surface

As a general rule the goal of specimen preparation is to consistently show the “True
Structure,” free of all artifacts. A specimen for automatic image analysis should also be
plane, without relief and edge rounding. All phases should be visible without smearing
or other artifacts; in inclusion rating even small scratches can disturb the measuring
共see Section 13.6兲.
Preparation of specimens suitable for quantitative analysis is described in Section
13.2.3 and in every quantitative standard under the jurisdiction of the ASTM Commit-
tee E-4 共see Section 12.4兲.
Etching
For a number of quantitative examinations, such as inclusion rating, etching should
not be used; the contrast developed obscures the features to be measured.
In other cases, etching has to be performed to obtain the contrast necessary to
show the structures of interest such as in steel grain size and banding measurements.
Reproducibility of the etching is very important in automatic image analysis so
that a uniform contrast can be developed. Variable and inconsistent etching will pro-
duce contrast irregularities which influence the measurements.
17.1.3 Calibration
Before making any measurement, it is essential to create calibrations for each instru-
ment 共microscope, video system, etc.兲 used to deliver an image. Calibration is the pro-
cess of establishing the graphical or mathematical relationship relating the desired
property 共expressed in a standard unit of measure such as ␮m兲 to the instrument out-
put 共instrument units such as filar divisions or pixels兲.
Although the operational requirements for equipment calibration differ widely,
the ASTM Standard Guide for Calibrating Reticles and Light Microscope Magnifica-
tions 共E 1951兲 provides an overview of calibration concepts and generalized calibration
procedures.
17.1.4 Field Selection—Bias

Quantitative measurement of a specimen surface will take place in microscopic fields
only representing a small part of the surface. To obtain a specific measurement accu-
racy, a number of fields must be examined. This number depends on the homogeneity
of the microstructure and the magnification. The higher the magnification observed
and the lower the homogeneity of the specimen, the higher the number of fields that
will be needed to accurately evaluate the microstructure, because at higher magnifica-
tion the area covered by the field is smaller and with a heterogeneous microstructure
the variations of the surface are higher. The number of fields is stated very often in the
specific standards. If not, the number should be calculated to obtain a reasonable rela-
tive accuracy.
As a rule, the fields should be placed randomly on the specimen surface. This can
be performed easily on an upright microscope, the specimen surface being visible 共see
Section 15.6兲. It is important that the operator does not look at the image when the
placement of the fields is decided on. This is the only way bias can be avoided.
17.2 Volume Fraction—Point Count

The volume fraction of a given phase or constituent in an alloy is one of the most impor-
tant and most common measurements in quantitative metallography/materialo-
graphy. This is because the amount of a second phase can have a strong influence on
the properties of the material.
The amount of a specific constituent 共second phase兲 is quantified by the volume
fraction. The volume fraction of a component ␣ is designated by VV, and is the ratio of
the volume of this component V␣ referred to the test volume VT 共total volume of the
specimen兲. This can be expressed:
VV = V␣/VT 共1兲
VV corresponds to the area fraction of the structural component ␣ that is visible
in the polished specimen surface and can be determined by planimetry. Because of
the valid relationship in the range of statistical scatter, AA 共area fraction兲 = LL
共lineal fraction兲 = PP 共point count兲, the volume fraction can also be determined from LL.
This is done by measurement of the fraction L␣ of a straight line LT that falls within the
component, or from the point fraction PP by counting the points P␣ of a point grid with
the point count PT that fall on the component. This can be expressed:
VV = V␣/VT = A␣/AT = L␣/LT = P␣/PT 共2兲

In ASTM Test Method for Determining Volume Fraction by Systematic Manual
Point Count 共E 562兲共see below兲, an efficient way for statistically estimating the volume
fraction of an identifiable constituent or phase from sections through the microstruc-
ture by means of a point grid, is described.
17.2.1 ASTM Test Method for Determining Volume Fraction by Systematic

Manual Point Count „E 562…
The test method may be used for all opaque materials 共see Section 12.4.3兲. The test
method is based on the stereological principle that a clear plastic test grid with a num-
ber of regularly arrayed points, when systematically placed over an image of a two-
dimensional section through the microstructure, can provide, after a representative
number of placements on different fields, an unbiased statistical estimation of the vol-
ume fraction of an identifiable component or phase. A grid of lines or curves is super-
imposed on a magnified image of a metallographic/materialographic specimen, and
the number of points falling within the microstructural component of interest is
counted and averaged for a selected number of fields. These points divided by the total
points in the grid is the point fraction PP 共see above兲. Based on PP the volume fraction
VV can be calculated.
17.3 Inclusion Rating

Inclusions can significantly influence the properties of a material. For this reason in-
clusion rating, especially of steel, is a very important quantitative method.
Inclusions can be exogenous like slag particles or indigenous, oxides, sulfides, sili-
cates, etc., developed in the material during the manufacturing process. Normally only
the indigenous inclusions, sulfides and oxides, are measured, quantifying the amount,
size, shape, and distribution. In a number of standards, ASTM E 45 共see below兲, SAE
J422a, and the German standard SEP 1570 共DIN 50602兲, the inclusions are determined
by using manual comparison chart methods based on volume fraction and point
counting. Since this involves a vast amount of counting time, image analyzers are often
used for inclusion rating 共see below兲.
17.3.1 ASTM Standard Test Method For Determining the Inclusion Content
of Steel „E 45…
ASTM E 45 covers a number of recognized methods for determining the nonmetallic
inclusion content of wrought steel.
The methods are both macroscopical and microscopical; only the latter shall be
shortly described here.
Comparison charts, mostly based on JK charts, as described above in this chapter,
are used. The inclusions are separated into four categories, A, B, C, and D and are
graded by calculating a severity level based on width and length 共for D types the count兲
of inclusions in 0.50 mm2 fields within a 160 mm2 specimen surface area. In Method A
共Worst Field兲 the inclusions are assessed qualitatively, seeking out and reporting only
the field with the highest severity rating. In Method D the length or count and the width
of inclusions are examined and the severity level of each inclusion type for each field of
view is determined and reported for a 160 mm2 specimen surface area. The Methods B
and C require that a specimen area be surveyed and inclusions greater than a certain
length and those of the maximum length be reported.
Manual performance of E 45 共especially Method D兲 involves much work to obtain
an acceptable measurement accuracy; therefore, the use of digital image analysis
equipment has become more common 共see Section 18.5.2兲.
17.3.2 ASTM Practice for Obtaining JK Inclusion Ratings Using Automatic

Image Analysis „E 1122… „withdrawn 2006, replaced by E 45…
This practice covers procedures to perform JK-type inclusion ratings using automatic
image analysis in accordance with microscopical methods A and D of E 45.
E 1122 is further described in Section 18.5.2.
17.3.3 ASTM Practice for Determining the Inclusion or Second-Phase

Constituent Content of Metals by Automatic Image Analysis „E 1245…
The practice describes a procedure for obtaining stereological measurements that
quantify basic characteristics of the morphology of indigenous inclusions in steels and
other metals using image analysis. The practice can be applied to provide such data for
any discrete second-phase constituent in any material.
ASTM E 1245 is further described in Section 18.5.2.
17.4 Grain Size

A very high number of metallographic/materialographic examinations are performed
to determine the grain size of the material; this parameter to a high degree influences
the material properties.
Three procedures for determining grain size are described in ASTM E 112 共see be-
low兲, the comparison procedure does not require counting of either grains, intercepts,
or intersections but only involves comparison of the grain structure to a series of
graded images. The planimetric procedure involves an actual point count of the num-
ber of grains within a known area, NA. NA is used to determine the ASTM grain size
number, G 共see below兲. The intercept procedure involves an actual count of the number
of grains intercepted by a test line or the number of grain boundary intersections with a
test line, per unit length of line, used to calculate the mean lineal intercept length, l. l is
used to determine the ASTM grain size number, G 共see below兲.
17.4.1 ASTM Test Methods for Determining Average Grain Size „E 112…
ASTM E 112 includes the comparison procedure, the planimetric procedure, and the
intercept procedures. The methods apply chiefly to single-phase grain structures in
metallic materials, but they can be applied to determine the average grain, crystal, or
cell size in nonmetallic materials like ceramics.
ASTM E 112 is a very comprehensive standard covering the earlier mentioned pro-
cedures, a description of the ASTM Grain Size Number, and a number of annexes de-
scribing how to establish the grain size for a number of materials.
ASTM Grain Size Number

This number, the G number, is defined as:
NAE = 2G−1 共3兲

where NAE is the number of grains per square inch at 100⫻ magnification. To obtain the
number per square mm at 1⫻, NA, NAE is multiplied by 15.50. The International Standard
Organization (ISO) and in several national standards, the metric grain size number, GM, is
based on the number of grains per mm2, at 1⫻, and this gives the equation:
NA = 8共2GM兲共4兲
The metric grain size number, GM, is a little lower than the ASTM grain size num-
ber, G, for the same microstructure:
G = GM + 0.046 共5兲
Comparison Procedure
The comparison procedure, as mentioned above, does not require counting of grains,
intercepts, or intersections, but involves comparison of the grain structure to a series of
graded images, either in the form of a wall chart, clear plastic overlays, or an eyepiece
reticle. Experience has shown that unless the standard image reasonably well ap-
proaches that of the specimen, errors may occur. To minimize such errors, the com-
parison charts are presented in four categories: Plate I—Untwinned grains 共flat etch兲
1 1 1 1 1 1 1 1 1
includes grain size numbers 00, 0, 2 , 1, 1 2 , 2, 2 2 , 3, 3 2 , 4, 4 2 , 5, 5 2 , 6, 6 2 , 7, 7 2 , 8, 8 2 , 9,
1
9 2 , 10, at 100⫻. Plate II—Twinned grains 共flat etch兲 includes grain size numbers 1, 2, 3,
4, 5, 6, 7, 8, at 100⫻. Plate III—Twinned grains 共contrast etch兲 includes nominal grain

diameters of 0.200, 0.150, 0.120, 0.090, 0.070, 0.060, 0.050, 0.045, 0.035, 0.025, 0.020,
0.015, 0.010, 0.005 mm at 75⫻. Plate IV—Austenite grains in steel 共McQuaid-Ehn兲 in-
cludes grains size numbers 1, 2, 3, 4, 5, 6, 7, 8, at 100⫻. As an example, Plate III is used
for twinned copper and brass with a contrast etch.
Repeatability and reproducibility of comparison chart ratings are generally ±1
grain size number.
Planimetric Procedure
As mentioned above, the planimetric procedure, also called Jeffries’ procedure, in-
volves an actual count of the number of grains within a known area 共circle or rect-
angle兲. The number of grains per unit area, NA, is used to determine the ASTM grain
size number, G. The precision of the method is a function of the number of grains
counted, and a magnification shall be selected which gives at least 50 grains in the field
to be counted 共a minimum of three fields兲. When the counting is done, the figure is mul-
tiplied by Jeffries’ multiplier, f, that is a factor relating to the magnification used, M.
The number of grains per square mm at 1⫻, NA is calculated from:
NA = f共NInside + NIntercepted/2兲共6兲
where f is the Jeffries' multiplier taken from a table in the standard, NInside is the number
of grains completely inside the test circle and NIntercepted is the number of grains that inter-
cept the test circle.
A precision of ±0.25-grain size units can be attained with a reasonable amount of
effort. Results are free of bias and repeatability and reproducibility are less than
±0.5-grain size units. An accurate count does require marking off the grains as they are
counted.
Intercept Procedure
The intercept procedure, also called Heyn’s procedure, is more convenient to use than
the planimetric procedure. With the intercept method an accurate estimate of the grain
size can be obtained in a fraction of the time used with the planimetric method. As
mentioned above, the intercept method involves an actual count 共at least 50 intercepts兲
of the number of grains intercepted by a test line or the number of grain boundary in-
tersections with a test line, per unit length of test line, used to calculate the mean lineal
intercept length, l−. l− is used to determine the ASTM grain size number, G.
The precision of the method is a function of the number of intercepts and intersec-
tions counted. An intercept is a segment of test line overlaying one grain. An intersec-
tion is a point where a test line is cut by a grain boundary. Experiments have shown that
a test pattern consisting of three concentric and equally spaced circles having a total
circumference of 500 mm gives satisfactory results. Based on the calculation of the
number of intercepts, NL and the number of intersections, PL, the mean lineal intercept
value for each field, l can be calculated:
l = l/NL = 1/PL 共7兲

A precision of better than ±0.25-grain size units can be attained with a reasonable
amount of effort. Results are free of bias; repeatability and reproducibility are less than
±0.5-grain size units. Because an accurate count can be made without the need of
marking off intercepts and intersections, the intercept method is, as mentioned, faster
than the planimetric method for the same level of precision.
ASTM E 1382 describes determining average grain size using semiautomatic and
automatic image analysis 共see below兲.
17.4.2 ASTM Test Methods for Estimating the Largest Grain Observed in a
Metallographic Section „ALA Grain Size… „E 930…
Commercial material specifications sometimes include, in size limits for grain struc-
tures, the need for identification of the largest grain observed in a sample, often ex-
pressed in ALA 共as large as兲 grain size. ASTM E 930 is used when the number of large
grains is too few for measurement with ASTM E 112.
The test methods are simple manual procedures, using comparison and measur-
ing. The measuring procedure is recommended for greater accuracy.
17.4.3 ASTM Test Methods for Characterizing Duplex Grain Sizes „E 1181…
The above-mentioned test methods for determination of average grain size covers ma-
terials assumed to contain a single log-normal distribution of grain sizes. ASTM E 1181
is set forth to characterize grain size in products with any other distributions of grain
size. The term “duplex grain size” is chosen to describe any of these other distributions
of grain size, because of its common usage and familiarity. However, the use of that
term does not imply that only two-grain size distributions exist.
Duplex grain size may occur in some metals and alloys as a result of their thermo-
mechanical processing history, and these methods are made for these materials, but
they can also be used for other materials with a similar microstructure. Duplex grain
structures 共for example, multiphase alloys兲 are not necessarily duplex in grain size, and
as such not covered by these methods.
The test methods use a comparison procedure, a point count procedure based on
ASTM E 562 共see above兲, a planimetric procedure, and a direct measurement pro-
cedure.
17.4.4 ASTM Test Methods for Determining Average Grain Size Using
Semiautomatic and Automatic Image Analysis „E 1382…
These test methods may be used to determine the mean grain size, or the distribution of
grain intercept lengths, or areas in metallic and nonmetallic polycrystalline materials.
The methods may be applied to specimens with equiaxed or elongated grain structures
with either uniform or duplex grain distribution. Either semiautomatic or automatic
image analysis devices may be utilized to perform the measurements.
The semiautomatic procedure is based on a digitizing tablet with a measurement
resolution of at least 0.1 mm. A variety of approaches can be employed: The simplest is
to fix a photograph to the tablet surface and place a suitable grid over the photograph,
tape down the corners of the grid, and use the cursor, fitted, with fine cross hairs, to
measure the appropriate features. Alternatively, the grid can be placed on an eyepiece
reticle. The cursor is moved over the table surface and the microscopist can see the
illuminated cross hairs in the cursor through the eyepieces over the field of view and
grid pattern. A third approach is to transfer the microstructural image, the test grid
image, and cursor image to a television monitor. The microscopist moves the cursor
across the tablet surface while watching the monitor to make the appropriate measure-
ments.
The automatic procedure is described in Section 18.5.3.
17.5 Banding
A banded microstructure is caused by segregation that occurs during the dendritic so-
lidification of metals and alloys and is aligned by subsequent deformation. Solid-state
transformations may be influenced by the resulting microsegregation pattern leading
to development of a layered or banded microstructure. The most common example of
banding is the layered ferrite-pearlite structure of wrought low-carbon and low-carbon
alloy steels. Other examples of banding include carbide banding in hypereutectoid tool
steels and martensite banding in heat-treated alloy steels.
Microstructural banding influences the uniformity of mechanical properties of
the material, and ASTM E 1268 describes a number of procedures for testing of banded
microstructures.
17.5.1 ASTM Practice for Assessing the Degree of Banding or Orientation

of Microstructures „E 1268…
This practice describes a procedure to qualitatively describe the nature of banded mi-
crostructures and stereological procedures for quantitative measurement of the degree
of microstructural banding or orientation. The practice also includes a procedure us-
ing microindentation hardness testing. Only the stereological procedure will be dis-
cussed here.
The stereological measurements are made on an etched specimen by superimpos-
ing a test grid 共consisting of closely spaced parallel lines of known length兲 on the pro-
jected image of the microstructure or on a photomicrograph. Measurements are made
with the test lines parallel and perpendicular to the deformation direction.
The stereological measurements may be made using a semiautomatic tracing type
image analyzer. The test grid is placed over the image projected onto the digitizing tab-
let and a cursor is used for counting. For certain microstructures where the contrast
between the banded or oriented constituents is adequate, an automatic image analyzer
may be used for counting 共see Section 18.5.4兲.
17.6 Porosity in Thermal Spray Coatings

Thermal spray coatings are susceptible to the formation of porosity due to a lack of
fusion between sprayed particles or the expansion of gases generated during the spray
process. The determination of area percent porosity is important to monitor the effect
of variable spray parameters and the suitability of a coating for its intended purpose.
Depending on application, some or none of this porosity may be tolerable. In Test
Methods for Determining Area Percentage Porosity in Thermal Sprayed Coatings 共E
2109兲, two methods are indicated for the determination of the porosity 共see below兲.
17.6.1 ASTM Test Methods for Determining Area Percentage Porosity in

Thermal Sprayed Coatings „E 2109…
These test methods cover the determination of the area percentage porosity of thermal
sprayed coatings. Method A is a manual, direct comparison method using seven stan-
dard images shown on figures in the standard. These figures depict typical distribu-
tions of porosity in thermal spray coatings. Method B is an automated technique re-
quiring the use of a computerized image analyzer 共see Section 18.5.1兲. The methods
quantify area percentage porosity only on the basis of light reflectivity from a metallo-
graphically polished cross section. In ASTM Guide E 1920 共see Section 12.4.3兲, a num-
ber of preparation procedures are recommended 共see also Material/Preparation Tables
12–15兲.
17.7 Decarburization—Case Depth—Coatings

The measurement of thickness 共depth兲 of surface phenomena like decarburization,
carburizing, nitriding, and coatings 共surface layers兲 is a common metallographic/
materialographic procedure. Normally a specimen is prepared and examined in an op-
tical microscope using an ocular micrometre reticle or other measuring instrument
共see below兲. The automatic image systems are also able to measure these surface phe-
nomena 共see Section 18.5.5兲.

For all measurements on layers, etc., mentioned above, the quality of the prepared
specimen is of utmost importance. The plane of the cross section must be perpendicu-
lar to the plane of the surface phenomenon to secure measurement of the true thick-
ness. The preparation must be performed so that the specimen surface is flat without
edge rounding and the surface shall be without artifacts such as smearing of a softer
coating. For correct preparation see Table 11.1 and Section 13.5/6.
17.7.2 ASTM Test Methods for Estimating the Depth of Decarburization of

Steel Specimens „E 1077…
These test methods cover procedures for estimating the depth of decarburization of
steels irrespective of the composition, matrix microstructure, or section shape. The fol-
lowing basic procedures may be used: Screening methods, microscopical methods, mi-
croindentation hardness methods, and chemical analysis methods. Only the micro-
scopical methods will be discussed here.
Microscopical methods are most suitable for measuring the depth of decarburiza-
tion of as-hot rolled, as-forged, annealed, or normalized specimens. These methods
can also be applied to heat-treated specimens, although with less certainty in deter-
mining the maximum affected depth. Spheroidized-annealed or cold-worked speci-
mens can also be evaluated, but detection of structural variations due to decarburiza-
tion is more difficult than with hot-worked or fully annealed structures. Measurement
is done on an etched specimen and based on evaluation of the variation in the micro-
structure at the surface due to change in carbon content.
Measurements are made on a microscope using an ocular reticle, a screw 共Filar兲
micrometre ocular, or with a scale placed against a ground glass projection screen.
For use of automatic image analysis see Section 18.5.5.
17.7.3 Case Depth

The measurement of the often very thin zone developed by carburizing, nitriding, etc.,
is done in much the same way as decarburization and coatings 共see below兲. The speci-
men preparation can be difficult because the often very hard zone will create problems
with the planeness of the specimen 共see above兲. For very low depths, taper sectioning
may be used 共see Section 3.11.1兲.
For the use of automatic image analysis see Section 18.5.5.
17.7.4 ASTM Test Method for Measurement of Metal and Oxide Coating
Thickness by Microscopical Examination of a Cross Section „B 487…
This test method covers measurement of the local thickness of metal and oxide coat-
ings by the microscopical examination of cross sections using an optical microscope.
Under good conditions, when using an optical microscope, the method is capable of
giving an absolute measuring accuracy of 0.8 ␮m.
A carefully prepared specimen 共cross section兲 is used 共see above兲. A special prob-
lem when preparing specimens with soft coatings is embedded abrasives 共see Section
13.5/6兲.
The measuring device may be a screw 共Filar兲 micrometre ocular or a micrometre
eyepiece. An image splitting eyepiece is advantageous for thin coatings on rough sub-
strate layers. The measuring device shall be calibrated at least once before and once
after the measurement using a stage micrometre. The magnification should be chosen
so that the field of view is between 1.5 and 3⫻ the coating thickness.
17.7.5 ASTM Test Methods for Thickness of Diffusion Coating „C 664…

These test methods cover two procedures for measuring the thickness of diffusion
coatings.
Method A is the determination of the difference in the thickness of the part before
and after coating.
Method B is the determination of total coating thickness, defined as the distance
between the observably unaffected substrate and the exterior surface of the coating.
The total coating thickness is determined by cross-sectioning the coating, preparing a
metallographic/materialographic specimen, and microscopically measuring the coat-
ing thickness.
17.8 Other ASTM Standards for Quantitative Materialography

Below follows the designations of a number of ASTM standards relating to quantitative
metallography/materialography. For further information see the Document Summa-
ries in Section 12.4 共the CD-ROM included with this manual兲.
For other standards 共ISO, DIN, BSI, etc.兲 see Appendix I.
ASTM Practice for Petrographic Examination of Hardened Concrete 共C 856兲
ASTM Test Method for Quantitative Analysis of Textiles 共D 629兲
ASTM Test Method for Fiber Analysis of Paper and Paperboard 共D 1030兲
ASTM Test Method for Microscopical Determination of the Reflectance of Vitrin-
ite in a Polished Specimen of Coal 共D 2798兲
ASTM Practice for Calculating Sample Size to Estimate, with a Specified Tolerable
Error, the Average for Characteristic of a Lot or Process 共E 122兲
18
Automatic Image Analysis
18.1 Introduction
THE NEED TO CONSIDER DIGITAL IMAGING SYSTEMS IS PREDICATED ON
recognition of stereological principles and quantitative metallography/materialo-
graphy as essential concepts in materials science. The application of quantitative
metallography/materialography in materials science requires the measurement of mi-
crostructures. It may be argued that the study of materials cannot be termed a “sci-
ence” if it does not use quantitative methods.
Equipment using digital imaging technology is not essential to the implementa-
tion of quantitative metallographic/materialographic methods. Quantitative metallo-
graphy/materialography can be practiced using nondigital methods 共see Chapter 17兲.
Digital imaging technology is applied to materials science to expeditiously pro-
duce the structural measurements required by quantitative metallographic/materialo-
graphic standards. Performing image analysis is not a goal; rather it is a means of
achieving a goal. To hear a laboratory technician or manager discuss the need to “do
image analysis” is disturbing. What actually needs to be performed in a materials sci-
ence laboratory is the measurement of microstructures, i.e., quantitative metallo-
graphy/materialography. The required products of quantitative metallography/
materialography are the measured dimensions of microstructural features, numerical
values that describe the physical extent of the structures. The goals of quantitative
metallography/materialography can be more easily achieved through the use of digital
image measurement technologies to simplify and maximize control of the measure-
ment process. In the most basic sense an image analysis system is nothing more than a
gage; principally no different than a micrometre, scale, or other device used to extract
physical dimensions from any object. An image analysis system is nothing more than a
tool designed to deliver digital images, extract the structural measurement data re-
quired by quantitative metallography/materialography and, as a bonus, process and
manage the data. Primarily, such a system offers the possibility of making accurate and
reproducible measurements of microstructural features. The availability of relatively
inexpensive digital imaging equipment greatly facilitates the extraction of data from
microstructural images as well as producing data that are immediately ready to be
stored and analyzed using a wide variety of common information management tools.
18.2 Qualitative and Quantitative Metallography/

Materialography
18.2.1 The Transition to Quantitative Standards
The barriers to implementing quantitative methods are primarily the continued exis-
tence of qualitative standards; lack of cost effective and efficient instrumentation; and
perhaps most significantly, the existence of procedural obstacles. Bringing rigorous
quantitative methods to metallography/materialography necessitates the existence of
specifications and standards requiring these methods, the equipment and operational
577
procedures to produce the results specified in the standards, and, finally, the organiza-
tional desire to institute these methods.
Nearly all of the more recent standard test methods produced by ASTM Interna-
tional, as well as other standards organizations and private industry, are quantitative in
nature and require the actual measurement of structural features rather than the tradi-
tional chart comparison or other subjective methods. New standards generally tend to
eliminate the use of chart comparison and rating or indexing schemes. Instead they
report the actual measured values for length, width, area, etc., as well as appropriate
statistical values. In many cases, the quantitative standard actually simplifies the test
method.
The equipment necessary to perform the operations required by quantitative
methods is readily available. In addition to a microscope, the components needed to
assemble an image analysis system generally include: computer with monitor, camera,
and printer. Early implementations of image analysis systems required specialized and
relatively expensive hardware components. Fortunately, the exponential rise in con-
sumer use of computers and digital cameras has benefited the use of image analysis in
materials science. Many of the technologies used in consumer imaging products are
directly transferable to microstructural image analysis systems. For example, the
availability of mass-produced personal computer components and image sensor chips
have resulted in dramatically lower system hardware costs.
A certain symbiosis exists between the advancement of digital imaging component
technology and the propagation of quantitative standards. Technological develop-
ments and component cost reductions have facilitated the adoption of more quantita-
tive standards by virtue of easing the efforts and costs of implementing the standards.
Conversely, the increased number of quantitative standards has expanded industry de-
mand for more efficient and cost-effective systems to perform the measurements incor-
porated in these standards.
Perhaps the most significant remaining barrier to the use of quantitative methods
is organizational 共procedural兲 in nature. While the imprecision and the shortcomings
of nonquantitative methods are widely recognized, there remains in many metallo-
graphic/materialographic laboratories a strong inertia slowing the adoption of new
standards. The advancement of quantitative materials science often suffers from a bur-
densome process of new standards approval. In many organizations the effort required
to secure organizational approval of new standards is difficult, tedious, and presents a
formidable barrier to what is technically and logically obvious. None the less, quantita-
tive methods and standards are gradually replacing qualitative procedures, driven by
the issuance by industry leaders, both public and private, of quantitative standards and
the constantly improving price/performance ratio of the equipment necessary to con-
veniently implement the standards.
18.2.2 Structure, Stereology, and Statistics

What structural parameters should be quantified? Physical metallurgy and the study of
microstructure property relationships provide the answers. An obvious problem is that
the preparation of materials for microscopic observation and quantification yields a
planar, two-dimensional surface on which three-dimensional phase and structural fea-
tures are displayed in some cross-sectional views. The solution lies in the body of ste-
reological principles that provide a scientific basis extrapolating planar measurement
data to yield valid volumetric material structure information.1 The physical extent of
microstructures as shown by metallographic preparation including feature number,
Chapter 18 Automatic Image Analysis 579
length, width, and area, are the primary structural dimensions of importance. Nearly
all standards for the measurement of materials microstructures call for the determina-
tion of some or all of these parameters. Several other measurements are sometimes
required including perimeter as well as calculated data such as percent area, density,
distance from a surface, aspect ratio, and shape factor. For most quantitative standards
the data extraction requirements are very basic. Commonly, in the implementation of
quantitative standards using image analysis software, far more effort is required in the
processing of the measurement data to provide reporting in the format required by the
standard. This situation is particularly encountered when translating the older qualita-
tive standards 共for example, ASTM Standard Test Method for Determining the Inclu-
sion Content of Steel 共E 45兲兲 that rely on rating or other manipulations to produce re-
sults expressed as an index or relative value rather than as stereological data.
An extremely important aspect of quantitative standards is the role of statistical
concepts. Not only is the validity of stereological principles predicated on meeting cer-
tain statistical conditions, but the results to be calculated also consist almost entirely of
statistical parameters, such as mean standard deviation and confidence interval. It is
vital that the laboratory personnel who are engaged in the performance and use of
quantitative methods have a basic understanding of statistical concepts in order to ob-
tain accurate results.
This chapter will cover the basic elements of image analysis systems and their
practical application to several of the most common quantitative standards. The sec-
tions below present an overview of image analysis functions that are frequently found
to be useful in quantitative metallography/materialography. This overview is not de-
signed to be a detailed examination of the vast array of image processing functions. For
a thorough discussion of many of these processing functions see the work of John C.
Russ.3
18.3 Principles of Digital Imaging

18.3.1 What is Digital Image Analysis?
Because the terminology used in describing digital imaging equipment and systems is
confusing, often ambiguous, and because of rapid changes in technology, prone to
short-term obsolescence the discussion that follows minimizes reference to specific
components.
How is digital image analysis applied to materials science? Image analysis is a set
of software functions that can be used to extract quantitative data from microstruc-
tural images. Digital imaging technology integrated into a “system” is used as a tool to
provide the measurement of microstructures as required by quantitative methods.
Employing the power of digital imaging technology, the extraction of data is accom-
plished in a more timely and efficient manner.
18.3.2 Image Acquisition

Generally an image of materials microstructure consists of a rectangular or square
area showing physical structure 共voids or grain boundaries兲 or material phases embed-
ded in a matrix. In most cases the objective of quantitative analysis is to measure the
physical extent of the structure or phase, most commonly length, width, or area. In
doing so it is necessary to remove the matrix portion of the image from consideration.
For this reason all of image processing is essentially a data reduction problem. Even for
a standard NTSC format camera the number of pixels in an image is 307 200. Every
step in the image acquisition and processing is performed with the objective of remov-
ing pixels representing matrix material information from consideration. Ironically
the large format digital cameras capable of delivering images having more than
1 000 000 pixels 共one mega pixel兲 provide an even greater amount of data that must be
eliminated to produce the quantitative information required. The argument can be
made that more pixels are not always a benefit in the extraction of measurements from
materials microstructure. Very little work has been done on identifying the level on
imaging digitization that is optimal for the data extraction job at hand. The assump-
tion that more pixels are better is not a universal truth, i.e., it should not be applied to
all analysis situations. Rather, the minimum number of pixels needed to quantify the
structure, based on the requirements of the standard should be taken into account
when selecting a camera. The more image data captured beyond that required to pro-
vide the measurement tolerances required by the standard, the more elaborate and,
therefore, more exposed to error the image processing 共data reduction兲 will be.
18.3.3 Image Digitization—Gray Scale

Digitization is the process of converting a continuous scene 共microscopic field of view兲
into a block of numerical values 共a number of horizontal rows and a number of vertical
columns兲. Individual units in the rows and columns are picture elements 共pixels兲. Pix-
els are the basic unit of digital images. Pixels have a location within the image. X is the
horizontal position and Y is the vertical position. Each pixel also has a brightness, illu-
mination intensity, or color value. These numerical values associated with each pixel
constitute a digital image. After a structural field of view has been digitized, all image
processing and measurement is based on the quantitative values of each pixel. A dis-
cussion of the details of image digitization can easily fill a volume, but an in-depth
knowledge of the technology is not necessary. See the excellent work of Inoue and
Spring for a detailed discussion of image digitization.4
The X, Y positional information associated with a pixel is straightforward. The
pixels into which the image is divided form an array or grid. The relative position of
each pixel within the overall grid 共image兲 can be expressed as a coordinate location.
Once a calibration has been established the position of each pixel can be expressed as a
real distance from the coordinate system origin or from any other point 共pixel兲 in the
array. The least common denominator for an image pixel array as produced from an
NTSC standard video camera has dimensions of 640 pixels in each horizontal row and
480 pixels in each vertical column. A so-called mega pixel image has upwards of 1000
horizontal by 1000 vertical pixels.
The third value possessed by every pixel is a measure of its illumination level. This
value is a quantification of the relative amount of light found at that location of the
image. The range of values possibly varies and is dependent on technical specifications
of the camera and digitizing components used to perform digitizing. In digitizing the
total range of illumination from no light 共pure black兲 to the maximum amount of light
共pure white兲 is divided into an equal number of levels. Commonly, an image from a
monochrome camera is digitized into 256 distinct levels, beginning with 0 for no light
up to a maximum of 255 for the maximum amount of light. In this scheme every level of
illumination has a value from 0–255. This range of digital illumination values is called
the gray scale. A gray scale having a range of from 0–255 is an 8-bit gray scale, since a
digital computer represents numbers as “bits” and to count to 255 requires 8 bits. Im-
age illumination may be digitized into ranges other than 0–255. The wider the range of
Fig. 18.1a—Base line image.
digital illumination levels, the more bits are required to count them. The number of
bits used in digitizing illumination is called the bit depth. To digitize a true color image
requires at least 24 bits and produces a total of 16.7 million possible illumination 共or
color兲 levels.
18.3.4 The Histogram

Digitization of the illumination levels within a microstructural field of view is in fact a
measurement of the illumination. Taken together, the pixel illumination measure-
ments show a pattern of variation representing the various phases and structures
within the image. By counting the number of pixels at each illumination value in a digi-
tized image, an illumination frequency distribution can be produced. The frequency or
quantitative distribution is a basic statistical method for summarizing data. Once a
microstructural field of view has been digitized its distribution of illumination values
can be viewed graphically by constructing a histogram.5 The typical image illumina-
tion histogram uses the gray scale range as the horizontal, X axis, and the count of pix-
els falling into each of the gray scale levels as the vertical, Y axis. In fact, the frequency
distribution of illumination presents the raw image data upon which all image process-
ing is based and from which all materials structure measurements are extracted. If the
structural features to be measured are not represented in the initial raw data of the
illumination quantitative distribution, then measurement of those features will not be
possible. The shape and position of the illumination histogram provides important in-
formation about the brightness, contrast, and measurability of the image.
18.3.5 The Effects of Brightness and Contrast on Illumination Distribution

The effects of different illumination 共brightness兲 levels on quantitative distribution can
be seen as measurability by considering the example of an image of a thermally
sprayed coating structure digitized to a depth of 8 bits, having a possible range of mea-
sured illumination values of 0–255 共displayed in Fig. 18.1共a兲兲.
A histogram of the pixel brightness distribution of this field of view is shown at the
right in Fig. 18.1共b兲. Digitized pixel brightness values are shown on the horizontal X
axis beginning with a value of 0 at the left end of the axis. The vertical Y axis shows the
number of pixels at each gray scale value. An inspection of the distribution reveals sev-
eral things. First, notice that this distribution is approximately normal; it has the shape
of the classic “bell” curve of a normal distribution. There is also a small but prominent
Fig. 18.1b—Base image illumination.
“spike” or relatively high number of pixels at the 0 or black gray scale level. Addition-
ally, the majority of the brightness measurements are clustered somewhat to the right,
or bright end of the distribution, at around the 180 level. To show the effects of a change
in illumination levels on the resultant distribution, the brightness level was decreased
by 15 % for the same field of view. The image and its associated histogram are shown in
Fig. 18.2.
Notice that the distribution is basically the same shape but it has shifted to the left
or darker end of the scale and that the most frequent illumination value is now approxi-
mately 140. Also, the number of pixels at the 0 illumination level has increased nearly
three times.
Next the image brightness level was increased by 15 %. The average brightness
level of the resultant image is approximately 213 and the brightest areas within the im-
age have been set to 255, the highest possible level 共saturation兲. Note in Fig. 18.3 that
the distribution is shifted so far to right end of scale that a portion of the distribution
has been clipped. This means that at the higher illumination levels some data repre-
senting the brightest structural features have been lost. In most cases the loss of raw
image illumination data due to excessive or insufficient image brightness should be
avoided.
Fig. 18.2a—Brightness decreased.

Fig. 18.2b—Histogram shifted left.
Now let us examine the effects on the image illumination distribution of changes
to the field of view contrast. Contrast is a measure of the range of illumination values
Fig. 18.3a—Brightness increased.
Fig. 18.3b—Histogram shifted right.

Fig. 18.4a—Contrast decreased.
between the darkest and lightest areas within the field of view. Again, referring to the
distribution shown in Fig. 18.1共a兲, the range of brightness values extends across the
entire 0–255 gray scale range. The result of decreasing the contrast by 10 % is displayed
in Fig. 18.4共a兲.
Notice in Fig. 18.4共b兲 that the range of illumination values has been reduced and
the distribution no longer fills the gray scale with the lowest value somewhat above 0
and the highest values somewhat below the 255 maximum. A decrease in contrast has
the effect of compressing the illumination distribution. Increasing the contrast by 10 %
produces the image and distribution displayed in Fig. 18.5.
In this case, the distribution range has been expanded or stretched. Note the gaps
in the bars plotted in Fig. 18.5共a兲, indicating that after increasing contrast some illumi-
nation levels are not present in the image. See more on “stretching” in the Image Pro-
cessing section of this chapter. Based on these examples, several generalizations can be
made about the optimal illumination conditions for extracting measurement data
from digital images. First, the illumination 共brightness兲 level selected for the image
should provide the broadest possible range of values in the distribution histogram
while avoiding clipping at either end of the gray scale. Also the contrast level should be
selected to maximize the range of illumination values present in the gray scale distribu-
Fig. 18.4b—Distribution decreased.

Fig. 18.5a—Contrast increased.
tion. The reason for seeking these conditions is simply to create an image that provides
the maximum amount of raw data to be used to define and measure the material micro-
structure.
Controlling illumination is essential. And while image processing software in-
cludes many powerful methods for altering digital image brightness and contrast,
these mathematical techniques must be considered as secondary tools. The primary
and most powerful control for controlling microstructure illumination is the micro-
scope or metallograph used to obtain the images. No software alteration of image illu-
mination characteristics should be undertaken prior to a thoughtful use of microscope
illumination controls including illumination level, aperture, filtering, etc., to produce
an image possessing the illumination conditions optimal for the intended use of the
image. During the process of setting illumination conditions with the microscope the
operator may quickly digitize candidate images and use the imaging software to dis-
play a distribution histogram. A series of microscope illumination adjustments should
be made and checked by viewing the histogram until the illumination distribution is
optimized. Only after such a process should additional software illumination adjust-
ment be undertaken if necessary.
The state of the image illumination distribution along with the intended uses of
Fig. 18.5b—Distribution stretched.

the digitized image determines what, if any, image processing can or should be
performed.
18.3.6 Image Processing and True Microstructure

The phrase image processing describes a wide range of operations, implemented by
software programs and designed to transform a digital image into another image by
performing one or more mathematical calculations upon the image pixel data. There is
only one goal in applying any image processing function and that is to produce an im-
age that more clearly represents the microstructure of interest. To achieve this single
result, image processing functions are commonly used in microstructural images for
the removal of artifacts that obscure the image structures of interest and to enhance or
exaggerate image structures so as to maximize the possibility of uniquely delineating
共and therefore more accurately measuring兲 the structures.
The goals of image processing should be identical to those of materialography, that
is, to produce a visible microstructure with no artifacts that is the truest possible depic-
tion of the material structure for the intended purpose. The application of modern con-
trolled metallographic/materialographic processes results in observable microstruc-
tures that optimally reveal the material structural or phase constituents, or both.
Consequently, materialography or metallography is actually the most powerful image
processing tool available, in that the mechanical or chemical processes employed are
designed to physically produce “true microstructure,” whereas software-based image
processing relies on mathematical calculations performed upon an image to produce a
new image displaying a structure which in fact does not exist physically.
All applications of image processing will alter the image illumination distribution.
Therefore, any image that exists as the result of image processing is not “true micro-
structure.” Such an image is not necessarily bad. But recognizing this simple truth
leads to the inescapable conclusion that in all cases electronic image processing should
be strictly limited to only those operations without which the original image would
remain unmeasureable or for purposes of human visualization to enhance the struc-
ture visibility. In regard to quantitative materials science, image processing operations
should be applied only in so far as they render the image more measurable or more
viewable. So the application of image processing processes is determined by the state
of the real world image and the use to which the digital image is to be put. In furthering
the purpose of materialography or metallography, that is to reveal microstructure for
subsequent measurement or examination, digital image manipulation is nothing more
than another process for materials specimen preparation. Digital 共image兲 preparation
should be used as a secondary class of techniques to be applied only if the primary class
共physical metallographic/materialographic methods兲 has failed to provide the required
structural visibility.
There are a very large number of image processing functions available in most im-
age analysis software products. Of the many possible image processing operations a
relatively few provide useful results in preparation of materials microstructure images.
Presented here is a short list of several image processing functions that are frequently
applied to improving microstructural images. For an extensive discussion of many
more image processing techniques see Russ.3
Background Correction
A common artifact resulting from poor microscope illumination alignment is observ-
able as bright or dark areas within the image. Background correction is an image pro-
Fig. 18.6a—Unevenly illuminated image.
cessing program that is used to reduce uneven image illumination due to misalignment
of microscope lighting. Microscope illumination alignment must always be centered.
All possible physical positioning and optical path alignment adjustments must be
made to the microscope or metallograph prior to performing software-based back-
ground correction. A common method of software background correction performs a
subtraction of a poorly illuminated image with a second copy of the same image show-
ing only the background. The background-only image can be produced by digitizing an
image of a uniform white surface or by defocusing the optics to obliterate all image
features. A background correction operation yields a resultant image that has been cor-
rected. The images in Fig. 18.6 illustrate this process.
Figure 18.6共c兲 clearly shows that the dark edge seen in Fig. 18.6共a兲 has been re-
moved by the background correction. Also note that several dust particles present
within the lenses of the microscope or camera used to capture the image are visible in
both Fig. 18.6共a兲 and 18.6共b兲 and have been removed by the correction software. A side
effect or artifact of the background correction process is that the right edge of the im-
age is now slightly brighter than the balance of the image. It is a near universal truth
that the application of image processing functions seldom provides results that are
wholly without artifacts. The existence of some degree of nonuniform image illumina-
Fig. 18.6b—Background only copy of Fig. ???

Fig. 18.6c—Resultant image after applying background correction.
tion may be acceptable provided it does not interfere with the measurement of the
structures of interest.
Contrast Stretching
Once digitized the image brightness and contrast may be altered using image process-
ing software. Again, it is important to use the illumination controls found on the imag-
ing system microscope being able to optimize image brightness and contrast before
resorting to software processing functions. Adjustments to brightness and contrast
should always be performed to increase the amount of illumination data available. See
Section 18.3 for examples of brightness and contrast changes to the amount and range
of data in the digitized image.
Stretching techniques increase image contrast by expanding the brightness values
found in the original image into a wider range of values. Stretching is generally applied
to images that display a narrow range of illumination levels in their initial digitized
state. One approach to stretching determines the minimum and maximum illumina-
tion levels within the image and mathematically extrapolates these values to cover the
maximum possible range, 256 values in an 8-bit gray scale image, as seen in Fig. 18.7.
Notice that there are no 0 or 255 brightness level pixels within the image 共extreme
left and right ends of the distribution in Fig. 18.7共a兲兲. Figure 18.7共b兲 displays the same
image after applying a contrast-stretching program to radically expand the illumina-
tion range 共contrast兲. In addition to increasing contrast across the entire image illumi-
nation range, it is possible to increase the contrast within a specific part of the illumina-
tion range. Stretching of this type may be helpful if several material phases have nearly
contiguous or slightly overlapping illumination ranges. This enhancement is per-
formed by dividing the histogram into three sections: brightness values that have a
value below a dark-end threshold 共some value greater than the minimum illumination
values in the image兲; brightness values above a bright-end threshold 共some illumina-
tion level less than the maximum兲; and brightness values lying between the dark and
bright thresholds. brightness values that lie below the dark threshold are assigned a
new value of 0. Similarly, values that lie above the bright threshold are assigned a value
of 255. The remaining values between the dark and bright threshold are assigned new
brightness levels between 0 and 255, according to a linear mathematical extrapolation
and are thereby stretched slightly to provide a calculated set of structural brightness
levels. The histograms in Fig. 18.8 display the effects of this type of stretching.
Fig. 18.7a—Narrow illumination range.
This form of histogram stretching eliminates low and high pixel brightness values
that do not represent the structures of interest by setting them to 0 or 255. Notice the
high pixel counts at the extreme ends of the distribution.
Fig. 18.7b—Entire range stretched.
Fig. 18.8a—Original image.

Fig. 18.8b—Middle values expanded.
Watershed Filter
The watershed filter is a mathematical function that transforms an image containing
individual particles that are touching or fused together into a new image wherein the
touching or fused objects have been separated. This is a very useful tool because several
quantitative metallography/materialography standards require the measurement of
individual objects. In material microstructure analysis the watershed filter can be ap-
plied to grain size measurement as well as to other structures where it is desirable to
measure individual particles within the unprocessed image that are touching. ASTM
Standard Test Methods for Determining Average Grain Size Using Semiautomatic and
Automatic Image Analysis 共E 1382兲 for grain size measurement by image analysis de-
scribe procedures incorporating individual grain area measurement. To achieve maxi-
mum accuracy each grain must be separated.
Figure 18.9共a兲 shows a steel grain boundary structure. Notice that the dark linear
grain boundaries are broken and do not completely delineate the individual grains.
Frequently the condition of uneven and incomplete grain boundary definition is pro-
Fig. 18.9a—Gray scale image showing incomplete grain boundaries.

Fig. 18.9b—Binary version of Fig. ??? after watershed separation operation to fill in missing
boundaries.
duced when revealing grain boundaries by chemical etching. The watershed filter can
be applied to such images and ideally will produce an image such as seen in Fig.
18.9共b兲, which shows all the grain boundaries completed. Such an image can be easily
measured using automated methods 共see Section 18.5.3 for additional discussion of
grain size measurement兲.
Another example will illustrate risks of applying image processing functions as
well as demonstrate another function that occasionally is useful in materials measure-
ment. In Fig. 18.10共a兲 below, a materials image showing darker second phase particles
within a light gray matrix has been digitized. To accurately count or measure the indi-
vidual particles a watershed separation processes has been performed. The resultant
binary image with particles assigned to white and the matrix to black is shown in Fig.
18.10共b兲.
The separation function has been fairly successful, having split many of the previ-
ously touching particles by constructing a black line between them. Note that the con-
Fig. 18.10a—Touching particles.

Fig. 18.10b—After separation.
structed separations tend to give angular and geometric rather than smoothly curving
edges to the particles. This type of mathematical artifact is typical of many image pro-
cessing operations and while the results are less than perfect, the slight distortion in
particle boundaries is more than offset by the overall improvement in particle measur-
ability. However, the separation has produced two relatively serious errors. In one in-
stance, near the upper center part of the image, a small triangular “particle” has been
created in the separation process that clearly does not exist in reality. Also, near the
lower right corner of the image a small particle has been incorrectly cracked in half.
Close examination of the Fig. 18.10共a兲 image reveals that small bright dots are found
within the particles at the site of the incorrect separations. In fact, just as in materials
where small voids or impurities can produce structural weaknesses that act as origin
sites for failures, these bright spots within the image have served as nuclei for the fail-
ure of the separation process. Caution should be used in the application of the separa-
tion function since the manufactured boundaries may result in the separated particles
having slightly altered dimensions. As discussed below, applying additional image pro-
cessing operations prior to running the separation program can minimize the occur-
rence of these errors.
Smoothing
There are a large number of processing operations designed to alter individual pixel
brightness values based upon the values of surrounding pixels. Such spatial filtering
operations exist for increasing or decreasing illumination changes within pixel neigh-
borhoods. When separating touching particles, a prior filtering operation that reduces
or smoothes illumination variability can eliminate bright spots that may lead to errors.
Applying such a filter results in the image shown in Fig. 18.10共c兲. Compare Fig. 18.10共c兲
with Fig. 18.10共a兲, nothing that the smoothing filter has remove the bright spots. Apply-
ing the watershed separation operation to the image in Fig. 18.10共c兲 yields the image
shown in Fig. 18.10共d兲.
Figure 18.10共d兲 displays a very good separation of the particles with no grossly in-
accurate particle shapes. This example has demonstrated the ability of image process-
ing programs to both reduce as well as increase artifacts present within an image as
Fig. 18.10c—Smoothed image.
well as the potential benefits of performing a series of image processing operations to

achieve an optimal result. Developing a multi-stage image processing procedure is
much like developing a metallographic/materialographic specimen preparation proce-
dure. It is extremely important to note, however, that since the outcome of any given
image processing operation is directly dependent upon the level of illumination in the
original image, any change to the illumination level may result in an entirely different
result.
Sharpening
Sharpening is an image processing operation that is designed to accentuate the edges
of objects within the image. It can be thought of as a way to bring an object into sharper
focus. The figures below illustrate the visual as well as quantitative effects of sharpen-
ing. Figure 18.11共a兲 shows a portion of a micron scale. Figure 18.11共b兲 is a plot of the
pixel brightness levels measured along the horizontal section line drawn in Fig.
18.11共a兲. Note that the brighter scale lines result in spikes on the illumination value
plot.
Fig. 18.10d—More accurate separation.

Fig. 18.11a—Scale with section line.
A typical sharpening function has been applied to the same image and the results
are displayed in Figs. 18.11 and 18.11共c兲 and 18.11共d兲.
Visually the scale lines in Fig. 18.11共c兲 are more prominent and show more con-
trast between the lines and the gray matrix areas. The plot in Fig. 18.11共d兲 shows a dis-
tinct dip at the base of the spikes indicating a greater illumination difference in the
pixels at the boundary where the scale lines and the matrix meet. These visual and
quantitative changes are characteristic of the image sharpening process. By blowing
up a section of the image the effects of sharpening can be seen in detail.
Note the exaggerated black to white illumination transition along the edges of the
sharpened image scale line in Fig. 18.11共f兲. Also notice the visible pixel brightness arti-
facts created in the matrix area immediately above the scale line in the sharpened im-
age. Exaggerating minor image brightness variations may cause difficulties depending
on the ultimate goals of the analysis. Sharpening filters can be valuable in enhancing
images for human viewing and can be helpful in reducing the so-called halo effect
when performing automatic detection of objects for measurement 共see ASTM Stan-
dard Practice for Obtaining JK Inclusion Ratings Using Automatic Image Analysis 共E
1122兲兲.
Fig. 18.11b—Plot of illumination along section line.

Fig. 18.11c—Sharpened image.
Many other image processing functions including filters and morphological op-
erations exist and are commonly found in commercially available image processing
software. For a thorough discussion of many of these processing functions see the
work of John C. Russ.2
18.3.7 Image Calibration

To measure the physical extent of structural features within a digital image, it is neces-
sary to create a spatial calibration. The process of calibration is the method by which
actual measurements may be extracted from any object displayed within an image. A
calibration is a numerical ratio that defines the relationship between a pixel and a real
world measurement unit such as a millimetre. Recall that a pixel is the unit building
block from which the entire digital image is formed. Spatial calibration provides a
height and width dimension for the image pixel. Within any digital image, all pixels are
identical in horizontal and vertical dimension. By assigning horizontal and vertical
pixel dimensions, structural features can be measured by counting the number of pix-
els within the feature and multiplying by the appropriate spatial calibration factors.
Pixel calibration factors are generally created for each of the magnification options
Fig. 18.11d—Exaggerated illumination at edges.

Fig. 18.11e—Unsharpened blowup.
available through the microscope or other device that is used to acquire images for
analysis. A calibration must be associated with an image prior to performing any mea-
surements within the image. A notable exception to this requirement is the case of per-
cent area or other relative measurements wherein the desired data are expressed as a
ratio and can be calculated by pixel counting.
The general process of creating a calibration involves the digitization of an image
of a scale or other object for which a dimensional distance is known. In microscopy this
is usually a slide micrometre having an etched scale in inches, millimetres, or microns,
or a geometric shape such as a circle or square with a known dimension. Figures
18.12共a兲, 18.12共b兲, 18.12共c兲, and 18.12共d兲 illustrate the calibration process. First a slide
micrometre is placed on the microscope stage, aligned, and the image is digitized.
After the scale image is digitized the operator initiates a series of steps that include
Fig. 18.11f—Sharpened blowup.

Fig. 18.12a—Image of portion of slide micrometre scale.
drawing a calibration line on the image across some distinct distance on the scale as
seen in Fig. 18.12共b兲.
Next the software prompts the operator to enter the length of the calibration line in
real world units, such as millimetres, as shown in Fig. 18.12共c兲.
The image analysis system software uses this information to calculate the calibra-
tion factor. Figure 18.12共d兲 shows a typical software control where the resultant cali-
bration factor is displayed as a ratio of pixels per unit measurement.
Note that in the example a calibration factor is shown for both the X 共horizontal兲
and Y 共vertical兲 pixel dimensions. If the image pixels are square and have an aspect
共height to width兲 ratio of 1 then the X and Y calibration factors are the same. The pixel
aspect ratio is a function of the camera and digitizing hardware. It is very important to
Fig. 18.12b—Scale with calibration line overlay.
Fig. 18.12c—Operator input of calibration line distance.

Fig. 18.12d—Typical operator for control for creating spatial calibration.
determine the pixel aspect ratio and if it is not 1 then the X and Y calibration factors
must be calculated independently. Another feature on the calibration display panel of
importance is the name of the calibration. This name could include information about
how the calibration is configured, including optics, measurement units, etc. An addi-
tional essential item of information displayed and adjustable from this control is the
origin of the XY coordinate grid of pixels into which the image is divided.
Although not specifically written for use with digital imaging systems, ASTM Stan-
dard Guide for Calibrating Reticles and Light Microscope Magnifications 共E 1951兲,
provides relevant information on the calibration process 共see Section 12.4兲.
18.4 Image Measurement

Once calibration has been established it becomes possible to extract data from an im-
age. It is at this point that digital image analysis becomes a tool to implement quantita-
tive metallography/materialography. Assuming that the metallographic/materialo-
graphic specimen preparation and digitization processes have yielded an image that
displays the microstructure clearly, the next task to be performed is the delineation of
the features to be measured. A typical materials image is composed of a relatively large
area of matrix or background material within which one or more structural features
having one or more individual occurrences are distributed. To extract measurements it
is necessary to separate the pixels that represent the features of interest from the pixels
that represent the matrix or background material. This is a data reduction operation to
separate pixel data that are associated with the microstructure of interest from all
other pixel data.
It is interesting to note that from this point forward what is taking place is data
processing—not image processing.
There are two basic approaches to defining and separating the features within the
Fig. 18.13a—Grain diameters measured.
image to be measured. In the more basic method the equipment operator interactively
delineates the points, lines, or areas to be measured.
18.4.1 Manual Measurements „Operator Defines Points, Lines, or Areas…

Manually indicating what is to be measured by operator interaction is a simple yet use-
ful method of extracting measurements from microstructural images. In general there
are three possible forms to be delineated by direct operator interaction, points, lines,
and areas. Figure 18.13共a兲 shows an image of a grain boundary structure. Exercising
the line feature creation tool available with nearly all image measurement software the
operator can use the computer system mouse to position the cursor on a grain bound-
ary, then click the mouse button and drag the cursor to another point on the grain
boundary. Another mouse click and the image measurement software immediately
counts the number of pixels in the line, calculates the length of the line, and notes the
distance on the image.
A slightly different implementation of the same techniques allows the operator to
trace an outline of a complete grain boundary and the measurement software can im-
mediately calculate the grain area as shown in Fig. 18.13共b兲.
While manual measurement techniques are basic and require operator input, they
should not be overlooked as a viable means for accurately extracting measurement
data from materials structure.
Fig. 18.13b—Grain boundaries traced and grain areas measured.

Fig. 18.14a—Segmentation control showing distribution of image illumination.
18.4.2 Automatic Measurements „Objects Defined by Image

Segmentation…
Of all the many advantages of digital image analysis, possibly the single most powerful
is the process of delineating and measuring structural features over multiple fields of
view without the necessity of operator interaction. The ability to measure dozens, hun-
dreds, and even thousands of individual occurrences of structural features without
constant operator involvement is a strong incentive for the implementation of image
analysis for quantitative metallography/materialography. Such automation of extract-
ing data from materials images based upon the concept of image segmentation. Seg-
mentation provides a means whereby, after initial operator setup, features can be de-
lineated and thus measured without additional operator input. In segmentation the
image is divided into the structural features of interest and the matrix or image back-
ground based upon the pixel illumination values. The division is based on the histo-
gram showing the distribution of image pixel illumination values. The process of seg-
mentation produces a range of values having a lower limit and an upper limit within
the overall image illumination distribution. The segmentation range is set to match as
closely as possible the pixel illumination values of the structure to be measured. The
success of this process is directly dependent upon the degree to which the structures to
be measured are represented by an exclusive set of pixel brightness values. Ideally the
structure to be measured is represented within the image by a distinct range of the pixel
illumination values different from the pixel illumination values of the matrix. All image
analysis software provides a control mechanism to allow the operator to interactively
adjust the segmentation levels to detect the features of interest. Commonly, the control
will display a histogram showing the image illumination distribution with the upper
and lower segmentation range limits superimposed as a pair of vertical lines. The im-
age itself may also be shown with a color overlay corresponding to the current segmen-
tation range settings. In effect, the color will show exactly what part of the image is
being detected. Figure 18.14共a兲 shows a portion of a typical segmentation control panel
provided with image analysis software.
In this example the histogram of an image digitized to 8 bits 共0 = black to 255
= white兲 is displayed. Notice also the bar along the top of the control; the size and posi-
tion of this bar relative to the distribution histogram is a visual indicator of the current
segmentation range setting. The 0–255 setting shown is actually detecting the entire
image and is simply the starting point for segmentation adjustment. The operator, us-
ing a combination of cursor positioning and mouse clicks, must move either or both of
the segmentation limits set to achieve detection of the features of interest. Figure 18.14
共b兲 shows the image under analysis.
The darker gray objects are to be detected for measurement. Since the objects are
Fig. 18.14b—Segmentation control showing the image under analysis.
relatively darker than the surrounding matrix material, the upper segmentation limit
must be adjusted to a lower level to exclude the brighter pixels representing the matrix.
Using the software control the upper segmentation limit can be reduced. As the limit is
moved lower, the pixels falling within the range are indicated by the bar and with a
color overlay on the actual image. This color-coding method allows the operator to
clearly see the results of segmentation at each possible level. The segmentation limit
must be lowered until the best possible delineation of the objects is achieved. Figures
18.14共c兲 and 18.14共d兲 show the final segmentation setting on the distribution plot and
the image with the red overlay indicating objects detected for measurement.
It is important to note two items regarding the setting of segmentation levels. First,
while automatic software-controlled segmentation can be performed by virtually all
image analysis software, the accuracy of the segmentation operation and therefore all
subsequent measurements, are primarily the responsibility of the operator and in most
cases are based upon a subjective judgment concerning the optimal limit settings. Sec-
ondly, if a relatively clear distinction between object feature illumination levels and
matrix illumination levels does not exist, the process of segmentation may be difficult
and in some cases it may be impossible to set with adequate accuracy to produce mean-
ingful measurement results. If the structures to be measured cannot be cleanly delin-
eated by segmentation further metallographic/materialographic specimen prepara-
tion or additional image processing must be considered. It is possible that micro-
structures of certain materials, regardless of preparation and processing, do not lend
themselves to the use of segmentation to delineate features for measurement. In such
Fig. 18.14c—Illumination distribution with segmentation range set.

Fig. 18.14d—Image showing detected objects with red overlay.
cases extraction of measurements must be accomplished interactively.

Once structural objects have been defined by segmentation, the extraction of mea-
surement data are almost trivial. All image analysis software includes a variety of mea-
surements that may be extracted from defined objects. In most cases the variety of mea-
surements possible greatly exceeds the requirements of common quantitative metallo-
graphic/materialographic standards. Structure area, diameter, length, width, perim-
eter, and many other measurement types can be made. In the next section the applica-
tion of these measurement methods to several of the most commonly employed quanti-
tative standards will be discussed.
18.5 Digital Imaging Applied to Quantitative Materialography

This section is composed of a series of detailed discussions of several of the most com-
monly practiced quantitative materials standards. The Annual Book of ASTM Stan-
dards, Volume 03.01—Standards Relating to Metals-Mechanical Testing; Elevated and
Low-Temperature Tests; Metallography 共see Part II, Section 12.4兲 contains the major-
ity of standards written by this body that are applied to quantitative materials micro-
structural analysis. Other standards not found in this volume but applicable to micro-
structural measurements include: ASTM Standard Test Method for Evaluating the
Microstructure of Graphite in Iron Castings 共A 247兲 and ASTM Standard Specification
for Compacted Graphite Iron Castings 共A 842兲. One or two other quantitative methods
for which specific standards do not exist are included based upon their widespread use.
18.5.1 Percent Area „Volume Fraction…

One of the simplest and most widely used forms of quantitative metallography/
materialography is area, or volume fraction. To perform percent area measurements
requires image digitization but does not require calibration, since the required out-
come is a ratio. The manual standard for implementing this quantitative method is
ASTM Standard Test Method for Determining Volume Fraction by Systematic Manual
Point Count 共E 562兲. This standard relies upon the use of a grid consisting of “equally
spaced points formed by the intersection of fine lines.” This, of course, is a method of
digitizing the microstructure. Interestingly, ASTM E 562 references ASTM Practice for
Inclusion or Second-Phase Constituent Content of Metals by Automatic Image Analy-
sis 共E 1245兲 for the “use of automatic image analysis to determine the volume fraction.”
Another standard, ASTM Test Methods for Determining Area Percentage Porosity in
Thermally Sprayed Coatings 共E 2109兲, describes the use of digital imaging to measure
percent area of a specific structural feature. Performed either manually or by com-
puter, the point counting technique is the essence of percent area or volume fraction
measurement. By definition a digitized image is composed of a number of pixels that
are, in fact, a grid of equally spaced points. All that is necessary is to count the pixels
共grid points兲 that fall within the structure of interest and divide that value by the total
number of pixels in the entire field of view. In order for the software to calculate the
percentages, the operator must use the system segmentation control to detect the
phase 共or phases兲 to be measured. The detection operation is the key step in the proce-
dure and all concerns relative to segmentation discussed in Section 18.3.6 apply. Inevi-
tably, microstructures will be encountered in which the pixel illumination values of the
structure to be measured and the matrix have some overlap with no distinct boundary.
In these cases setting the segmentation range necessarily requires a subjective judg-
ment on the part of the operator. The reliability of the calculated volume fraction may
be improved by employing a technique of setting several segmentation ranges to detect
the same structure. Since most imaging systems have the capability of measuring more
than one segmented range simultaneously, it is a simple matter to set several ranges for
the same structure and take the statistical average for the reported result. This ap-
proach of taking a larger sample of data is consistent with statistical thinking and the
additional measurements and calculations necessary are easily performed by analysis
software. There are other advantages to using digital image measurement software for
percent area 共volume fraction兲 as well as other measurements. The possibility of apply-
ing a color overlay to the image to highlight the measured phases provides an excellent
visual aid to the operator and yields highly informative images for inclusion in the re-
sults report.
Another advantage is the capability of the image measurement software to pro-
duce data that may be exported directly to external analysis and reporting software
such as database, statistical process control, and spreadsheet programs.
18.5.2 Inclusion Rating

Inclusions are occurrences of precipitates or other products of indigenous processes
that result in random distributions of observable particles in the matrix material. Be-
cause of the significance of inclusions in influencing material properties, methods of
classifying and determining the level of inclusions present in materials have been de-
veloped and widely used, primarily in steel, as a major determining factor of quality.
A number of published standards employing manual comparison as well as quan-
titative methods for determining the content of inclusions exist. ASTM Volume 03.01
includes three standards, ASTM Standard Test Methods for Determining the Inclusion
Content of Steel 共E 45兲, ASTM Standard Practice for Obtaining JK Inclusion Rating
Using Automatic Image Analysis 共E 1122兲共withdrawn 2006, replaced by E 45兲 and
ASTM Standard Practice for Determining the Inclusion or Second Phase Constituent
Content of Metals by Automatic Image Analysis 共E 1245兲 for determining inclusion
content.
ASTM E 45 is the original manual comparison method. Of the several methods
found in this standard by more widely practiced microscopic methods are Method A
and Method D. The heart of these methods involves classifying inclusions into four
types 共A, B, C, and D兲 based upon inclusion morphology, separating each type into a
thin and heavy series based upon inclusion width and assigning each type a Severity
Level 共1 / 2 to 5兲 based upon the total length or number of inclusions in a field of view.
The Method A requires the reporting of the inclusion rating for the field of view with the
most severe rating for each inclusion type. The compilation of these four ratings is the
“worst field.” In Method D a specimen surface area of 160 mm2 must be covered using
individual fields of view of 0.05 mm2. This results in the requirement to cover 320 fields
of view, each to be rated for the severity level of all types. ASTM E 45 includes a series of
drawings showing the amount of inclusions at each severity level for each inclusion
type and requires that the operator judge the best comparison and record the observa-
tions.
Obviously this manual approach is quite labor intensive and has the potential to
generate subjective results particularly in the Method D rating of 320 fields. ASTM E 45
is one of the best examples of a standard that has been significantly improved by con-
verting to more quantitative and automatable methods. While incorporating the meth-
ods of E 45, ASTM E 1122 defines inclusion typing and rating in a sufficiently quantita-
tive way so as to enable these classifications to be performed by image analysis
software. Although eliminating the reliance on chart comparison, ASTM E 1122 pre-
serves the traditional severity level-rating scheme rather than requiring a more statisti-
cally robust results report. In recognition of this short-coming ASTM E 1245 has been
published and provides a thoroughly quantitative method with statistically relevant re-
porting of results.
Following the ASTM E 45/E 1122 standard to perform the severity level rating of
inclusions using digital imaging software requires first the separation of the inclusions
from the matrix by the process of segmentation. The matrix of the steel microstructure
after specimen preparation has a very high illumination level nearly white. The type A
sulfide inclusions are generally quite high in illumination levels and appear in a gray
scale digital image as light gray. A-type inclusions may be close to the matrix in illumi-
nation level and therefore the requirements for specimen preparation and lighting op-
timization are critical. Background correction may be required to ensure that the A
types can be successfully segmented without detection of bits of the matrix. Inclusion
types B, C, and D are the oxide types and generally appear as black objects in the ma-
trix. The B types are sometimes described as broken stringers and occur as a series of
three or more particles strung out in a line; C types are single particles called stringers
having an elongated form with an aspect ratio of greater than designated in the stan-
dard. The D types are globular oxides and are circular with aspect 共length to width兲
ratios of less than designated in the standard. The B, C, and D oxide type inclusions
must also be separated from the matrix by segmentation. Normally segmentation to
separate the B, C, and D types is not difficult due to their high contrast with the bright
matrix.
Separation of the sulfide A type inclusions from the B, C, and D oxide types is gen-
erally straightforward since the A types appear as brighter objects than the darker ox-
ide types. Once segmentation is established the measurement of length and width of all
inclusion types and counting of the D types must be performed. These data are then
used to calculate the severity levels for each inclusion type. For many image analysis
systems, the specimens must be oriented on the microscope stage such that the elon-
gated inclusions are aligned horizontally or parallel to the X axis of stage movement.
Several difficulties can be encountered when implementing this standard. To begin
with, inclusion ratings must be made for a specific field area 共0.05 mm2兲. If this area
cannot be displayed in a single digitized image, it is necessary to digitize and measure a
sequence of images until the 0.50 mm2 area has been achieved before a rating can be
calculated. The need to measure and accumulate data over multiple images requires
more complex software and will be more time consuming. To improve efficiency an
attempt should be made to choose a combination of camera lens and microscope ob-
jective magnification to yield a digitized image area of 0.50 mm2. Another difficulty
may be encountered because of the standard requirement that inclusions as thin as
2 ␮m be measured. Such small objects can be difficult to distinguish from commonly
occurring artifacts that possess illumination levels similar to the inclusion types. Any
scratches visible on the specimen surface after materialographic preparation may be
detected as an elongated A or C type inclusion, although generally imaging software is
designed to eliminate such artifacts due to their orientation. A more common problem
is the misdetection of small circular artifacts as D type inclusions. It is nearly impos-
sible to separate with software filtering legitimate D types from artifacts of this class
and therefore it is absolutely essential to perform inclusion measurement only on
specimens that are freshly prepared in order to minimize the occurrence of corrosion,
oxidation, or staining. Another issue arises from the requirement to measure a rela-
tively large specimen area, 160 mm2.
As mentioned earlier 320 images are needed to cover this area at 0.50 mm2 per
image. Obtaining such a large number of images can obviously take a significant
amount of time and has naturally led to the use of motorized microscope stages that
can be programmed to move the necessary number of fields without the need for
manual operator interaction. While without question an improvement, the use of mo-
torized stage movement along with motorized focusing procedures to eliminate opera-
tor interaction during the inclusion measurement process can also lead to problems. It
is inevitable that an unattended, fully motorized, and automatic inclusion rating pro-
cess will produce some field ratings that are incorrect. Two types of errors are com-
monly encountered. Excessively high severity levels can be calculated because image
artifacts 共scratches, dust, oxidation spots, stains, etc.兲 have been measured as inclu-
sions. Also slightly out-of-focus images can be digitized to display inclusions with exag-
gerated dimensions that produce results higher than actual severity levels. More rarely,
the focus is so far off so as to cause complete failure to detect any inclusions present in
the image. Falsely high field measurements can be flagged and the images stored sepa-
rately so at the conclusion of specimen measurement the operator may check the list of
suspect rating data and review the associated images. Any images displaying obvious
artifacts may then be removed from the rating database. Incorrectly under rated im-
ages are impossible to discover, short of an operator examination of every image rated.
This of course is impractical and completely defeats the desire to eliminate direct op-
erator involvement in the measurement process. Several additional error sources can
be identified including misclassification of inclusion type by the software. In contrast
to ASTM E 45 and ASTM E 1122 the ASTM E 1245 provides another approach to inclu-
sion rating.
ASTM E 1245 is a primary example of a stereologically and statistically robust
quantitative microstructural quality standard. The Procedures Section of E 1245 lists
the Measurement of Stereological Parameters including volume fraction of the inclu-
sions, the number of inclusions per field, and the number of interceptions of the inclu-
sions per unit length of test line. Additional individual inclusion feature measurements
may be made. From these basic measurements, statistical parameters such as aver-
ages, standard deviations, 95 % confidence interval, and percent relative accuracy are
to be calculated for each type of inclusion detected. An important aspect of this stan-
dard that is significantly different from its predecessors is the elimination of separating
inclusion types into thin and heavy and calculation of severity levels.
The stereological and statistical procedures embodied in the ASTM E 1245 stan-
dard make it an important addition to the traditional severity rating level methods.
18.5.3 Grain Size

Grain size is a key determiner of materials properties. Several standards, both qualita-
tive and quantitative exist that describe methods for determining grain sizes 共see Sec-
tion 17.3兲. ASTM Standard Test Methods for Determining Average Grain Size Using
Semiautomatic and Automatic Image Analysis 共E 1382兲 is a quantitative standard writ-
ten for implementation via digital image analysis that is based on many of the same
measurement parameters described in the quantitative methods of the ASTM Stan-
dard Test Methods for Determining Average Grain Size 共E 112兲. The several variations
in methods described in both of these standards are derived from measurement of ei-
ther grain interior areas, grain boundary lengths, or the interceptions of these features
with some pattern of test lines. The chief difficulty in applying digital image analysis to
grain size determination arises from the problem of grain boundary delineation. To
show the grain boundaries in most materials requires some form of chemical etching.
Acidic etch compounds may erode the material at the structurally weaker boundary
between grains producing a slight “groove” that has a lower illumination level when
viewed with a microscope 共see Part II, Chapter 13兲. Some acidic etchants, such as Nital,
when applied to steel, chemically dissolve grains at different rates based on each grain’s
crystal orientation. This difference in attack creates differences in elevations at the
boundaries between adjacent grains resulting in what appears to be, in bright-field illu-
mination, black lines at the boundaries between grains. In practice the precise and uni-
form application of etchants is difficult to achieve and along with naturally occurring
variations in material etching rates, results in grain boundary visibility and appear-
ance that is highly variable. Even within a single microscopic field of view it is common
to observe strongly etched boundaries immediately adjacent to areas that display
faintly or incomplete boundary delineation. In fact, the preparation of microstructural
specimens with 100 % grain boundary delineation is uncommon. The boundary delin-
eation issue is so significant that the ASTM E 1382 standard prefaces all discussion of
digital image measurement methods with the statement “The precision … of grain size
measurements using automatic image analysis is highly dependent on the quality of
the etch delineation of the grain boundaries. The grain boundaries should be fully and
uniformly delineated.” If the boundary between adjacent grains is incomplete when
using a grain area method, the separate grain areas will be measured as one, resulting
in erroneously high grain area data. Similarly, missing boundaries will produce an in-
accurately low measurement when employing a grain boundary length method of
grain size determination.
In nearly every case the application of a watershed type digital image filter must be
applied to improve grain boundary delineation before measuring grain features with
digital imaging systems. This process is commonly referred to as grain boundary re-
construction; see Section 18.3.6 for a discussion of the watershed filter. It is important
to note that the watershed filter can be too aggressive in defining boundaries; the filter
typically connects truncated grain boundaries but also tends to connect any dots ap-
pearing in the grain interiors to form boundary networks. This action can result in a
virtual “fracturing” of grains into small pieces.
Minimization of this effect can be achieved by careful operator adjustment of the
segmentation levels. Most implementations of this filter require that the operator set
the segmentation levels to select the grain interiors. In practice it may be advantageous
to set the segmentation range to over detect the grains, i.e., include some of the lighter
boundaries 共and grain interior artifacts兲 along with the grain interiors. Observing the
results of boundary reconstruction at several different segmentation levels and select-
ing the most accurate level should be a part of the standard analysis procedure. It may
also be necessary to run one or more digital image processing functions designed to
eliminate grain interior artifacts that can serve as sites for nonexistent boundary con-
struction. Ultimately, it may be necessary for the operator to manually insert, via a soft-
ware drawing function, missing boundary sections. This operation obviously lacks effi-
ciency and should be avoided. In reality, boundaries have no dimensions, but in any
graphical representation they will have some width. Depending on the magnification,
the grain size and the width of the boundaries, an area reduction introduced by the
boundary delineation could be significant, thus the boundary thickness should be kept
to a minimum.
After performing the appropriate image processing steps to “reveal” the complete
grain boundary network in a specific image, the image processing software can pro-
duce a binary, or black and white image with only the boundaries shown. An image
composed of only test lines in any orientation and density, linear or circular 共or virtu-
ally any other configuration兲 can be constructed by software. This test line image can
be mathematically combined with the grain boundary image using a class of image
processing functions commonly termed “image arithmetic.” The imaging software can
produce a resultant image showing just the points where the test lines intercept the
boundaries. This is accomplished by checking pixels at exactly the same coordinate
location in both images and if the location is occupied by a boundary and by a test line
it is counted. Alternatively other image arithmetic functions may be performed to yield
an image showing just the lengths of the test lines falling within the grain interiors. The
grain intercept lengths displayed in these images can be measured to provide the mean
lineal intercept length, a method of grain measurement described in ASTM E 1382 as
well as in ASTM Standard Test Methods for Characterizing Duplex Grain Sizes
共E 1181兲.
In reality, perfect grain boundary delineation is not necessary. It is perfectly ac-
ceptable that over any given number of fields measured there will be some over and
some under-measured grain areas or boundary lengths. Since the statistical reporting
requirements of the quantitative standards provide methods for determining measure-
ment accuracy based on statistical parameters such as confidence interval and percent
relative accuracy, if, after measuring a specimen area, appropriate statistical signifi-
cance levels are not produced, then it is necessary to measure more grains in more im-
ages. Typically, imaging system software accumulates the grain feature measurements,
as they are collected over multiple images. Based on these raw measurements the re-
quired statistical parameters are calculated. One advantage in delineating and collect-
ing individual grain areas for average grain size determination is that in the same
dataset the largest grain area and clusters of grains can be found. The largest grain area
can be used to satisfy the requirements of ASTM Standard Test Methods for Estimating
the Largest Grain Observed in a Metallographic Section 共ALA Grain Size兲共E 930兲. Even
Table 1 of ASTM E 930 listing the relationship of the ALA grain area to the grain size
number can be created easily in software such that the grain size number can be auto-
matically reported, further streamlining the performance of ALA grain size analysis.
Grain area cluster data can be useful in characterizing duplex grain sizes as described
in ASTM E 1181.
18.5.4 Degree of Banding

The nature and importance of quantifying banding in microstructures is discussed in
Section 17.5. ASTM Standard Practice for Assessing the Degree of Banding or Orienta-
tion of Microstructures 共E 1268兲 provides quantitative as well as qualitative methods
for assessing the degree of banding. The standard requires the measurements of vol-
ume fraction and count of feature interior interceptions or feature boundary intersec-
tions with superimposed test grid lines. Both of these operations have been discussed
共see Sections 18.5.1 and 18.5.3兲; they can be performed using digital imaging tech-
niques providing the banded structures exhibit a sufficiently high degree of illumina-
tion contrast to enable successful segmentation. Application flexibility is increased and
segmentation requirements relaxed if the imaging software provides the option for di-
rect operator insertion or deletion of the test line-feature interceptions or intersec-
tions. The only other condition to be satisfied for banding measurements is to orient
the image so that the deformation axis seen in the structure is aligned horizontally or
vertically in the digitized image. While image rotation can be performed by software to
avoid introduction of image processing artifacts, it is preferable to achieve the required
structure alignment by physically rotating the material specimen on the microscope
stage.
18.5.5 Depth or Thickness Measurements

Several standards exist that address the linear measurement of depth or thickness of
structures, zones, and layers. These include ASTM Standard Test Methods for Estimat-
ing the Depth of Decarburization of Steel Specimens 共E 1077兲 and ASTM Standard Test
Method for Measurement of Metal or Oxide Coating Thickness by Microscopical Ex-
amination of a Cross Section 共B 487兲. These standards rely primarily on the use of eye-
piece reticles or filar micrometres to perform the necessary measurements. Digital im-
aging offers several approaches to emulate the nondigital quantitative procedures.
When measuring the depth or thickness of structures that exhibit a strong contrast
with surrounding or adjacent material the “segment and combine” techniques de-
scribed in Section 18.5.3 may be used. Briefly, an image of the segmented layer to be
measured is mathematically combined with an image of a set of section lines. A result-
ant image is produced that displays only that portion of each section line that lies on
the segmented layer and these lines are measured. While section lines may be discon-
tinuous, the image analysis software calculates the overall length of each horizontal
row of line segments no matter how many segments into which the line is broken. The
actual thickness measurement is made starting from the left end point of the left-most
segment in each row and finishes at the right end point of the right-most segment in the
row. Figures 18.15共a–e兲 depict this process.
For structures lacking the contrast to use the segmentation approach the measure-
ments can be made using operator interactive methods to construct point-to-point dis-
tances or parallel lines that are measured by the software. These methods are the digi-
tal equivalents of positioning filars for thickness measurement, with the operator using
the computer mouse to position filar lines on the digital image as displayed in Figs.
18.16共a兲 and 18.16共b兲.
Fig. 18.15a—Image of coating.
Fig. 18.15b—Binary 共segmented兲
Fig. 18.15c—Binary section line image.

Fig. 18.15d—Combined 18.15b and c.
One of the additional advantages in using digital imaging systems for thickness-
type measurements is that annotations showing measurement lines as well as the mea-
sured distances can be added to the image automatically by the software.
18.5.6 Graphite in Iron Castings

ASTM Standard Test Method for Evaluating the Microstructure of Graphite in Iron
Castings 共A 247兲 is essentially a qualitative chart comparison standard, applied to duc-
tile, gray and malleable irons. For nodular 共ductile兲 and flake 共gray兲 iron particles a size
共maximum diameter or length兲 classification chart is given. Much could be done to im-
prove this standard by introducing additional quantitative procedures. The highly con-
trasted nature of microscopically observed graphite in prepared cast iron specimens
make the use of segmentation-based digital image measurement of these structures
quite straightforward. Well prepared specimens that do not exhibit graphite smearing
seldom require extensive image processing since the dark 共nearly black兲 graphite
shapes are strongly contrasted with the bright white of the cast iron ferrite matrix.
One problem that may hinder automatic measurement is the possibility, particu-
larly in gray iron, of touching graphite particles. The application of a separation filter
Fig. 18.15e—Section lines over coating.

Fig. 18.16a—Vertical filar.
may reduce these occurrences and as a final solution manual editing of the image may
be undertaken to separate massively touching particles.
Ductile Cast Iron

Although not incorporated into any ASTM standard, an important factor in determin-
ing ductile or nodular iron product acceptability is the percentage of graphite particles
that are nodular. Digital imaging systems provide outstanding capabilities for calculat-
ing the percent nodularity. The classic function used to calculate particle roundness
共nodularity兲 is the shape factor. While several equations exist for calculating shape fac-
tor the most commonly used is:
Shape Factor = 4*Pi* Particle Area/Particle Perimeter2

To calculate nodule shape factor the area and perimeter of each graphite particle is
Fig. 18.16b—Horizontal point-to-point.

Fig. 18.17a—8-line perimeter.
measured. These values are entered into the equation and the shape factor number is
produced. Possible shape factor values range from 1.0 for a perfectly circular particle
downward towards 0 for increasingly “uncircular” shapes. Some shape factor level
must be chosen as a lower limit to define the most “uncircular” shape to be considered
nodular. This value is often set to 0.6, so that graphite particles have a shape factor
equal to 0.6 or greater are nodules, and those with shape factors less than 0.6 are not.
Percent nodularity can then be easily calculated by dividing the total count of nodules
by a count of all graphite particles. The precision with which the imaging software de-
fines the particle perimeter length has a significant effect on the outcome of the calcula-
tions. In particular, the measuring of small undulations in perimeter can significantly
alter the percent nodularity since the perimeter is squared in the calculation of shape
factor. Figure 18.17共a兲 shows a nodule in an enlarged portion of a digital image. In this
view the imaging software was adjusted to measure the graphite perimeter using just
eight line segments seen as dark lines around the perimeter.
In Fig. 18.17共b兲 the software was readjusted to use 128 line segments to define the
object perimeter. The 8-line delineation yields a perimeter of 0.47953 mm while the
Fig. 18.17b—128-line perimeter.

128-line perimeter is 0.51311 mm in length. The shape factor of Fig. 18.17共a兲 is 0.929
while the shape factor of Fig. 18.17共b兲 is 0.869, a significant difference. This example
illustrates the importance of the software algorithms used to define objects and extract
measurements. The algorithms are in fact critical functions in the process of data pro-
duction. As such their contribution to the end result must be understood and con-
trolled if reproducible structure measurements are to be achieved. Attention to such
internal software methods is especially important when results produced by several
separate digital imaging systems are to be compared.
Gray Cast Iron

The length of graphite flakes in gray iron can normally be readily measured from digi-
tal images. The lengths can be input to calculations of the percentage of the flakes fall-
ing in each of the size classes listed in ASTM A 247. However, the task of digitally classi-
fying the “Graphite Distribution Patterns” as types of graphite flakes described in the
standard is beyond the capability of common image analysis techniques.
Compacted Graphite
Compacted graphite cast iron contains graphite particles in shapes that are intermedi-
ate between flake and spheroid shapes. This type is defined by the ASTM Standard
Specification for Compacted Graphite Iron Castings 共A 842兲 as “The acceptable graph-
ite formation in the microstructure shall contain 80 % minimum Type IV graphite as
depicted in ASTM A 247 which may be arrived at by using…automatic image analysis
methods.” Also, this type is “described as cast iron with the graphite in compacted 共ver-
miform兲 shapes and essentially free of flake graphite.” Based upon these guidelines it is
possible to produce imaging software to calculate the percentage of graphite that is not
spheroid 共calculate shape factor as in ductile cast iron except the percent particles that
are not spherical is found兲. Also, to ensure that there is no flake graphite present, the
aspect 共length to width兲 ratio may be calculated. In this case since the standard does
not provide a quantitative value to separate compacted from flake graphite, a reason-
able value must be assumed and used in the software to calculate the presence of any
flake graphite.
18.6 Digital Imaging Technology
18.6.1 Hardware
Several distinct hardware components are required to perform image digitization, pro-
cessing, and analysis. Microscopes and other optical devices are not discussed here.
The basic imaging system hardware components are: computer, camera, and printer.
Recently all hardware components needed for image digitization have become avail-
able as “off-the-shelf” items and the need for specialized hardware components for all
common materials structure measurements is nonexistent. A general philosophy con-
cerning selection of digital imaging systems should be based upon using the most stan-
dard components available. It is no longer necessary or even desirable to purchase pro-
prietary, single purpose, single source, and fully integrated systems. Such systems
inevitably have limited shelf life, provide functionality that is behind the curve of hard-
ware capabilities available on the open market, and provide very limited 共and expen-
sive兲 upgrade possibilities. With the possible exception of image measurement soft-
ware there is no component necessary for assembling a state-of-the-art digital imaging

system that is not widely available commercially.
Because the same technologies developed and priced for mass-marketed con-
sumer cameras, computers, and printers are used in industrial grade digital imaging
systems, the cost of the hardware components needed to provide image digitizing func-
tions continues to decline while the capabilities of the components continue to
improve.
Computer
Today, computers designed for normal business 共or even home兲 use have more than
adequate power and information processing capabilities to run even the most sophisti-
cated materials analysis software. It is not necessary or even desirable to procure cus-
tom designed or nonstandard computers to power digital imaging systems. All of the
computer peripherals present in a typical home computer system designed for Internet
access and game playing should in most cases be present on a system for image mea-
surement. Several specific components can be briefly commented upon. For viewing
images 共especially those delivered by large format digital cameras兲, relatively large
monitors are helpful. Monitors of 19 in. or larger display size and to save laboratory
bench space 共albeit at a premium price兲 flat, active matrix LCD monitors should be
considered. Efficient management of digital images does require relatively large capac-
ity computer memory, high processing speed, and extensive file storage space. Fortu-
nately, computer processors, memory chips, and disk drive components are among the
most cost effective of all equipment needed for digital imaging. Rapid technological
development and a long history of downward trending prices in these devices are pri-
mary reasons to avoid imaging systems based upon private label and custom designed
hardware that cannot be readily upgraded or enhanced with standard components.
Cameras
No other single component required to perform digital imaging is more widely avail-
able than the camera. There are literally hundreds of camera models available. Of this
vast array there are two basic types: analog and digital. The analog camera outputs an
analog electronic signal that is essentially a television signal; it is not in digital form
and requires that image digitization be performed by a video digitizing or frame grab-
ber circuit board installed in the computer.4 Digital cameras are designed to digitize
the image signal internally and output a digital format data stream to the computer.
The key element in cameras is the sensor that converts light into an electronic signal. At
this time the predominant sensor technology is the charged coupled device or CCD sili-
con chip. Another type of image sensor becoming increasingly available is the Comple-
mentary Metal Oxide Semiconductor or CMOS. Among the specifications that differ-
entiate cameras, the physical size of the chip is one of the more significant. Chip sizes
generally range from 41 , 31 , 21 , 32 , up to 1 in. or more. Chip size is important because all
other components remaining equal, the size of the chip is directly proportional to the
size of the digital image field of view. A system equipped with a camera featuring one of
1 1
the smaller chip sizes 共 4 or 3 in.兲 may not be capable of delivering the required field of
view area.
Obviously the quality of the image produced by the camera is important. But other
factors such as image size, ease of operation, cost, and most importantly, how the im-
ages are to be used should be considered.
Analog Cameras
Analog cameras output a video signal that can be displayed in real time, that is, the
image signal is output fast enough to refresh the monitor display at approximately 30
times a second. For viewing images on a monitor at a display rate that produces no
noticeable delay or jerky movement when the field of view is moved or the image focus
is adjusted, in general an analog camera performs better than a digital camera. Since
analog cameras contain a minimal amount of circuitry the physical size of the camera
can be relatively small. In general, the more digitizing and signal processing that is
done within the camera, the larger the camera body.
To digitize an image the analog camera must be connected to a digitizing circuit
board mounted inside the computer. Digitizing boards can display a live signal from
the camera along with digitizing the image for storage, processing, and measurement
共see Inoue and Spring for a detailed discussion of digitizing boards4兲. There are a wide
variety of digitizing boards available. When selecting a digitizing board it is important
to match the board input and digitizing capabilities with the signal output of the ana-
log camera. Many digitizing boards are available with the capability of being con-
nected to multiple cameras. This feature is useful in laboratories requiring cameras to
be mounted on a microscope, a stereoscope, a microhardness tester, and more.
Digitizing boards are supplied with software for adjusting the board to accept vari-
ous camera signal formats, for capturing images, and perhaps for image file manage-
ment. Digitizing board products may also include software programs called drivers
that are designed to enable the board to work directly with specific digital imaging soft-
ware. There is an industry standard digitizer-to-imaging software driver called TWAIN.
Digitizing boards and imaging software products providing the TWAIN interface can
work together and do not require any additional special software drivers. Analog
camera/digitizing board combinations provide a fast and efficient means for digitizing
images. For most material microstructure digitizing applications high-resolution ana-
log camera/digitizing board combinations are the best all around choice.
Digital Cameras
Digital cameras digitize the image signal output from the image sensor chip before it
enters the computer. Digital cameras connect to the computer using a variety of com-
puter ports or circuit boards, some standard and some custom designed. Digital cam-
eras are available with large format image sensor chips and can digitize images into a
very large number of pixels. With their high pixel counts digital cameras can provide
excellent quality images and are generally capable of displaying fine structural details
more sharply than an analog camera/board combination. As with digitizing boards,
digital cameras will be supplied with software for image acquisition and the availabil-
ity of TWAIN software is equally important. While providing high quality images, it
should be noted that many digital cameras are slower to capture images than analog
cameras.
The real time image display rate is 30 times a second for analog output while digi-
tal cameras may require up to several seconds to display a full image. In general, the
greater the number of pixels the digital camera offers, the longer the image capture
time. Delays in refreshing the computer image display are particularly noticeable dur-
ing focusing of the image. Additionally, digital cameras may be more complex to oper-
ate than analog systems. Digital cameras should be considered when the primary use
for the digitized images is viewing, particularly when the images are to be printed. Of
course, the quality of printed images is also a function of the printer used and printers
are briefly discussed in this section.
Black and White or Color

For extracting structural measurements from most materials a gray scale 共8 bit or 256
levels of pixel illumination兲 is adequate. In a few materials segmentation to separate a
structure for automatic delineation may require the use of a 24 bit 共16.7 million levels兲
true color image. Due to the increased difficulty in setting color segmentation levels
and inefficiencies attendant to managing color images, the use of color images for ex-
tracting measurements is only recommended if the measurements are not possible
with gray scale images. Color images are recommended when the primary use of the
image is for publication and human viewing.
Printers
As with cameras, a very large number of computer printers are available for use with
digital imaging systems. The growth in consumer digital photography has impacted
the quality of prints and the price of image printers very positively. Inkjet type printers
that can produce “photographic quality” images continue to become less expensive.
The primary printer specification used to judge the potential quality of printed images
is the number of ink dots per inch the printer is capable of putting on the paper. A count
of 2400 by 1200 dots per inch is dense enough to produce high quality prints. For the
highest quality images coated photographic type paper must be used. Another type of
printer technology known as thermal dye diffusion can produce a continuous-tone
print with resolution of 300 pixels-per-inch. The quality of these prints is termed “pro-
fessional grade” and these printers have prices in the range of one order of magnitude
higher than ink jet printers. Specifications and pricing level aside, it is recommended
that actual prints of material microstructures be viewed prior to making a decision on
printer acquisition.
18.6.2 Software
There is an enormous variety of digital imaging software available. A recent search of
the Internet yielded the following results:
Search Phrase: digital imaging software Web Page Matches over 50 000
Search Phrase: image acquisition software Web Page Matches over 2400
Search Phrase: imaging editing software Web Page Matches over 400
Search Phrase: image archiving software Web Page Matches over 400
Search Phrase: image measurement software Web Page Matches over 300
Although not designed specifically for materialographic structure imaging, the
number of “image software” product sources is significant. Many of the products, con-
cepts, techniques, and software modules developed for other digital imaging applica-
tions can be used in metallographic/materialographic systems. This results in the avail-
ability of constantly improving software functionality at competitive prices. Of course,
several software systems have been designed particularly for materials science applica-
tions. These should provide minimum basic image processing functions as well as the
modules to perform one or more of the metallographic/materialographic test methods
described in Section 18.5, depending on the requirements of the individual laboratory.
It is a near certainty that most imaging software packages will provide far more pro-
cessing and measurement capabilities than are normally needed in all but the most
diverse research and development environments. One of the challenges in selecting
software for materials analysis uses is in identifying products that provide the func-
tions needed to perform structural imaging tasks without the presence of extraneous
software capabilities that may complicate operation and inflate costs. A few general
guidelines can be suggested.
Obviously the most important consideration is that the software is capable of per-
forming the required tasks. What may not be so apparent is what those tasks are 共see
Section 18.7 for additional comments concerning software selection兲. The same gen-
eral criteria used in selecting any type of software are applicable. Avoid software that
can only be used with a specific computer or other hardware components. The soft-
ware should provide an open architecture that permits exchange of data and interac-
tion with other software products such as database, spreadsheet, and statistical pro-
cess control programs. The software must also follow industry standards for data and
image file formats, user interface control designs, and device connectivity. In most
cases it is advisable to avoid proprietary designs that create a “sole source” supplier
dependency.
Open Source/Public Domain Software

It is possible to obtain open source/public domain software like NIH Image from Na-
tional Institutes of Health for image processing/analysis. However, it should be noted
that the basic philosophy of open source software requires a strong commitment to
maintain and support the software on the part of the user. Often the typical
metallographic/materialographic laboratory is not able or willing to perform such
tasks.
18.7 Digital Imaging System Implementation

The selection of software should always be based on a thorough and realistic study of
current organizational tasks, established laboratory procedures and a realistic ap-
praisal of future requirements. A digital imaging system is not a stand-alone device; it
is a tool to facilitate the operation of a quantitative microstructural quality control pro-
gram. The same care and attention to detail should be accorded the selection of a digi-
tal imaging system as to other organizational information management or quality con-
trol systems. An imaging system is part of a bigger organizational structure.
In a well designed system implementation project three distinct phases can be
identified. The purpose of Phase 1 is to produce a master plan based on an analysis of
existing metallographic/materialographic operations and a definition of objectives.
Part of this phase is actually a traditional systems analysis study, undertaken to define
in some detailed and formal manner the procedures and work flow of the existing
metallographic/materialographic operations. This information can serve as a base line
for integration of new equipment. A clear understanding of the standards to be fol-
lowed, the type of measurements necessary, and the volume of current as well as pro-
jected work are among the many questions to be answered. It is also essential to consult
with engineers, information technology personnel, and others within the organization
who will be in any way impacted by the new system. A very important factor in the
successful implementation of a digital imaging system is the skill level required by the
system operator. Efficient operation of the imaging system may require a more techni-
cal background than general lab work; in particular a firm understanding of basic com-
puter operation techniques is essential. Since quantitative metallography/materialo-
graphy is based on stereological and statistical principles the system operators must
also possess an understanding of these subjects. If an evaluation of potential system
operators reveals a deficiency in these areas, suitable training programs should be re-
quired. The system suppliers should provide training in the operation of specific imag-
ing systems and software. However, general computer and quantitative methods
knowledge are a prerequisite and remedial instruction in these topics, if necessary, is
not the responsibility of equipment vendors. One important result of the initial phase
should be the generation of a set of expectations or specifications that define the func-
tions required of the imaging system.
The purpose of Phase 2 is to use the requirements, priorities, and specifications
generated in Phase 1 to determine which of the many commercially available systems
will best meet the current and future requirements of the company. This phase may
include identification of potential suppliers, compilation of a list of products available,
demonstrations, circulation of a Request for Quotation, and of course, final system se-
lection.
Phase 3, the last step of the process, is actually placing the system into operation.
The process of converting to digital imaging from qualitative or manual quantitative
methods should have been defined in Phase 1. Implementation of new technology will
almost certainly necessitate changes in the procedures used to employ that technology.
Common procedural points that may need changing include:
1. Specific orientation and positioning of specimen may be required by standards or
by equipment.
2. Selection of microscope objective magnification may be significant, i.e., field of
view area required by standard.
3. Upgrading of preparation standards to eliminate artifacts that defeat automatic
imaging.
Often results obtained from image analysis equipment will not match historical
results based on qualitative estimates or chart comparison methods. In these cases it
may become necessary to devise a strategy to correlate pre-and post-digital imaging
results. Ideally, major issues arising during implementation will have been identified,
and the new system will be placed into operation in an efficient and cost-effective man-
ner. Even with flawless planning it is to be expected that the full use of the system at
maximum efficiency will require a “learning” period.
ASTM Standard Guide for Laboratory Information Management Systems 共LIMS兲
共E 1578兲, offers many insightful guides for the selection of a Laboratory Information
Management System. Many of these concepts may be adapted for use in selecting a
system for digital imaging and an examination of ASTM E 1578 is suggested. A particu-
larly useful idea found in ASTM E 1578 is the need to focus on functions, not technol-
ogy. Additionally, see ASTM E 2066-00 Standard Guide for Validation of Laboratory
Information Management Systems.
In conclusion, the objective of this chapter was to highlight some of the digital im-
aging functions that are commonly applied to materials structure images and to pro-
vide an overview of the use of image measurement techniques to implement selected
standard test methods. It is also hoped that these comments have initiated an aware-
ness of the necessity of quantitative metallography/materialography and also that digi-
tal imaging systems are but a part of an overall program for the improvement of prod-
uct quality.
19
Digital Image Management
„Archiving…
A DIGITAL IMAGE ARCHIVING SYSTEM MAY INCLUDE ALL OF THE FEA-
tures and components of a full image measurement system, the difference being that
the primary purpose of archiving is to provide efficient and convenient yet powerful
methods for capturing, identifying, storing, and retrieving digital images and associ-
ated information rather than to extract structure measurement data. Such a system
may include sophisticated database software or simple filing schemes for identifying
images by a range of user definable classifications and keyword associations. As with
digital image measurement systems the selection of archiving must be based upon an
evaluation of existing and projected needs.
A broader view of laboratory digital imaging possibilities must include consider-
ation of the ASTM Standard Guide for Laboratory Information Management Systems
共LIMS兲共E 1578兲共see Sections 12.4.2/3兲. ASTM E 1578 provides a detailed discussion of
LIMS concepts. Laboratory information management systems are designed to provide
total data management from initial material sample receipt through logging of all
specimen preparation procedures, recording of image acquisition parameters such as
microscope magnification brightness, contrast, segmentation levels, calibration, and
any image processing functions performed along with the original, intermediate, and
final images as well as final structural measurements data and many others. In short,
these systems aspire to compile a complete record of all possible information related to
the processing of the specimen within the laboratory along with the ability to search,
retrieve, and report selected views or dynamic combinations of the information from
these records. These systems represent the most ambitious and sophisticated level of
digital system possible in the laboratory. The demands of design and implementation
of digital systems are increased by levels of magnitude when considering a LIMS. At
the most advanced implementation level, the LIMS must provide electronic integra-
tion of the technologies of many diverse instruments, requires the use of local as well as
wide area networking, and employs sophisticated database technologies. And because
they provide the several functional LIMS components as defined in ASTM E 1578 such
as data/information capture, data analysis, and reporting, systems for digital image ar-
chiving and structural measurement may be considered components or subsystems of
a LIMS.
References „Part IV…

关1兴 Underwood, E. E., Quantitative Stereology, Addison-Wesley Publishing Company, Reading,
MA, USA, 1970.
关2兴 Friel, J. J., et al., Practical Guide to Image Analysis, ASM International, Materials Park, OH,
USA, 2000.
关3兴 Russ, J. C., The Image Processing Handbook, 3rd ed., CRC Press, Boca Raton, FL, USA, 1998.
关4兴 Inoue, S. and Spring, K. R., Video Microscopy, Plenum Press, New York, NY, USA, 1997.
关5兴 Freund, J. E., Statistics: A First Course, 2nd ed., Prentice Hall Inc., Englewood Cliffs, New
Jersey, USA, 1970.
619
Part V: Hardness Testing
20
Introduction
HARDNESS IS AN IMPORTANT PROPERTY WHEN JUDGING THE QUALITY
and possible applications of a material. It can also give indications concerning the ten-
sile strength, ductility, or wearing quality of the material.
Beginning in approximately 1822, quantitative evaluation of hardness was carried
out based on the hardness scale developed by F. Mohs. He ordered known minerals so
that the harder mineral scratched the one preceding it.
TABLE 20.1—Mohs Hardness Scale.

Mohs Standard Equivalent Knoop
Mohs Scale Mineral Hardness Number
1 Talc 2
2 Gypsum 32
3 Calcite 120
4 Fluorite 150
5 Apatite 400
6 Feldspar 560
7 Quartz 700
8 Topaz 1300
9 Corundum 1800
10 Diamond 6000
It must be noted that the differences in hardness between the individual steps of
the scale are not equal. For example, the difference between steps 9 and 10 is substan-
tially greater than that between 1 and 9.
Around 1900, further testing procedures were developed for technical purposes. In
these procedures, hardness is not determined by scratching, but rather by indenting
the material to be tested with very hard objects of a specified size and shape. The
Brinell, Rockwell, Vickers, and Knoop hardness testing procedures are the best known
of these techniques.
Already in 1900, Martens suggested the following definition of hardness for techni-
cal purposes:
Hardness is the resistance of a material to penetration by another 共harder兲 mate-
rial.
This simple conceptualization remains the basis of our understanding of hardness
even today.
20.1 Indentation Hardness

Figure 20.1 schematically shows the significant elements of indentation hardness test-
ing. A particular indenter 共1兲, attached to the lower end of a press, is pressed into the
623
Fig. 20.1—Schematic drawing of hardness tester indicating force, indenter 共1兲 specimen 共2兲 and
support 共3兲.
specimen surface 共2兲 with a particular test force 共in N or kgf兲 and then pulled back. The
indentation that is created can then be measured.
The shape and size of the indenter are decisive for indentation resistance. With
ball-shaped indenters, the specimen material is pushed away sideways and down-
wards through plastic and elastic deformation. Angular or needle-shaped indenters
can, in addition to the deformation, cause separation processes like cracks, especially
in brittle materials 共ceramics兲.
Depending on the characteristics of the material being tested, various mostly non-
homogeneous deformation processes with multiple axes and varying degrees of elas-
ticity and plasticity occur with penetration.
The speed of penetration also influences the behavior of the material being tested.
For these reasons, the guidelines for the hardness testing procedures, including equip-
ment construction, indenter, penetration speed, optical system, and evaluation are of
particular importance.
Hardness is a distinguishing feature of a material. It is usually measured quantita-
tively according to the following general relationship:
Hardness value = Test force/indentation size 共1兲

Beginning in 1940, hardness testing procedures in which the penetration depth is
measured during application of a test force and then used to determine hardness were
developed. These procedures quickly gained in importance.
We differentiate among:
Hardness testing procedures with static load action.
Hardness testing procedures with dynamic load action.
Special hardness testing procedures.
The most important of these will be shortly described below.
20.2 ASTM Standards

To be able to compare hardness values, the equipment, testing procedures, testing
method, and evaluation must correspond to particular standards. The following ASTM
standards describe the various hardness testing procedures. See Section 12.4.2 for
more standards on hardness.
Standard Practices for Force Verification of Testing Machines 共E 4兲
Standard Test Method for Brinell Hardness of Metallic Materials 共E 10兲
Standard Test Methods for Rockwell Hardness and Rockwell Superficial Hardness
of Metallic Materials 共E 18兲
Standard Test Method for Rapid Indentation Hardness Testing of Metallic Materi-
als 共E 103兲
Standard Test Method for Indentation Hardness of Metallic Materials by Portable
Hardness Testers 共E 110兲
Hardness Conversion Tables for Metals 共Relationship Between Brinell Hardness,
Vickers Hardness, Rockwell Hardness, Rockwell Superficial Hardness, Knoop Hard-
ness and Scleroscope Hardness兲共E 140兲
Standard Practice for Scleroscope Hardness Testing of Metallic Materials 共E 448兲
Standard Test Method for Microindentation Hardness of Materials 共E 384兲
Standard Test Method for Vickers Hardness of Metallic Materials 共E 92兲
21
Static Hardness Testing Procedures
21.1 Brinell Hardness Testing
THE FIRST STATIC HARDNESS TESTING METHOD WAS INTRODUCED BY J.
A. Brinell, a Swedish researcher, at the 1900 Paris World Exposition. A hardened steel
ball or tungsten carbide ball with a diameter 共D兲 of 1, 2, 2.5, 5, or 10 mm was used as
indenter. This was pressed into the smooth, clean specimen surface with a test force
共F兲. Figure 21.1 shows the principle of test with test force F 共N兲, D the diameter of the
ball 共mm兲, d the mean diameter of the indentation 共mm兲, and h the depth of the inden-
tation 共mm兲. It is important that the specimen rests on a rigid support, and that the
indenter contacts the specimen without being shaken or jolted. The test force is then
increased to the predetermined maximum value within 2 – 10 s and held for 10– 15 s. If
the duration of load application falls outside of this range, this must be indicated. For
example, for nonferrous materials, the duration may be as long as 180 s.
Depending on the elastic-plastic behavior of the material, the indentation may
vary. Figure 21.2 shows an ideal indentation, 共a兲, an indentation with sink-in due to a
high degree of elasticity 共b兲 and an indentation with pile-up due to a high degree of
plasticity 共c兲.
21.1.1 Calculations and Procedures

The spherically shaped indentation that is created is measured. The Brinell hardness is
calculated from the mean indentation diameter according to the following equation:
F 2F
HBS or HBW = 0.102 = 0.102 ⫻ 共1兲
A ␲D共D − 冑D2 − d2兲
where
HBS= Brinell hardness with steel ball as indenter
HBW= Brinell hardness with tungsten carbide ball as indenter
F = test force in N
A = indentation surface in mm2
Fig. 21.1—Brinell hardness testing, test principle. Force, kgf 共F兲, diameter of ball, mm 共D兲, mean
diameter of indentation, mm 共d兲, depth of indentation, mm 共h兲共ASTM Standard E 10兲.
626
Chapter 21 Static Hardness Testing 627
Fig. 21.2—Ball-shaped indentation shapes. Ideal indentation 共a兲, indentation with sink-in 共b兲
and indentation with pile-up 共c兲.
D = ball diameter in mm
d = arithmetical mean value of two measured indentation diameters in mm
The test force F is multiplied by 0.102 共⬃1 / 9.80665= 1 / g兲 to get the calculated
hardness as a unitless numerical value.
Specimen thickness should be at least ten times the expected indentation depth. If
the expected hardness of a material can be estimated, then the minimum specimen
thickness can also be estimated.
For the indentation depth, it can be assumed that
A = D␲h 共2兲
The minimum thickness S of the specimen is then
S = 8共0.102F/␲DHB . . . 兲共3兲
Steel balls can be recommended as indenters for Brinell hardness values of up to
350. They are permitted up to HBS= 450. When testing harder materials, elastic defor-
mations of the ball must be expected. These lead to increased indentation diameters
and thus to erroneously elevated measured values. Tungsten carbide balls may be used
up to HBW 650.
Test results are given as follows:
Duration of test load application 共25兲
Test force identifying value 0.102 F 共3000兲
Ball diameter in mm 共10兲
Identifying marking of indenter 共in this case tungsten carbide兲
共W兲
Abbreviation for Brinell hardness 共HB兲
Determined Brinell hardness value 共410兲
The relatively large indentations are an advantage of the Brinell hardness testing
method. They ensure representative hardness values even when heterogeneous materi-
als are tested.
TABLE 21.1—Stress Level and Recorded Hardness Range for Various Materials.
Stress Level Hardness Range, HB Material
30 70–600 Steel, Iron ⬎140 HB
10 22–315 Ti, Ni-, Co, Cu-Alloys ⬎200 HB
5 11–158 Nonferrous metals and their
alloys
2.5 6–78 Bearing metals
1.25 3–39 Lead, tin
It is important that the ball creates an easily measurable indentation. For that rea-
son, it is stipulated that the indentation diameter lies between 0.24 D and 0.6 D. If dif-
ferent ball diameters are used on the same material, the measured values can only be
compared when the indentations are geometrically similar. Accordingly, the test force
F must be appropriate for the ball diameter D. For comparison of hardness values, the
optimum stress level 0.102F / D must therefore be closely adhered to. Table 21.1 shows
the relationship between stress level and measured hardness range for various mate-
rial categories.
If the material to be tested, and therefore the load ratio and the diameter D of the
test ball selected 共10, 5, 2.5, or 1.25 mm兲, are known, then the test force F can be set on
the testing apparatus.
The minimum distance from the middle of an indentation to the edge of the speci-
men should be at least 2.5 d for steel, gray cast iron, copper, and copper alloys. The
distance between adjacent indentations must be ⬎4 d.
For light alloys, Pb, Zn, and their alloys, the respective distances should be ⬎3 d
共specimen edge兲 and ⬎6 d 共adjacent indentations兲.
21.1.2 Brinell Hardness Testers

Figure 21.3 schematically shows the construction of a Brinell hardness testing ma-
chine with hand wheel 共1兲, support 共2兲, specimen 共3兲, objective 共4兲, indenter 共5兲, loading
system 共7兲, and screen for measuring the projected Brinell indentation 共6兲.
Figure 21.4 shows a modern Universal Hardness Tester for Vickers, Knoop,
Brinell, and Rockwell. It has unattended testing and analysis cycle via fully automated
image analysis for Brinell/Vickers and automatic focusing. The test load ranges are
9.81 N to 2450 N or 49 N to 7350 N.
Testing procedure details can be found in the directions for use of the equipment
and in the procedural and material-specific norms, for example, the ASTM Test
Method for Brinell Hardness of Metallic Materials 共E 10兲. Internal company proce-
dural guidelines should also be observed.
21.2 Vickers Hardness

Smith and Sandland developed the Vickers method 共named for the English company
Vickers兲 in 1925. The reason for this development was the fact that Brinell hardness
only provided usable results up to HBS= 450, because higher test forces cause defor-
mation of the steel ball to begin to occur.
In Vickers Hardness Testing, the indenter is a regular four-sided diamond pyramid
Fig. 21.3—Schematic drawing of Brinell hardness testing machine with hand wheel 共1兲, support
共2兲, specimen 共3兲, objective 共4兲, disengaged indenter 共5兲, screen for projection of the
indentation 共6兲, and loading system 共7兲.1
with an interfacial angle, ␣, of 136°. The geometry of this Vickers pyramid produces a
good correlation between the Vickers values HV and the Brinell hardness values HBS
between 350 and 400.
The Vickers pyramid is pressed vertically into the specimen with a test force P 共kgf兲
共2兲 shown schematically in Fig. 21.5. ␣ 共1兲 is the face angle of the diamond 共136°兲, d1 and
d2 共3兲 are the diagonals of the impression 共mm兲. The mean diagonal diameter d of the
indentation is used to calculate the Vickers hardness.
P 2P sin共136 ° /2兲 P
HV = 0.9272 = 2 ⬇ 1.8544 2 共4兲
A d d
where
HV= Vickers hardness
P = test force in kgf
Fig. 21.4—Universal hardness tester for all standard testing processes such as Vickers, Knoop,
Brinell, and Rockwell. Unattended testing and analysis cycle via fully automated image analysis
for Brinell and Vickers. Automatic focusing. Test load ranges: 9.81 N to 2450 N or 49 N to
7350 N.2
A = indentation surface in mm2

d = arithmetical mean value of the measured indentation diagonals in mm
For Vickers Hardness, given in GPa units, we find that
HV = 0.0018544 ⫻ P2/d22 共5兲
with force P2 in N and the mean length of indentation diagonals in mm.

Because of the pyramidal geometry, the relationship between the indentation
depth and the indentation diagonals is h = d / 7.0006.
For Vickers macrohardness testing, the test load must normally also be selected
such that the indentation diagonals are relatively large in comparison to the phase
components. The diagonal d should be a maximum of 2 / 3 of the specimen thickness,
and the penetration depth thus 1 / 10 of the specimen thickness, to exclude influence
from the specimen support. This is important when testing thin sheets or layers 共see
below兲.
Fig. 21.5—Vickers hardness testing, test principle 共ASTM Standard E 92兲.

Duration of test load application in s 共25兲
Test load identifying value 共100兲
Abbreviation for Vickers hardness 共HV兲
Measured Vickers hardness value 共780兲
Figure 21.6 shows the ideal indentation 共a兲 and possible undesirable indentations
with sink-in 共b兲, pile-up 共c兲 formation and “kite” shape 共d兲.
For high-test forces, determination of Vickers hardness is independent of the test
force. However, for test forces P ⬍ 5N the calculated Vickers hardness becomes test
force dependent. This phenomenon is known as Indentation Size Effect 共ISE兲. Its influ-
ence is particularly disruptive in microhardness testing, where HV values that have
been measured for the same specimen with differing test forces are no longer compa-
rable. The cause can be tension induced when the Vickers pyramid is imposed or sur-
faces that have stabilized dissimilarly during metallographic/materialographic prepa-
ration.
For this reason, hardness value classification is divided into test ranges.
Following the ASTM Standard Test Method for Vickers Hardness of Metallic Mate-
rials 共E 92兲, Vickers Hardness Tests are performed with test forces of from 1 to 120 kgf.
The ASTM Standard Test Method for Microindentation Hardness of Materials 共E
384兲 specifies a test force range of 1–1000 gf for microindentation hardness testing with
Vickers indenters 共see Section 21.5兲.
At Vickers hardness testing 共E 92兲 the distance between the center of the indenta-
tion and the specimen edge and between the center of two indentations should be
⬎2.5d. When laminated material is tested, a bond surface shall be considered as an
edge for spacing of indentation calculations.
In hardness testing of small parts, thin sheets, layers or foils, low-test forces should
be used to avoid the so-called anvil effect. The anvil effect is caused by use of a test force
Fig. 21.6—Vickers indentation shapes. Ideal indentation 共a兲, indentation with sink-in 共b兲,
indentation with pile-up 共c兲, and kite-shaped indentation 共d兲.
that is too high when testing a thin specimen, resulting in a bulge or shiny spot on the
underside of the specimen. Also a force that is too high may cause edge effects, a plastic
deformation in the direction towards the edge. For this reason an indentation shall be
in a certain distance to the edge as mentioned above. The use of low-test forces also
applies to the determination of hardness of individual structural constituents.
As the test force or indentation size, or both, decrease, the influence of the speci-
men surface increases. A carefully smoothed and cleaned surface is sufficient when
macro testing, but when micro testing, the specimen must be metallographically/
materialographically prepared to remove any disruptive roughness or solidified sur-
face layers. If smoothing and polishing are insufficient, the surface can be electrolyti-
cally or chemically treated to have access to mechanically undisrupted areas. If
individual structural constituents are to be tested, additional phase contrasting, for ex-
ample by means of etching, is necessary.
21.2.2 Vickers Hardness Tester

The hardness tester shown in Fig. 21.4 can easily be converted for use in Vickers macro-
hardness measurements. The indenter is exchanged and the appropriate test force in-
crements selected. Measurement takes place on the screen or automatically.
Depending on the producer, the machines differ in various ways. For example, the
test force may be produced mechanically or hydraulically in different increments, the
test method may be more or less automated and special testing needs may be met by
means of additional equipment.
Fig. 21.7—Knoop diamond pyramid and indentation 共ASTM Standard E 384兲.
21.3 Knoop Hardness Testing

Special machines were developed for low load, microindentation hardness, and ultra-
microindentation hardness testing in order to further decrease potentially disruptive
device-related influences and better measure very small indentations. Essentially, how-
ever, the testing procedure corresponds to that of macrohardness testing.
In 1932, Knoop, Emerson, and Peters introduced a method developed specifically
for low load and microindentation hardness testing. In Knoop hardness testing, a
rhombic-based pyramidal-shaped diamond indenter with edge angles of 172° 30⬘ 共⬔A兲
and 130° 共⬔B兲 is used. In Fig. 21.7, the pyramidal-shaped diamond is shown with the
two angles and the long diagonal, d 共␮m兲. As in the Vickers method, this pyramid is
pressed vertically into the specimen surface. Knoop hardness in kgf/ mm2 is calculated
by means of the long indentation diagonal d in ␮m, which is 7.114 times longer than
the short diagonal of the Knoop indentation.
The following equation applies:
HK = 14.229P1/d12 共6兲
where
HK= Knoop hardness in kgf/ mm2
P1 = test force in kgf
d1 = long indentation diagonal in mm
Knoop hardness in GPa units is determined as follows:
HK = 0.014229 ⫻ P2/d22 共7兲

where
P2 = test force in N
d2 = long indentation diagonal in mm
650 HK 0.5/ 30
Duration of test force application in seconds; not recorded if

between 10 and 15 s 共30兲
Test force identifying value: 0.102F 共F in N兲共0,5兲
Abbreviation for Knoop hardness 共HK兲
Measured Knoop hardness value 共650兲
Knoop hardness measurements are primarily taken using hardness testers devel-
oped for low load and microindentation hardness testing. In such machines, the load
system is changed accordingly and adjusted for small test forces. The screen onto
which the indentation is projected is exchanged for a measuring ocular.
Due to the measurement length that is greater than that of a comparable Vickers
indentation, measurement error is smaller in the Knoop method. Therefore, even very
thin layers or foils can be tested better. The Knoop method is also advantageous with
brittle materials, as cracks form more easily around a Vickers indentation.
The Knoop indenter does not produce a geometrically similar indentation as a
function of test force. Consequently, the Knoop hardness will vary with test force.
Due to the elongated shape of the Knoop diamond, any anisotropy that may exist
in individual structural constituents can be ascertained. When this is the case, different
measurements of the crystallite are taken and the specimen is appropriately rotated
before every new measurement.
Knoop hardness testing is described in ASTM Standard Test Method E 384 共see
Section 21.5兲.
21.4 Rockwell Hardness Testing

Due to a number of disadvantages of the Brinell hardness test and the limitations re-
garding testing of steels with high hardness, Stanley P. Rockwell developed a hardness
testing method in 1919. In this method, the hardness of a material is determined by
means of measured indentation depth. A diamond indenter is used for Rockwell C 共see
Fig. 21.8兲 or a tungsten carbide/steel ball is used for Rockwell B. In Fig. 21.8 the follow-
ing symbols and designations are used:
1: Angle of the top of the diamond indenter 共120°兲; 2: Radius of the curvature at the
tip of the cone 共0.200 mm兲; 3: P0, Preliminary test force; 4: P1, Additional force; 5: P,
Total test force 共P0 + P1兲; 6: Depth of penetration under preliminary test force; 7: In-
crease in depth under additional force; 8: e, Permanent increase in depth of penetration
under preliminary test force after removal of additional force, the increase being ex-
pressed in units of 0.002 mm; 9: xxHRC, Rockwell C hardness= 100− e.
It can be seen that the indenter is first pressed a small distance into the material; in
this way the influence of the specimen surface can be excluded.
Rockwell hardness value is calculated by means of a process internal to the ma-
chine with the help of a scale division factor S and a numerical value N.
The simple equation for determining Rockwell hardness is:
HR = N − e/S 共8兲
where
HR= Rockwell hardness
N = Numerical value tied to S
e = Remaining indentation depth in mm
Fig. 21.8—Rockwell C hardness test with diamond indenter, test principle, see text 共ASTM
Standard E 18兲.
S = Scale division in mm
The standard indenters are a diamond cone with 120° apical angles and tungsten
carbide balls with diameters of 1.588, 3.175, 6.350, and 12.70 mm.
The preliminary test force for the Rockwell Standard Method is 98 N 共10 kgf兲; the
possible total force is 589 N 共60 kgf兲, 981 N 共100 kgf兲, 1471 N 共150 kgf兲.
For the Rockwell Superficial Hardness test, the preliminary force is 29 N 共3 kgf兲
and the possible total force is 147 N 共15 kgf兲, 294 N 共30 kgf兲 and 441 N 共45 kgf兲.
Corresponding scales are available for different application purposes and material
groups 共see Table 21.2兲.
Lower test forces are used in Rockwell Superficial Hardness Testing. The prelimi-
nary test force is 29 N and the total test force can be 147 N, 294 N, and 441 N.
Rockwell scales B 共for the steel ball of 1.588 mm diameter兲 and C 共for the diamond
cone兲 are the most frequently used. As in Brinell hardness testing, however, it must be
noted that deformation of the ball can occur in very hard materials with HRB. There-
fore, use of the B steel ball for materials harder than 100 HRB is not recommended.
The test object should lie solidly on the support table 共anvil兲 so that it cannot slip
during the test method. Care must be taken to select the correct indenter and force
when working with thin specimens so that the hardness value of the specimen is not
falsified due to the influence of the support table, the so-called anvil effect. Specimen
thickness should be ⬎15 times the depth of indentation when using a ball indenter and
⬎10 times the depth of indentation with a diamond cone. As a rule, no deformation
should be visible on the back of the work piece after the test.
Indentations should be made at a distance of at least 2.5 times the indentation di-
ameter from the specimen edge. The distance between adjacent indentations should be
three times the indentation diameter.
The preliminary test force F should be produced within 3 s. The usual duration of
stress by the additional force is 1 – 8 s.
Further information about the method can be found in ASTM Standard Test
Method E 18.
TABLE 21.2—Rockwell Scales and Test Conditions for Various Groups of Materials.
Scale Symbol Indenter (Diam.) Total Test Force kgf Application Example
B Steel 共1.588 mm兲 100 Moderately hard, soft steels; brass, bronze, Al
alloys
C Diamond 150 Hardened, tempered steel; hard casting,
materials harder than HRB 100
A Diamond 60 Sintered carbides as well as HRC with low
specimen thickness
D Diamond 100 Thin steel sheets, case-hardened layers
E Steel 共3.175 mm兲 100 Cast iron, Al and Mg alloys, bearing metals
F Steel 共1.588 mm兲 60 Thin, soft steel sheets, annealed copper alloys
G Steel 共1.588 mm兲 150 Copper-nickel-zinc, hard bronzes
H Steel 共3.175 mm兲 60 Aluminum, zinc, lead
K Steel 共3.175 mm兲 150
L Steel 共6.350 mm兲 60
M Steel 共6.350 mm兲 100 Soft bearing metals and thin specimens, very
small balls and heaviest load that does not
give an anvil effect
P Steel 共6.350 mm兲 150
R Steel 共12.70 mm兲 60
S Steel 共12.70 mm兲 100
V Steel 共12.70 mm兲 150
Designation of Rockwell hardness is made by supplying the hardness value fol-

lowed by the abbreviation HR 共for Rockwell hardness兲 and the scale symbol. This gives
information about the indenter and the force. For example, 80 HRC means a Rockwell
hardness value of 80 on the C scale using the diamond cone as indenter.
21.4.2 Rockwell Hardness Testers

Figure 21.9 shows a basic Rockwell hardness testing machine. The testing procedure
differs in two significant ways from the Brinell and Vickers methods described previ-
ously. First, with the help of a hand wheel, the specimen is pressed against the indenter
until the meter indicates the desired preliminary force F0. Then, the additional force F1
is applied for the specified length of time. A further difference lies in the fact that the
Rockwell hardness value HR can be read from the meter immediately after withdraw-
ing the major force.
The significant advantages of Rockwell hardness testing compared to the Vickers
and Brinell procedures include the simpler machine construction without optical mea-
suring equipment, the direct readability of the hardness values, and the less stringent
quality requirements for the specimen surface.
For these reasons, the Rockwell method was quickly adopted and is used primarily
for simple and fast quality control in production.
21.5 Microindentation Hardness

21.5.1 Methods
Measuring methods and machines must be appropriately adapted to perform hardness
measurements on very small objects, thin layers, surface-treated materials, or indi-
vidual structural constituents.
Fig. 21.9—Rockwell hardness tester.2
Microindentation hardness, also often called microhardness, means the determi-

nation of hardness values with low test forces. Compared to the macrohardness testing
methods described previously, the test force range in microhardness testing is very
small. Following the ASTM Standard Test Method for Microindentation Hardness of
Materials 共E 384兲 the range is between 1 and 1000 gf 共9.8⫻ 10−3 and 9.8 N兲, and the
indentations are correspondingly small.
In practice, the geometric forms of the Vickers and Knoop diamond indenters have
proved successful. In addition, the Berkovich diamond indenter must be mentioned.
This is a regular three-sided pyramid with an angle of 142° between the lateral edge and
the opposite lateral face. The indentation surface is an equilateral triangle; the lengths
of its sides are measured.
The hardness value that has already been described, is in any case ascertained by
dividing the test force by the remaining indentation surface.
It is especially important to monitor the loading system regularly, since the hard-
ness error percentage is directly proportional to force error. The total force should be
applied within 10 s, while the duration of the force can range from 10 to 15 s. For
steels, 10 s are sufficient. If longer load times are necessary for softer materials, this
must be indicated in the test protocol.
Vibrations and shaking of the machine must be avoided during measurement.

To achieve precise measurement values, the polished and cleaned specimen surface
should be set up perpendicularly to the direction of indentation. This is the only way to
achieve clearly defined indentations that can be evaluated to a microscopically exact
degree. The smaller the test force and the indentation, the greater the influence of
specimen preparation. For example, excessive polishing can cause cold work of the sur-
face material 共see Part II, Section 13.16兲. Whenever possible, the surface should not be
etched since the indentation otherwise becomes uneven due to the attacked surface
and may be difficult to measure.
See Part II, Table 11.1 and Chapter 13.2.3 for information regarding suitable speci-
men preparation. Small unevenly shaped specimens must be mounted or fastened into
specimen holders. It is important to ensure that the specimen cannot move under the
effects of the force.
21.5.3 Taking the Measurements

The microindentation hardness measurement method takes place in the following
way:
Turn on lighting system and the calibrated hardness tester
Select, carefully clean and apply an indenter
Set or fasten specimen material on table surface
Focus a low-enlargement lens on the specimen surface
Select indentation area, adjust contrast and resolution to optimal values
Remove lens from and move indenter into the operating position
Select force
Activate test, adhere to specified force times
After withdrawing the force, disengage indenter and move lens into measuring
mode
Check indentation for desired position and symmetry
Evaluate
Nonsymmetrical indentations can be caused by the following:
Indenter does not penetrate specimen surface perpendicularly
Specimen surface is not level
Material is textured
Anisotropy of structural constituents
Because microindentation hardness values are strongly influenced by different
components and their size and distribution in the material, it is advisable, depending
on the task at hand, to make several indentations under otherwise identical conditions.
The distance between two Knoop indentations shall lengthwise be ⱖ1.5 d 共length of
Knoop diagonal兲, side by side be ⱖ4 w 共width of Knoop diagonal兲 and the distance to
the edge of the specimen shall be ⱖ3w. The distance between the center of two Vickers
indentations shall be ⱖ4 d 共length of Vickers diagonal兲, and the distance to the edge of
the specimen shall be ⱖ2d.
In ceramics or other brittle substances, the indentation can cause cracks. The
ASTM Test Method for Knoop Hardness for Advanced Ceramics 共C 1326兲 and the
ASTM Test Method for Vickers Hardness for Advanced Ceramics 共C 1327兲 address
more closely the consideration of such special circumstances.
When test forces and indentations are so small, high demands are placed on the
indenter in terms of precision, particularly where the four faces meet. For the Knoop
indenter the line of junction between opposite faces 共offset兲 shall be not more than
1 ␮m in length for indentations greater than 20 ␮m in length, as shown in Fig. 21.7.
For Vickers indenters the offset shall be not more than 0.5 ␮m. Formation of an offset
between the faces cannot occur with the Berkovich indenter, as it has only three faces.
Indenters should be examined periodically and replaced if they become worn,
dulled, chipped, cracked, or separated from the mounting material.
Fig. 21.10—Microhardness testing machine.3
21.5.4 Microindentation Hardness Testers

Figure 21.10 shows a modern microhardness tester. With this machine, Vickers,
Knoop, Berkovich, and Brinell testing procedures can be carried out with adherence to
the most recent ISO and ASTM standards. Machines of this kind operate completely
automatically with motorized lens carousel and autofocus 共motorized z-axis兲. The load
production and the load changes among nine increments 共from 98.07 mN to 19.61 N兲
take place automatically when the duration of load application is between 5 and 999 s.
With the help of a video camera and appropriate measuring and controlling software,
the image of the indentation surface can be transferred to a PC and evaluated there.
Serial measurements are possible in addition to individual tests. Measurement values
can be statistically evaluated 共maximum, minimum, mean values, standard deviation,
histogram兲. Conversion of hardness values 共HR, HB, MPa, etc.兲 occurs automatically.
21.5.5 Examples of Indentations

Figure 21.11 gives four examples of indentations. In Fig. 21.11 共a兲 shows three indenta-
tions in differential interference contrast 共DIC兲; 共b兲 shows Vickers indentations in steel,
indicating the softer ferrite and the harder pearlite; 共c兲 shows the hardness progression
in case hardened steel; and 共d兲 the indentation is in a ceramic material, Si3N4. The
brittle material causes cracks at the corners of the indentation.
21.6 Universal Hardness—Martens Hardness—Instrumented

Indentation Testing—Nano Indentation
The extent of elastic and plastic deformation varies greatly among technical materials.
In rubber, for example, elasticity predominates, and the indentation regresses almost
completely when the load is removed, whereas in materials like lead the hardness in-
dentation is retained. The hardness values of the two materials can therefore not be
compared to each other.
Comparison is possible when the Universal hardness, HU, is calculated. In this
procedure that has been known since 1940, the Vickers hardness is measured under
force. The Universal hardness is calculated from the maximal test force Pmax and the
indentation depth hmax. Universal hardness is now known as Martens hardness, HM
共see below兲.
Fig. 21.11—Examples of Vickers and Knoop indentations. Three Vickers indentations in DIC,
220X 共a兲, indentations in steel indicating ferrite and pearlite, BF 500X 共b兲, progression of
hardness in a case hardened steel, BF, 100X 共c兲, and a Vickers indentation in silicon nitride with
cracks at the corners, DIC, 200X 共d兲.
By means of this procedure, hardness values from all material types can be com-
pared on one scale, which is a great advantage, particularly for industrial purposes.
The Vickers procedure’s visual evaluation of the indentation, along with its possibility
of error, is hereby eliminated. The indentation depth is recorded by measuring tech-
niques that make possible the automation of the procedure.
Additional valuable quantitative information about a material’s elastic and plastic
behavior can be extracted from load-indentation depth curves, Fig. 21.12, that are a
schematic representation of the test force 共indentation-load兲, F, versus depth of inden-
tation 共displacement兲, h. The diagram shows that the depth of indentation 共displace-
ment兲 increases with increasing load. At unloading only the elastic portion of the dis-
placement is recovered, which allows for separation of the elastic properties of the
material from the plastic properties. Based on the maximum depth, hmax and the maxi-
mum load, Fmax, the Martens hardness, HM, previously Universal hardness, can be de-
fined 共see below兲. It is also possible from Fig. 21.12 to calculate the elastic modulus
共Young’s modulus兲 based on the slope of the unloading curve.
Fig. 21.12—Schematic representation of indentation force—depth of indentation 共displace-

ment兲 data during one complete cycle of loading and unloading.
21.6.1 Instrumented Indentation Testing—Nano Indentation

In classical light-optical microhardness testing, even when using automatic machines
with high-grade optical measurement systems, a Vickers or Knoop diagonal length is
recordable to at most 2 – 3 ␮m. This is due to the limited resolution capability. When
working with microcrystalline materials and extremely thin layers, however, hardness
indentations of substantially smaller indentation size are required. This is achieved by
using the testing principle, Instrumented Indentation Testing 共IIT兲, also called nano
indentation. IIT is used for determination of Martens hardness, HM, Indentation hard-
ness, HIT, and Indentation modulus, EIT. The indentation depth 共h兲 is measured and
used to calculate the hardness value. In this way, indentation depths to 0.1 nm can be
recorded and evaluated in adherence to international standards 共see below兲.
Martens Hardness Scale: The Martens hardness value is calculated by dividing the
test force F by the surface area of the indenter penetrating beyond the original surface
of the test piece As共h兲.
For Vickers indenter:
HM = F/As共h兲 = F/26.43h2 共9兲

For Berkovich indenter:
HM = F/As共h兲 = F/26.44h2 共10兲

Indentation Hardness Scale: The indentation hardness HIT is calculated from the
test force, F, divided by the projected area of the indenter in contact with the test piece
at maximum load:
HIT = F/A共hc兲共11兲

where the projected contact area A共hc兲 is calculated from knowledge of the geometry of
the indenter and the stiffness of the contact.
During the indentation the force-trajectory progression can be recorded that gives
significantly more information about elastic-plastic behavior than does a classical in-
dentation for which the size is evaluated. In this way, hardness, elasticity, or viscoelas-
tic properties of paint, varnish, or synthetic layers, galvanized layers, carbide layers of
TiN or TiC, diamond and anodized layers as well as fibers and foils can be determined
and compared. Also, the hardness and elastic modulus of a single grain in a microstruc-
ture can be measured. Fully automated measurement and evaluation ensure high re-
producibility and prevent subjective error.
Instruments for IIT work with test forces down to 1 nN and indentation depths
共displacement兲 down to 0.1 nm. HM can be measured with Vickers and Berkovich in-
denters. For measurements in the nano range the Berkovich indenter, having only
three faces 共see Section 21.5.3兲 is preferred, but other geometries like sphero-conical
indenters are also used.
Instrumented Indentation Testing is described in ASTM Work Item, Practice for
Instrumented Indentation Testing 共WK 382兲 and in the Standard ISO 14577.
21.7 Precision of Hardness Values

The hardness testing procedure takes place in two steps: The production of the hard-
ness indentation and its measurement. The measurement value that is obtained in the
presence of known standard testing machine and specimen conditions is influenced by
the geometric precision of the indentation specimen and by penetration direction, test
force, test time, penetration speed, and temperature. This can lead to constant or vari-
able errors.
For this reason the testing machine shall be verified. The direct verification of the
hardness tester includes the inspection of the force application, the indenters, and the
measuring device at regular intervals. If the test force or the indenter is changed, a new
verification must be performed.
Indirect verification takes place by making a series of at least five test impressions
on a standardized hardness test block. The closer the mean values of the test impres-
sions are to the hardness of the test block, the more exact the hardness tester functions.
The difference in hardness values around a mean value may be an indication of the
precision of the hardness tester: The less difference the higher precision.
A verification report often should be worked out after the verification. The test re-
port should contain the following information: Reference to the ASTM test method.
Method of verification. Identification of the hardness testing machine. Means of verifi-
cation. Type of indenter and test force. The result obtained. Date of verification and
reference to the calibration institution. Identity of the person performing the verifica-
tion.
For specification regarding the single hardness testing method, see the relevant
ASTM standard stated in Section 20.2.
21.8 Conversion of Hardness Values

The conversion back and forth among Brinell, Vickers, or Rockwell hardness values is
possible with the help of conversion tables 共see below兲. The conversion values are solely
empirical in nature.
In certain cases the following equations can be used; these should be considered as
rules of thumb, not as exact as the equations stated in the conversion tables mentioned
below.
Simple Hardness Conversion Equations:
From HB to HV: HB⬃ 0.95 HV

From HRB to HB: HRB⬃ 176– 1165/冑HB
From HRC to HV: HRC⬃ 116– 1500/冑HV
From HV to HK: HV⬃ HK 共in low load range兲
Procedural information can be found in the ASTM Standard Hardness Conversion
Tables for Metals 共Relationship between Brinell Hardness, Vickers Hardness, Rockwell
Hardness, Rockwell Superficial Hardness, Knoop Hardness, and Scleroscope Hard-
ness 共E 140兲. Please refer to ASTM E 140 in the CD-ROM included with this manual.
Values that have been estimated using the equations given above or taken from the
conversion tables should be indicated, stating the original hardness value.
22
Dynamic Hardness Testing
Procedures
IN DYNAMIC HARDNESS TESTING PROCEDURES, THE INDENTER HITS
the specimen surface with impact. The specimen material can thereby be elastically
and unelastically deformed. Deformation that arises due to the kinetic energy of the
indenter and remains can be measured. In such dynamic-plastic procedures, the hard-
ness value is the quotient of the test force and the indentation size. We distinguish be-
tween fall hardness testing and impact hardness testing 共see Fig. 22.1兲.
In the fall hardness testing method 共a兲, an object of defined mass falls freely onto
the specimen along with the indenter 共ball兲 and creates an indentation. In the impact
hardness testing method 共b兲, the ball rests on the specimen surface. Triggered by a
hammer blow or by spring force, an object of known mass is thrust onto the indenter,
which then penetrates the specimen.
One such instrument is the Poldi impact hardness tester, Poldi hammer for short.
The indenter is pressed, by means of a hammer blow, simultaneously into the specimen
and into a comparison rod of known Brinell hardness. The HBP hardness can then be
determined by comparison.
With the Baumann hammer, the indenter is driven into the specimen surface by
means of spring force. The indentation is measured and assigned a corresponding
Brinell hardness value.
Fig. 22.1—Principles of dynamic hardness testing procedures, schematic. Rebound with drop
共a兲, and rebound with spring loaded hammer and ball placed on the work piece 共b兲.
644
Chapter 22 Dynamic Hardness 645
Fig. 22.2—Types of rebound hardness testers, schematic. Hardness value based on height of
rebound 共a兲, and hardness value based on rebound angle 共b兲.
In dynamic-elastic hardness test procedures, the rebound height, or rebound

angle is measured 共see Fig. 22.2兲. In materials with low deformation potential, such as
tungsten carbide or rubber, the indenter, which hits the specimen surface at a defined
velocity, springs back. We can infer a hardness value from the rebound height that is
proportional to the rebound energy. Such dynamic-elastic procedures also include the
Shore hardness testing method and the Equotip method.
The Scleroscope functions according to the drop hammer principle. The indenter
is either a rounded diamond point of a particular size and shape or a steel ball that rests
on a drop hammer. This falls through a pipe vertically onto the specimen and rebounds
again up to a particular height 共Fig. 22.2共a兲兲. This rebound height is a measure of hard-
ness that is given in Shore hardness values. In the Model C Scleroscope, a high-
precision, low-friction glass pipe is used. The rebound height can be recorded on a
scale of 0–140, and the hardness can be read in HSc. In the Model D Scleroscope, the
hammer is automatically detained after reaching the rebound height, and height and
hardness are then recorded using technical measuring instruments. Since the hammer
is larger and heavier compared to the one used for the Model C, the fall height can be
reduced without changing the impact energy. The hardness values are given in HSd.
Depending on the machine model, application, and test material, various indenters
and scales are used. More exact guidelines are found in the ASTM Standard Practice E
448.
The Equotip tester functions according to the drop hammer principle. A carbide
ball 3 mm in diameter is used as indenter. After the release of a preloaded spring, the
indenter is thrust against the test specimen. Impact and rebound velocity of the ball are
electronically measured at a distance of 1 mm above the test surface. From the rela-
tionship between these two velocities we can ascertain an L hardness value 共named
after D. Leeb, the machine’s inventor兲. Hardness measurements of up to approximately
1200 HV can be calculated with this method.
The advantages of the portable machines described above include their suitability
for use on slanted surfaces and the short duration 共only a few seconds兲 of the test proce-
dure. The disadvantage is that these methods do not supply the hardness values with
the same high precision as the static hardness testers.
23
Special Methods for Hardness
Testing
SPECIAL HARDNESS TESTING PROCEDURES INCLUDE THE MARTENS
scratch hardness determination as well as the Mohs scratch hardness. In the Martens
procedure, a specimen surface under a specified test force is scratched by a diamond
cone with a 90-deg apical angle. The test force F is varied until a scratch width of 10 ␮m
is microscopically measured. In this way, a particular scratch hardness value can be
attributed to the specimen.
There are continuous test procedures that allow us to record hardness progression
curves for case-hardened or nitrided steels. In these, the width of the scratch that ap-
pears is evaluated, at a constant test force, in light of the scratch length. Or, the force
trajectory-dependent indentation process may be recorded by means of technical mea-
surement instruments, much as is done in instrumented indentation testing 共see Sec-
tion 21.6.1兲.
References „Part V…
关1兴 Courtesy of Deutscher Verlag für Grundstoffindustrie.
关2兴 Courtesy of Emco-Test Prüfmaschinen GmbH.
关3兴 Courtesy of Struers A/S.
646
Part VI:
The Metallographic/Materialographic
Laboratory
24
Introduction
24.1 Establishing a Metallographic/Materialographic Laboratory
WHEN ESTABLISHING A METALLOGRAPHIC/MATERIALOGRAPHIC LABO-
ratory, many conditions have to be taken into consideration. The two main conditions
are: 共1兲What is the purpose of the metallographic/materialographic examination? Is it
quality control, research, education, etc.?; 共2兲 What is the specimen volume; few or
many specimens per day?
Another important condition is the degree of automation of the preparation pro-
cess. This really depends on the volume of specimens to be prepared and the size of the
specimens, as well as the specimen quality 共reproducibility兲. The occupational situa-
tion for the persons performing the preparation should also be taken into consider-
ation.
Chapter 25 discusses the above-mentioned conditions and other important mat-
ters connected to planning for and establishing a metallographic/materialographic
lab, and suggestions for a number of laboratories suited for different purposes and ca-
pacities will be given.
24.2 Running a Metallographic/Materialographic Laboratory

The metallographic/materialographic laboratory should be considered a production
unit, producing specimens of the desired quality at the lowest price. This means that
correct planning must be made, covering both the day-to-day operation and preventive
maintenance.
24.3 Occupational Safety and Health

The work in the laboratory involving machines, chemicals, etc., makes it imperative
that all relevant rules and regulations covering occupational safety are followed. This
subject is described in Chapter 26.
649
25
How to Build a Metallographic/
A LABORATORY IS SELDOM BUILT FROM SCRATCH. AN EXISTING LABORA-
tory should usually be changed, possibly moved to other locations, etc. In all these
cases it is very useful to analyze a number of factors regarding the laboratory so that
the right changes, gradually, can be made.
25.1 Purpose
The purpose of the laboratory as part of a larger organization should be considered.
The purpose may be quality inspection of parts from a running production, meaning
that the preparation with examination result should be finished in a short time, or a
research lab with large test series that can be prepared at a steady speed with ample
time available.
Three purposes together with the capacity, number of specimens to prepare per
week, should be discussed here.
25.1.1 Quality Control „QC…

The laboratory performing quality inspection ranges from the relatively small sub-
supplier, who prepares a few specimens per week, to the large lab with several hundred
specimens per week.
In both cases, the specimen size and the materials to be prepared are known and
often of a limited number. This means that fixed documented procedures can be estab-
lished. This ensures the reproducibility that is very important if the analysis over a pe-
riod of time shall provide a true picture of the product quality.
Although a smaller lab with few specimens per week could prepare the specimens
by hand and still be rational, the preparation should be performed with a small semiau-
tomatic grinder/polisher to secure the reproducibility. This also makes it possible to
use a rather untrained person for the preparation, which can be of advantage, when the
specimen volume is low, and it is not possible to have a full-time person on the job.
A lab with higher volume will use semiautomatic or fully automatic equipment to
have rational specimen production, at the same time securing reproducibility and a
programmed process.
The “cost per specimen” is important 共see Section 25.2.2兲.
If preparation time is important, electrolytic polishing should be considered if the
materials are suited for this 共see Chapter 8兲.
A QC lab often will have the advantage of digital imaging connected to a system for
registration, connecting the metallographic/materialographic analysis with other tests
like hardness, etc. 共see Chapter 19兲.
If a QC lab also makes failure analysis, this might indicate other types of equip-
ment 共see below兲.
650
Chapter 25 How to Build 651
25.1.2 Research and Education
Research
Like the QC lab, the research lab needs a high reproducibility to secure correct inter-
pretation of the materials being developed. For this reason, semiautomatic equipment
should be used. This equipment should have a reasonable capacity, but the production
of specimens can usually be planned for and “high-production” equipment is not
needed.
For research, typically a wide spectrum of materials should be prepared and the
equipment should preferably be for mechanical preparation. Electrolytic polishing
and thinning 共TEM兲 could be interesting also, electrolytic polishing resulting in
“deformation-free” specimens 共see Chapter 8兲.
Education
As part of education in physical metallurgy, the students often have to prepare one or
more materials, both to experience the metallographic/materialographic process and
to be able to see a prepared microstructure in a microscope with their own eyes.
A group of students usually works with specimen preparation at the same time,
and this can be done on a number of small grinder/polishers, either by hand or with a
simple semiautomatic specimen mover.
Education is often connected to a research lab, but equipment used for research
should not be used by the students for educational purposes.
25.1.3 Testing and Inspection Laboratories—Failure Analysis

Laboratories established for preparation of specimens for customers should be able to
prepare “all materials” for a wide number of examinations. The job may be just one
specimen representing a failure, a special case 共archaeology, forensic兲, or a series of
specimens. For this reason, equipment for both mechanical preparation and electro-
lytic polishing should be available, “high productivity” playing a minor role, with the
possibility of preparing all difficult materials playing a major role. Preparation of
specimens for failure analysis is often difficult because the specimen is not “regular,”
but has to be taken from a work piece at a special location, and the area to be prepared
is often difficult to establish. In certain cases hand preparation is preferred, but in most
cases the specimen can be mounted so that a semiautomatic grinder/polisher can be
used. Therefore, even large laboratories with advanced automatic equipment, some-
times engaged in failure analysis, need a small semiautomatic machine for single
specimens.
25.2 Rationalization and Automation

The demand for more cost-efficient processes and procedures has been increasing in
all parts of the society for a long time. In the metallographic/materialographic lab, the
focus is on “cost per specimen,” including all the costs covering manpower, equipment,
consumables, locations, administration, energy consumption, etc.
Examples are changes in the production, the organization, or the requirements to
documentation. As a result, the lab has to produce more specimens without increasing
the personnel, or the quality of the specimens should be improved because an auto-
matic image analyzer has been installed. Improvements in quality have to be made very
often without a similar increase to the budget.
The demand for a higher specimen quality and a better reproducibility is also in-
creasing because of quality standards like ISO 9000 and IS 9000.
Rationalization can often be made in all steps from the work piece/specimen arriv-
ing in the lab to the finished report leaving the lab. This can be in specimen handling,
choice of equipment, preparation procedures, and administrative routines, including
writing of reports and filing the micrographs. At the same time the occupational safety
can very often be improved.
Automation according to the “state-of-the-art” is limited to the preparation pro-
cess from plane grinding to the finished specimen and to the automatic printing of mi-
crophotographs through digital systems 共see below兲. In case of image analysis, this can
also be automatic 共see Part IV兲.
25.2.1 Reproducibility—Standards—Occupational Safety

Basically the only assurance that a microstructure is “true” depends on the evaluation
done by the person who is interpreting the structure. In most technical matters, the
result can be measured and the correctness be verified, but this is not possible with a
microstructure. A high element of subjectivity is present when it should be decided
whether a microstructure is “true.” It is very possible, of course, to measure the struc-
ture using image analysis, but whether the microstructure being measured is the true
structure representing the work piece material, or not, is based on the evaluation of an
experienced person.
For this reason, it is very important that methods are developed, documented, and
followed when making a preparation. A proven method “guaranteeing” the true struc-
ture, executed on a machine with constant parameters and uniform consumables,
makes it possible 共with a high certainty兲 to say that a running production of specimens
is correct. As soon as human treatment is involved, the risk of an incorrect result will
increase.
In modern quality control 共QC兲, according to standards like ISO 9000 and IS 9000,
the correct measurement of all results is very important. Therefore, in the case of
metallography/materialography, the microscope should be calibrated regularly to en-
sure that the analysis is correct. It is very difficult, however, to give correct “measuring
data” for the preparation process, securing a correct preparation, as mentioned above.
Therefore, the responsibility of the correct structure is transferred to the skilled person
evaluating the microstructure, and to support this, a documented procedure using
semiautomatic or automatic preparation equipment should be worked out.
In a number of ASTM standards, such as Standard Test Methods for Determining
Average Grain Size Using Semiautomatic and Automatic Image Analysis 共E 1382兲, the
preparation is part of the standard, spelling out that the “true structure” must be avail-
able at a high reproducibility. In most cases, however, the methods for a given material
must be worked out in the laboratory 共see Section 13.2.3兲.
Occupational safety and health play an increasing role, both regarding the physi-
cal work done by the operator and the total laboratory environment 共see Chapter 26兲.
Using semiautomatic or fully automatic equipment for cutting-off, mounting, and
preparation will reduce the amount of physical power needed and, when possible, the
equipment can be connected to an exhaust system to avoid contaminating the air.
25.2.2 Productivity—Cost Per Specimen

Essentially the preparation of a specimen can be seen as a “production” as any other
item made in a production facility. This means that preparation should be constantly
analyzed according to the following demands:
• Increased productivity
• Improved quality
• Cost reduction
The increase in productivity can be obtained by analyzing the whole preparation
process and calculating the cost per specimen 共see below兲.
Improved quality can often be achieved by using semiautomatic or automatic
equipment. This also usually provides increased productivity. Cost reduction can often
be obtained by reducing the cost per specimen, but other factors should also be ana-
lyzed to give the most cost-efficient function of the total metallographic/material-
ographic lab.
The following should be taken into consideration:
Development of the correct application for each material: It is very important that
the optimum process is found for a given material. One or more preparation steps can
often be omitted or times can be reduced.
Training of Personnel: The persons responsible for the preparation should be
trained to optimize the use of equipment and consumables.
Service: The equipment should be serviced regularly 共preventive servicing兲 to
avoid breakdowns. If breakdowns happen, a service support should be available from
the supplier, keeping the downtime short.
Cost per Specimen

A cost-savings analysis must be made to decide on the present cost per specimen and a
possible lower cost per specimen.
The analysis is supposed to show all costs involved in making a specimen.
• Operator costs
• Consumable costs
• Depreciation of equipment
The first step in the analysis is to decide on the actual costs.
Operator costs are calculated for the total operator time used per specimen from
receiving the work piece 共specimen兲 through to a prepared specimen that is ready for
the microscope. Consumable costs are calculated by listing all consumables used for
each preparation step and calculating the amount used per step.
For the equipment, the service costs and depreciation costs are calculated, the lat-
ter based on the total investment in equipment, time of depreciation, and the interest
rate.
The cost per specimen will usually be lower when using more automatic prepara-
tion equipment, and often depends on the number of specimens made per day. In Fig.
25.1, two curves are shown indicating the cost per specimen for a highly automated
machine 共Equipment 1兲 and a relatively simple piece of equipment 共Equipment 2兲. It
can be seen that around 55 specimens per day, the price per specimen is lower using the
expensive machinery.
The Payback Time is interesting too. This indicates the time for how long the new
equipment should operate before the savings are so high that the investment is “paid
back.” Figure 25.2 shows an example of Equipment 1 mentioned earlier. The Payback
Fig. 25.1—Cost per specimen. Comparison between preparation with a highly automated
machine 共Equipment 1兲 and a relatively simple piece of equipment 共Equipment 2兲.
Time shows that the expensive 共automatic兲 equipment 共Equipment 1兲 is paid back in
one year when approximately 38 specimens are prepared per day.
Additionally, the advantage of having a higher certainty for correctly prepared
specimens should be taken into consideration also, supporting the procurement of au-
tomatic equipment.
25.3 Planning the Metallographic/Materialographic Laboratory

25.3.1 Basic Planning
The metallographic/materialographic lab, like all other investments, should be subject
to a total cost-benefit analysis. It is, however, not as easy to calculate as the more
straightforward processes like a production facility. The lab is a mixture of production
共specimen preparation兲, analysis, reporting, and other administrative work, often with
a high variation in the work load.
The metallographic/materialographic lab is established like any other lab, but a
number of specific features should be evaluated.
The lab should be split into several rooms, the basic parts including a room for
cutting, a room for preparation, and a microscope room.
Fig. 25.2—Payback time. Payback time in years in relation to number of specimens per day for
Equipment 1 in Fig. 25.1.
A good workflow should be secured. Considering the number of apparatus, the in-
stallation of electric power 共both 1-phase and 3-phase兲, compressed air, water drains,
and ventilation should be made flexible and easy to maintain The floor load should also
be taken into consideration.
Because of the relatively large machines used in materialographic preparation, the
passages and doors need to be wide enough so that machines up to 1.3 m 共4.3 ft兲 can
pass through.
A person’s workplace in the lab should have the best possible lighting 共daylight兲,
low noise level, and correctly placed fume hoods.
A 20–25 % spare area should be designed, if possible, to make room for future ex-
pansion.
It is important to consider all demands regarding safety 共cupboard for first aid,
etc.兲共see Chapter 26兲.
With both basic and detailed planning it is important that the personnel already
using the lab, or intending to work in the new lab, participate in the planning work.
This ensures that a lot of problems are solved in the planning stage and the most effi-
cient function is obtained.
25.3.2 Detailed Planning

Factors like type of specimen material, number of specimens to prepare, etc., will influ-
ence the details in the lab.
Specimen Material
The specimen material influences the type of equipment used. If only one type of mate-
rial is to be prepared, relatively simple machinery may be used. In the case of a vast
spectrum of materials, more machinery may be needed because of the different prepa-
ration methods needed.
Number of Specimens
The average number of specimens per day will vary very much from lab to lab. A QC lab
might have a hundred or more specimens per day, maybe in working shifts. In this case,
a very rational preparation can take place 共see Section 25.2兲. In a research lab perhaps
only ten specimens per day are made on average, but the materials span widely so that
several types of preparation processes are available.
In some cases with very few specimens, the preparation might be performed in the
“Chemical Lab” or “Materials Testing Lab.”
The Specimen Size and Shape

In some cases the lab receives the specimens cut to the right size. In other cases large
work pieces, machine parts, or stock material are received and the lab should take care
of cutting out the specimen. This may require a special room for cutting, often with
large machines.
The mounting of the specimen will vary. In mounting a large number of speci-
mens, a special room for hot mounting presses should be considered. In the case of
cold mounting, fume hoods must be available.
Type of Examination
For labs working with QC or other types of inspection, the lab might be under time
pressure, being required to deliver an analysis result in a given period of time. This
influences how the lab is organized, securing fast results and reporting, effective com-
munication, etc. In some cases, the metallographic/materialographic analysis is com-
bined with other examinations, like hardness testing, and care should be taken that
these other instruments are integrated in the best possible way in the lab. In some labo-
ratories, the specimens, before or after preparation, have to be treated in other labora-
tories and a rational cooperation must be secured. Using a digital camera, the images
often necessary for reporting can easily be communicated, avoiding the more tedious
photographic work.
Personnel
Persons with different educational background and training are needed in the
metallographic/materialographic lab. Cutting, mounting, and preparation work can
be done by persons with little or no metallographic/materialographic background. For
persons without knowledge of metallography/materialography, they should be trained
thoroughly before starting the work because lack of knowledge may jeopardize the
preparation result.
Interpreting the microstructure, working out reports, etc., should be performed by
persons with the necessary education in metallography/materialography. In spite of
the increasing use of semiautomatic equipment, it should be emphasized that the per-
sonnel should be well trained and be allowed to develop experience over a long period
of time.
25.4 Equipment and Laboratory Layout

A large selection of equipment for preparation, examination, and reporting 共IT兲 is
available in the market. The tendency goes towards automation both regarding prepa-
ration and analyzing, where the result will now be electronically communicated in IT
networks.
It is important to select the right equipment, both to secure a high quality, cost-
efficient production of specimens and to secure a certain flexibility 共increase兲 in the
number of specimens to be prepared and analyzed. Table 25.1 gives an overview of the
equipment needed for a metallographic/materialographic lab, and in the following sec-
tions examples for different labs are given.
The layout of the lab with several rooms and the correct installations, etc., also
plays an important role to ensure an efficient specimen production. This will be dis-
cussed below.
25.4.1 Equipment—Table 25.1

The basic equipment is stated in Table 25.1, but in each category several models are
available, e.g., a grinder/polisher can be hand-operated or automatic 共see Chapter 7兲.
In the following sections some examples are given for different sizes of labs, indi-
cating the types of machines.
Small Laboratory
A laboratory with only one to ten specimens per day can be defined as a small lab. This
type of lab can be at a sub-supplier to a large company, where a metallographic/
materialographic examination is part of the specifications for the supplied product.
The following equipment should be available:
TABLE 25.1—Equipment, Accessories, and Consumables for a Metallographic/Materialographic Laboratory.

Accessory/
Preparation Stage Process Equipment Consumable
Sectioning Wet abrasive cutting Cut-off machine Cut-off wheels,
Precision cutting Precision cutter additive for cooling
fluid
Shearing Shear
Sawing Hacksaw Saw blades
Bandsaw Saw bands, cutting fluid
Wire cutting Wire cutter Wire
Mounting Hot compression Hot mounting press Hot mounting resins
mounting
Cold (castable) Mounting molds Cold mounting resins
mounting
Heating of epoxy Small oven Cold mounting epoxy
Clamping (sheets) Clamp
Impregnation Vacuum impregnation Resins with low viscosity
apparatus
Vacuum pump Dye
Marking Engraving Engraver Engraving needless
Surface preparation— Grinding Plane grinder with Grinding stones,
mechanical grinding stone additive for cooling fluid
Grinder/Polisher/ Disks (platens),
sample mover rigid composite disks
(RCD),
wet grinding papers,
diamond disks
Belt grinder Grinding belts
Mechanical polishing Grinder/polisher/sample Disks (platens),
mover polishing cloths,
Vibratory polisher diamond consumables,
lubricants,
oxide consumable
(Al2O3, SiO2)
Dispensing of diamond Dosing unit Diamond suspension
suspension
Surface preparation— Electrolytic polishing Electropolisher Electrolytes
electrolytic Electrolyte containers
Thinning for TEM Electrolytic polishing Jet-thinning apparatus Electrolytes
Cleaning Ultrasonic cleaning Ultrasonic apparatus Cleaning liquids
Ethanol, cotton
Drying Drying apparatus
(hair dryer)
Conservation Desiccator Desiccants
Special cupboard Protective media
Etching Chemical etching Plastic container, pair of Etchants
tongs
Electrolytic etching DC-power supply with Etchants
pair of tongs
Accessory/
Preparation Stage Process Equipment Consumable
Potentiostatic etching Potentiostat
Thermal etching Oven
Vapor deposition Vacuum chamber
Sputtering
Ion etching
Examination Optical microscopy Magnifying glass, Objectives
Light microscope, small, Eyepieces
medium, large
Stereomicroscope
Image analysis system
Electron microscopy SEM Sample mounts
EPMA
TEM
STEM Sample mounts
Documentation Microscopy Macro camera Films, paper
Micro camera
Polaroid camera
Digital camera
PC with monitor
Video equipment
Printer
Cutter
Refrigerator
Indentation hardness Vickers/Knoop Microhardness tester Indenters
testing microindentation
hardness
Brinell/Vickers hardness Universal hardness tester Indenters
Rockwell hardness Rockwell hardness Indenters
tester
Sectioning: Cut-off machine, table top, hand operated, cut-off wheel diameter
200– 250 mm 共8 – 10 in兲. For an examination of sheet products, a hand shear should be
available. A vertical band saw might be useful also.
Mounting: Cold mounting materials with mounting cups or a hot mounting press,
or both, if the investment is justified. In the case of sheet specimens, a clamp can be
used for manual preparation.
Plane grinding/Fine grinding/Polishing: Rotating grinder/polisher 共2 speeds兲, 200
or 250 mm 共8 or 10 in兲 disk diameter. This is sufficient for manual preparation, but to
ensure highest reproducibility and avoid tedious work, a small specimen mover for
three or six specimens should be mounted on the grinder/polisher. This also ensures a
relatively high quality of the specimens, even with a relatively unskilled operator. A
dosing unit, adding diamond suspension and lubricant in an optimal way, will also im-
prove quality and economy.
Microscope/Documentation: A small or medium-sized light microscope with
bright field/dark field and differential interference contrast 共DIC兲 is recommended 共see
Part III兲. For making images for reporting, a Polaroid 共4 in⫻ 5 in兲 or digital camera
should be used, the latter in connection to a PC and a printer.
Medium-Sized Laboratory
A medium-sized lab will prepare three to fifty specimens a day, mounted or unmounted
共see Table 25.1兲.
The following equipment can be recommended:
Sectioning: Cut-off machine, table top or floor model, automatic feed, cut-off
wheel diameter 250– 350 mm 共10– 14 in兲. For large work pieces, larger automatic ma-
chines with a wheel diameter up to 600 mm 共24 in兲 are needed 共see Section 2.5兲. If pre-
cision cutting or cutting with lowest possible deformation of the cut surface is needed,
a precision cutter should be available. A bandsaw can also be useful, and a hand shear
can be used for sheet products.
Mounting: One or two hot mounting presses and consumables for cold mounting.
A vacuum impregnation apparatus and a small oven for accelerating the curing of ep-
oxy cold mounting resins might be included.
Plane grinding: With large specimens and a relatively high production with the
specimens fixed in holders, a special plane grinding machine is recommended using a
grinding stone. In most cases, however, the plane grinding can take place on the same
machine as for fine grinding/polishing.
Fine grinding/polishing: This is preferably done on a table model, semiautomatic
system, consisting of a grinder/polisher with a 250 or 300 mm 共10 or 12 in兲 disk and
specimen mover with specimen holders for fixed or single specimens, or both, which
can prepare up to six to eight specimens at a time. To obtain the highest reproducibility
a semiautomatic, programmable system with a dosing unit included is recommended.
In case of a relatively high production of larger specimens, a floor-based, program-
mable grinder/polisher, using specimens fixed in a holder is recommended.
To save manpower and increase the reproducibility, a fully automatic preparation
system could be used. A fully automatic system might show a favorable cost/benefit
共see Section 25.2兲, especially for difficult to prepare materials.
An electropolisher could be of advantage as a supplement to the mechanical
preparation equipment, depending on the type of material to be prepared 共see Chapter
8兲.
Etching: Chemical etching is typically used and needs only a very low investment
共see Table 25.1兲. If other contrasting methods should be used, like thermal etching or
interference layers, special equipment must be procured 共see Table 25.1 and Chapter
9兲.
Microscopy/Documentation: A good quality light microscope with good optics
should be available. This shall have bright field/dark field, polarized light, differential
interference contrast 共DIC兲, and fluorescence.
For documentation one or more of the following cameras should be available:
A normal, single lens reflex camera 共35 mm兲, a Polaroid camera 共4 in⫻ 5 in兲, or a
digital camera. For all types, an automatic control unit should be connected to the mi-
croscope. For a digital camera, a PC with monitor should be available and a printer.
For macro work, a stereomicroscope with camera connection should be available.
A camera for macrophotography should be available also.
Large-Sized Laboratory
The large laboratory has from 10– 100/ 200 specimens per day, and the specimens pro-
duced are very often for quality control relating to a production. Therefore, the main
concern is to have a fast, efficient flow of prepared specimens.
The following equipment can be recommended:
Sectioning: The conditions are the same as mentioned above under the Medium-
Sized Laboratory.
Mounting: The conditions here are also close to the medium-sized lab, only a
larger number of mounting presses may be needed.
Plane grinding: With a large number of specimens and using specimen holders
with fixed specimens, plane grinding can be a bottleneck; therefore, a special plane
grinding machine is recommended, using a grinding stone. In some cases, the plane
grinding will be part of a fully automatic system 共see below兲.
Fine Grinding/Polishing: With a large number of specimens, handling, manual
cleaning, etc., should be avoided to save time. Therefore, fully automatic systems with
a high number of preparation programs and built-in dosing and cleaning are recom-
mended. These systems can be used for both “normal” specimen sizes and for large,
unmounted specimens. The only manual handling is placing the specimens in a holder
and removing the finished specimen ready for etching/microscopy from the holder.
An alternative is one or more of the systems described above under Medium-Sized
Labs. Electropolishing may be useful also, as mentioned above.
Etching/Microscopy/Documentation: This is the same as mentioned under
Medium-Sized Labs.
25.4.2 Layout—Furniture—Installations
The layout of a metallographic/materialographic lab should include several rooms,
making it possible to keep the different activities separated. The furniture should be
appropriate and the installations specifically made to ensure an effective working pro-
cedure.
The space between tables and machines should be so that several persons can
work and move around in the lab without disturbing each other. During planning,
space should also be reserved for extension considering a period of three to five years,
often, a relatively new lab gets crammed after a few years.
Rooms
A metallographic/materialographic lab should have at least three rooms, each con-
nected with a door for easy passage from room to room. A lab for quality control pur-
poses could have three rooms, and a research lab, covering a wide material field and
many different processes might have four rooms.
Room 1: This is the room for “dirty” processes, sectioning, and mounting. If cold
mounting is performed in this room, a fume hood should be installed. Plane grinding
also may be done in this room if a special machine is available for plane grinding. A
sink should be installed in this room, and the idea is that a specimen, leaving the room,
is clean and ready for the proper preparation in Room 2.
Room 2: This is the main area of the lab, containing a preparation area and possi-
bly an area for the personnel for working out preparation reports, etc. 共see below兲. Ma-
chines for preparation should be placed so that persons passing by do not disturb the
operator. Table space around a machine should be 80– 100 cm 共3 – 4 ft兲 to ensure an
efficient working order and make room for possible service work on the machine.
At least one or two sinks should be placed very close to the grinder/polisher. It must
be understood that cleaning is a very important part of the preparation process, and the
operator should be able to clean the specimens when only moving a few steps.
Another sink is placed under a fume hood to be used for chemical etching. The
same hood, if large enough, can be used for electrolytic polishing, with the polishing
table being placed under the hood.
A small, low cost, upright or inverted microscope, placed near the preparation ma-
chines, is also useful to examine the specimens between the preparation steps. Other
instruments like hardness testers are also placed in this room. Space should be avail-
able for desks with PCs for the personnel, preferably separated from the machine area,
if these are not placed in connection with Room 3 together with the microscopes.
Room 3: This is the microscope room with a large microscope and possibly a
stereomicroscope and other examining instruments. The working places for the per-
sonnel can be placed in this room also, separated from the microscopes, preferably as a
separate “office.” In the ideal microscope room, an air conditioning system keeps a
constant temperature. Specimens can also be stored in this room in a desiccator 共one
for each metallographer兲 or a special cupboard.
Room 4: In certain cases, a fourth room may be recommended. This room will take
over the “etching functions” of Room 2. The room will have one or two fume hoods for
etching, electro polishing, and other processes that must be kept under strict control.
Darkroom: For photographic work, one or two darkrooms will be necessary, but
this won’t be necessary if only digital photography is used.
Furniture
Laboratory furniture is available from many suppliers, but it should be taken into con-
sideration that this furniture is made typically for chemical labs, not metallographic/
materialographic labs. The most important points to observe are the following: The
metallographic/materialographic machine has a certain height, and the working area
of the machine is often too high for convenient work if the table is a normal lab table.
The surfaces of tables, etc., should be resistant to acids, alcohol, etc. Drawers for the
grinding/polishing disks should be available, preferably placed under the tabletops
very close to the machines. Shelves for consumables like cut-off wheels, grinding pa-
per, etc., and storing space for other consumables, specimen holders, etc., should be
close to the machines, and correctly made storage space for chemicals, glass articles,
etc., should be close to fume hoods. Channels for taking pipes, tubes, and cables to the
machines should be made in the tables.
Other furniture is solid tables for microscopes, special cupboards for storing of
specimens, cupboards for archiving, etc., shelves for a small library, and a refrigerator
for storing of polaroid films, etc.
Installations
The metallographic/materialographic lab should have the following installations:
Hot/cold water at all sinks and compressed air preferably at all sinks and at all
tables and places to be used for equipment. The compressed air should be clean, pass-
ing a water/oil separator and a particle filter. Adequate three-phase and one-phase elec-
tricity should be taken to all tables and places to be used for equipment, especially cut-
off machines require a high amperage.
Drainage should be installed in all tables and places to be used for equipment. The
drainage should be made according to the regulations of the local authorities, taking
into consideration that acid and other chemicals together with debris from the prepa-
ration process will flow in the drainage system.
For installations regarding protection of personnel see Chapter 26.
25.5 Maintenance
The most obvious reason for maintaining the laboratory in good working order is
economy. A badly organized laboratory that cannot carry out its work properly and
timely can cause unnecessary additional lab expenses and costs due to delayed produc-
tion.
Another important reason to focus on quality inspection and competitiveness is
that the laboratory is a showcase for the company. Any manufacturing company that
wants to attract customers and convince them of the quality of its goods needs a well
equipped and presentable laboratory. A well run metallographic/materialographic
laboratory with a good working atmosphere will reflect positively on the company’s
image.
The maintenance can be split into organizing, cleaning, and servicing.
25.5.1 Organizing
Accessories and consumables for machines should be in easy reach of the operators.
Special lab furniture or wall shelves help to keep grinding paper, cut-off wheels, polish-
ing cloths, and disks out of the way but still accessible. In a metallographic/materialo-
graphic lab a large variety of small items are needed in everyday operation. Small tool
or tackle boxes help to keep screws, tweezers, springs, rings, “dummy” samples in or-
der. Wire racks over the sink are essential for storing wet glassware.
It is always important to have enough consumables available to guarantee uninter-
rupted work.
Large quantities of consumables should not be stocked in the laboratory, but in the
main storeroom because they take up too much of the valuable space in the lab.
25.5.2 Cleaning
Keeping the machines and work area clean is one of the most important matters in a
metallographic/materialographic laboratory. Every machine should be wiped clean
with a wet cloth before the staff leaves in the afternoon. This should also be done before
shift change, so that the incoming operators start with clean machines. If this routine is
not possible, a specific day or time should be set aside each week for cleaning the ma-
chines.
Recirculation cooling units have to be cleaned and refilled at regular intervals, at
least once a month depending on the workload. The spray nozzles of certain automatic
diamond dispensing systems must be cleaned occasionally to avoid drying of the dia-
mond suspensions inside the nozzles.
As a rule, rigid composite disks 共RCDs兲 and polishing cloths should not be cleaned
regularly. However, they can be cleaned with water/soap or ethanol, or both, if too
much debris has built up on the surface and stops them from grinding/polishing prop-
erly, or if they are contaminated.
25.5.3 Servicing
Regular service checks ensure that the equipment is always in a correct working condi-
tion. This is crucial because correct maintenance is the basis of reliability, avoiding
irritating stops, and reproducibility, and securing the correct preparation result, even
over a long period of time.
26
Occupational Safety and Health in
the Metallographic/
OCCUPATIONAL SAFETY AND HEALTH ARE IMPORTANT IN A METALLO-
graphic/materialographic labs considering the use of machines, chemicals, plastics,
etc.
The dangers in the metallographic/materialographic laboratory will be discussed,
and a special section will describe dangerous and hazardous materials. In Section
26.1.8 the ASTM Guide for Metallographic Laboratory Safety 共E 2014兲 will be shortly
described, the only standard specifically covering the safety in the metallographic/
materialographic lab. The standard is stated in full in the CD-ROM included in this
manual.
At the end of this chapter, the most important rules and regulations for safety and
health covering the metallographic/materialographic lab will be stated.
26.1 Dangers in the Metallographic/Materialographic

Laboratory
The laboratory having functions like cut-off, specimen preparation, and etching in-
volves a number of potential dangers. In the following the most important precautions
regarding safety and health are mentioned, not claiming that all potential dangers and
necessary safety and health measures are mentioned.
26.1.1 Sectioning
Eye protection and gloves should be used when working with machines and tools for
sectioning. Abrasive cut-off machines will have a hood 共shield兲 protecting the operator
against cooling fluid, pieces from a broken cutting wheel, etc. According to safety regu-
lations, the machine can only be started when the hood is closed. When cutting with
bakelite or rubber wheels, fumes develop, and at larger machines the cutting chamber
should be connected to an exhaust system.
For bandsaws, the operator will guide the work piece into the band, and it is very
important that this is done indirectly using a distance piece or a special holder for the
work piece.
A Standard Operating Procedure 共SOP兲, including a Job Safety Analysis 共JSA兲共see
Section 26.2.3/4兲 should be completed for each piece of equipment being used for
sectioning.
26.1.2 Mounting
With hot compression mounting, the main danger is the high temperatures used in the
mounting presses. Gloves should be used for handling of the hot mounts, and when
664
Chapter 26 Occupational Safety and Health 665
filling mounting material such as bakelite powder into the press, inhalation of dust
should be avoided.
A SOP, including a JSA, should be completed for each piece of equipment.
At cold 共castable兲 mounting there are several potential dangers. The cold mount-
ing resins are potentially dangerous to health 共see Section 26.1.7兲, and therefore all
handling should be done with rubber 共latex兲 gloves to avoid skin contact and the mixing
and hardening shall take place under a fume hood. When using an oven for accelerat-
ing the hardening of epoxy, gloves should be used.
MSDS information should be available for all mounting resins 共see Section
26.2.2兲.

The semiautomatic preparation machines are basically safe to use. If a specimen is
slung away from the specimen holder during rotation, the specimen will usually be
kept inside the machine, and the speeds of the disks and holders are relatively low. To
avoid dirty hands, especially when using rigid composite disks that create a very fine
sludge that is difficult to remove from the skin, rubber or plastic gloves should be used.
For large machines using a flammable alcohol-based lubricant, the alcohol fumes can
be rather strong, and the machine should be placed in connection to a fume exhaust
system. A better solution might be to change the lubricant to a water-based type.
When working with semiautomatic machines, a laboratory coat should be used to
avoid that ties or other pieces of clothing get into contact with the rotating specimen
holder.
Fully automatic systems are totally enclosed and will not operate if the protective
shields are not closed.
At manual grinding/polishing, care should be taken that a specimen released by
the operator and flying from the grinding/polishing disk will not injure other persons.
A SOP, including a JSA, should be completed for all mechanical and polishing
equipment.
26.1.4 Electrolytic Polishing/Etching

The most serious potential danger at electrolytic polishing and etching is the mixing,
handling, use, and storing of electrolytes 共see Section 26.1.5兲. During the polishing pro-
cess, care should be taken to avoid heating of the electrolyte that may cause a fire or
even an explosion. It is important to keep a correct level of electrolyte in the electrolyte
container because too little electrolyte might give air pockets in the polishing chamber
causing a spark between anode and cathode, which might ignite the alcohol in the elec-
trolyte.
A SOP, including a JSA, should be completed for each electropolisher.
26.1.5 Etching—Etchants—Electrolytes
The etching procedure should be performed using gloves and eye protection under a
fume hood. The most serious potential dangers are connected to the mixing, handling,
and storing of the chemicals used for etchants, and the same is the case for electrolytes.
The user should have sufficient information on all the chemicals used from training
and MSDSs, which should be available in the laboratory 共see Section 26.2兲. Etchants/
electrolytes are mostly solution mixtures of different materials mixed in the laboratory.
During the mixing, very dangerous reactions can be established like fire, explosion, and
dissolution, creating dangerous substances. The etchants are generally more danger-
ous than the electrolytes because they contain very oxidizing substances.
As a rule, the mixing should always start with the water 共alcohol兲 and then mix the
other ingredients into this. A special procedure, however, should often be followed to
obtain the necessary safety, and certain combinations of chemicals are known to be
dangerous. Information on this must be available in the laboratory. A number of the
most hazardous materials are mentioned below, and further information can be ob-
tained in the Standard Guide on Metallographic Laboratory Safety 共E 2014兲 in Section
26.1.8 of this book.
Acetic Acid: Extreme care should be taken when mixing with other acids like per-
chloric acid and nitric acid. Mixtures of acetic acid and perchloric acid should be
avoided.
Chromic Acid: Very strong oxidation substance, very strong reaction with organic
or easy to oxidize material and it cannot be safely mixed with acetic acid and most or-
ganic liquids, such as alcohols or glycerol. Poisonous.
Nitric Acid: Strong oxidizing acid, creating gases with many organic materials and
metals. Do not store solutions of more than 3 % nitric acid in ethanol.
Perchloric Acid: Very aggressive acid that can cause serious explosions at higher
concentrations. Very dangerous at contact with metals that oxidize easily, such as bis-
muth. Contact to organic material should also be avoided; if absorbed in organic mate-
rial the material must be placed in water. Organic material should never be used to
wipe up perchloric acid.
Picric Acid: Aggressive oxidizer and should always be stored in wet condition. In
dry condition the risk of explosion is high. Storage should be cool and fire safe.
Toxic Substances
Toxic materials are substances that, when inhaled or taken in by the mouth or by the
skin, can lead to death or serious damage to the health. These substances are listed by
official organizations like the National Institute for Occupational Safety and Health
共NIOSH兲共see Section 26.5兲, and rules are defined for their use, storing, handling and
disposal. Also, for many substances the permissible exposure through air and skin is
stated 共see Section 26.5兲.
A number of toxic substances with CAS Nos. 共see Section 26.5.1兲 often used in a
metallographic/materialographic laboratory are mentioned below.
Chemicals based on the metals Be, Pb, Cr, Cu, Ag, U, Sn, Zn 共not ZnO2兲: Poisonous
as liquids or as vapor.
Chlorinated Carbohydrates: These solvents are very dangerous to inhale.
Cyanides 共CAS No. 460-19-5兲: These react strongly with acids, even the CO2 con-
tent in humid atmospheric air gives a reaction. Very poisonous.
Hydrofluoric Acid, Anhydrous 共CAS No. 7647-01-0兲: In concentration higher than
0.5 % the acid is very dangerous, making very serious damage to tissue. Attacks almost
all metals and glass. Very dangerous.
Mercury 共CAS No. 7439-97-6兲: Chemicals bond on mercury and mercury vapor are
poisonous.
Methanol 共CAS No. 67-56-1兲: Poisonous.
Oxalic Acid 共CAS No. 144-62-7 共Anhydrous兲兲共CAS No. 6153-56-6 共Dihydrate兲兲: In
concentrations higher than 5 % oxalic acid is poisonous.
Phosgen 共Carbonyl Chloride兲共CAS No. 75-44-5兲: Very dangerous to the respiratory
system.
Flammable Liquids
Flammable liquids are used in metallographic/materialographic preparation for elec-
trolytic polishing, lubrication, etching, and cleaning.
OSHA 共see Section 26.5兲 defines flammable liquids. “Class I liquids” as any liquid
having a flashpoint below 100° F 共37.8° C兲, except any mixture having components
with flashpoints of 100° F 共37.8° C兲 or higher, the total of which make up 99 % or more
of the total volume of the mixture.
Liquids, which are somewhat harder to ignite, with a flash point above 100° F
共37.8° C兲 are called combustible liquids, “Class II liquids.” These are defined by OSHA
as liquids with flashpoints at or above 100° F 共37.8° C兲 and below 140° F 共60° C兲, except
any mixture having components with flashpoints of 200° F 共93.3° C兲 or higher, the vol-
ume of which make up 99 % or more of the total volume of the mixture.
“Class III liquids” are even harder to ignite and are defined by OSHA as “liquids.”
Class IIIA liquids include those with flashpoints 140° F 共60° C兲 or above and below
200° F 共93.3° C兲, except any mixture having components with flashpoints of 200° F
共93.3° C兲, or higher, the total volume of which make up 99 % or more of the total volume
of the mixture.
Class IIIB liquids include those with flashpoints at or above 200° F 共93.3° C兲.
When a combustible liquid is heated for use to within 30° F 共16.7° C兲 of its flash-
point, it should be handled in accordance with the requirements for the next lower
class of liquids.
All containers with flammable liquids should be marked 共see Section 26.5.3兲.
The number of flammable liquids stored in the lab should be kept at a minimum
and carefully protected against heat and against possible ignition.
All rules and regulations should be followed carefully when handling flammable
liquids. Heating in open containers should be done with special care, using a fume
hood and special electric heating plates.
The flammable liquids are also very often dangerous to health and precautions
should be taken according to the MSDS for the liquid 共see Section 26.2.2兲.
Disposal can be a problem and should be done according to rules and regulations
by local authorities.
26.1.6 Dust
Dust can be developed from specimen material, abrasives, or powders used for mount-
ing. This should be suppressed as much as possible, because even if not toxic, the dust
can give respiratory problems. Dust from metals can be toxic and should be avoided.
26.1.7 Cold „Castable… Mounting Resins

All the cold 共castable兲 mounting resins described in Section 3.8 are potentially danger-
ous to health.
Epoxy
This material, both resin and hardener, can damage the skin, causing allergic reac-
tions. The material should never come in contact with skin and the vapors should not
be inhaled. All work with epoxy should take place under a fume hood using personal
protective equipment 共PPE兲 specified in the MSDS. It is recommended that containers
and stirring pins are disposed of after mixing.
The epoxy is not dangerous when it has fully hardened.
Fig. 26.1—The NFPA diamond symbol: 1兲 Indication of color and type of hazard of the four
small diamonds. 2兲 Example of number ratings and symbol.
Acrylics and Polyesters

Mixing should always take place under a fume hood and gloves should be used when
handling these materials to avoid inhalation and skin contact.
26.1.8 Standard Guide on Metallographic Laboratory Safety „E 2014…

This ASTM guide covers the outline of the basic safety guidelines to be used in a
metallographic/materialographic laboratory. Safe working habits are discussed for
various tasks performed in the laboratory and the guide goes into more details of the
work than stated above in this chapter. Please refer to ASTM E 2014 in the CD-ROM
included with this book.
26.2 Safety Information

It is very important that the user of a chemical substance is informed on all important
facts regarding the substance. According to the OSHA Standard 29 CFR 1910.1200 共see
Section 26.5.3兲, any chemical should be labeled for safe identification and a Material
Safety Data Sheet 共MSDS兲 should be available on the working place for any chemical.
26.2.1 Identification
It is important that the dangerous materials can be identified. Materials that are in one
way or another hazardous should be marked with a label according to a system, as
stated in the standards 共see Section 26.5兲. This label must express a number of facts
regarding the substance so that the user is able to evaluate the possible hazard. The
container with the substance is usually labeled by the supplier, but in cases where
chemicals are taken into smaller containers in the lab and in other cases where the
original container is not used, a new label must be used.
Below two “official” identification systems, NFPA and EU 共EC兲, used by suppliers
of chemicals and one system, HMIS, developed for use in the laboratory, are described.
NFPA 704 Hazard Identification Ratings System

This identification system, developed by the National Fire Protection Association
共NFPA兲 uses the “Hazard Diamond” 共see Fig. 26.1兲 for identification of health, flamma-
bility and instability 共reactivity兲共see also Section 26.5.11兲. The diamond is broken into
four smaller diamonds one each blue, red, yellow, and white. The numbers in the three
colored diamonds range from 0 共least severe hazard兲 to 4 共most severe hazard兲. The
fourth 共white兲 diamond is left blank and is used only to devote special fire fighting
measures/hazards, indicated with special symbols.
Meaning of Colors—Ratings of Numbers

Red: FLAMMABILITY 共Instability兲 is the degree of susceptibility to burning.
0 Will not burn.

1 Must be preheated to burn. Flash point above 200° F 共93.5° C兲.
2 WARNING: Ignites with moderate heat. Flash point 100° F – 200° F 共38– 93.5° C兲.
3 HAZARDOUS: Ignites at room temperature. Flash point 73° F – 99° F 共23– 37° C兲.
4 EXTREMELY DANGEROUS: Highly flammable liquids and explosive gases. Flash
point below 73° F 共23° C兲.
Yellow: REACTIVITY 共Instability兲 is the degree of susceptibility of materials to re-

lease energy.
0 Normally stable at all temperatures. Not reactive with water.

1 CAUTION: May become unstable when heated or mixed with water.
2 HAZARDOUS: Normally unstable or may have violent chemical change when mixed
with water.
3 DANGEROUS: Explodes with exposure to confined heat, shock, or when mixed with
water.
4 EXTREMELY DANGEROUS: Explodes at room temperature.
Blue: HEALTH HAZARD is the degree of injury from burning materials.
0 Creates no unusual hazard.

1 CAUTION: Causes irritation or minor injury.
2 HAZARDOUS: Intense exposure may be harmful.
3 EXTREMELY DANGEROUS: Avoid skin contact and inhalation.
4 FATAL: Too dangerous to enter without specialized protective equipment.
White: OTHER indicates special warnings.
ACID acid
ALK alkali
COR corrosive
OXY oxidizing chemicals
䊏䊏 radiation
P subject to polymerization when mixed with water
—
W do not use water
EU „EC… Identification System

The European Union 共EU兲 has issued a directive, Council Directive 67/548/EEC of 27
June 1967, covering classification, packaging, and labeling of dangerous substances.
According to this directive, all dangerous substances sold in the EU, the European
Economic Area and selected other countries, should be marked with a labeling symbol
and one or more Risk Phrases and Safety Phrases.
Labeling Symbols
The symbols indicate the basic serious dangers, expressed in a figure, and a short text
expressing the Category of Danger, Symbol Letter, and Indication of Danger 共see Fig.
26.2兲.
Risk Phrases—Safety Phrases

To give further information to the user of the substance, one or more Risk Phrases 共R
Phrases兲 and Safety Phrases 共S Phrases兲 should be indicated. The phrases are often
combined 共see below兲. A high number of R and S phrases are available and a few ex-
amples are given below, indicating the number of the phrase.
Examples of R Phrases:
R1 Explosive when dry

R10 Flammable
R20 Harmful by inhalation
R21 Harmful in contact with skin
R20/21 Harmful by inhalation and in contact with skin
R24 Toxic in contact with skin
R25 Toxic if swallowed
R24/25 Toxic in contact with skin and if swallowed
Examples of S Phrases:
S1 Keep locked up
S15 Keep away from heat
S20 Do not eat or drink when using
S24 Avoid contact with the skin
S25 Avoid contact with eyes
S24/25 Avoid contact with skin and eyes
S36 Wear suitable protective clothing
S37 Wear suitable gloves
HMIS: Hazardous Materials Identification System

In case the user makes the labeling, this can be supported by systems developed for this
purpose.
HMIS® is a complete program that helps employers comply with OSHA’s Hazard
Communication Standard 共HCS兲. The program uses a numerical hazard rating system,
labels with colored bars giving information on health, flammability, and reactivity haz-
ards. Training material is provided to inform workers of chemical hazards in the work-
place 共see Section 26.5.12兲.
26.2.2 Material Safety Data Sheet „MSDS…

A Material Safety Data Sheet 共MSDS兲 is designed to provide both laboratory personnel
and emergency personnel with the proper procedures for handling or working with a
Fig. 26.2—EU labeling system. Symbols 共pictograms兲 with words and letters indicating
categories of danger.
particular substance. MSDSs include information such as physical data, health effects,
first aid, reactivity, storage, disposal, protective equipment, and spill/leak procedures.
These are of particular use if a spill or other accidents occur.
MSDSs are made according to the OSHA Standard on Hazard Communication
共HCS兲 or the EC Directive on Safety Data Sheets 共see Section 26.5兲.
MSDSs are meant for:
• Employees who may be occupationally exposed to a hazards at work.

• Employers who need to know the proper methods for storage, etc.
• Emergency responders such as fire fighters, hazardous material crews, emergency
medical technicians, and emergency room personnel.
MSDSs are not meant for consumers. An MSDS reflects the hazards of working
with the material in an occupational fashion. For example, an MSDS for a given paint
is not highly pertinent to someone who uses a can of paint once a year, but is extremely
important to someone who does this in a confined space for 40 hours a week.
The MSDS Format

The formats of MSDSs tend to vary, but they usually convey the same basic kinds of
information.
Supply of MSDS
MSDSs should be kept at the workplace. They are usually delivered by the supplier of a
given product. If it is not delivered, ask the supplier for immediate delivery. For com-
monly known substances, MSDSs can be obtained from an OSHA office or science li-
brary. Many organizations and chemical suppliers, like Cornell University and Sigma-
Aldrich have databases with MSDS on the Internet.
26.2.3 Standard Operating Procedure „SOP…

Standard Operating Procedures 共SOPs兲 can be made for chemicals or processes and
shall contain the operating procedure in relative detail so that an operator can perform
the procedure in a satisfactory way without risk. Often at procedures involving hazard-
ous materials or other potential risks a Job Safety Analysis 共JSA兲 is included in the SOP
共see below兲.
26.2.4 Job Safety Analysis „JSA…

The Job Safety Analysis 共JSA兲 is a very effective means of helping reduce accidents and
injuries in the workplace. Any job that has hazards or potential hazards is a candidate
for a JSA. Based on the operating procedure 共SOP兲, the potential hazards for each step
in the working process are identified. It is very important to look at the entire environ-
ment to determine every hazard that might exist. Based on the steps in the working
process and potential hazards, it is decided what actions are necessary to eliminate,
control, or minimize hazards that could lead to accidents, injuries, damage to the envi-
ronment, or possible occupational illness.
26.3 Disposal of Chemicals

Disposal of chemicals should follow the local rules and regulations. These can vary
very much from place to place and therefore it is very important to obtain the rules
from the local authorities.
As a common rule, the chemicals should be kept separated. Strongly oxidizing
chemicals especially should not be mixed with other chemicals. The chemicals for dis-
posal should be carefully categorized so that no mistake can take place when the waste
is transported and treated further.
Typical categories could be:
共1兲 Chlorinated hydrocarbons like trichloroethylene
共2兲 Hydrocarbons containing aromatic solvents like xylene, terpentine, kerosene

共3兲 Hydrocarbons not containing aromatic solvents like acetone, ketones, alcohols
共4兲 Acidic, aqueous solutions containing chromium compounds
共5兲 Acidic, aqueous solutions containing nitric acid, but not hydrofluoric acid
共6兲 Acidic, aqueous solutions containing hydrofluoric acid or HF salts
共7兲 Acidic, aqueous solutions containing hydrochloric acid, sulfuric acid or phos-
phoric acid
共8兲 Basic aqueous solutions containing metal compounds but not cyanide
共9兲 Metal sludge containing chromium, copper, nickel, zinc, lead, cadmium and silver
26.4 Occupational Safety in General

26.4.1 Standards
In the sections above, the hazards of chemicals and machines have been discussed.
As a rule, the machines and apparatus are designed and manufactured according
to relevant standards. These are the “technical” standards, “safety” standards, and “oc-
cupational” standards. The “occupational” standards, describing the conditions, when
working in the laboratory concerning machines and chemicals, can be the OSHA stan-
dards No. 29 CFR 1910.212, General Requirements for All Machines, No. 29 CFR
1910.215, Abrasive Wheel Machinery, No. 29 CFR 1910.95, Occupational Noise Expo-
sure, No. 29 CFR 1910.120, General Description and Discussion of the Levels of Protec-
tion and Protective Gear, and the important Hazard Communication standard, No. 29
CFR 1910.1200 共see Section 26.5兲.
26.4.2 Training
It is very important that the personnel be trained, both in using the machines and other
equipment, and in health and safety precautions. Not only the training in the practical
use, but an education in the correct attitudes is also important.
26.4.3 Maintenance and Service

It is important that all equipment, building parts, and installations are kept in good
working order and repair is made immediately in case of failure.
Unauthorized personnel should not perform repair work.
26.5 Standards and Regulations—Organizations

A number of American and International organizations are responsible for issuing
standards and regulations connected to occupational safety and health in the
metallographic/materialographic laboratory.
The first section below states a number of abbreviations used in connection with
safety and health.
26.5.1 Designations and Abbreviations Used to Describe a Chemical

Substance
Ca: A substance NIOSH 共see below兲 considers a potential occupational carcinogen
CAS Number: Chemical Abstract Service Registry Number. This number identifies
each chemical. The Chemical Abstracts Service is a division of the American Chemical
Society
IDLH: Immediately Dangerous to Life or Health Concentrations

PEL: Permissible Exposure Limit
PPE: Personal Protective Equipment
REL: Recommended Exposure Limit
RTECS: Registry of Toxic Effects of Chemical Substances 共see Section 26.5.4兲
STEL: Short-Term Exposure Limit as designated by “ST” preceding the value
TLV: Threshold Limit Value, issued by ACGIH 共see Section 26.5.8兲
TWA: Time-Weighted Average 共used in REL兲
UN Number: Four digit number to identify hazardous chemicals 共transport兲.
26.5.2 ASTM Standard

The only standard that directly describes the safety in the metallographic/material-
ographic laboratory is issued by ASTM.
Standard Guide on Metallographic Laboratory Safety 共E 2014兲 covers the outline
of the basic safety guidelines to be used in a metallographic/materialographic labora-
tory. This standard is stated with its full text in the CD-ROM included with this book
共see Section 26.1.8兲.
All other standards 共see below兲 are directed towards the problems in general and
specific matters inside and outside the metallographic/materialographic lab. E 2014,
being specific regarding metallographic/materialographic labs, makes it an important
document that should be followed by all metallographic/materialographic labora-
tories.
26.5.3 OSHA—OSHA Standards

In 1970, the Occupational Safety and Health Act was passed by the U.S. Congress, es-
tablishing NIOSH 共see below兲 and OSHA.
Occupational Safety and Health Administration 共OSHA兲 in the U.S. Department of
Labor has issued a number of regulations 共standards兲 covering occupational safety and
health in laboratories in general, these also covering the metallographic/material-
ographic laboratory.
In the following, the most important standards are described in short form, with
the important Hazard Communication Standard in relative detail.
Standard Title: Hazard Communication Standard

Standard Number: 29 CFR 1910.1200
The Hazard Communication Standard 共HCS兲, sometimes called the Right to
Know law or HazCom, is a set of regulations first promulgated in 1988 by the Office of
Occupational Safety and Health Administration 共OSHA兲. HCS’s purpose is to ensure
that the hazards of workplace chemicals are evaluated, and that information on the
hazards is provided to employers and employees. Details of the standard are provided
in parts 1910.1200 of the Code of Federal Regulations 共CFR兲 of Chapter XVII of Title 29
under the Department of Labor. HCS covers nearly all employers and is applicable to
most work operations where hazardous materials are present.
Contents:
In short, the standard requires that every affected employer must establish a pro-
gram to inform the employees of the hazards associated with the materials in their
workplace. The program must have five main components as follows:
• Written Hazard Communication Program documentation
• Identifying and keeping an inventory of hazardous chemicals
• Obtaining and keeping material safety data sheets 共MSDS兲 on the identified haz-
ards
• Ensuring that the hazardous materials are labeled with name and hazard
• Training employees on the standard, safety information, labeling, and protective
measures
Hazardous Chemicals/Materials
The HCS covers chemicals in all physical forms—liquids, solids, gases, vapors, fumes,
and mists—whether they are “contained” or not. The hazardous nature of the chemical
and potential for exposure are the factors that determine whether a chemical is cov-
ered. If it is hazardous and there is potential for exposure, the rule applies.
Written Program
Under the standard each laboratory 共employer兲 must complete and keep a written Haz-
ard Communication Program. The written program describes how the requirements
for labels and other forms of warning, material safety data sheets 共MSDSs兲, and em-
ployee information and training are implemented in the workplace. It indicates who is
responsible for MSDSs, labels, warning signs, and training, as well as the location of
the inventory. MSDSs and other information and resources pertaining to hazardous
chemicals and safety measures. An inventory list of hazardous chemicals is required to
be maintained as part of the written program.
Chemical Inventory
The person working in the laboratory needs to know about the hazards to be able to
protect oneself. The leader of the laboratory is responsible for establishing an inven-
tory of hazardous chemicals.
All potentially hazardous chemicals in containers should be registered and chemi-
cals possibly generated in work operations should be included, including vapor, fumes,
dust, etc. In the inventory, information based on the labels and the MSDSs made avail-
able by the supplier of the chemical is stated.
MSDS
The role of the MSDS is to provide detailed information on each hazardous chemical,
including its potential hazardous effects, its physical and chemical characteristics, and
recommendations for appropriate protective measures. This information is useful for
designing protective programs, as well as informing the chemical user of the hazards.
MSDSs must be readily accessible to users when they are in their work areas. Some
laboratories keep the MSDSs in a binder in the individual work area or in a central
location in the department.
An MSDS should be available for each hazardous chemical used in the lab. The
MSDS must be in English. The MSDS should be delivered by the supplier, and it should
include all of the information required under the rule. If an MSDS is not supplied auto-
matically it should be requested for. If an MSDS is obviously inadequate an appropri-

ately complete one should be requested.
Employees should not use or be exposed to any chemicals for which the safety data
have not been reviewed and appropriate safety measures implemented.
Labels
Containers of hazardous chemicals must be labeled, tagged, or marked with the iden-
tity of the material and appropriate hazard warnings. The original label must include
the identity of the material, appropriate hazard warnings, and the manufacturer name
and address. The identity used by the supplier may be a common or trade name, or a
chemical name. The hazard warning is a brief statement of the hazardous effects of the
chemical 共“flammable,” “causes lung damage”兲. Labels frequently contain other infor-
mation, such as precautionary measures 共“do not use near open flame”兲. Labels must
be legible and prominent.
Secondary Containers Label and Signs

If materials are transferred from the original container into other containers, these
must be labeled as well. Depending on the employers written plan, the secondary labels
may be warning symbols, text, or use a numerical hazard rating system, such as HMIS
and NFPA 共see Section 26.2兲.
Large containers or storage units containing hazardous chemicals or mixtures
must also be labeled or have warning signs. It is strongly recommended that other
warning or caution signs be placed in the work areas to remind individuals of the haz-
ards and of the protective equipment that may be necessary in the area.
Employee Information and Training

An employee working with hazardous chemicals must receive both information and
training on the hazard communication.
Information and training may be done either by individual chemical, or by catego-
ries of hazards 共such as flammability or carcinogenicity兲. If there are only a few chemi-
cals in the laboratory, each chemical may be discussed individually. Where there are
large numbers of chemicals, or the chemicals change frequently, training may be based
on the hazard categories 共e.g., flammable liquids, corrosive materials, carcinogens兲.
Employees must have access to the substance-specific information on the labels and
MSDSs.
The underlying purpose of the HCS is to reduce the incidence of chemical source
illnesses and injuries. In general, the most important aspects of training are to ensure
employees are aware that they are exposed to hazardous chemicals, that they know
how to read and use labels and material safety data sheets, and that, as a consequence
of learning this information, they are following the appropriate protective measures
共e.g., personal protective equipment, safe procedures, engineering controls兲.
Frequently Asked Questions on HCS „HAZCOM…

HCS being an important standard, the answers to a number of questions can be of
interest.
What are the containers labeling requirements under HCS?

Under HCS, the manufacturer, importer, or distributor is required to label each con-
tainer of hazardous chemicals. If the hazardous chemicals are transferred into un-
marked containers, these containers must be labeled with the required information,
unless the container into which the chemical is transferred is intended for the immedi-
ate use of the employee who performed the transfer.
Can MSDSs be stored in a computer to meet the accessibility requirements

of HCS?
If the employee’s work area includes the area where the MSDSs can be obtained, then
maintaining MSDSs on a computer would be in compliance. If the MSDSs can only be
accessed out of the employee’s work area共s兲, then the employer would not be in compli-
ance with HCS.
When is the supplier required to distribute MSDSs?

Hazard information must be transmitted on Material Safety Data Sheets 共MSDSs兲 that
must be distributed to the customer at the time of first shipment of the product. The
Hazard Communication Standard also requires that MSDSs be updated by the chemi-
cal manufacturer or importer within three months of learning of “new or significant
information,” regarding the chemical’s hazard potential.
What is considered proper training under HCS?

Employees are to be trained at the time they are assigned to work with a hazardous
chemical. The intent of this provision is to have information prior to exposure to pre-
vent the occurrence of adverse health effects. This purpose cannot be met if training is
delayed until a later date.
The training provisions of the HCS are not satisfied solely by giving the employee
the data sheets to read. An employer’s training program is to be a forum for explaining
to employees not only the hazards of the chemicals in their work area, but also how to
use the information generated in the hazard communication program. This can be ac-
complished in many ways 共audiovisuals, classroom instruction, interactive video兲, and
should include an opportunity for employees to ask questions to ensure that they un-
derstand the information presented to them.
Training need not be conducted on each specific chemical found in the workplace,
but may be conducted by categories of hazard 共e.g., carcinogens, acutely toxic agents兲
that are or may be encountered by an employee during the course of his duties.
Furthermore, the training must be comprehensible. If the employees receive job
instructions in a language other than English, then the training and information to be
conveyed under the HCS will also need to be conducted in a foreign language.
What are the requirements for refresher training or retraining a new hire?
Additional training is to be done whenever a new physical or health hazard is intro-
duced into the work area, not a new chemical. For example, if a new solvent is brought
into the workplace, and it has hazards similar to existing chemicals for which training
has already been conducted, then no new training is required. As with initial training,
and in keeping with the intent of the standard, the employer must make employees
specifically aware which hazard category 共i.e., corrosive, irritant, etc.兲 the solvent falls
within. The substance-specific data sheet must still be available, and the product must
be properly labeled. If the newly introduced solvent is a suspect carcinogen, and there
has never been a carcinogenic hazard in the workplace before, then new training for
carcinogenic hazards must be conducted for employees in those work areas where em-
ployees will be exposed.
It is not necessary for the employer to retrain each new hire if that employee has
received prior training by a past employer, an employee union, or any other entity. Gen-
eral information, such as the rudiments of the HCS could be expected to remain with
an employee from one position to another. The employer, however, maintains the re-
sponsibility to ensure that their employees are adequately trained and are equipped
with the knowledge and information necessary to conduct their jobs safely. It is likely
that additional training will be needed since employees must know the specifics of their
new employer’s programs such as where the MSDSs are located, details of the employ-
er’s in-plant labeling system, and the hazards of new chemicals to which they will be
exposed.
Do you need to keep MSDSs for commercial products such as Windex®

and “White-out®”?
OSHA does not require that MSDSs be provided to purchasers of household consumer
products when the products are used in the workplace in the same manner that a con-
sumer would use them, i.e., where the duration and frequency of use 共and therefore
exposure兲 is not greater than what the typical consumer would experience. This ex-
emption in OSHA’s regulation is based, not on the chemical manufacturer’s intended
use of his product, however, but on how it actually is used in the workplace. Employees
who are required to work with hazardous chemicals in a manner that results in a dura-
tion and frequency of exposure greater than what a normal consumer would experi-
ence have a right to know about the properties of those hazardous chemicals.
What are the requirements and limits to use generic MSDSs?

The requirements for MSDSs are found in paragraph 共g兲 of the standard. MSDSs must
be developed for hazardous chemicals used in the workplace, and must list the hazard-
ous chemicals that are found in a product in quantities of 1 % or greater, or 0.1 % or
greater if the chemical is a carcinogen. The MSDS does not have to list the amount that
the hazardous chemical occurs in the product.
Therefore, a single MSDS can be developed for the various combinations of chemi-
cals, as long as the hazards of the various mixtures are the same. This “generic” MSDS
must meet all of the minimum requirements found in HCS, including the name, ad-
dress, and telephone number of the responsible party preparing or distributing the
MSDS who can provide additional information.
What is the application of HCS to an office environment?

Office workers who encounter hazardous chemicals only in isolated instances are not
covered by the rule. OSHA considers most office products 共such as pens, pencils, adhe-
sive tape兲 to be exempt under the provisions of the rule, either as articles or as con-
sumer products. OSHA has previously stated that intermittent or occasional use of a
copying machine does not result in coverage under the rule. However, if an employee
handles the chemicals to service the machine, or operates it for long periods of time,
then the program would have to be applied.
Is an MSDS required for a nonhazardous chemical?

MSDSs that represent nonhazardous chemicals are not covered by the HCS. Para-
graph 29 CFR 1910.1200 共g兲共8兲 of the standard requires that “the employer shall main-
tain in the workplace copies of the required MSDSs for each hazardous chemical, and
shall ensure that they are readily accessible during each work shift to employees when
they are in their work area共s兲.” OSHA does not require nor encourage employers to
maintain MSDSs for nonhazardous chemicals. Consequently, an employer is free to
discard MSDSs for nonhazardous chemicals.
Standard Title: Occupational Exposure to Hazardous Chemicals in

Laboratories
Standard Number: 29 CFR 1910.1450
Scope and Application

The standard covers all laboratories engaged in the laboratory use of chemicals defined
as hazardous by this standard, generally, superseding provisions of all other health
standards except in specific instances. The obligation to maintain employee exposures
at or below the permissible exposure limits 共PELs兲 specified in the air contaminants
standard and in substance specific standards is retained.
It does not apply to users of hazardous chemicals, which do not meet the definition
of laboratory use, and in such cases, the employer must comply with the relevant stan-
dard even though use occurs in a laboratory.
The standard does not apply for laboratory use of hazardous chemicals that pro-
vide no potential for employee exposure such as procedures using chemically impreg-
nated test media and commercially prepared test kits.
Employee Exposure Determination

The employer must measure the employee’s exposure periodically to any substance
regulated by a standard which requires monitoring if there is reason to believe that
exposure levels for that substance routinely exceed the action level 共or in the absence of
an action level, the PEL兲. The employer must notify the employee of the results within
15 working days after receipt of the monitoring results.
Chemical Hygiene Plan

Where hazardous chemicals are used a laboratory covered by this standard the em-
ployer must develop and carry out the provisions of a written Chemical Hygiene Plan
共CHP兲. The CHP must include the necessary work practices, procedures, and policies
to ensure that employees are protected from all potentially hazardous chemicals in use
in their work area. The plan must be available to employees, to employee representa-
tives, and to the Assistant Secretary for Occupational Safety and Health.
Employee Training and Information

The employer must provide employees with information and training to ensure that
they are aware of the hazards of the chemicals present in their work area. This informa-
tion must be provided at the time of an employee’s initial assignment to a work area
where hazardous chemicals are present and prior to assignments involving new expo-
sure situations.
Employees must be informed of:
• The contents of this standard and its appendices must be made available to them
• The location and availability of the employer’s Chemical Hygiene Plan
• The permissible exposure limits for OSHA
• Signs and symptoms associated with exposures to hazardous chemicals used in

the laboratory
• The location and availability of known reference material on the hazards, safe han-
dling, storage, and disposal of hazardous chemicals found in the laboratory includ-
ing, but not limited to Material Safety Data Sheets 共MSDS兲 received from chemical
suppliers
Medical Consultation and Examinations

All employees who work with hazardous chemicals must be given the opportunity to
receive medical attention, including any follow-up examinations, which the examining
licensed physician determines to be necessary under certain circumstances. Medical
examinations and consultants must be provided without cost to the employee, without
loss of pay, and at a reasonable time and place.
The employer must provide certain information to the physician, including the
identity of the hazardous chemicals, a description of the conditions under which the
exposure occurred, and a description of the signs and symptoms of exposure that the
employee is experiencing.
Hazard Identification
Labels on incoming containers of hazardous chemicals must not be removed or de-
faced. MSDSs on incoming hazardous chemicals must be retained and made available
to lab employees.
Respirator Use
Where the use of respirators is necessary to maintain exposure below permissible ex-
posure limits, the employer must provide, at no cost to the employee, the proper respi-
rator equipment.
Record Keeping
The employer must establish and maintain for each employee an accurate record of
any measurements taken to monitor employee exposure and any medical consultation
and examination including tests or written opinions.
Standard Title: List of Highly Hazardous Chemicals, Toxics and Reactives

Standard Number: 29 CFR 1910.119 App A
The standard contains a listing of toxic and reactive highly hazardous chemicals
that present a potential for a catastrophic event at or above the treshold of quantity.
Chemical name, CAS number 共Chemical Abstract Service Number兲 and Treshold
Quantity in Pounds are stated in the list.
Standard Title: Flammable and Combustible Liquids

Standard Number: 29 CFR 1910.106.
The standard defines “flammable” and “conbustible” 共see Section 26.1.5兲 and
states the rules and regulations regarding safety and health, using flammable liquids in
general.
Standard Title: General Description and Discussion of the Levels of

Protection and Protective Gear
Standard Number: 29 CFR 1910.120 App B
Scope and Application

The standard gives information about personal protective equipment 共PPE兲 protection
levels, which may be used to assist employers in complying with the PPE requirements.
As required by the standard, PPE must be selected, which will protect employees
from the specific hazards, which they are likely to encounter during their work on-site.
Selection of the appropriate PPE is a complex process, which should take into con-
sideration a variety of factors. Key factors involved in this process are identification of
the hazards, or suspected hazards; their routes of potential hazard to employees 共inha-
lation, skin absorption, ingestion, and eye or skin contact兲; and the performance of the
PPE materials 共and seams兲 in providing a barrier to these hazards. The amount of pro-
tection provided by PPE will protect well against some hazardous substances and
poorly, or not at all, against others.
Standard Title: Availability of NIOSH Registry of Toxic Effects of Chemical

Substances „RTECS… „non-mandatory….
Standard Number: 29 CFR 1910.1020 App. B
The standard applies to all employee exposure and medical records, and analyses
thereof, of employees exposed to toxic substances or harmful physical agents 共para-
graph 共b兲共2兲. The term “toxic substance or harmful physical agent” is defined by para-
graph 共c兲共13兲 to encompass chemical substances, biological agents, and physical
stresses for which there is evidence of harmful health effects. The regulation uses the
latest printed edition of the National Institute for Occupational Safety and Health
共NIOSH兲共see below兲, Registry of Toxic Effects of Chemical Substances 共RTECS兲 as one
of the chief sources of information as to whether evidence of harmful health effects
exists. If a substance is listed in the latest printed RTECS, the regulation applies to ex-
posure and medical records 共and analyses of these records兲 relevant to employees ex-
posed to the substance.
It is appropriate to note that the final regulation does not require that employers
purchase a copy of RTECS, and many employers need not consult RTECS to ascertain
whether their employee exposure or medical records are subject to the rule. Employers
who do not currently have the latest printed edition of the NIOSH RTECS, however,
may desire to obtain a copy. The RTECS is issued in an annual printed edition as man-
dated by section 20 共a兲共6兲 of the Occupational Safety and Health Act 共29 U.S.C. 669 共a兲
共6兲兲.
26.5.4 National Institute for Occupational Safety and Health „NIOSH…

National Institute for Occupational Safety and Health 共NIOSH兲 is, like OSHA estab-
lished according to the Occupational Safety and Health Act of 1970. They are, however,
two distinct agencies with separate responsibilities, NIOSH is in the U.S. Department
of Health and Human Services.
NIOSH is the Federal agency responsible for conducting research and making rec-
ommendations for the prevention of work-related disease and injury.
NIOSH works with the Health Hazard Evaluation Program, investigating poten-
tially hazardous working conditions and with the NIOSH Publications Office supply-
ing information on hazardous materials. NIOSH has a number of other activities.
NIOSH Pocket Guide

NIOSH Pocket Guide to Chemical Hazards is a useful book that can be obtained from
NIOSH. It includes the following:
Chemical Names, synonyms, trade names, conversion factors, CAS, RTECS, and
DOT Numbers
NIOSH Recommended Exposure Limits 共NIOSH, RELS兲
Permissible Exposure Limits 共PELs兲
NIOSH Immediate Dangerous to Life and Health values 共NIOSH IDLHs兲.
A physical description of the agent with chemical and physical properties
Measurement methods
Personal Protection and Sanitation Recommendations
Respirator Recommendations
Information on Health Hazards including route, symptoms, first aid, and target
organ information.
RTECS® Database
The Registry of Toxic Effects of Chemical Substances 共RTECS®兲 is a database of toxi-
cological information compiled, maintained, and updated by the NIOSH. RTECS®
contains over 133 000 chemicals as NIOSH strives to fulfill the mandate to list “all
known toxic substances … and the concentrations at which … toxicity is known to oc-
cur.”
RTECS® is a compendium of data extracted from the open scientific literature.
The data are recorded in the format developed by the RTECS® staff and arranged in
alphabetical order by prime chemical name. No attempt has been made to evaluate the
studies cited in RTECS®. The user has the responsibility of making such assessments.
26.5.5 International Chemical Safety Cards „ICSCS…

The International Chemical Safety Cards are worked out by an international group of
experts under The International Programme on Chemical Safety under the World
Health Organization 共WHO兲.
The ICSCs are based on standard phrases, the criteria for which are given in the
Compiler’s Guide. A certain number of Cards are available in 22 languages and their
translation into a further eight languages is on-going.
The first edition of the Compiler’s Guide and ten series, representing over 900
Cards, have been published as hard copies in English, Spanish, Japanese, Chinese, and
Polish, and about 1300 Cards are available in electronic form. Cards in English are
available on the ILO Web site: www.ilo.org/public/english/protection/safework/cis/
products/icsc
An ICSC summarizes essential health and safety information on chemicals for
their use at the “shop floor” level by workers and employees in factories, agriculture,
construction, and other work places.
ICSCs are not legally binding documents, but consist of a series of standard
phrases, mainly summarizing health and safety information collected, verified, and
peer reviewed by internationally recognized experts, taking into account advice from
manufacturers and Poison Control Centers.
The identification of the chemicals on the Cards is based on the UN numbers, the
Chemical Abstracts Service 共CAS兲 number, and the Registry of Toxic Effects of Chemi-
cal Substances 共RTECS/NIOSH兲 numbers. It is thought that the use of those three sys-
tems assures the most unambiguous method of identifying the chemical substances
concerned, referring as it does to numbering systems that consider transportation
matters, chemistry, and occupational health.
ICSCs and Material Safety Data Sheets

Great similarities exist between the various headings of the ICSC and the manufactur-
ers’ Safety Data Sheet 共SDS兲 or Material Safety Data Sheet 共MSDS兲 of the International
Council of Chemical Associations. However, MSDSs and the ICSCs are not the same.
The MSDS, in many instances, may be very complex technically and too expensive for
shop floor use, and secondly it is a management document. The ICSCs, on the other
hand, set out peer-reviewed information about substances in a more concise and
simple manner. Although not a legal document, the ICSC is an authoritative document
emanating from WHO/ILO/UNEP. This is not to say that the ICSC should be a substi-
tute for an MSDS, nothing can replace management’s responsibility to communicate
with workers on the exact chemicals, the nature of those chemicals used on the shop
floor and the risk posed in any given work place. Indeed, the ICSC and the MSDS can
even be thought of as complementary. If the two methods for hazard communication
can be combined, then the amount of knowledge available to the safety representative
or shop floor workers will be more than doubled.
26.5.6 Environmental Protection Agency „EPA…

The U.S. Environmental Protection Agency is to protect human health and to safe-
guard the natural environment—air, water, and land—which life depends on.
EPA administrates important laws like Occupational Safety and Health Act and
Toxic Substances Control Act, both important in relation to metallographic/material-
ographic laboratories.
26.5.7 National Technical Information Service „NTIS…

The National Technical Information Service 共NTIS兲 is the largest, central resource for
government-funded scientific, technical, engineering, and business information avail-
able in United States.
Toxic Substances Control Act 共TSCA兲 Chemical Substances Inventory—Revised
Inventory Synonym and Preferred Name File: This inventory list covers more than
65 000 chemicals as defined under TSCA.
26.5.8 American Conference of Government Industrial Hygienists „ACGIH…

The American Conference of Governmental Industrial Hygienists, Inc. 共ACGIH兲, is an
organization open to all practitioners in industrial hygiene, occupational health, envi-
ronmental health, or safety.
ACGIH publishes over 400 titles in occupational and environmental health and
safety. They are best known for their Treshold Limit Values publication that lists the
TLVs for over 700 chemical substances and physical agents, as well as 50 Biological
Exposure Indices for selected chemicals.
26.5.9 National Toxicology Program „NTP…

The National Toxicology Program is an organization under U.S. Department of Health
and Human Services 共DHHS兲 to coordinate toxicological testing programs.
NTP has collected health and safety data on over 2000 chemicals.
26.5.10 Agency for Toxic Substance and Disease Registry „ATSDR…

The Agency for Toxic Substances and Disease Registry 共ATSDR兲 is an agency under
U.S. Department of Health and Human Services.
The mission is to prevent exposure and advise human health effects associated
with exposure to hazardous substances.
ATSDR TOX FAQs is a series of summaries about hazardous substances. Each fact
sheet serves as a quick and easy to understand guide, 共www.atsdr.cdc.gov/toxfaq.html兲.
26.5.11 National Fire Protection Association „NFPA…

The National Fire Protection Association 共NFPA兲 is a nonprofit organization that is re-
sponsible for over 300 codes covering basic fire safety, electricity, and other topics.
The NFPA 704 Hazard Identification Ratings System is described in Section 26.2.
26.5.12 National Paint and Coatings Association „NPCA…—HMIS

The National Paint and Coatings Association 共NPCA兲 has established a complete pro-
gram, HMIS, 共Hazardous Materials Identification System兲 that helps employers com-
ply with OSHA’s Hazard Communication Standard 共HCS兲共see Section 26.2兲.
26.5.13 BSI—ISO
British Standards Institution is the independent national body responsible for prepar-
ing British Standards. BSI cooperates with ISO 共International Standard Organization兲
and EU 共European Union兲.
The British Standard BS 7750 on Environmental Management has been used as
the basis for the standard, BS EN ISO 14001: 1996, Environmental Management Sys-
tems. This standard covers all sides of environmental management and connects to the
quality standard BS EN ISO 9000: 2000.
The standard BS 8800: 1996, Guide to Occupational Health and Safety Manage-
ment Systems, puts emphasis on OHS management. Two standards are established
based on this standard:
OHSAS 18001: 1999, Occupational Health and Safety Management Systems
Specifications.
OHSAS 18002: 2000, Occupational Health and Safety Management Systems.
Guidelines for the implementation of OHSAS 18001.
An important factor in OHSAS 18001: 1999 is “Risk Assessment” defined as “The
overall process of estimating the magnitude of risk and deciding whether or not the risk
is tolerable or acceptable.” Risk assessment involves three basic steps: 共1兲 identify haz-
ards; 共2兲 estimate the risk from each hazard—the likelihood and severity of harm; 共3兲
decide if the risk is tolerable.
26.5.14 EU
The European Union 共EU兲共European Community 共EC兲兲 has established a number of
directives, covering occupational safety.
The directive 67/548/EEC on dangerous substances is described further in Section
26.2.
26.6 Literature on Laboratory Safety

Literature can be seen in References of the Standard Guide on Metallographic Labora-
tory Safety 共E 2014兲 in the CD-ROM included with this manual 共see Section 26.1.8兲. In
addition the books by Petzow and Vander Voort 共Refs 2 and 9, Part I兲 can be recom-
mended.
27
Literature
27.1 Books
THE BOOKS LISTED BELOW COVER THE FIELD OF METALLOGRAPHIC/
materialographic preparation and examination. They are intended as a supplement to
this book and should not be considered as a complete list of books on these subjects.
Amelinckx, S., Van Dyck, D., Van Landuyt, J., and Van Tendeloo, G., Handbook of Microscopy: Applications in
Materials Science, Solid-State Physics, and Chemistry. Wiley-VCH, New York, N.Y., USA, 1997.
Beraha, E. and Shipgler, B., Color Metallography, ASM Materials Park, Ohio, USA, 1977.
Bjerregaard, L., Geels, K., Ottesen, B., and Rückert, M., Metalog Guide, Struers A/S, Copenhagen, Denmark,
2000.
Bousfield, B., Surface Preparation and Microscopy of Materials, John Wiley & Sons, Chichester, UK, 1992.
Bramfitt, B. L. and Benscoter, A. O., Metallographer’s Guide—Practices and Procedures for Iron and Steels, ASM
International, Metals Park, Ohio, USA, 2001.
Burgess, D. and Blanchard, R. A., Wafer Failure Analysis for Yield Enhancement, Accelerated Analysis, Half
Moon Bay, California, USA, 2001.
Bühler, H. E. and Hougardy, H. P., Atlas of Interference Layer Metallography, Deutsche Gesellschaft für Met-
allkunde, Oberursel, Germany, 1980.
Durand-Charre, M., Microstructure of Steels and Cast Irons, Springer-Verlag New York, Inc., New York, NY, USA,
2004.
Durand-Charre, M. and Durand-Charre, M., Microstructure of Superalloys, Taylor & Francis, Inc., Philadelphia,
PA, USA, 1998.
Elssner, G., Hoven, H., Kiessler, G., and Wellner, P., Ceramics and Ceramic Composites: Materialographic Prepara-
tion, Elsevier Science, Inc., New York, NY, USA, 1999.
Freund, J. E., Statistics: a First Course, 2nd ed., Prentice Hall, Englewood Cliffs, New Jersey, USA, 1970.
Friel, J. J., et al., Practical Guide to Image Analysis, ASM International, Materials Park, Ohio, USA, 2000.
Handbook of Thermal Spray Technology, ASM International, Materials Park, Ohio, USA, 2004.
Higginson, R. L. and Sellars, C. M., Worked Examples in Quantitative Metallography, Maney Publishing, Cam-
bridge MA, USA, 2003.
Inoue, S. and Spring, K. R., Video Microscopy, Plenum Press, New York, NY, USA, 1997.
Kapitza, H. G., Microscopy from the Very Beginning, Carl Zeiss, Jena, Germany, 1994.
Metals Handbook, Metallography and Microstructures, Vol. 9, ASM International, Materials Park, Ohio, USA,
2004.
Petzow, G., Metallographic Etching, ASM International, Materials Park, Ohio, USA, 1999.
Ross, Boit, and Staab, 共edit.兲, Microelectronics Failure Analysis, ASM International, Materials Park, Ohio, USA,
1999.
Rostoker, W. and Dvorak, J. R., Interpretation of Metallographic Structures, Elsevier Science, Inc., New York, NY,
USA, 1990.
Russ, J. C., The Image Processing Handbook, 3rd ed., CRC Press, Boca Raton, FL, USA, 1998.
Samuels, L. E., Metallographic Polishing by Mechanical Methods, ASM International, Materials Park, Ohio, USA,
2003.
Schumann, H. and Oettel, H., Metallografie, Wiley-VCH Verlag, Weinheim, Germany, 2004 共In German兲.
Tegart, Mc.G., The Electrolytic and Chemical Polishing of Metals in Research and Industry, Pergamon Press, Lon-
don, UK, 1959.
Tomer, A., Structure of Metals through Optical Microscopy, ASM International, Materials Park, Ohio, USA, 1990.
Underwood, E. E., Quantitative Stereology, Addison-Wesley Publishing Company, Reading, MA, USA, 1970.
685
Vander Voort, G. V., Metallography Principles and Practice, ASM International, Materials Park, Ohio, USA, 1999.
Waschull, H., Präparative Metallographie, Wiley-VCH Verlag, Weinheim, Germany, 1993 共In German兲.
Weck, E. and Leistner, E., Metallographic Instructions for Colour Etching by Immersion, Part I 共1982兲, II 共1983兲,
III 共1986兲, Deutscher Verlag für Schweisstechnik GmbH, Düsseldorf, Germany.
27.2 Periodicals
THE PERIODICALS STATED IN THIS LIST COVER THE FIELD OF METALLO-
graphic/materialographic preparation and interpretation, but it should not be consid-
ered a complete list of all periodicals covering these subjects.
Advanced Functional Materials, English/18 issues yearly, Wiley-VCH, P.O. Box 191161, D-69451, Weinheim, Germany.
Advanced Materials, English/24 issues yearly, Wiley-VCH, P.O. Box 191161, D-69451, Weinheim, Germany.
Advanced Materials and Processes, English/monthly, ASM International, Materials Park, OH 44073, USA.
Advanced Engineering Materials, English/monthly, Wiley-VCH, P.O. Box 191161, D-69451, Weinheim, Germany.
Alloy Digest, English/bimonthly, ASM International, Materials Park, OH 44073, USA.
Electronic Device Failure Analysis, English/quarterly, ASM International, Materials Park, OH 44073, USA.
International Materials Reviews, English/bimonthly, ASM International, Materials Park, OH 44073, USA.
JOM, English/monthly, TMS 共The Minerals, Metals and Materials Society兲, 184 Thorn Hill Road, Warrendale, PA 15086, USA.
Journal of Electronic Materials, English/monthly, TMS 共The Minerals, Metals and Materials Society兲, 184 Thorn Hill Road,
Warrendale, PA 15086, USA.
Journal of Failure Analysis and Prevention, English/bimonthly, ASM International, Materials Park, OH 44073, USA.
Journal of Materials Engineering and Performance, English/bimonthly, ASM International, Materials Park, OH 44073, USA.
Journal of Phase Equilibria and Diffusion, English/bimonthly, ASM International, Materials Park, OH 44073, USA.
Journal of the American Ceramic Society, English/monthly, American Ceramic Society, P.O. Box 6136, Westerville, OH 43086-
6136, USA.
Journal of Thermal Spray Technology, English/quarterly, ASM International, Materials Park, OH 44073, USA.
Materials Characterization, English/10 issues yearly, Elsevier Science Publishing Co. Inc., 655 Avenue of the Americas, New
York, NY 10010, USA.
Metallurgical and Materials Transactions A, English/bimonthly, ASM International, Materials Park, OH 44073, USA.
Metallurgical and Materials Transactions B, English/bimonthly, ASM International, Materials Park, OH 44073, USA.
Praktische Metallographie/Practical Metallography, bilingual, German/English/monthly, Carl Hanser Verlag, Kolbergstrasse
22, 81679 München, Germany.
SlipLines, newsletter, English/quarterly, IMS 共International Metallographic Society兲, ASM International, Materials Park, OH
44073, USA.
Structure, English/German/French editions, twice a year, Struers A/S, Pederstrupvej 84, 2750 Ballerup, Denmark.
Welding Journal, English/monthly, AWS 共American Welding Society兲, 550 N.W. LeJeunne Road, Miami, FL 33126, USA.
Appendixes
Appendix I: Other Standards on Metallography/

Materialography
A NUMBER OF STANDARDS, OTHER THAN ASTM, COVERING METALLO-
graphy/materialography from ISO 共International Standard Organization兲 and a num-
ber of important industrial countries are listed below. The list is not complete.
ISO standards/National standards: The national standards, which are local ver-
sions of ISO standards, are not indicated below.
CEN 共European Committee for Standardization兲 is involved in European Stan-
Chapter 27 Books 687
dards 共EN兲, Technical Specifications 共CEN TS兲, Technical Reports 共CEV TR兲 and CEN
Work Agreements 共CWA兲. All documents are supplied by the national members of CEN.
ISO 共INTERNATIONAL STANDARD ORGANIZATION兲

ISO 643 Steels—Micrographic determination of the ferritic or
austenitic grain size
ISO 945 Cast iron—Designation of microstructure of graphite
ISO 1083 Spheroidal graphite cast irons—Classification
ISO 1463 Metallic and oxide coatings—Measurements of thickness—
Microscopical method
ISO 2064 Metallic and other inorganic coatings—Definitions and
conventions concerning the measurement of thickness
ISO 2624 Copper and copper alloys—Estimation of average grain size
ISO 2639 Steel—Determination and verification of the effective depth
of carburized and hardened cases
ISO 3057 Nondestructive testing—Metallographic replica techniques
of surface examination
ISO 3082 Iron ores—Sampling and sample preparation procedures
ISO 3085 Iron ores—Experimental methods for checking the
precision of sampling, sample preparation and
measurement
ISO 3754 Steel—Determination of effective depth of hardening after
flame or induction hardening
ISO 3763 Wrought steels—Macroscopic methods for assessing the
content of nonmetallic inclusions
ISO 3887 Steels—Determination of depth of decarburization
ISO 4499 Hard metals—Metallographic determination of
microstructure
ISO 4505 Hard metals—Metallographic determination of porosity and
uncombined carbon
ISO 4524-1 Metallic coatings—Test methods for electrodeposited gold
and gold alloy coatings—Part 1 Determination of coating
thickness
ISO 4967 Steel—Determination of content of nonmetallic inclusions—
Micrographic method using standard diagrams
ISO 4968 Steel—Micrographic examination by sulfur prints
共Baumann method兲
ISO 4969 Steel—Macroscopic examination by etching with strong
mineral acids
ISO 4970 Steel—Determination of total or effective thickness of thin
surface-treated layers
ISO 5949 Tool steels and bearing steels—Micrographic method for
assessing the distribution of carbides using reference
photomicrographs
ISO 6196 Micrographics—Vocabulary—Part 1: General terms
ISO 8036 Optics and photonics—Microscopes—Immersion liquids for

light microscopy
ISO 9042 Steels—Manual point counting method for statically
estimating the volume fraction of a constituent with a point
grid
ISO 9220 Metallic coatings—Measurement of coating thickness—
Scanning electron microscope method
ISO 11567 Carbon fibre—Determination of filament diameter and
cross-sectional area
ISO 13520 Determination of ferrite content in austenitic stainless steel
castings
ISO 14250 Steel—Metallographic characterization of duplex grain size
and distribution
ISO/TR 14321 Sintered metal materials, excluding hardmetals—
Metallographic preparation and examination
ISO 14703 Fine ceramics 共advanced ceramics, advanced technical
ceramics兲—Sample preparation for the determination of
particle size distribution of ceramic powders
ISO 14923 Thermal Spraying—Characterization and testing of
thermally sprayed coatings
ISO 16793 Nuclear fuel technology—Guide for ceramographic
preparation of UO2 sintered pellets for microstructure
examination
ISO 17642-2 Destructive tests on welds in metallic materials—Cold
cracking tests for weldments—Arc welding processes—Part
2: Self-restraint tests
ISO 20160 Implants for surgery—Metallic materials—Classification of
microstructures for alpha⫹beta titanium alloy bars
ISO 21227 Paints and varnishes—Evaluation of defects on coated
surfaces using optical imaging—Part 1: General guidance
FRANCE
NF A04-105 Iron and steel. Methods of determination of the
nonmetallic inclusion content of wrought steels. Part 1:
Macroscopic methods.
NF A04-106 Iron and steel. Methods of determination of content of
nonmetallic inclusions in wrought steel. Part II:
Micrographic method using standards diagrams.
NF A04-107 Iron and steel. Micrographic method of dtermination of the
nonmetallic inclusion content of unalloyed wire rod.
NF A04-108 Iron and steel. Characterization of sulfide shapes in
structural steels with improved machinability using
standard diagrams. Micrographic method.
NF A04-110 Iron and steel. Wire rods of non-alloy general purpose steel
for wire drawing. Surface examination.
NF A04-111 Iron and steel. Micrographic determination of the extent of
decarburization of non-alloy high carbon steel wire rod.
NF A04-112 Iron and steel. Macrographic method of showing and

describing the chemical heterogeneity of effervescent steel
wire rod.
NF A04-113 Iron and steel. High carbon steel wire rod derived from
ingots. Macrographic method of showing and describing
the chemical heterogeneity.
NF A04-114 Iron and steel. High carbon continuous cast steel wire rod.
Macrographic method of showing and describing the
chemical heterogeneity.
A04-115 Iron and steel. Characterization of sulfide shapes in
free-cutting steels using standards diagrams. Micrographic
method.
NF A04-203 Steel products. Determination of the effective hardening
after flame or induction hardening.
NF A04-204 Steel products. Determination of the total or conventional
thickness of surface hardened thin layers.
NF A04-503 Semi-products made from aluminum, copper, nickel and
their alloys. Determination of grain size. Aluminium and
aluminium alloys.
NF A05-150 Steel products. Techniques of micrographic examination.
NF A05-151 Steel products. Macrographic examination by sulfur print
共Baumann method兲.
NF A05-152 Steel products. Macroscopic examination by etching with
strong mineral acids.
NF A05-153 Iron and steel. Macroscopic examination by means of
copper salt etching.
NF A05-154 Steel products. Metallographic replica techniques 共optical
examination兲.
NF A05-156 Iron and steel. Macrographic examination by sodium sulfur
print 共so-called lead print method兲.
A05-165 Steel products. Manual point counting method for
statistically estimating the volume fraction of a constituent
with a point grid.
NF A95-342 Powder metallurgy. Sintered materials including
hardmetals. Micrographic examination techniques.
NF EN 1321 Destructive tests on welds in metallic materials.
Macroscopic and microscopic examination of welds.
NF EN 12797 Brazing—Destructive tests of brazed joints.
NF EN 24499 Hard metals. Metallographic determination of
microstructure.
NF EN 24505 Hard metals. Metallographic determination of porosity and
uncombined carbon.
XP ENV 10247 Micrographic examination of the nonmetallic inclusion
content of steels using standard pictures.
GERMANY
DIN V ENV 共Pre-standard兲 Advanced technical ceramics—Methods of

1071-5 test for ceramic coatings—Part 5: determination of porosity
DIN CEN/TS Advanced technical ceramics—Methods of test for ceramic
1071-10 coatings—Part 10: determination of coating thickness by
cross sectioning
DIN EN 1321 Destructive tests of welds in metallic materials—
macroscopic and microscopic examination of welds
DIN EN Aerospace series—Test methods for aluminium and
2004-10 aluminium alloy products; Part 10: preparation of
micrographic specimens for aluminium alloys
DIN EN 2007 Aerospace series—Test methods for aluminium and
aluminium alloy products—metallographic determination
of cladding thickness and copper diffusion in the cladding
for rolled products
DIN EN 3684 Aerospace series—Test methods—titanium alloy wrought
products—determination of beta transus temperature;
metallographic method
DIN EN 10247 Micrographic examination of the nonmetallic inclusion
content of steels using standard pictures
DIN 50192 Determination of the depth of decarburization
DIN 50600 Testing of metallic materials; metallographic micrographs;
picture scales and formats
DIN 50601 Metallographic examination; determination of the ferritic
or austenitic grain size
DIN 50602 Metallographic examination; microscopic examination of
special steels using standard diagrams to assess the content
of non-metallic inclusions
DIN 54150 Nondestructive Testing Impression Methods for Surface
Examination
JAPAN
JIS H 0501 Methods for estimating average grain size of wrought
copper and copper alloys
JIS G 0551 Steels—Micrographic determination of the apparent grain
size
JIS G 0552 Method of ferrite grain size test for steel
JIS G 0553 Macrostructure detecting method for steel, Edition 1
JIS G 0555 Microscopic testing method for the non-metallic inclusions
in steel
JIS Z 6014 Micrographics—Test charts for digitizing image—
Description and use in electronic imagery
UNITED KINGDOM
BS M 37 Method for the etch inspection of metallic materials and
components
BS EN 1321 Destructive test on welds in metallic materials.
Macroscopic and microscopic examination of welds
BS 4490 Methods for micrographic determination of the grain size

of steel
BS 5710 Macroscopic assessment of the nonmetallic inclusion
content of wrought steels
BS 6285 Macroscopic assessment of steel by sulfur print
BS 6286 Measurement of total or effective thickness of thin
surface-hardness layers in steel
BS 6479 Determination and verification of effective depth of
carburized and hardened cases of steel
BS 6481 Determination of effective depth of hardening of steel after
flame or induction hardening
BS 6533 Guide to microscopic examination of steel by etching with
strong acids
BS 6617 Determination of decarburization in steel. Methods for
determining decarburization by microscopic and
microhardness techniques
BS 7590 Method for statistically estimating the volume fraction of
phases and constituents by systematic manual point
counting with a grid
BS 7590 A Worksheet for the determination of volume fraction by
systematic manual point count
BS 10247 Micrographic examination of the nonmetallic inclusion
content of steels using standard pictures
BS EN 10328 Iron and steel—determination of the conventional depth of
hardening after surface heating
93/7105316 DC Aerospace series. Test methods for aluminium and
aluminium alloy products. Metallographic determination of
cladding thickness and copper diffusion in the cladding for
rolled products 共prEN 2007兲
94/710839 DC Aerospace series. Test methods. Titanium alloy wrought
products. Determination of primary ␣ content. The point
count method and line intercept method 共prEN 3683兲
94/710840 DC Aerospace series. Test methods. Titanium alloy wrought
products. Determination of ␤ transus temperature.
Metallographic method 共prEN 3684兲
Appendix II: Other Standards on Hardness Testing

A number of standards, other than ASTM, covering hardness testing from ISO 共Inter-
national Standard Organization兲 and a number of important industrial countries are
listed below. The list is not complete.
ISO standards/National standards: The national standards, which are local ver-
sions of ISO standards, are not indicated below.
CEN 共European Committee for Standardization兲 is involved in European Stan-
dards 共EN兲, Technical Specifications 共CEN TS兲, Technical Reports 共CEV TR兲 and CEN
Work Agreements 共CWA兲. All documents are supplied by the national members of CEN.
ISO „International Standard Organization…

A number of standards covering hardness testing from ISO are listed below. The list is
not complete.
ISO 共INTERNATIONAL STANDARD ORGANIZATION兲

ISO 48 Rubber, vulcanized or thermoplastic—Determination of
hardness 共hardness between 10 IRHD and 100 IRHD兲
ISO 3738-1 Hard metals—Rockwell hardness test 共scale A兲—Part 1:
Test method
ISO 3738-2 Hard metals—Rockwell hardness test 共scale A兲—Part 2:
Preparation and calibration of standard test blocks
ISO 3878 Hard metals—Vickers hardness test
ISO 4384-1 Plain bearings—Hardness testing of bearing metals—Part
1: Compound materials
ISO 4384-2 Plain bearings—Hardness testing of bearing metals—Part
2: Solid materials
ISO 4498 Sintered metal materials, excluding hardmetals—
Determination of apparent hardness and microhardness
ISO 4498-1 Sintered metal materials, excluding hardmetals—
Determination of apparent hardness—Part 1: Materials of
essentially uniform section hardness
ISO 4498-2 Sintered metal materials, excluding hardmetals—
Determination of apparent hardness—Part 2:
Case-hardened ferrous materials, surface enriched by
carbon or carbon and nitrogen
ISO 4507 Sintered ferrous materials, carburized or carbonitrided—
Determination and verification of hardening depth by a
microhardness test
ISO 4516 Metallic and other inorganic coatings—Vickers and Knoop
microhardness tests
ISO 4545 Metallic materials—Hardness test—Knoop test
ISO 4546 Metallic materials—Hardness test—Verification of Knoop
hardness testing machines
ISO 4547 Metallic materials—Hardness test—Calibration of
standardized blocks to be used for Knoop hardness testing
machines
ISO 6506-1 Metallic materials—Brinell hardness test—Part 1: Test
method
ISO 6506-2 Metallic materials—Brinell hardness test—Part 2:
Verification and calibration of testing machines
ISO 6506-3 Metallic materials—Brinell hardness test—Part 3:
Calibration of reference blocks
ISO 6507-1 Metallic materials—Vickers hardness test—Part 1: Test
method
ISO 6507-2 Metallic materials—Vickers hardness test—Part 2:
Verification of testing machines
ISO 6507-3 Metallic materials—Vickers hardness test—Part 3:

Calibration of reference blocks
ISO 6508-1 Metallic materials—Rockwell hardness test—Part 1: Test
method 共scales A, B, C, D, E, F, G, H, K, N, T兲
ISO 6508-2 Metallic materials—Rockwell hardness test—Part 2:
Verification and calibration of testing machines 共scales A,
B, C, D, E, F, G, H, K, N, T兲
ISO 6508-3 Metallic materials—Rockwell hardness test—Part 3:
Calibration of reference blocks 共scales A, B, C, D, E, F, G,
H, K, N, T兲
ISO 9015-1 Destructive test on welds in metallic materials—Hardness
testing—Part 1: Hardness test on arc welded joints
ISO 9015-2 Destructive tests on welds in metallic materials—Hardness
testing—Part 2: Microhardness testing of welded joints
ISO 9385 Glass and glass-ceramics—Knoop hardness test
ISO 14271 Vickers hardness testing of resistance spot, projection and
seam welds 共low load and microhardness兲
ISO 14577-1 Metallic materials—Instrumented indentation test for
hardness and materials parameters—Part 1: Test method
hardness and materials parameters—Part 2: Verification
and calibration of testing machines
hardness and materials parameters—Part 3: Calibration of
reference blocks
ISO 18571 Rubber, vulcanized or thermoplastic—Hardness testing—
Introduction and guide
France
NF A95-329 Powder metallurgy. Sintered metal materials excluding
hardmetals. Measurement of Vickers microhardness
NF A95-348 Powder metallurgy. Sintered ferrous materials, carburized
or carbonitried. Determination of effective case depth by
the Vickers microhardness testing method.
Germany
DIN EN 1043-2 Destructive test on welds in metallic materials—Hardness
test—Part 2: Micro hardness testing on welded joints
DIN CEN/TS 共Pre-standard兲 Advanced technical ceramics—Methods of
1071-7 test for ceramic coatings—Part 7: Determination of
hardness and Young’s modulus by instrumented
indentation testing
DIN CEN/TS 共Pre-standard兲 Advanced technical ceramics—Methods of
1071-8 test for ceramic coatings—Part 8: Rockwell indentation
test for evaluation of adhesion
Japan
JIS Z 2255 Method for ultra-low loaded hardness test
JIS Z 2255 Method for ultra-low loaded hardness test
JIS R 1623:1995 Testing method for Vickers hardness of fine ceramics at

elevated temperatures
JIS B 7724:1999 Brinell hardness test—Verification of testing machines
JIS B 7726 Rockwell hardness test—Verification of testing machines
JIS B Shore hardness test—Verification of testing machines
7727:2000
JIS B 7730 Rockwell hardness test—Calibration of reference blocks
United Kingdom
BS DD ENV Advanced technical ceramics—monolithic ceramics—
843-4 mechanical properties at room temperature—Part 4.
Vickers, Knoop and Rockwell superficial hardness tests
BS 1881 P 202 Recommendations for surface hardness testing by rebound
hammer
BS 2782 P3 Determination of Rockwell hardness
METH 3665 C
BS 3900-E12.1 Methods of test for paints—determination of Knoop
hardness by measurement of the indentation length using
a microscope
BS 4443 P2 Method 7, indentation hardness tests
BS 5411 P6 Vickers and Knoop microhardness tests
BS 5600 P4 S4.5 Powder metallurgical materials and products—methods of
testing and chemical analysis of hardmetals—Rockwell
hardness test 共scale A兲
BS 6431 P13 Method for determination of scratch hardness of surface
according to Mohs
BS 6617 Determination of decarburization in steel. Method for
determining decarburization by microscopic and
micro-hardness techniques
BS 7442 P3 S3.2 Determination of Shore hardness
BS EN 23878 Hardmetals—Vickers hardness test
BS EN 24428-1 Sintered metal materials, excluding hardmetals—
determination of apparent hardness—Part 1. Materials of
essentially uniform section hardness
Appendix III: Hardness Conversion Tables for Metals „E 140…

共Included on CD-Rom in back of this book.兲
Appendix IV: SI Quick Reference Guide: International System of

Units „SI…
共Included on CD-Rom in back of this book.兲
Glossary
Abrasion The process of rubbing, grinding, or wearing away by the
use of abrasives; a roughening or scratching of a surface due
to abrasive wear [1].
Abrasive A substance capable of removing material from another
substance in machining, abrasion, or polishing that usually
takes the form of several small, irregular shaped particles of
hard material [1].
Abrasive disk (1) Grinding wheel mounted on a steel plate, with the
exposed flat side being used for grinding. (2) Grinding disk
with a layer of abrasive product [1].
Abrasive paper See Grinding paper.
Abrasive wet cutting Cutting method for almost all solid materials using
mechanical friction and wear with abrasives bonded in a
cut-off wheel (similar to grinding) [3].
Achromatic Literally, color-free. A lens or prism is said to be achromatic
when corrected for two colors. The remaining color seen in
an image formed by such a lens is said to be secondary
chromatic aberration [2]. See Achromatic objective.
Achromatic objective An objective that is corrected chromatically for two colors,
and spherically for one, usually in the yellow-green part of
the spectrum [2].
Acid A chemical substance that yields hydrogen ions 共H+兲 when
dissolved in water gives a pH of less than 7 [1]. See also
Base.
Age hardening Hardening through aging, usually after rapid cooling or cold
working [1]. See also Precipitation hardening.
Aging A change in the property of certain metals and alloys that
occurs at room temperature or slightly elevated
temperatures, after hot working or heat treatment, or after
cold working. The aging is usually due to phase changes
(precipitation) [1]. See also Precipitation hardening.
Air-hardening steel A steel containing sufficient carbon and other alloying
elements to harden fully during cooling in air or other
gaseous media from a temperature above its transformation
range. Same as self-hardening steel [1].
Alloy A substance having metallic properties and being composed
of two or more chemical elements of which at least one is an
elemental metal [1].
Alloying element An element added to a metal (and which remains within the
metal) to effect changes of properties [1].
Alloy steel Steel containing significant quantities of alloying elements
(other than carbon and the commonly accepted amounts of
manganese, copper, silicon, sulfur, and phosphorus) to
improve the mechanical properties [1].
Alpha brass Solid solution phase of one or more alloying elements in
copper and having the same crystal lattice as copper [2].
Alpha iron „Fe… Solid phase of pure iron [2].
Amalgam Alloy with mercury and one or more other metals [3].
Amorphous Not having a crystal structure; noncrystalline [1].
695
Anisotropy Characterized by having different values of a property in

different crystallographic directions [1].
Annealing Heating to and holding metals and alloys at a suitable
temperature followed by cooling at a suitable rate, used
primarily to soften metals, but also to simultaneously
produce desired changes in properties or in microstructure
[3].
Anode Electrode where electrons leave (current enters) an
operating system (battery, X-ray tube, electrolytic cell) [3].
See also Cathode.
Anode corrosion The dissolution of a metal acting as an anode [3].
Anodic etching See Electrolytic etching.
Anvil effect The effect caused by use of too high a load, or when testing
the hardness of too thin a specimen, resulting in a bulge or
shiny spot on the underside of the specimen [2].
Aperture, optical The working diameter of a lens or a mirror [2].
Apochromatic An objective with longitudinal chromatic correction for red,
objective green, and blue, and spherical chromatic correction for
green and blue. This is the best choice for high resolution or
color photomicrography [2].
Arc cutting A group of cutting processes that melts the metals to be cut
with the heat of an arc between an electrode and the base
material [1].
Artifact A false microstructural feature that is not an actual
characteristic of the specimen; it may be present as a result
of improper or inadequate preparation, handling methods,
or optical conditions for viewing [2].
Attack polishing Simultaneous etching and mechanical polishing by adding a
weak etching solution to the polishing compound [1]. See
also Chemical mechanical polishing.
Austenite A face-centered cubic solid solution of carbon or other
elements in gamma iron [2].
Austenitic steel An alloy steel whose structure is austenitic at room
temperature [1].
Automatic image A device which can be programmed to detect and measure
analysis features of interest in an image. It may include accessories
such as automatic focus and an automatic traversing stage to
permit unattended operation [2].
Glossary 697
Bainite—upper, Metastable microstructure or microstructures resulting from

lower, intermediate the transformation of austenite at temperatures between
those which produce pearlite and martensite. These
structures may be formed on continuous (slow) cooling if
the transformation rate of austenite to pearlite is much
slower than that of austenite to bainite. Ordinarily, these
structures may be formed isothermally at temperatures
within the above range by quenching austenite to a desired
temperature and holding for a period of time necessary for
transformation to occur. If the transformation temperature
is just below that at which the finest pearlite is formed, the
bainite (upper bainite) has a feathery appearance. If the
transformation temperature is just above that at which
martensite is produced, the bainite (lower bainite) is
acicular, resembling slightly tempered martensite. At the
higher resolution of the electron microscope, upper bainite
is observed to consist of plates of cementite in a matrix of
ferrite. These discontinuous carbide plates tend to have
parallel orientation in the direction of the longer dimension
of the bainite areas. Lower bainite consists of ferrite needles
containing carbide platelets in parallel array cross-striating
each needle axis at an angle of about 60°. Intermediate
bainite resembles upper bainite; however, the carbides are
smaller and more randomly oriented [2].
Banded structure Alternate bands parallel with the direction of working
„banding… resulting from the elongation of segregated areas [2].
Band saw Mechanical cutting method using an endless steel saw blade.
Base A chemical substance that yields hydroxyl ions 共OH−兲, when
dissolved in water gives a pH of more than 7 [1].
Base metal (1) After welding, that part of the metal which was not
melted. (2) A metal that readily oxidizes, or that dissolves to
form ions [1]. See also Noble metal.
Beilby layer A layer of amorphous or amorphous-like character
developed on the surface of a specimen during mechanical
polishing. Theory by G. Beilby, but later research has shown
that the layer does not exist.
Beta structure Structurally analogous body-centered cubic phases (similar
to beta brass), or electron compounds, that have ratios of 3
valence electrons to 2 atoms [2].
Binder Cementing medium holding together mixtures of particles
or powder [3].
Blow torch Method for cutting metal using an acetylen burner, with the
possibility of adding an extra flow of oxygen, melting, and
blowing away the material. Also called oxyacetylen torching.
Bond The material that binds the abrasive in a cut-off wheel and in
other abrasive products.
Brass Alloy consisting of copper (over 50 %) and zinc, to which

small amounts of other elements may be added [3].
Brightfield For reflected light, the illumination which causes specularly
illumination reflected surfaces normal to the axis of a microscope to
appear bright. For transmission electron microscopy, the
illumination of an object so that it appears on a bright
background [2].
Brinell hardness Hardness test performed by forcing a hard steel or tungsten
testing carbide ball of specified diameter into a material [3].
Brittleness The tendency of a material to fracture without first
undergoing significant plastic deformation [1]. See also
Ductility.
Bronze Copper-tin alloy with or without small amounts of other
alloying elements such as phosphorus and zinc [3].
Burning Can occur in cutting and grinding, when sufficient heat is
metallography/ generated on the surface of the work piece to cause
materialography… discoloration or a change of the microstructure by
tempering or hardening [1].
Calibration (1) The act or process of determining the relationship
between a set of standard units of measure and the output
of an instrument or test procedure. (2) The graphical or
mathematical relationship relating the desired property
(expressed in a standard unit of measure such as
micrometres or Kg/ mm2) to the instrument output
(instrument units such as filar divisions or pixels) [2].
Carbide A compound of carbon with one or more elements, which,
in customary formulation, are considered as being more
positive than carbon [2].
Carbide tools Cutting or forming tools, usually made of tungsten, titanium,
tantalum, or niobium carbides or a combination of them in
a matrix of cobalt, nickel, or other metals. Carbide tools are
characterized by high hardness and compressive strength
and may be coated to improve wear resistance [1].
Carbon steel Steel containing carbon up to 2 % [3].
Carbonitriding A case-hardening process by which a suitable ferrous metal
is heated in a gaseous atmosphere. Through the gas, the
metal surface will absorb carbon and nitrogen by diffusion
and form a very hard compound layer [1].
Carburizing Absorption and diffusion of carbon into solid ferrous alloys
by heating to a temperature usually above Ac3, in contact
with a suitable carbonaceous material. A form of case
hardening [1]. See also Case hardening.
Case In a ferrous alloy, the outer portion that has been made
harder than the inner portion as a result of altered
composition, or structure, or both, from treatments such as
carburizing, nitriding, and induction hardening [2]. See also
Core.
Glossary 699
Case hardening A generic term covering several processes applicable to steel

that change the chemical composition of the surface layer
by absorption of carbon, nitrogen, or a mixture of the two
by diffusion. It is also called carburizing, nitriding,
carbonitriding, cyaniding, nitrocarburizing, and quench
hardening [1].
Cast iron Generic term of a large family of cast ferrous alloys
containing 2.5–4 % carbon and about 1–3 % silicon. The
carbon content exceeds the solubility of carbon in austenite
that exists at the eutectic temperature, which is usually more
than 2 % [3].
Cast structure The structure, on a macroscopic or microscopic scale, of a
casting [2]. See also Dendrites.
Cathode Electrode where the electrons enter (current leaves) an
operating system [3]. See also Anode.
Cemented carbides Material made by pressing and sintering a powder of one or
„sintered carbides… more metallic carbides with a small amount of metal
(cobalt) serving as a binder [1].
Cementite A very hard and brittle compound of iron and carbon
corresponding to the empirical formula Fe3C. It is
commonly known as iron carbide and possesses an
orthorhombic lattice. In “plain-carbon steels” some of the
iron atoms in the cementite lattice are replaced by
manganese, and in “alloy steels” by other elements such as
chromium or tungsten. Cementite will often appear as
distinct lamellae or as spheroids or globules of varying size
in hypo-eutectoid steels. Cementite is in metastable
equilibrium and has a tendency to decompose into iron and
graphite, although the reaction rate is very slow [2].
Ceramic Inorganic, nonmetallic material with crystalline and
noncrystalline structures (for instance: metal carbides,
oxides, nitrides, and borides are ceramics) [3].
Cermets Powder metallurgy product consisting of ceramic particles
bonded with metal [1].
CG iron Same as compacted graphite cast iron [1]. See also
Compacted cast iron.
Chemical deposition Precipitation of a metal from solutions of its salts through
the introduction of another metal or reagent to the solution
[1].
Chemical etching Develops the microstructure by using an electrochemical
process, which takes advantage of the differences in the
electrochemical potentials of the various constituents in the
structure [3].
Chemical polishing Improving the surface luster of a metal by chemical
treatment [1]. See also Chemical mechanical polishing.
Chemical Using a combination of a chemical solution (usually an

mechanical etchant) with an oxide suspension on a polishing cloth,
polishing resulting in a scratch free surface. Mainly used for very soft
or ductile metals [3]. See also Oxide polishing.
Chips Pieces of material removed from a work piece by cutting
tools or by an abrasive medium [3].
Clad metal A composite metal containing two or three layers that have
been bonded together. The bonding may have been
accomplished by co-rolling, welding, casting, heavy chemical
deposition, or heavy electroplating [1].
Clay Earthy or stony mineral aggregate, which is plastic when
sufficiently pulverized and wetted, rigid and dry, and
vitreous when fired at a sufficiently high temperature [3].
Cold etching Reveals the microstructure at room temperature and below
[4].
Cold rolled sheet Sheets of metal made by feeding metal through mill rolls at
room temperature [3].
Cold worked A microstructure resulting from plastic deformation of a
structure metal or alloy below its recrystallization temperature [1].
Combined carbon That part of the total carbon in steel or cast iron that is
present as other than free carbon [1]. See also Free carbon.
Comet tails Artifact in the form of unidirectional scratches developed by
mechanical polishing of a metallographic/materialographic
surface.
Compacted graphite Cast iron having a graphite shape intermediate between the
cast iron flake form typical of gray cast iron and the spherical form of
fully spherulitic cast iron. Also known as CG iron [1].
Component One of the independently variable substances by means of
which the composition of each phase of a system of
heterogeneous equilibrium may be described completely;
usually an element, or a compound that remains
undissociated throughout the range of temperature and
pressure concerned [2].
Composite material A heterogeneous, solid structural material consisting of two
or more distinct components that are mechanically or
metallurgically bonded together (such as a cermet, or boron
wire embedded in a matrix of epoxy resin) [1]. See also
Cermet.
Condenser A term applied to lenses or mirrors designed to collect,
control, and concentrate radiation in an illumination system
[2].
Constant feed speed In cutting: Cutting principle where the movement of the
specimen or the cut-off wheel is kept constant throughout
the cutting process. This cutting principle is preferred to the
principle of Constant force as it will produce the least
deformation possible while still achieving the shortest
cutting times [3]. See also Constant force.
Glossary 701
Constant force In cutting: Cutting principle where the force applied is kept
constant throughout the cutting process. Constant force can
produce damage to the sample especially at sample entry
and exit [3].
Constituent A phase, or combination of phases, which occurs in a
characteristic configuration in an alloy microstructure [2].
Contamination (1) Debris from grinding or dust from the lab environment
„metallography/ contaminating a polishing cloth resulting in scratches of the
materialography… specimen surface. (2) Material from a source other than the
specimen itself, which is deposited on the specimen surface
during preparation [3].
Continuous phase The phase forming the matrix or background in which other
phases may be dispersed as isolated units [2].
Controlled etching Electrolytic etching with selection of suitable etchant and
voltage, resulting in a balance between current and dissolved
ions [4].
Conversion, The exchange of a hardness number determined by one
hardness method for an equivalent hardness number of a different
scale [2].
Coolant See Cutting fluid.
Core (1) Case hardening—interior portion of unaltered
composition, or microstructure, or both, of a case-hardened
steel article. (2) Clad products—the central portion of a
multilayer composite metallic material [2].
Corrosion Deterioration of a metal by chemical or electrochemical
reaction with its environment [1].
Corrosion The chemical or electrochemical reaction between a
embrittlement material, usually a metal, and its environment that produces
a deterioration of the material and its properties [1].
Corrosion fatigue Cracking produced by the combined action of repeating and
fluctuating stress and a corrosive environment [1].
Coupon A piece of material especially made for testing. Known from
printed circuit boards, where a coupon is made together
with the board.
Creep Time-dependent strain occurring under stress [1].
Crystal A solid composed of atoms, ions, or molecules arranged in a
pattern which is periodic in three dimensions [2].
Crystallite A crystalline grain not bounded by habit planes [2].
Cut-off wheel Abrasive wheel consisting of an abrasive in a bond for
cutting any material or part [3].
Cutting Sectioning of a piece of material to obtain a specimen [3].
„metallography/ See also Cut-off wheel.
materialography…
Cutting fluid Fluid used to cool a work piece, wash chips away, and
improve surface finish and cut-off wheel lifetime [3].
Cutting speed The linear or peripheral speed of relative motion between

the tool and work piece in the principal direction of cutting
[1].
Darkfield The illumination of an object such that it appears
illumination illuminated with the surrounding field dark. This results
from illuminating the object with rays of sufficient obliquity
so that none can enter the objective directly. As applied to
electron microscopy, the image is formed using only
electrons scattered by the object [2].
Decarburization Loss of carbon from the surface of a carbon-containing alloy
due to a reaction with one or more chemical substances in a
medium that contacts the surface. Decarburization may be
either (1) partial. That is, where carbon content is less than
the unaffected interior but greater than the room
temperature solubility limit of carbon in ferrite or (2)
complete. That is, where carbon content is less than the
solubility limit of carbon in ferrite so that only ferrite is
present [2].
Deep drawing Forming of deeply recessed parts by means of plastic flow of
the material [1].
Deep etching Macroetching; etching preliminary to macro-examination,
intended to develop gross features such as segregation, grain
flow, cracks, or porosity [2]. See also Macroetching.
Deformation Plastic deformation, which may also be referred to as cold
„metallography/ work, can result in subsurface defects after grinding,
materialography… lapping, or polishing. Remaining plastic deformation can
first be seen after etching. Plastic deformation (deformed
layer) is an artifact that has to be removed during sample
preparation [3].
Deformation bands Bands produced within individual grains during cold
working which differ variably in orientation from the matrix
[2].
Dendrites Crystals, usually formed during solidification or sublimation,
which are characterized by a tree-like pattern composed of
many branches; pine-tree or fir-tree crystals [2].
Depth of field The depth or thickness of the object space that is
simultaneously in acceptable focus [2].
Diamond polishing Polishing using diamond as abrasive. Removes scratches
introduced during fine grinding. Makes the specimen
suitable for microscopic observation [3]. See also Final
polishing, Polishing.
Diamond wheel A grinding wheel in which crushed and sized industrial
diamonds are held in a resinoid, metal, or vitrified bond [1].
Diaphragm A fixed or adjustable aperture in an optical system.
Diaphragms are used to intercept scattered light, to limit
field angles, or to limit image-forming bundles or rays [1].
Glossary 703
Differential A microscopical technique employing a beam-splitting

interference contrast double-quartz prism; that is a modified Wollaston prism
illumination „DIC… placed ahead of the objective with a polarizer and analyzer
in the 90° crossed positions. The two light beams are made
to coincide at the focal plane of the objective, thus rendering
height differences visible as variations in color. The prism
can be moved, shifting the interference image through the
range of Newtonian colors [2].
Diffraction (1) A modification which radiation undergoes, as in passing
by the edge of opaque bodies or through narrow slits, in
which the rays appear to be deflected. (2) Coherent
scattering of X-radiation by the atoms of a crystal which
necessarily results in beams in characteristic directions.
Sometimes called reflection. (3) The scattering of electrons,
by any crystalline material, through discrete angles
depending only on the lattice spacings of the material and
the velocity of the electrons [2].
Diffusion The spontaneous movement of atoms or molecules to new
sites within a material [1].
Direct cut Cutting mode in which the cut-off wheel cuts directly
„metallography/ through the work piece; also called chop cutting [3].
materialography…
Dislocation A linear imperfection in a crystalline array of atoms [1].
Dislocation etching Reveals exit point of dislocations on the specimen surface
[4].
Dissolution etching Reveals the microstructure by surface removal [4].
Double etching Two etchants are used sequentially; the second one will
accentuate a particular microstructural feature [4].
Drawing Forming recessed parts of metal by pressing them in or
through a die. Reducing cross section of a wire or tube by
pulling it through a die [1].
Drop etching Placing a drop of an etchant on a selected area of the
specimen surface to develop the microconstituents [4].
Dry etching Develops the microstructure by gaseous exposure [4].
Ductile cast iron A cast iron that has been treated while molten with an
element such as magnesium or cerium to induce the
formation of free graphite as nodules or spherulites, which
imparts a measurable degree of ductility to the cast metal.
Also known as nodular cast iron, cast iron with spheroidal
graphite and SG iron [1].
Ductility Ability of a material to deform plastically without fracturing,
measured by elongation or reduction of area in a tensile test
[1]. See also Brittleness.
Duplex A two-phase structure [2].
microstructure
Dye penetrant Color spray used in nondestructive testing to find cracks in
surface of parts [3].
Elastic deformation Change of dimensions of a piece of material under stress.

Upon release of stress original dimensions are restored
again (example: elastic band which takes its original shape
after it has been stretched) [3].
Elasticity Ability of a solid to deform in direct proportion to and in
phase with increases or decreases in applied force [3].
Electrical discharge Removal of stock from an electrically conductive material by
machining „EDM… rapid, repetitive spark discharge through a dielectric fluid
flowing between the work piece and a shaped electrode [1].
Electrolyte Liquid, most often a solution, that will conduct an electric
current [1].
Electrolytic cell An assembly consisting of a vessel, electrodes (anode and
cathode) and an electrolyte in which electrolysis can be
carried out [1].
Electrolytic etching Development of microstructure by selective dissolution of
the polished surface under application of a direct current
[1]. Also called anodic etching.
Electrolytic A metallographic preparation procedure where metal is
polishing preferentially dissolved from high points on an anodic
surface by passage of an electric current through a
conductive bath, to produce a specular reflecting surface.
Used as an alternative to mechanical polishing [2].
Electron microscopy The study of materials by means of the electron microscope
[2]. See also SEM and TEM.
Embedded abrasives Loose abrasive particles pressed into the surface of a
specimen. This happens mainly with soft or ductile
materials, or both. Abrasives can be embedded when using a
small abrasive particle size, the grinding or polishing cloth
used has a low resilience or a lubricant with a low viscosity
is used or a combination of these conditions takes place [3].
Equiaxed grain A polygonal crystallite, in an aggregate, whose dimensions
are approximately the same in all directions [2].
Equilibrium diagram A graphical representation of the temperature, pressure, and
composition limits of phase fields in an alloy system, as they
exist under conditions of complete equilibrium [1].
Etchant Chemical substance or mixture used for etching [1].
Etch figures Markings formed on a crystal surface by etching or chemical
solution and usually related geometrically to the crystal
structure [2].
Etching Controlled preferential attack on a metal surface for the
purpose of revealing structural details [2].
Eutectic Phase consisting of intermixed solid constituents formed by
a eutectic reaction, (pearlite= ferrite end cementite). The
number of solids being the same as the number of
components in the system [3].
Eutectic structure The structure resulting when an alloy has passed through a
eutectic equilibrium upon freezing [2].
Glossary 705
Exogenous A nonmetallic constituent produced by entrapment of

inclusions foreign material in the melt [2]. See also Inclusions,
Nonmetallic inclusions.
Eyepiece The lens system used in an optical instrument for
magnification of the image formed by the objective [2].
Fatigue Process by which repeated or fluctuating stress, or both,
leads to fracture [3].
Feed speed Rate by which a tool or cut-off wheel advances along or into
the surface of a work piece [3].
Ferrite Designation commonly assigned to alpha iron containing
alloying elements in solid solution. Increasing carbon
content markedly decreases the high-temperature limit of
equilibrium [2].
FG Fine Grinding. Reduces surface roughness of a specimen to
a degree that is suitable for polishing [3].
Field The portion of the object in view [2].
Field metallography Metallographic techniques carried out in the field when the
part or component is too large to bring to a metallographic
laboratory or a specimen cannot be removed [1].
Filar An eyepiece equipped with a fiducial line in its focal plane,
which is movable by means of a calibrated micrometre
screw, in order to make accurate measurements of length
[2].
Filler Material used to increase the bulk of a product without
adding to its effectiveness in functional performance [3].
Final polishing The final step in a specimen preparation process producing
a surface suitable for microscopic examination.
Flame spraying Coating technique in which the coating material is fed as
wire or powder into a flame and sprayed in the molten state
against the surface to be coated [3].
Flow lines A fiber pattern, frequently observed in wrought metal, which
indicates the manner in which the metal flowed during
deformation [2].
Fluorescent screen A sheet of material which emits visible light when exposed to
invisible radiation [2].
Foil A thin sheet of a material, usually a metal, not exceeding
0.13 mm 共0.005 in.兲 in thickness [2].
Forging Process of plastically deforming metal, usually hot, into a
desired shape with compressive force, with or without dies
[1].
Formability Relative ease with which a metal can be shaped through
„workability, plastic deformation [1].
drawability…
Fractography Description of fractures with macrographs 共⬍25⫻ 兲 and
micrographs at high magnification 共⬎25⫻ 兲 from the optical
microscope and the SEM [3].
Fracture test Test in which a specimen is broken and its fracture surface
examined to determine such factors as composition, grain
size, case depth, or soundness [1].
Free carbon Part of the total carbon in steel or cast iron that is present in
elemental form as graphite [1]. See also Combined carbon.
Free machining Machining capabilities of an alloy to which one or more
ingredients have been introduced to produce small broken
chips, better surface finish, and longer tool lifetime during
the machining process [1].
Galvanizing Coating the surface of iron or steel with zinc applied
electrolytically or by hot dipping [3].
Goniometer An instrument devised for measuring the angle through
which a specimen is rotated [1].
Grain An individual crystallite in metals [2].
Grain boundary An interface separating two grains, where the orientation of
the lattice changes from that of one grain to that of the
other. When the orientation change is very small the
boundary is sometimes referred to as a subboundary [2].
Grain boundary Reveals the intersections of the individual grains. Grain
etching boundaries have a higher dissolution potential than the
individual grains because of their high density of structural
defects. Accumulation of impurities in grain boundaries
increases this effect [4].
Grain size (1) Measure of the areas or volume of grains in a
polycrystalline material, usually expressed as an average
when the individual sizes are fairly uniform. In metals
containing two or more phases, grain size refers to that of
the matrix unless otherwise specified. Grain size is reported
in terms of number of grains per measuring unit area or
volume, average diameter, or as a grain size derived from
area measurements. See also ASTM Standard E 112. (2)
Dimension of one individual particle of an abrasive,
measured in micrometres, ␮m [1]. See also Grit size.
Grain-contrast Etching the surface of the grains according to their crystal
etching orientation. They become distinct by the different reflectivity
caused by reaction layers or surface roughness [4].
Graphite The polymorph of carbon with a hexagonal crystal structure
[1]. See also CG iron, Gray cast iron, Nodular cast iron,
Spheroidal cast iron.
Graphitic carbon Free carbon in steel or cast iron [1].
Graticule A scale on glass or other transparent material placed in the
eyepiece or at an intermediate plane on the optic axis of a
light microscope for the location and measurement of
objects (a graticule is different than a reticle) [2]. See also
Reticle.
Glossary 707
Gray cast iron or Cast iron that looks gray on the fractured surface due to the
gray iron presence of free graphite. Contains carbon as graphite in
form of flakes or nodules [3].
Grinding The removal of material from the surface of a specimen by
abrasion through the use of randomly oriented
hard-abrasive particles bonded to a suitable substrate, such
as paper or cloth, where the abrasive particle size is
generally in the range of 60 to 600 grit (approximately
150 to 15 ␮m) but may be finer [2].
Grinding paper Coated abrasive product in which paper is used as a backing
material [3].
Grit size Nominal size of abrasive particles in a grinding wheel,
corresponding to the number of openings per linear inch in
a screen through which the particles can just pass.
Sometimes but inadvisably called “grain size” [1]. See Grain
size.
Half moon Appears mainly when using wet grinding disk and coarse
phenomenon SiC-paper for plane and fine grinding of specimens clamped
in a specimen holder. This phenomenon is due to the fact
that the abrasive grains of the SiC-paper are not getting
worn down at the edge of an SiC-paper as fast as in the
middle, combined with the higher speed at the periphery of
the disk [3].
Hardening Increasing hardness of a metal with a suitable treatment,
usually through heating and fast cooling [1].
Hardness Resistance of a metal to plastic deformation, usually by
„indentation… indentation. However, the term may also refer to resistance
to scratching, abrasion, or cutting. Indentation hardness may
be measured by various hardness testing methods, such as
Brinell, Rockwell, Vickers, Knoop, and Scleroscope [3].
Heat-resistant alloy Alloys used for applications for which resistance against
high temperature and corrosion, combined with high
stresses are required. They are usually high nickel alloys [1].
Heat tinting Coloration of a metal surface through a thin oxide film,
formed by heating in oxidizing atmosphere, to reveal details
of the microstructure [1].
Heat treatment Heating and cooling a solid metal or alloy in such a way that
desired properties are obtained [1].
Heterogenous Nonuniform in microstructure or composition [2].
High alloy steel Contains up to 2.5 % carbon and more than 6 % metallic
alloying elements, mainly chromium (Cr), nickel (Ni),
vanadium (V), tungsten (W), and manganese (Mn). Very hard
tool steels and ductile stainless steels are high alloy steels
[3].
Homogenizing Holding at high temperature to eliminate or decrease
chemical segregation by diffusion [1].
Hot dip coating Metallic coating obtained by dipping the basic metal into a
molten metal [1].
Hot etching Development and stabilization of the microstructure at
elevated temperature in etching solutions or gases [4].
Identification Etching for the identification of particular microconstituents
„selective… etching without attacking any others [4].
Image A representation of an object produced by means of
radiation, usually with a lens or mirror system [2].
Image processing, in The computer modification of a digitized image on a
image analysis pixel-by-pixel basis to emphasize or de-emphasize certain
aspects of the image [2]. See also Automatic image analysis.
Immersion etching The specimen is immersed in the etchant with the polished
surface up and is agitated. This is the most common etching
method [4].
Immersion objective An objective in which a medium of high refractive index is
used in the object space to increase the numerical aperture
and hence the resolving power of the lens [2].
Impact test A test to determine the behavior of materials when subjected
to high rates of loading, usually bending, tension, and
torsion. The quantity measures the energy absorbed in
breaking the specimen by a single blow, as in Charpy and
Izod tests [1].
Impregnation Process of filling voids and cracks under vacuum with a
„metallography/ sealing medium, for instance, epoxy cold mounting resin [3].
materialography…
Impression (1) Electron microscopy. The reproduction of the surface
contours of a specimen formed in a plastic material after the
application of pressure and heat, or both.
(2) Hardness. The imprint or dent made in the specimen by
the indenter of a hardness-measuring device [2].
Impurities Elements or compounds whose presence in a material is
undesired [1].
Inclusions Foreign material held mechanically, usually referring to
nonmetallic particles, such as oxides, sulfides, silicates, etc.
[2]. See also Exogenous inclusions, Nonmetallic inclusions.
Indentation Resistance of a material to indentation. This is the usual type
hardness of hardness test, in which a pointed or rounded indenter is
pressed into a surface under a substantially static load [3].
See also Hardness.
Indigenous A nonmetallic material that precipitates from the melt [2].
„endogenous… See Inclusions.
inclusion
Induction hardening Surface hardening in which only the surface layer of a
suitable ferrous work piece is heated by electrical induction
to hardening temperature and then quenched [3].
Ingot Casting of a simple shape suitable for hot working or
remelting [1].
Glossary 709
Intercrystalline Between crystals, or between grains of a metal, the same as

intergranular [1].
Intercrystalline Cracks or fractures that occur between the grains or crystals
cracks in a polycrystalline aggregate [2].
Interdendritic Corrosive attack that progresses preferentially along an
corrosion interdendritic path [1].
Interface Surface that forms the boundary between phases or systems,
or both [1].
Intergranullar A preferential attack at the grain boundaries [2].
corrosion
Intracrystalline Within or across the crystals or grains of a metal, same as
transcrystalline and transgranular [1].
Inverted microscope A microscope so arranged that the line of sight is directed
upwards through the objective to the object [2].
Ion etching Surface removal by bombardment with accelerated ions in a
vacuum 共1 to 10 kV兲 [4].
Iron Iron-based metals not falling into the steel category, such as
pure iron, gray iron, pig iron, white cast iron, etc. [3].
Isotropy The condition of having the same values of properties in all
directions [2].
Kikuchi lines Light and dark lines superimposed on the background of a
single crystal electron diffraction pattern caused by
diffraction of diffusely scattered electrons within the crystal
[2].
Koehler illumination A specular illumination system. In reflected-light
microscopy, used directly for the brightfield mode, and as a
preliminary setup for all other modes except darkfield. The
image of the field diaphragm is focused on the specimen
surface and the image of an undiffused lamp source is
focused in the plane of the aperture diaphragm [2].
Knoop hardness Microhardness determined from resistance of a metal to
indentation using a rhombic-based pyramidal diamond
indenter, which makes an impression with one long and one
short diagonal [3].
Lamellar structure A microstructure consisting of parallel plates of a second
phase [3]. See Pearlite.
Laminate (1) A composite material, usually in the form of sheet or bar,
composed of two or more materials bonded to form a solid
structure. (2) Product of two or more bonded metal layers
[3].
Lapping The abrasive removal of material using graded abrasive
particles in a loose form as in a liquid slurry on a platen [2].
Lapping tracks Indentations on the specimen surface made by abrasive
particles moving freely on a hard surface. These are not
scratches from a cutting action, but are the distinct tracks of
particles tumbling over the surface without removing
material [3].
Light metal Low density metal such as aluminum, magnesium, titanium,

beryllium, or their alloys [1].
Light micoscopy See Optical microscope.
Long-term etching Etching times of a few minutes to several hours [4].
Lubricant Any substance used to reduce friction between surfaces in
contact. Liquid used for cooling and lubricating. Depending
on the type of material and the preparation stage, different
types of lubricants can be used for grinding and polishing
[3].
Machining Removing surface material in the form of chips, usually with
a mechanical tool [3].
Macroetching Controlled etching of the surface of a metallic specimen,
intended to reveal a structure which is visible at low
magnifications (not usually greater than ten times) [2]. See
also Deep etching.
Macroscopic Observation using the naked eye or magnifications up to
10–30 times [3].
Macrostructure Structure of metals as revealed by macroscopic examination
of the etched surface of a polished specimen [1].
Magnetic-particle A nondestructive method of inspection for determining the
inspection existence and extent of possible defects in ferro-magnetic
materials. On the surface of a magnetized part fine magnetic
particles are attracted to areas where the magnetic field is
displaced or interrupted, such as cracks or pores [1].
Malleability The characteristic of metals that permits plastic deformation
in compression without rupture [1].
Malleable cast iron A cast iron made by prolonged annealing of white cast iron
in which decarburization or graphitization, or both, takes
place to eliminate some or all of the cementite [1].
Martensite Metastable phase resulting from the diffusionless athermal
decomposition of austenite below a certain temperature
known as the Ms temperature (martensite start
temperature). It is produced during quenching when the
cooling rate of a steel, in the austenitic condition, is such
that the pearlite and bainite, or both, transformation is
suppressed. The composition of the martensite is identical
with that of the austenite from which it transformed. Hence,
martensite is a super-saturated solid solution of carbon in
alpha iron (ferrite) having a body-centered tetragonal lattice.
It is a magnetic plate-like constituent formed by a
diffusionless shear type of transformation. These plates may
appear needle-like or veriform in cross section [2].
Glossary 711
Materialography Materialography is defined as an investigative method of

materials science. It emcompasses the optical examination
of microstructures, and its goal is a qualitative and
quantitative description of the microscopic structural
analysis of solid materials. Materialography includes
metallography, ceramography, plastography, and mineralogy
[4]. See also Metallography.
Matrix The continuous phase [2]. See Continous phase.
Mechanical Specimen preparation process using finer and finer
polishing abrasives, mostly diamond, to obtain a surface suited for
microscopic examination.
Mechanical The properties of a material that reveal its elastic and
properties inelastic behavior when force is applied, by indicating its
suitability for mechanical applications; for example,
modulus of elasticity, tensile strength, elongation, hardness,
and fatigue limit [1]. Compare with Physical properties.
Mechanical testing Determination of mechanical properties [1].
Mechanical twin A twin formed in a crystal by simple shear under external
loading [1]. See also Twin bands.
Metallograph An optical instrument for the examination of metallographic/
materialographic specimens. In principle it consists of a
light source, a microscope, and a camera.
Metallography That branch of science which relates to the constitution and
structure, and their relation to the properties, of metals and
alloys [2]. See also Materialography.
Metallurgy The science and technology of metals and alloys [1].
Metastable A state of apparent equilibrium which has a higher free
energy than has the true equilibrium state; usually applied to
a phase existing outside its temperature and pressure span
of equilibrium existence, by reason of a greatly delayed
transformation [2].
Microetching Development of microstructure for microscopic
observation.The usual magnification exceeds 25⫻ (50⫻ in
Europe) [1].
Micrograph A graphic reproduction of an object as seen through the
microscope or equivalent optical instrument, at
magnifications greater than ten diameters [2].
Micro indentation Hardness of a material determined by forcing an indenter
hardness into the polished surface of a material under very light load
„microhardness… using a microhardness tester [3]. See also Micro penetration
hardness.
Micro penetration The hardness number obtained by use of a low load tester
hardness whose indentation is usually measured with a high power
microscope [2]. See also Micro indentation hardness.
Microscopy The science of the interpretive use and applications of
microscopes [1].
Microstructure The structure of a suitably prepared specimen as revealed by

a microscope [2].
Mineralogy Scientific study of minerals [3]. See also Petrographic
examination.
Modulus of elasticity The measure of rigidity or stiffness of a metal; the ratio of
„E… stress, below the proportional limit, to the corresponding
strain. In terms of stress-strain diagram, the modulus of
elasticity is the slope of the stress-strain curve in the range of
linear proportionality of stress to strain. Also known as
Young's modulus [1].
Monochromatic Of the same wavelength [2].
„homogeneous…
Monocrystalline A solid composed of a unique crystal [3].
Morphology The shape characteristics of a structure; the form and
orientation of specific phase or constituent [2].
Mounting To embed the specimen in resin to facilitate the further
handling during grinding and polishing, and to improve the
preparation result [3].
Multiple etching A specimen is etched sequentially with the specific etchants
to reveal certain constituents [4].
Nitriding Nitriding is a form of surface hardening. By exposing a
ferrous part at a certain temperature to nitrogenous
materials, nitrogen will diffuse into the surface of the part
and form hard nitrides [3].
Nitrocarburizing Any of several case-hardening processes in which both
nitrogen and carbon are absorbed into the surface layers of
a ferrous material at a certain temperature. Nitrocarburizing
improves fatigue resistance [1].
Noble metal (1) A metal whose potential is highly positive relative to the
hydrogen electrode. (2) A metal with marked resistance to
chemical reaction, particularly to oxidation and to solution
by inorganic acids. The term as often used is synonymous
with precious metal [1].
Nodular cast iron Also called ductile cast iron; trace amounts of magnesium
are added to the melt to induce formation of free graphite
in the form of nodules. See also Spheroidal cast iron.
Nonmetallic Particles of impurities (usually oxides, sulfides, silicates, and
inclusions such) that are held mechanically or are formed during
solidification or by subsequent reaction within the solid
metal [2]. See also Exogenous inclusions, Inclusions.
Nondestructive Inspection by methods that do not destroy the part in order
testing to determine its suitability for use [1]. See also Field
metallography.
Normalizing Heating a ferrous alloy to a suitable temperature above the
transformation range and then cooling it in air to a
temperature substantially below the transformation range
[1].
Glossary 713
Numerical aperture The sine of half the angular aperture of an objective lens
„NA… multiplied by the refractive index of the medium between
the lens and the sample [2].
Objective The primary magnifying system of a microscope [1].
Ocular See Eyepiece.
Optical etching Develops the microstructure by using special illumination
techniques (dark field, interference contrast, polarized light,
phase contrast) [4].
Optical microscope Instrument containing one or more lenses which uses
artificial light to produce an enlarged image of an object
placed in the focal plane of the lens(es) [3].
Ore A natural mineral that may be mined and treated for the
extraction of any of its components, metallic or otherwise
[3].
Organic materials For example, wood, bone, tissue, teeth, paper.
Orientation The angular position of a crystal described by the angles
which certain crystallographic axes make with the frame of
reference. In hardness measurements, the relationship
between the direction of the axes of the indenter of a
hardness tester and the direction of nonhomogeneous
properties of the specimen [2].
Overheating (1) In ferrous alloys, heating to an excessively high
temperature such that the properties/structure undergo
modification. The resulting structure is very coarse-grained.
Unlike burning, it may be possible to restore the original
properties/structure by further heat treatment or mechanical
working, or a combination thereof. (2) In aluminum alloys,
overheating produces structures that show areas of
resolidified eutectic or other evidence that indicates the
metal has been heated within the melting range [2].
Oxide polishing Process used for the final polishing of a specimen with a
suspension containing fine abrasive particles of oxides
(aluminum oxide, silicon dioxide) with or without chemicals
of different pH. See also Final polishing.
Oxidation (1) A reaction in which there is an increase in valence
resulting from a loss of electrons. (2) A corrosion reaction in
which the corroded metal forms an oxide; usually applied to
reaction with a gas containing elemental oxygen, such as air
[1].
P Polishing (mechanical) taking place as the last steps (P1, P2,
P3, etc.) of metallographic/materialographic preparation to
obtain a surface suited for microscopic examination. See
also Final polishing, Oxide polishing, Polishing.
Particle size The controlling linear dimension of an individual particle,
such as of a powdered metal, as determined by analysis with
screens or other suitable instruments [1].
Pearlite A metastable microstructure formed when local austenite

areas attain the eutectoid composition in alloys of iron and
carbon containing greater than 0.025 % but less than 6.67 %
carbon. The structure is an aggregate consisting of alternate
lamellae of ferrite and cementite formed on slow cooling
during the eutectoid reaction. In an alloy of given
composition, pearlite may be formed isothermally at
temperatures below the eutectoid temperature by quenching
austenite to a desired temperature (generally above 550° C)
and holding for a period of time necessary for
transformation to occur. The interlamellar spacing varies
directly with the transformation temperature; that is, the
higher the temperature the greater the spacing [2].
Petrographic Methods of examining nonmetallic matter under suitable
examination microscopes to determine structural relationships and to
identify the phases or minerals present. With transparent
materials, the determination of the optical properties, such
as the indices of refraction and the behavior in transmitted
polarized light, serve as means of identification. With
opaque materials, the color, hardness, reflectivity, shape, and
etching behavior in polished sections serve as means of
identification. Metallographic applications include
examination of particles mechanically or chemically
separated from the metal by these methods [2].
PG Plane (planar) grinding. Removes damage introduced by
cutting, and levels specimens clamped in a holder for
automatic grinding [3]. See also Planar grinding.
pH The negative logarithm of the hydrogen-ion activity. It
denotes the degree of acidity or basicity of a solution. At
25° C 共77° F兲, 7.0 is the neutral value. Lower values than 7.0
indicate acidity and higher values increasing basicity [1].
Phase A physically homogeneous and distinct portion of a material
system [1].
Phase contrast A special method of controlled illumination, ideally suited
microscopy for observing thin, transparent objects whose structural
details vary only slightly in thickness or refractive index. This
can also be applied to the examination of opaque materials
to determine surface elevation changes [2].
Photo micrograph See Micrograph.
Physical etching Develops the microstructure through removal of surface
atoms, lowering the grain surface potential and deposition
of interference layers [4].
Physical properties Properties, other than mechanical properties, that pertain to
the physical nature of a material; for example, density,
electrical conductivity, thermal expansion, reflectivity
magnetic susceptibility, and so on [1]. See also Mechanical
properties.
Glossary 715
Physical testing Determination of physical properties [1].

Pig Metal casting poured from the melting furnace, used for
remelting [3].
Pitting Forming small sharp cavities in a metal surface if
„metallography… electrolytic polishing is not performed correctly.
Pixel „picture Smallest spatial unit of an image [2].
element…
Planar grinding The first step in a preparation procedure used to bring all
specimens into the same plane of polish. It is unique to semi
or fully automatic preparation equipment that utilize
specimen holders [2]. See also PG.
Plane grinding See PG.
Plasma spraying Coating technique in which the coating material is fed as
powder into an ionized gas atmosphere (plasma) and
sprayed in the molten state onto the surface to be coated [3].
Plastic Any of various organic compounds produced by
polymerization, capable of being molded, extruded, cast into
various shapes and films, or drawn into filaments used as
textile fibers [3].
Plastic deformation Deformation that remains or will remain permanent after
release of the stress that caused it [1].
Plasticity The capacity of a material to deform nonelastically without
rupturing [1].
Plating Forming an adherent layer of metal on metal, usually
through a galvanic process. Any adherent layer of metal on
other material can also be called plating [3].
Plowing In tribology, the formation of grooves by plastic deformation
of the softer of two surfaces in relative motion [1].
Polarized light A method of illumination in which the incident light is plane
illumination polarized before it impinges on the specimen [2].
Polishing A mechanical, chemical, or electrolytic process or
combination thereof used to prepare a smooth reflective
surface suitable for microstructure examination, free of
artifacts or damage introduced during prior sectioning or
grinding [2]. See also Final polishing, Oxide polishing,
Polishing cloth.
Polishing artifact A false structure introduced during a polishing stage of a
surface preparation sequence [1]. See also Artifact.
Polishing cloth A substrate, mostly a textile or a nonwoven material, used
for polishing of specimens with selected abrasives. See also
Final polishing, Oxide polishing, Polishing.
Polishing rate The rate of which material is removed from a surface during
polishing. It is usually expressed in terms of the thickness
removed per unit of time or distance traversed [1].
Polycrystalline Characteristic of an aggregate composed of more than one,
and usually of a large number, of crystals [2].
Polymers Plastics, for instance polyethylene, epoxy, polyester and

polyacryl, and polyamide (Nylon) [3].
Pores Small voids in the body of a material [1].
Porosity Holes in a solid, not necessarily connected [2].
Potentiostatic Anodic development of the microstructure at a constant
etching potential enables a defined etching of singular phases [4].
Powder Particles of a solid characterized by small size, nominally
within the range from 0.1 to 1000 ␮m [3].
Powder metallurgy Production and use of metal powders, which are hot pressed
and sintered into solid materials and shaped objects [1].
Precious metals Gold, silver, and platinum-group metals [3].
Precipitation Separation of a new phase from solid, liquid, or gaseous
solutions, usually with changing conditions of temperature
or pressure, or both [2].
Precipitation etching Develops the microstructure by the formation of reaction
products at the specimen surface [4].
Precipitation Hardening caused by precipitation of a constituent from a
hardening supersaturated solid solution [1]. See also Age hardening,
Aging.
Primary crystals The first type of crystals that separates from a melt on
cooling [2].
Primary etching Develops the cast microstructures including coring [4]. See
also Secondary etching.
Pull-out Void existing on the plane of polish of a metallographic
specimen caused by the dislodging of a particle or
constituent during the grinding or polishing operation [2].
Quantitative Determination of specific characteristics of a microstructure
metallography by making quantitative measurements on micrographs or
metallographic/materialographic images. Quantities so
measured include volume concentration of phases, grain
size, particle size, and surface-area-to-volume ratios of
micro-constituents, particles, or grains [1]. See also
Automatic image analysis.
Quenching Rapid cooling, usually in water [3].
Quenching crack A crack formed as a result of thermal stresses produced by
rapid cooling from a high temperature, not to be confused
with fire crack [2].
Ram Moving part in e.g, the cylinder of a mounting press [3].
Rare earth metals One of the group of 15 chemically similar metals with
atomic numbers 57 through 71, commonly referred to as the
lanthanides [1].
RCD Rigid composite disk, hard or soft, used for fine grinding.
See also Rigid grinding disk.
Recarburize (1) Increase the carbon content of molten cast iron or steel
by adding carbonaceous material, high-carbon pig iron or a
high carbon alloy. (2) Carburize a metal part to return
surface carbon loss in processing [1].
Glossary 717
Recrystallization The formation of a new grain structure through nucleation

and growth commonly produced by subjecting a metal, that
may be strained, to suitable conditions of time and
temperature [3].
Reflected light In the metallographic/materialographic microscope the
specimen is illuminated with reflected (incident) light. For
examination of mineralogical thin sections and in biology
the transmitted light is used.
Refractory (1) Material of very high melting point with properties that
make it suitable for furnace linings and kiln construction.
(2) Quality of resisting heat [1].
Refractory alloy (1) Heat-resistant alloy. (2) Alloy having an extremely high
melting point. (3) An alloy difficult to work at elevated
temperatures [1].
Refractory metal Metal with an extremely high melting point, above the range
of iron, cobalt, and nickel (Mo, V, W, Ta, Nb) [3].
Relief Due to varying hardness or wear rate of a matrix or
individual phases, or both; material is removed at different
rates, and relief is developed [3].
Removal rate The rate at which material is removed from a surface during
grinding and polishing. See also Polishing rate.
Replica A reproduction of a surface in a material, for example, a

plastic.
(1) Atomic. A thin replica devoid of structure on the
molecular level, prepared by the vacuum or hydrolytic
deposition of metals or simple compounds of low molecular
weight.
(2) Cast. A reproduction of a surface in plastic made by the
evaporation of the solvent from a solution of the plastic or
by polymerization of a monomer on the surface.
(3) Collodion. A replica of a surface cast in nitro-cellulose.
(4) Formvar. A reproduction of a surface in a plastic
Formvar film.
(5) Gelatin. A reproduction of a surface prepared in a film
composed of gelatin.
(6) Impression. A surface replica which is made by
impression. The results of making an impression.
(7) Molecular. The reproduction of a surface in a high
polymer such as collodion and other plastics.
(8) Negative. That replica which is obtained by the direct
contact of the replicating material with the specimen. In it,
the contour of the replica surface is reversed with respect to
that of the original.
(9) Oxide film. A thin film of an oxide of the specimen to be
examined. The replica is prepared by air, oxygen, chemical,
or electrochemical oxidation of the parent metal and is
subsequently freed either mechanically or chemically for
purposes of examination.
(10) Plastic. A reproduction in plastic of the surface to be
studied, prepared by evaporation of the solvent from a
solution of plastic, by polymerization of a monomer, or
solidification of a plastic on the surface.
(11) Positive. A replica, the contours of which correspond
directly to the surface being replicated; that is, elevations on
the surface are elevations on the replica.
(12) Preshadowed. A replica formed by the application of
the shadowing material to a surface to be replicated, before
the thin replica film is cast or otherwise deposited on the
surface.
(13) Pseudo. A replica which has portions of the material
being replicated embedded in it.
(14) Tape replica method (faxfilm). A method of producing a
replica by pressing the softened surface of a tape or sheet of
a plastic material on the surface to be replicated.
(15) Vapor deposited—a replica formed of a metal or a salt
by the condensation of the vapors of the material onto the
surface to be replicated [2].
Glossary 719
Reproducibility The ability to achieve the same result every time. In

specimen preparation reproducibility is crucial, as specimen
preparation is often employed in quality inspection and
failure analysis. Reproducibility can be ensured by using
consumables of high standard and uniform quality, and by
using automatic preparation equipment which controls
preparation parameters, e.g., rotational speed, force, dosing
levels, and time [3].
Resolution The fineness of detail in an object which is revealed by an
optical device. Resolution is usually specified as the
minimum distance by which two lines or points in the object
must be separated before they can be revealed as separate
lines or points in the image. The theoretical limit of
resolution is determined from the equation:
d = 0.61␭/共n sin A.A./2兲
where
d = minimum distance between object points
observed as distinct points in the image;
␭ = wavelength of the radiation employed;
n = the minimum refractive index of the media
between the object and the objective lens;
A.A. = the angular aperture 关2兴. See also Resolving
power.
Resolving power The ability of a given lens system to reveal fine detail in
an object 关2兴. See also Resolution.
Reticle A system of lines, circles, dots, cross hair or wires, or
some other pattern, placed in the eyepiece or an
intermediate plane on the optic axis which is used as a
measuring reference, focusing target, or to define a
camera field of view 共a reticle is different than a graticule兲
关2兴. See also Graticule.
Rigid grinding disk A nonfabric support surface, such as a composite of
metal/ceramic or metal/polymer, charged during use with
an abrasive 共usually 6 to 15 micrometre diamond
particles兲 and used for grinding operations in a
metallographic preparation 关2兴. See also RCD.
Rockwell hardness Indentation hardness test based on the depth of
test penetration of a specified penetrator 共cone or ball兲 into a
specimen under a specified load 关3兴.
Roughness Relatively finely spaced surface irregularities, the heights,
width, and directions of which establish the predominant
surface pattern 关1兴.
Rough polishing A polishing process after fine grinding to remove the layer
of significant damage caused by the grinding. Rough
polishing is followed by the steps polishing and final
polishing to finish the specimen preparation. See also
Final polishing, Oxide polishing, Polishing.
Scanning An electron microscope in which the image is formed by a
microscope beam operating in synchronism with an electron probe
scanning the object. The intensity of the image forming
beam is proportional to the scattering or secondary
emission of the specimen where the probe strikes it 关2兴.
See also SEM.
Scratches A groove produced in a surface by an abrasive point 关1兴.
Secondary etching Develops the microstructures that differ from primary
structures through transformation and heat treatment in
the solid state 关4兴. See also Primary etching.
Segregation Concentration of alloying elements in specific regions in a
metallic object 关2兴.
Segregation „coring… Develops segregation 共coring兲 mainly in macrostructures
etching and microstructures of castings 关4兴.
SEM Scanning Electron Microscope is a type of electron
microscope capable of producing high resolution images
of a specimen surface. Due to the manner in which the
image is created, SEM images have a characteristic
three-dimensional appearance and are useful for judging
the surface structure of the specimen 关3兴. See also
Scanning microscope.
SG iron See Ductile cast iron.
Shear 共1兲 That type of force that causes or tends to cause two
contiguous parts of the same body to slide relative to each
other in a direction parallel to their plane of contact. 共2兲 A
type of cutting tool with which a material in the form of
wire, sheet, plate, or rod is cut between two opposing
blades. 共3兲 The type of cutting action produced by rake so
that the direction of chip flow is other than at right angles
to the cutting edge 关1兴.
Short-term etching Etching time of seconds to a few minutes 关4兴.
Shrinkage Reduction in volume of a material from beginning to end
of solidification 关3兴.
Shrinkage cavity A void left in cast metals as a result of solidification
shrinkage 关1兴.
Shrinkage gaps Gaps are voids between the mounting resin and sample
material caused by shrinkage of the mounting resin 关3兴.
Single specimen Single specimens can be prepared on preparation systems
using specimen mover plates. The specimens are not
clamped and force is applied to each individual specimen
关3兴.
Glossary 721
Sintering Bonding of particles in a mass of metal powder by

heating, usually with prior compacting 关3兴.
Slag Nonmetallic product resulting from the dissolution of flux
and nonmetallic impurities in smelting, refining, and
certain welding operations 关1兴. See also Inclusions.
Slip Translation of a portion of a crystal relative to the
adjacent portion 关2兴.
Slip lines Traces of slip planes observed at low magnifications on
the polished surface of a crystal which has been deformed
after polishing; since no differences in orientation exist,
repolishing will remove the traces. With increasing
resolving power and magnification, an individual line may
be revealed as a series of parallel lines. The “line” which is
visible at low magnifications is then described as a slip
band 关2兴.
Smearing Plastic deformation of a soft matrix or soft phases.
Instead of being cut, the material is pushed, moved across
the surface. Smearing occurs when the abrasive is too
small or when using the wrong lubricant or polishing
cloth, or a combination of these conditions, which
reduces the cutting effect of the abrasive 关3兴.
Soldering Bonding of metals using filler metals at temperatures
below 450° C 关3兴.
Specimen A test object, often of standard dimensions or
configuration, or both, which is used for destructive and
nondestructive testing. One or more specimens may be
cut from each unit of a sample 关1兴.
Specimen holder A holder in which 3–12 specimens are clamped. During
„metallography/ specimen preparation force is applied to the center of the
materialography… holder 关3兴.
Spheroidal cast iron Same as nodular cast iron or ductile cast iron. See also
„SG… Nodular cast iron.
Spheroidite A coarse aggregate of carbide and ferrite usually produced
by tempering martensite at temperatures slightly below
the eutectoid temperature. Generally, any aggregate of
ferrite and large spheroidal carbide particles no matter
how produced 关2兴.
Spheroidizing Heating and cooling to produce a spheroidizing or
globular form of carbide in steel 关1兴.
Stage A device for holding a specimen in the desired position in
the optical path 关2兴.
Stage micrometre A graduated scale used on the stage of a microscope for
calibration 关2兴.
Staining Staining is a discoloration of the specimen surface,
typically caused by water, alcohol, or etching solutions
关3兴.
Stainless steel Any of several steels containing 12 to 30 % chromium as

the principal alloying element 关1兴.
Steel Malleable iron-base alloy, containing carbon and other
alloying elements. Carbon and low-alloy steels contain a
maximum of 2 % carbon, high-alloy steels up to 2.5 %
carbon and over 8 % metallic alloying elements 关3兴.
Stereology The study of mathematical procedures used to derive
three-dimensional parameters describing a structure from
two-dimensional measurement 关2兴.
Stereomicroscope A light optical microscope that permits each eye to
examine the specimen at a slightly different angle, thereby
retaining its three-dimensional relationship 关2兴.
Strain hardening An increase in hardness and strength caused by plastic
deformation at temperatures below the recrystallization
range 关1兴.
Stringer A single, high-aspect ratio, elongated inclusion, two or
more elongated inclusions, or a number of small
nondeformable inclusions aligned in a linear pattern due
to deformation 关2兴. See also Inclusions.
Structure As applied to a crystal, the shape and size of the unit cell
and the location of all atoms within the unit cell. As
applied to microstructure, the size, shape, and
arrangement of phases 关2兴. See also True structure,
Polishing.
Subgrain A portion of a crystal or grain, with an orientation slightly
different from the orientation of neighboring portions of
the same crystal or grain 关1兴.
Substrate 共Substratum兲 that which lies under 关2兴.
Superalloy Same as heat-resistant alloy; superalloys are heat and
corrosion resistant and ductile and contain up to 20 %
chromium 共Cr兲关3兴. See also Heat-resistant alloy.
Swab etching Wiping the specimen surface with cotton saturated with
an etchant. This will simultaneously remove undesired
reaction products 关4兴.
Swarf Mixture of chips, abrasive material, and lubricating
medium developing during grinding/polishing.
Technical ceramics Pressed and sintered oxides, carbides, and nitrides. They
are very dense, insulators, highly wear resistant, and
resistant against chemicals: aluminum oxide 共Al2O3兲,
silicon carbide 共SiC兲, silicon nitride 共Si3N4兲, tungsten
carbide 共WC兲, titanium carbide 共TiC兲, boron carbide
共B4C兲, titanium boride 共TiB2兲, zirconium oxide 共ZrO2兲
关3兴.
Glossary 723
TEM The Transmission Electron Microscope is an imaging

instrument whereby a beam of electrons is focused onto a
specimen causing an enlarged version to appear on a
fluorescent screen or layer of photographic film or can be
detected by a CCD camera 关3兴. See also Thin foil,
Transmission microscope.
Tensile testing To determine the strength of a material by pulling a
sample applying equal and constant stress until it breaks.
The elongation of the sample is also measured. Also
known as tension testing 关3兴.
Thermal Any physical process taking place due to heat 关3兴.
Thermal etching Annealing the specimen in a vacuum or inert atmosphere.
This is a preferred technique for high-temperature
microscopy and for ceramics 关4兴.
Thermoplastic resins Mounting resins that soften or melt at elevated
temperatures and harden during cooling 关3兴.
Thermosetting Mounting resins that cure under heat and pressure and
resins cannot be melted after curing. They are also called
duroplastics 关3兴.
Thin foil A very thin specimen prepared for transmission
microscopy. See also TEM.
Tool steel Any of a class of carbon and alloy steels commonly used
to make tools. Tool steels are characterized by high
hardness and resistance to abrasion, often accompanied
by high toughness and resistance to softening at elevated
temperature. These attributes are generally attained with
medium carbon and high-alloy contents 关1兴.
Traditional ceramics Earthenware, brick, clay, porcelain 关3兴.
Transmission A microscope in which the image forming rays pass
microscope through 共are transmitted by兲 the specimen being observed
关2兴. See also TEM.
True structure The microstructure representing the material without any
influences from the preparation of the specimen. See also
Structure, Polishing.
Twin bands Bands across a crystal grain, observed on a polished and
etched section, the crystallographic orientations of which
have a mirror image relationship to the orientation of the
matrix grain across a composition plane which usually is
parallel to the sides of the band. 共1兲 Annealing twins—
twin bands which are produced during annealing
following cold work. 共2兲 Mechanical twins—twin bands
which are produced by cold work. 共3兲 Neumann bands—
mechanical twins in ferrite 关2兴.
Ultrasonic cleaning Immersion cleaning aided by ultrasonic waves that cause
microagitation 关1兴.
Ultrasonic testing Nondestructive test used on sound conductive materials to

locate cavities, cracks, and structural discontinuities by
means of ultrasonic impulse 关3兴.
Vibratory polishing Mechanical polishing process where one or several
specimens are moved around in a bowl through vibration
of the bottom of the bowl.
Vickers In a more restricted sense, the 136° diamond pyramid
indenter used in microindentation hardness tests 关2兴. See
also Micro indentation hardness, Micro penetration
hardness, Vickers hardness test.
Vickers hardness Indentation hardness test using a pyramid-shaped
test diamond indenter and variable loads which enables the
use of one hardness scale for all materials from very soft
lead to tungsten carbide 关3兴. See also Micro indentation
hardness, Micro penetration hardness, Vickers.
Weld Union between materials by welding 关3兴. See also Welding.
Welding Joining two or more pieces of metal by applying heat or
pressure, or both, with or without a filler material, to
produce a localized union through fusion or
recrystallization across the interface 关1兴.
Weld structure The microstructure of a weld deposit and heat-affected
base metal 关2兴. See also Welding.
Wet etching The specimen surface has to be wetted before immersion
into the etching solution. This is important for color
etchants 关4兴.
Whiskers Metallic or ceramic filaments, mostly microscopic, more
or less evenly distributed in a matrix 关3兴.
White cast iron Cast iron that shows a white fracture because the carbon
is present in the form of iron carbide, Fe3C, which gives
it its very high hardness and also brittleness 关3兴.
White metal A general term covering a group of white-colored metals
and their alloys of relatively low melting points 共lead,
antimony, tin, cadmium, bismuth, and zinc兲 and alloys
based on these metals 关1兴.
Wire cutting A cutting method mainly used for sectioning of small
specimens of various types of materials. A fine wire is
drawn along the work piece with a controlled force. The
abrasive is either diamond bonded to the wire, or an
abrasive slurry that is dripped continuously onto the wire
and drawn into the cut 关3兴.
Workability See Formability.
Work hardening A change in the hardness of a material as a result of
plastic deformation 关2兴.
Working distance The distance between the surface of the specimen being
examined and the front surface of the objective lens 关2兴.
Glossary 725
Wrought iron An iron produced by direct reduction or ore or by refining

molten cast iron under conditions where a pasty mass of
solid iron with included slag is produced. The iron has a
low carbon content 关1兴.
X-ray testing Using X-ray radiation to check work pieces for cavities,
cracks, pores, and overlaps. Especially used for checking
of welds 关3兴.
Young’s modulus A term used synonymously with modulus of elasticity. The
ratio of tensile or compressive stresses to the resulting
strain 关1兴. See also Modulus of elasticity.
References „Glossary…
[1] Benscoter, A. O. and Bramfitt, B. L., Metallographer’s Guide, Practices and
Procedures for Irons and Steels, ASM International, Materials Park, Ohio, USA, 2002.
Reprinted with permission of ASM International®. All rights reserved. www.
asminternational.org
[2] ASTM Standard, Terminology Relating to Metallography 共E 7兲, ASTM International,
West Conshohocken, Pennsylvania, USA, 2003.
[3] Terms defined by Struers in the on-line training material e-Education and e-Training
under www.struers.com.
[4] Petzow, G., Metallographic Etching, ASM International, Materials Park, Ohio, USA,
1999.
Subject Index
A Arc of contact, metallographic/
materialographic cutting
Abbreviations operation, 31
occupational safety and health, Archiving, 619
labs, 673–674 Artifacts of electrolytic polishing,
specimen preparation, 221 selection of preparation method, 7
Abrasive cut-off machines, 36–43 ASTM B 487, 576
design principles of wheel-work ASTM C 664, 576
piece contact, 36–39 ASTM E 45, 570
machine designs, 39–43 ASTM E 112, 571–573
Abrasive cut-off wheels, 32–36 ASTM E 562, 569
consumable wheels, 32–34 ASTM E 930, 573
slow consumable wheels, 34–36 ASTM E 1077, 575
Abrasives, 18–19 ASTM E 1122, 570
aluminum oxide, 18 ASTM E 1181, 573
cubic boron nitride, 18 ASTM E 1245, 570
diamond, 18–19 ASTM E 1268, 574
polishing, 129–132 ASTM E 1382, 573
silicon carbide, 18 ASTM E 1578, 619
wet abrasive cutting, ASTM E 2014, 668, 674
sectioning, 16–21 ASTM E 2109, 574–575
Acrylics ASTM standards
occupational safety and health, cutting fluids, wet abrasive
labs, 668 cutting, 29
specimen preparation, 436–439 hardness, 625
After preparation cleaning, 82–84 metallography, 188–193
Agency for Toxic Substance and Atomic force microscope 共AFM兲, 561
Disease Registry 共ATSDR兲, 683–684 Automatic grinding equipment,
Alcohol-based grinding/polishing 119, 135
fluids, 97 Automatic image analysis, 577–617
Alumina wet grinding paper, 105–106 analog cameras, 614–615
Aluminum automatic measurements,
electrolytic polishing and 600–602
etching, 464 background correction, 586–588
specimen preparation, 352–356 banding degree, 608
Aluminum alloys, 356–358 brightness and contrast, 581–586
Aluminum oxide cameras, 614–615
abrasive types, 18 compacted graphite, 613
grinding abrasives, 93 computers, 614
specimen preparation, 238–240 contrast stretching, 588–589
American Conference of Government depth measurements, 608–610
Industrial Hygienists 共ACGIH兲, 683 digital cameras, 615–616
Analog cameras, automatic image digital imaging, 579, 602–613
analysis, 614–615 digital imaging technology,
Anodic etching, 172–173 613–616
Anodized coatings, specimen ductile cast iron, 611–613
preparation, 247–251 grain size, 606–608
Anodizing, etching, 173 graphite in iron castings, 610–611
Antimony, specimen preparation, gray cast iron, 613
361–364 hardware, 613–616
727
histogram, 581 Bias, quantitative metallography/

image acquisition, 579–580 materialography, 568–569
image calibration, 595–598 Blades, bandsawing, 49–51
image digitization, 580–581 Bond materials
image measurement, 598–602 cut-off wheel, 20–21
image processing, 586–595 wet abrasive cutting, sectioning,
implementation, 617–618 16–21
inclusion rating, 603–606 Bones, specimen preparation, 427–430
manual measurements, 599–600 Boron carbide
open source/public domain grinding abrasives, 97
software, 617 specimen preparation, 227–232
percent area, 602–603 Brass, specimen preparation, 376–380
printers, 616 Brightness and contrast, automatic
sharpening, 593–595 image analysis, 581–586
smoothing, 592–593 Brinell hardness testing, 626–628
software, 616–617 British Standards Institution, 684
thickness measurements, 608–610 Brittle materials, grinding, 92–93
volume fraction, 602–603 Bronze
watershed filter, 590–592 electrolytic polishing
Automatic measurements, automatic and etching, 467
image analysis, 600–602 specimen preparation, 376–380
Automatic systems, polishing, 140–143 Building labs, 649, 650–663
Automation labs, 651–654
Availability of NIOSH Registry of Toxic
Effects of Chemical Substances, 681 C
Calcium oxide, specimen
B
preparation, 241
Background correction, automatic Calibration, quantitative
image analysis, 586–588 metallography/materialography, 568
Bacteria and fungi, cutting fluids, wet Cameras, automatic image
abrasive cutting, 28–29 analysis, 614–615
Bakelite bond, 20–21 Capacitors, specimen preparation,
Banding, quantitative metallography/ 298–300
materialography, 574 Carbonitrided steels, specimen
Banding degree, automatic image preparation, 339–342
analysis, 608 Cement clinker, specimen preparation,
Bandsawing, 48–52 346–349
blades, 49–51 Cemented carbides, 187
cutting fluids, 51 Ceramic capacitors, specimen
machines, 49–51 preparation, 281–284
safety, 49 Ceramic layers, specimen preparation,
tips, 51–52 268–270
Barium titanate, specimen Ceramic resistors, specimen
preparation, 241 preparation, 281–284
Baumann hammer, 644 Ceramics
Before preparation start cleaning, 82 deformation, grinding, 92–93
Beryllium, specimen preparation, specimen material, 182
365–367 specimen preparation, 232–235
Subject Index 729
Cerium oxide, specimen Color etching, 172

preparation, 241 Color ratings system, occupational
Chemical disposals, occupational safety safety and health, labs, 669
and health, labs, 672–673 Compacted graphite, automatic image
Chemical etching, 172 analysis, 613
Chemical mechanical polishing 共CMP兲, Comparison procedure, quantitative
7, 151–152 metallography/materialography,
Chemical microetching, examination 571–572
purpose, 194–217 Composites
Chemical polishing, 7 specimen material, 183
electrolytic polishing/etching, 168 specimen preparation, 276–281
Chips, sliding, plowing, grinding Compressed air, cleaning, 83
mechanics, 22 Computers, automatic image
Chromium analysis, 614
electrolytic polishing Concrete, specimen preparation,
and etching, 464–465 346–349
specimen preparation, 367–370 Confocal laser scan microscope,
Chromium carbide, specimen 552–555
preparation, 232–235 Consumable abrasive cut-off wheels
Chromium oxide, specimen storing, 33–34
preparation, 238–240 wheel dimensions, 33
Circular sawing, 48 wheel velocity, 32–33
Clamping, thermal damage, wet
Consumables, specimen preparation,
abrasive cutting, 24–25
221
Classical etching, 172
Contemporary grinding, 106–117
Classification of materials, specimen
diamond film, 109
material, 181
diamond pads, 109
Cleaning, 82–84
fine grinding cloths, 116
after preparation, 82–84
magnetic fixation, 106–107
drying, 83
metal-bonded diamond-coated
ethanol, 83
disks, 109
grinding disks, 84
resin-bonded diamond grinding
hand, 82–83
disks, 107–108
polishing cloths, 84
before preparation start, 82 resin-bonded SiC grinding
rubbing effect, 83 disks, 108
ultrasonic, 83 rigid composite disks, 109–116
ultrasonic apparatuses, 83 Contrast stretching, automatic image
Cleanliness, 84 analysis, 588–589
Cloths, polishing, 124–129 Cooling, cutting fluids, 26
Coatings, specimen material, 182–183 Cooling system, cutting fluids, wet
Cobalt abrasive cutting, 27–28
electrolytic polishing Copper
and etching, 465–466 electrolytic polishing
specimen preparation, 370–373 and etching, 466
Cobalt-based super alloys, specimen specimen preparation, 376–380
preparation, 373–376 Copper-bearing alloys, specimen
Cold mounting resins, occupational preparation, 380–383
safety and health, labs, 667 Cubic boron nitride, abrasive types, 18
Cubic boron nitride 共CBN兲, grinding Depth measurements, automatic image

abrasives, 97 analysis, 608–610
Cut-off grinding process, wet abrasive Design principles of wheel-work
cutting, sectioning, 15–16 piece contact
Cut-off wheel abrasive cut-off machines, 36–39
abrasive types, 18–19 direct cutting, 36
bond material, 20–21 oscillating cutting, 36–37
grade, 20 rotating work piece, 39
grain size, 19–20 step cutting, 38–39
rpm, 30 Diamond products
selection, 44–45 abrasive types, 18–19
specifications, 16–18 film, 109
structure, 20 fixed grains, 95
truing and dressing, 26 grinding abrasives, 94–96
wear, 25–26 loose grains, 95–96
wet abrasive cutting, sectioning, monocrystalline, 94
16–21 pads, 109
Cutting fluids, 26–29 pastes, 96
ASTM standards, 29 polycrystalline, 94
bacteria and fungi, 28–29 sprays, 96
bandsawing, 51 suspensions, 96
cooling system, 27–28 Differential interference contrast 共DIC兲,
grinding fluid application, 27 etching, 169
Diffusion coatings, specimen
grinding fluid concentration, 28
preparation, 251–254
grinding fluid disposal, 29
Digital cameras, automatic image
health and safety aspects, 29
analysis, 615–616
lubrication and cooling, 26
Digital image management, 619
synthetic grinding fluids-oil-
Digital imaging, automatic image
based, 26–27
analysis, 579, 602–613
water quality, 28
Digital imaging technology, automatic
CVD coatings, specimen preparation,
image analysis, 613–616
247–251
Diodes, specimen preparation, 281–284
Direct cutting, design principles of
D wheel-work piece contact, 36
Documentation, optical reflected light
Dangers, occupational safety and microscope, 550–552
health, labs, 664 Drying, cleaning, 83
Dark-field illumination 共DF兲, Ductile cast iron, automatic image
etching, 169 analysis, 611–613
Decarburization, quantitative Dust, occupational safety and health,
metallography/materialography, labs, 667
575–576 Dynamic hardness testing procedures,
Deformation, 89–93 644–645
brittle materials, 92–93
ceramics, 92–93
E
grinding, 86 Economy, grinding, traditional, 105
metals, 89–92 Edge retention, grinding, traditional,
polishing, 122–124 103–105
Subject Index 731
Education, labs, 651 electron microscope 共TEM兲, 167–168

Electric discharge machining 共EDM兲, Electrolytically deposited coatings,
sectioning by melting, 46 251–254
Electrolytes, polishing/etching, 163–164 Electron backscatter diffraction
Electrolytic polishing and etching, 共EBSD兲, 559–560
172–173, 453–475 polishing, 149–150
aluminum, 464 Electron microscopy, 558–561
bronze, 467 atomic force microscope 共AFM兲,
chromium, 464–465 561
cobalt, 465–466 electron backscatter diffraction
copper, 466 共EBSD兲, 559–560
gray cast iron, 459 electron probe microanalyzer
hard metals, 474–475 共EPMA兲, 560
heat treated steels, 459–460 energy dispersive spectroscopy
high carbon steels, 457 共EDS兲, 559
high-speed steels, 462–463 focused ion beam 共FIB兲, 560
iron, 462 magnetic force microscopy
lead, 467–468 共MFM兲, 561
low-alloyed tool steels, 463 scanning electron microscope
low carbon steels, 457–458 共SEM兲, 558–559
magnesium, 468–469 scanning probe microscopes
nickel, 469 共SPM兲, 560–561
silver, 469–470 scanning transmission electron
stainless steels, 460–461 microscope 共STEM兲, 558
super alloys, 461 transmission electron microscope
tin, 470–471 共TEM兲, 558
titanium, 471 Electron probe microanalyzer 共EPMA兲,
tungsten, 472 560
vanadium, 472–473 Electropolishing in practice, 164–165
zinc, 473 Energy dispersive spectroscopy 共EDS兲,
zirconium, 474 559
Electrolytic polishing/etching, 156–168 Engraving, marking, 80
chemical polishing, 168 Environment, grinding, traditional, 105
electrolytes, 163–164 Environmental Protection Agency
electrolytic thinning for 共EPA兲, 683
transmission electron microscope EPDM polymers, 430–436
共TEM兲, 167–168 Epoxy, occupational safety and health,
electropolishing in practice, labs, 667
164–165 Equipment
equipment, 165–166 electrolytic polishing/etching,
field metallography, 166–167 165–166
nondestructive electropolishing, labs, 656–660
166–167 Equotip tester, 645
occupational safety and health, Etchant names, examination purpose,
labs, 665 217
process, 156–163 Etching, 169–176
Electrolytic polishing etching, anodic, 172–173
artifacts, 7 anodizing, 173
Electrolytic thinning for transmission chemical, 172
classical, 172 electrolytic polishing/etching,

color, 172 166–167
dark-field illumination 共DF兲, 169 polishing, 150–151
differential interference contrast Field metallography/materialography,
共DIC兲, 169 specimen preparation, 475–476
electrolytic, 172–173 Field selection, quantitative
examination purpose, 194 metallography/materialography,
fluorescence, 170 568–569
grain boundary etching, 171 Fine grinding, 86, 119
grain contrast etching, 170–171 Fine grinding cloths, 116
heat tinting, 172 Fixed grains, diamond products, 95
ion, 173–174 Flammable and Combustible Liquids,
macroetching, 174–175 680
microetching, 169 Flammable liquids, occupational safety
microscope techniques, 169–170 and health, labs, 667
occupational safety and health, Fluorescence, etching, 170
labs, 665–666 Focused ion beam 共FIB兲, 560
physical, 173–174 Force
polarized light 共POL兲, 169–170 material removal, grinding, 89
potentiostatic, 173 metallographic/materialographic
precipitation, 172 cutting operation, 30
preparation process, 13 Fracturing, sectioning, 45
reactive sputtering, 174 Free cutting, 31–32
automatics, 32
relief polishing, 173
hand, 32
reproducibility, 171–172
sputtering, 174
thermal, 174 G
vapor deposition, 174
Ethanol, cleaning, 83 Galvanization, specimen preparation,
European Union 共EU兲, occupational 251–254
safety and health, labs, 669–670, 684 General Description and Discussion of
Examination purpose, 179, 188 the Levels of Protection and
ASTM standards, 188–217 Protective Gear, 680–681
chemical microetching, 194–217 General studies or routine work, 14
etchant names, 217 General use, machine designs, abrasive
etching practice, 194 cut-off, 40–41
Eyepieces, optical reflected light Generic methods, specimen
microscope, 535–536 preparation, 219
Germanium, specimen preparation,
288–291
F Glasses, specimen preparation,
244–247
Failure analysis, labs, 651 Gold, specimen preparation, 384–387
Feed speed, metallographic/ Grades
materialographic cutting operation, cut-off wheel, 20
30–31 hard, 20
Ferrous metals, specimen material, soft, 20
183–184 Grain boundary etching, 171
Field metallography Grain contrast etching, 170–171
Subject Index 733
Grain penetration, material removal, Grinding/polishing equipment, 117–119

grinding, 89 automatic grinding, 119
Grain shape, material removal, fine grinding, 119
grinding, 88 manual grinding, 117–119
Grain size plane grinding, 117–119
automatic image analysis, Grinding/polishing fluids, 89, 97–99
606–608 alcohol-based, 97
cut-off wheel, 19–20 oil-based, 98–99
quantitative metallography/ water-based, 97
materialography, 571–573 water-oil based, 98
Graphite in iron castings, automatic Grit number, 19
image analysis, 610–611
Gray cast iron H
automatic image analysis, 613
electrolytic polishing and etching, Hacksawing, 48
459 Hand cleaning, 82–83
specimen preparation, 315–318 Hard grade, 20
Grinding, 85–86 Hard metals, electrolytic polishing
chips, sliding, plowing, 22 and etching, 474–475
contemporary, 106–117 Hardness, 623–625
deformation, 86, 89–93 ASTM standards, 625
fine, 86 indentation, 623–624
material removal, 86–89 testing special methods, 646
plane, 85 Hardness values
traditional, 99–106 conversion, 642–643
wet abrasive cutting, sectioning, precision, 642
21–22 Hardware, automatic image
Grinding, traditional, 99–106 analysis, 613–616
alumina wet grinding paper, Hazard Communication Standard
105–106 共HCS兲, OSHA standard, 674–679
economy, 105 Health and safety aspects, cutting
edge retention, 103–105 fluids, 29
environment, 105 Heat tinting, etching, 172
relief, 103–105 Heat treated steels, electrolytic
SiC wet grinding paper, 100–105 polishing and etching, 459–460
stones/disks, 99–100 High-alloy steels, specimen
zirconia alumina wet grinding preparation, 325–328
paper, 105–106 High carbon steels
Grinding abrasives, 93–97 electrolytic polishing and etching,
aluminum oxide, 93 457
boron carbide, 97 specimen preparation, 307–311
cubic boron nitride 共CBN兲, 97 High-speed steels
diamond, 94–96 electrolytic polishing and etching,
silicon carbide, 93 462–463
Grinding disks cleaning, 84 specimen preparation, 343–346
Grinding fluid Histogram, automatic image analysis,
application, 27 581
concentration, 28 HMIS, occupational safety and health,
disposal, 29 labs, 670
Hot dip zinc coatings, specimen L

Human eye, light microscopy, 526–527 Laboratory information management
Hydroxyapatite 共HA兲 coating, specimen systems 共LIMS兲, 619
preparation, 223–226 Labs, 649
automation, 651–654
building, 649, 650–663
I education, 651
equipment, 656–660
Identification tag marking, 80
failure analysis, 651
Illumination, optical reflected light
layout, 660–662
microscope, 536–537
maintenance, 662–663
Image
occupational safety and health,
acquisition, 579–580
649, 664–684
calibration, 595–598
planning, 654–656
digitization, 580–581
purpose, 650
measurement, automatic image
quality control, 650
analysis, 598–602
rationalization, 651–654
processing, automatic image
research, 651
analysis, 586–595
running, 649
Implementation, automatic image
testing and inspection labs, 651
analysis, 617–618
Laser torching, sectioning by
Inclusion rating
melting, 46
automatic image analysis,
Layout, labs, 660–662
603–606
Lead
quantitative metallography/
electrolytic polishing and etching,
materialography, 570
467–468
Indentation hardness, 623–624
specimen preparation, 387–391
Instrumented indentation testing, Light microscopy, 525–527
641–642 human eye, 526–527
Integrated circuits. specimen magnification, 527
preparation, 301–305 magnifying lens and microscope,
Intercept procedure, quantitative 527
metallography/materialography, visible light, 525–526
572–573 List of Highly Hazardous Chemicals,
International Chemical Safety Cards, Toxics and Reactives, OSHA
682–683 standards, 680
Ion etching, 173–174 Literature, occupational safety and
Iron, electrolytic polishing and etching, health, labs, 684–686
462 Loose grains, diamond products, 95–96
Low-alloy steels, specimen preparation,
J 336–339
Low-alloyed steels, electrolytic
Job Safety Analysis 共JSA兲, 670–672 polishing and etching, 463
Low carbon steels
K 457–458
Knoop hardness testing, 633–634 Lubricants, 97–99
Subject Index 735
cutting fluids, 26 specimen or sample, 8–9

Materialography, 3
Mechanical damage, wet abrasive
M cutting, 22–23
Machine designs, 39–43 unplane surface, 23
general use, 40–41 waviness, 23
polishing, 135–139 Mechanical polishing artifacts,
precision, 41–43 selection of preparation method, 7
Machines, bandsawing, 49–51 Mechanical preparation, occupational
Macroetching, 174–175 safety and health, labs, 665
Magnesium Mechanical surface preparation. see
electrolytic polishing and etching, grinding
468–469 Medium carbon steels, specimen
specimen preparation, 391–394 preparation, 307–311
Magnesium oxide, specimen Metal-bonded diamond-coated disks,
preparation, 241 contemporary grinding, 109
Magnetic fixation, contemporary Metallographic/materialographic
grinding, 106–107 cutting operation
Magnetic force microscopy 共MFM兲, 561 arc of contact, 31
Magnification, light microscopy, 527 cut-off wheel rpm, 30
Magnifying lens and microscope, 527 feed speed, 30–31
Maintenance, labs, 662–663, 673 force, 30
Malleable cast iron, specimen free cutting, 31–32
preparation, 315–318 power, 31
Manganese, specimen preparation, wet abrasive cutting,
395–397 sectioning, 29–32
Manual grinding equipment, wheel velocity, 30
117–119, 135 Metallographic/materialographic
Manual measurements, automatic preparation, 5–6
image analysis, 599–600 Metallography, 3
Marking, 80 Metals, deformation, grinding, 89–92
engraving, 80 Microelectronic material, specimen
identification tag, 80 preparation, 291–293
stamping, 80 Microelectronic materials, polishing,
with waterproof ink, 80 143–147
Martens scratch hardness, 646 Microelectronic packages
Material exam, 179 polishing, 147–149
Material removal, 86–89 specimen preparation,
force on specimens, 89 295–298, 301–305
grain penetration, 89 Microetching, 169
grain shape, 88 Microindentation hardness, 636–639
grinding, 86 Microscopes
grinding/polishing fluids, 89 options, 537–538
polishing, 120–122 techniques, etching, 169–170
rake angle, 87–88 Microtomy, polishing, 155
Material Safety Data Sheet 共MSDS兲, Mineralogical materials, specimen
occupational safety and health, labs, material, 184
670–672 Minerals, ores, specimen preparation,
Materialographic specimen, 7–9 349–352
Mohs scratch hardness, 646 Protection and Protective Gear,

Molybdenum, specimen preparation, 680–681
398–401 Hazard Communication Standard
Monocrystalline, diamond products, 94 共HCS兲, 674–679
Mounting List of Highly Hazardous
occupational safety and health, Chemicals, Toxics and
labs, 664–665 Reactives, 680
preparation process, 11 Occupational Exposure to Hazardous
Chemicals in Laboratories, 679–680
Occupational safety and health labs,
N 649, 664–684
abbreviations, 673–674
National Fire Protection Association acrylics, 668
共NFPA兲, 684 Agency for Toxic Substance and
National Paint and Coatings Disease Registry 共ATSDR兲,
Association, 684 683–684
National Technical Information Service American Conference of
共NTIS兲, 683 Government Industrial
National Toxicology Program 共NTP兲, Hygienists 共ACGIH兲, 683
683 ASTM E 2014, 668, 674
NFPA 704 Hazard Identification British Standards Institution, 684
Ratings System, 668–669 chemical disposals, 672–673
Nickel cold mounting resins, 667
electrolytic polishing and etching, color ratings system, 669
469 dangers, 664
specimen preparation, 402–405 dust, 667
NIOSH standards, 681–682 electrolytic polishing/etching, 665
Nodular cast iron, specimen Environmental Protection Agency
preparation, 319–321 共EPA兲, 683
Nondestructive electropolishing, epoxy, 667
electrolytic polishing/etching, etching, 665–666
166–167 EU system, 669–670
Nonferrous metals, specimen material, European Union 共EU兲, 684
184–186 flammable liquids, 667
HMIS, 670
International Chemical Safety
O Cards, 682–683
Job Safety Analysis 共JSA兲,
Occupational Exposure to Hazardous 670–672
Chemicals in Laboratories, 679–680 literature, 684–686
Occupational Safety and Health maintenance and service, 673
Administration 共OSHA兲 standards Material Safety Data Sheet
Availability of NIOSH Registry of 共MSDS兲, 670–672
Toxic Effects of Chemical mechanical preparation, 665
Substances, 681 mounting, 664–665
Flammable and Combustible National Fire Protection
Liquids, 680 Association 共NFPA兲, 684
General Description and National Paint and Coatings
Discussion of the Levels of Association, 684
Subject Index 737
National Technical Information P

Service 共NTIS兲, 683
National Toxicology Program Paint layers, specimen preparation,
共NTP兲, 683 257–260
NFPA 704 Hazard Identification Palladium, specimen preparation,
Ratings System, 668–669 406–409
NIOSH standards, 681–682 Parameters, specimen preparation,
OSHA standards, 674–681 220–221
polyesters, 668 Pastes, diamond products, 96
risk phrases, 670 Path of light rays, optical reflected light
safety information, 668–672 microscope, 528
sectioning, 664 PCB coupon, specimen preparation,
Standard Operating Procedure 305–307
Percent area, automatic image analysis,
共SOP兲, 670–672
602–603
standards, 673
Phenolic bond, 20–21
toxic substances, 666
Physical etching, 173–174
training, 673
Pitting, 9
Oil-based grinding/polishing fluids, Plane grinding, 85, 117–119
98–99 Planimetric procedure, quantitative
Open source/public domain software, metallography/materialography, 572
image analysis, 617 Planning, labs, 654–656
Optical examination methods, reflected Plasma spray coatings, specimen
light microscope, 540–546 preparation, 265–267, 270–273
Optical fibers, specimen preparation, Plasma torching, sectioning by
244–247 melting, 46
Optical reflected light microscope, Plated coatings, specimen preparation,
528–555 251–254
confocal laser scan microscope, Point count, quantitative
552–555 metallography/materialography, 569
documentation, 550–552 Polarized light 共POL兲, etching, 169–170
eyepieces, 535–536 Poldi impact hardness tester, 644
illumination, 536–537 Polishing, 120–155
microscope options, 537–538 abrasives, 129–132
automatic grinding/polishing
optical examination methods,
equipment, 135
540–546
automatic systems, 140–143
path of light rays, 528
chemical mechanical polishing
practical use of microscope,
共CMP兲, 151–152
546–550 cloths, 84, 124–129
reflected-light microscope, deformation, 122–124
538–540 dynamics, 139–140
stereo microscopy, 555–557 electron backscatter diffraction
Ores, specimen preparation, 349–352 共EBSD兲, 149–150
Organic materials, specimen material, field metallography, 150–151
186–187 machine design, 135–139
Oscillating cutting, design principles of manual grinding/polishing
wheel-work piece contact, 36–37 equipment, 135
Oxyacetylene torching, 46 material removal, 120–122
microelectronic materials, Purpose, labs, 650

143–147 PVD coatings, specimen preparation,
microelectronic packages, 247–251
147–149
microtomy, 155
polishing dynamics, 139–140 Q
preparation methods, 132–134
printed circuit boards 共PCB兲, Quality control labs, 650
Quantitative metallography/
143
materialography, 565–576
rough, 120
ASTM B 487, 576
semiautomatic systems, 140–143
ASTM C 664, 576
thin sections, 152–154
ASTM E 45, 570
ultramilling, 155
ASTM E 112, 571–573
Polycrystalline diamond products, 94
ASTM E 562, 569
Polyesters, occupational safety and
ASTM E 930, 573
health, labs, 668
ASTM E 1077, 575
Polymers, specimen material, 187
ASTM E 1122, 570
Porosity in thermal spray coatings,
ASTM E 1181, 573
574–575
ASTM E 1245, 570
Potentiostatic etching, 173
ASTM E 1268, 574
Powder metals
ASTM E 1382, 573
specimen material, 187
ASTM E 2109, 574–575
banding, 574
Power, metallographic/
bias, 568–569
materialographic cutting
calibration, 568
operation, 31
comparison procedure, 571–572
Power hacksawing, 48
decarburization, 575–576
Practical use of microscope, 546–550
field selection, 568–569
Precipitation etching, 172 grain size, 571–573
Precision inclusion rating, 570
cut-off, slow consumable wheels, intercept procedure, 572–573
35 other standards, 576
machine designs, abrasive, 41–43 planimetric procedure, 572
Preparation methods point count, 569
polishing, 132–134 porosity in thermal spray
selection of preparation coatings, 574–575
method, 7 specimen preparation, 567–568
Preparation process, 9–13 stereology, 565–567
etching, 13 volume fraction, 569
mounting, 11
sectioning, 10–11
surface preparation, 11–13 R
Preservation, 81
Printed circuit boards 共PCB兲, Rake angle, material removal,
polishing, 143 grinding, 87–88
Printers, automatic image analysis, 616 Rationalization, labs, 651–654
Process, electrolytic polishing/etching, Reactive sputtering, etching, 174
156–163 Reflected-light microscope, 538–540
Punching, shearing, 47 Relief
Subject Index 739
grinding, 103–105 occupational safety and health,

polishing, 173 labs, 664
Reporting locations, 15 other methods, 45–53
Reproducibility, etching, 171–172 preparation process, 10–11
Research labs, 651 sawing, 47–52
Research studies, 14 sectioning by melting, 46
Resin-bonded diamond grinding disks, selection, 14–15
107–108 shearing, 46–47
Resin-bonded SiC grinding disks, 108 wet abrasive cutting, 15–32
Resistors, specimen preparation, wet abrasive cutting tips, 43–45
293–295 wire cutting, 52–53
Rigid composite disks, grinding, Sectioning by melting, 46
109–116 electric discharge machining
Risk phrases, occupational safety 共EDM兲, 46
and health, labs, 670 laser torching, 46
Rockwell hardness testing, 634–636
oxyacetylene torching, 46
Rotating work piece, 39
plasma torching, 46
Rough polishing, 120
Selection, sectioning, 14–15
Rubber bonds, 21
general studies or routine
Rubbing effect, cleaning, 83
work, 14
Running labs, 649
reporting locations, 15
research studies, 14
S section type, 14–15
study of failures, 14
Safety Selection of preparation method, 6–7
bandsawing, 49 artifacts of electrolytic
occupational safety and health,
polishing, 7
labs, 668–672
artifacts of mechanical
Sample, materialographic specimen,
polishing, 7
8–9
preparation methods, 7
Sawing
Semiautomatic systems, polishing,
bandsawing, 48–52
140–143
circular sawing, 48
Semiconductors, specimen
hacksawing, 48
power hacksawing, 48 preparation, 288–291
sectioning, 47–52 Sharpening, automatic image analysis,
Scanning electron microscope 共SEM兲, 593–595
558–559 Shearing
Scanning probe microscopes 共SPM兲, punching, 47
558–561, 560–561 sectioning, 46–47
Scanning transmission electron Si wafers, specimen preparation,
microscope 共STEM兲, 558 288–291
Scleroscope, 645 SiC fibers in Ti matrix, specimen
Section type, selection, sectioning, preparation, 273–276
14–15 SiC wet grinding paper, 100–105
Sectioning, 14–53, 15 Silicon, specimen preparation, 288–291
abrasive cut-off machines, 36–43 Silicon carbide
abrasive cut-off wheels, 32–36 abrasive types, 18
fracturing, 45 grinding abrasives, 93
Silicon nitride, specimen preparation, barium titanate, 241

235–237 beryllium, 365–367
Silicon oxide, specimen preparation, bones, 427–430
241 boron carbide, 227–232
Silver brass, 376–380
electrolytic polishing and etching, bronze, 376–380
469–470 calcium oxide, 241
specimen preparation, 409–412 capacitors, 298–300
Sintered carbides carbonitrided steels, 339–342
specimen material, 187 cement clinker, 346–349
specimen preparation, 443–447 ceramic capacitors, 281–284
Slow consumable wheels ceramic layers, 268–270
precision cut-off, 35 ceramic resistors, 281–284
storing, 36 ceramics, 232–235
truing and dressing, 34–35 cerium oxide, 241
use, 35 chromium, 367–370
wheel dimensions, 35 chromium carbide, 232–235
wheel velocity, 35 chromium oxide, 238–240
Smoothing, automatic image analysis, cobalt, 370–373
592–593 cobalt-based super alloys,
Soft grade, 20 373–376
Software, automatic image analysis, composites, 276–281
616–617 concrete, 346–349
Solder balls, specimen preparation, consumables, 221
295–298 copper, 376–380
Sorby, Henry Clifton, 5–6 copper-bearing alloys, 380–383
Special methods hardness testing, 646 CVD coatings, 247–251
Specimen material, 179, 181–187 diffusion coatings, 251–254
ceramics, 182 diodes, 281–284
classification of materials, 181 electrolytic polishing and etching,
coatings, 182–183 453–475
composites, 183 electrolytically deposited
ferrous metals, 183–184 coatings, 251–254
materialographic specimen, 8–9 EPDM polymers, 430–436
mineralogical materials, 184 field metallography/
nonferrous metals, 184–186 materialography, 475–476
organic materials, 186–187 galvanization, 251–254
polymers, 187 generic methods, 219
powder metals, 187 germanium, 288–291
sintered carbides, 187 glasses, 244–247
Specimen preparation, gold, 384–387
179–180, 218–521 gray cast iron, 315–318
abbreviations, 221 high-alloy steels, 325–328
acrylics, 436–439 high carbon steels, 307–311
aluminum, 352–356 high-speed steels, 343–346
aluminum alloys, 356–358 hot dip zinc coatings, 254–257
aluminum oxide, 238–240 hydroxyapatite 共HA兲 coating,
anodized coatings, 247–251 223–226
antimony, 361–364 integrated circuits, 301–305
Subject Index 741
lead, 387–391 transistors, 301–305

low-alloy steels, 336–339 trouble shooting, 476–521
low carbon steels, 311–314 tungsten carbide, 232–235
magnesium, 391–394 uranium, 447–450
magnesium oxide, 241 white cast iron, 322–324
malleable cast iron, 315–318 wrought aluminum alloys,
manganese, 395–397 359–361
medium carbon steels, 307–311 YBCO ceramic super conductors,
microelectronic material, 285–288
291–293 zinc, 420–423
microelectronic packages, zinc oxide, 241
295–298, 301–305 zirconium, 424–427
minerals, ores, 349–352 zirconium dioxide, 241
molybdenum, 398–401 Sprays, diamond products, 96
nickel, 402–405 Sputtering, etching, 174
nodular cast iron, 319–321 Stainless steels
optical fibers, 244–247 electrolytic polishing and etching,
paint layers, 257–260 460–461
palladium, 406–409 specimen preparation, 328–333
parameters, 220–221 Stamping, marking, 80
PCB coupon, 305–307 Standard Operating Procedure 共SOP兲,
plasma spray coatings, 670–672
265–267, 270–273 Standards, occupational safety and
plated coatings, 251–254 health, labs, 673
powder metals, 439–443 Static hardness testing, 626–643
PVD coatings, 247–251 Brinell hardness testing, 626–628
quantitative metallography/ hardness values conversion,
materialography, 567–568 642–643
resistors, 293–295 hardness values precision, 642
semiconductors, 288–291 instrumented indentation
Si wafers, 288–291 testing, 641–642
SiC fibers in Ti matrix, 273–276 Knoop hardness testing, 633–634
silicon, 288–291 microindentation hardness,
silicon nitride, 235–237 636–639
silicon oxide, 241 Rockwell hardness testing,
silver, 409–412 634–636
sintered carbides, 443–447 universal hardness, 639–642
solder balls, 295–298 Vickers hardness testing, 628–632
stainless steels, 328–333 Step cutting, design principles of
steps, 219–220 wheel, 38–39
super alloys, 333–335 Steps, specimen preparation, 219–220
teeth, 427–430 Stereo microscopy, 555–557
thermal spray coatings, 260–265 Stereology, 565–567
tin, 413–416 Stones/disks, grinding, 99–100
tin cubic boron nitride, 232–235 Storage, 81
tissue, 427–430 Storing
titanium, 416–420 consumable abrasive cut-off
titanium carbide, 232–235 wheels, 33–34
titanium nitride, 232–235 slow consumable wheels, 36
Structure, cut-off wheel, 20 Transistors, specimen preparation,

Study of failures, selection, sectioning, 301–305
14 Transmission electron microscope
Super alloys 共TEM兲, 558
electrolytic polishing and etching, Trouble shooting, specimen
461 preparation, 476–521
specimen preparation, 333–335 True microstructure, 5–6, 6
Surface preparation, 11–13 Truing and dressing
Suspensions, diamond products, 96 cut-off wheel wear, wet abrasive
Synthetic grinding fluids-oil-based, cutting, 26
26–27 slow consumable wheels, 34–35
Tungsten, electrolytic polishing and
etching, 472
T Tungsten carbide, specimen
Teeth, specimen preparation, 427–430
Testing and inspection labs, 651
Thermal damage, wet abrasive cutting, U
23–25
Ultramilling, polishing, 155
clamping, 24–25
Ultrasonic apparatuses cleaning, 83
wet cutting, 25
Ultrasonic cleaning, 83
Thermal etching, 174
Universal hardness, static hardness
Thermal spray coatings, specimen
testing, 639–642
Unplane surface, mechanical damage,
Thickness measurements, automatic
wet abrasive cutting, 23
image analysis, 608–610 Uranium, specimen preparation,
Thin sections, polishing, 152–154 447–450
Tin Use, slow consumable wheels, 35
470–471
specimen preparation, 413–416 V
Tin cubic boron nitride, specimen
preparation, 232–235 Vanadium, electrolytic polishing and
Tissue, specimen preparation, 427–430 etching, 472–473
Titanium Vapor deposition, etching, 174
electrolytic polishing Vickers hardness testing, 628–632
and etching, 471 Visible light, light microscopy, 525–526
specimen preparation, 416–420 Volume fraction
Titanium carbide, specimen automatic image analysis,
preparation, 232–235 602–603
Titanium nitride, specimen quantitative metallography/
preparation, 232–235 materialography, 569
Toxic substances, occupational safety
and health, labs, 666 W
Traditional grinding, 99–106
Traditional versus contemporary Water-based grinding/polishing fluids,
methods, specimen preparation, 218 97
Training, occupational safety and Water-oil based grinding/polishing
health, labs, 673 fluids, 98
Subject Index 743
Water quality, cutting fluids, wet slow consumable wheels, 35

abrasive cutting, 28 White cast iron, specimen preparation,
Waterproof ink marking, 80 322–324
Watershed filter, automatic image Wire cutting, 52–53
analysis, 590–592 Wrought aluminum alloys, specimen
Waviness, mechanical damage, wet preparation, 359–361
abrasive cutting, 23
Wet abrasive cutting, sectioning, 15–32
abrasives and bond materials, Y
16–21
cut-off grinding process, 15–16 YBCO ceramic super conductors,
cut-off wheel, 16–21 specimen preparation, 285–288
cut-off wheel wear, 25–26
cutting fluids, 26–29 Z
grinding mechanics, 21–22
mechanical damage, 22–23 Zinc
metallographic/materialographic electrolytic polishing and etching,
cutting operation, 29–32 473
thermal damage, 23–25 specimen preparation, 420–423
tips, 43–45 Zinc oxide, specimen preparation, 241
Wet cutting, thermal damage, 25 Zirconia alumina wet grinding paper,
Wheel dimensions 105–106
consumable abrasive cut-off Zirconium
wheels, 33 electrolytic polishing and etching,
slow consumable wheels, 35 474
Wheel velocity specimen preparation, 424–427
consumable abrasive cut-off Zirconium dioxide, specimen
wheels, 32–33 preparation, 241
metallographic/materialographic
cutting operation, 30

MNL46 - Metallographic and Materialographic Specimen Preparation, Light Microscopy, Image Analysis and Hardness Testing 2007

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MNL46 - Metallographic and Materialographic Specimen Preparation, Light Microscopy, Image Analysis and Hardness Testing 2007

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Metallographic and

Printed in City, State

The Metallographic/Materialographic Laboratory

AFM Atomic Force Microscope

EBSD Electron Backscatter Diffraction

3.1.3 Surface Flatness—Edge Retention. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

5 Cleaning and Cleanliness

7.2 Material Removal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 120

8.1.3 Electrolytic Etching. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159

Part II: Metallographic/Materialographic Specimen Preparation—A Hands-On

Part III: Light Microscopy

14.3 Magnifying Lens and Microscope. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 527

Part IV: Quantitative Metallography/Materialography— Automatic Image Analysis

17.1.2 Specimen Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 567

18.4 Image Measurement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 598

Part V: Hardness Testing

Part VI: The Metallographic/Materialographic Laboratory

Fig. 1.1—Metallography/materialography can be described as a bridge between engineering

Fig. 1.2—The constituents of a microstructure and the factors affecting them.

Fig. 1.3—Photomontage of a microsection of silicon nitride alloy superimposed upon a pile of

1.1 Metallographic/Materialographic Preparation—The True

1.1.1 Henry Clifton Sorby „1826–1908…

1.2 The True Microstructure

1.3 Selection of Preparation Method

The choice of preparation is usually between using mechanical or electrolytic pol-

Artifacts of Mechanical Polishing

Artifacts of Electrolytic Polishing

1.3.2 Preparation Methods

1.4 The Metallographic/Materialographic Specimen

Fig. 1.5—Mechanical polishing: the most common artifacts shown schematically.

both specimen preparation and examination, using an optical microscope or an SEM,

1.4.1 “Specimen” or “Sample”

Fig. 1.6—Electrolytic polishing: the most common artifacts shown schematically.

1.5 The Preparation Process

1.5.3 Preparation of the Surface

2.1.1 General Studies or Routine Work

2.1.2 Study of Failures

2.1.3 Research Studies

2.1.4 Type of Section

Estimating the Depth of Decarburization of Steel Specimens 共E 1077兲, Section

2.1.5 Reporting of Locations

2.3 Wet Abrasive Cutting

2.3.1 The Cut-off Grinding Process

2.3.2 The Cut-off Wheel—Abrasives and Bond Materials

Cut-off Wheel Specifications

with a short arc of contact.

2.3.3 Grinding Mechanics

Ft⬘ = u · d · l · b/v · l · b · C = 共d/v兲u/C 共3兲

Chips, Sliding, and Plowing

2.3.4 Mechanical Damage

2.3.5 Thermal Damage

cause a metallurgical transformation in the heat-affected zone 共see Section 13.6.2兲.

2.3.6 Cut-off Wheel Wear

Truing and Dressing

2.3.7 Cutting Fluids

Lubrication and Cooling

Synthetic Grinding Fluids—Oil-Based Fluids

Application of Grinding Fluid

The Cooling System