Data Conferma/Confirmation Date: 13 nov 2013

PRESCRIPTIONS FOR SAMPLING AND

Fiat Group PREPARATION OF SPECIMENS FOR
MATERIAL STANDARD

Automobiles MICROSCOPIC TEST OF METALLIC 50210

normazione MATERIALS Page: 1/5
1/3
Date: 10/23/2009
BOGGIO RICCARDO - RICCARDO.BOGGIO@CRF.IT
ROLLI RAFFAELLA - RAFFAELLA.ROLLI@CRF.IT

TMD
PURPOSE
To specify prescriptions for sampling and preparation of specimens for microscopic test of
metallic materials.

Code
-
Ch.
4
Change Date Description

= May '90 Edition 2 - Reorganized. (OR)

Edition
Supervisor
Author

= 07/12/05 Edition 3 - Completely revised. (FD)

= 10/23/09 Edition 4 - Completely revised. Title changed. (CL)

C.R.F. - Group Materials Labs Physical Analysis & Common Testings
C.R.F. - Group Materials Labs Physical Analysis & Common Testings

DISPUTE THE ONLY VALID REFERENCE IS THE ORIGINAL ITALIAN EDITION

PARTIES WITHOUT PRIOR WRITTEN CONSENT BY FIAT AUTO S.P.A. IN CASE OF
THIS DOCUMENT MUST NOT BE REPRODUCED OR CIRCULATED TO THE THIRD
CONFIDENTIAL
Supervisor department
Author Department

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 Page 2
50210 Change

1
GENERAL

This standard covers metallographic specimen preparation from sampling to etching.

a) sampling
b) mounting
c) grinding and polishing
d) etching

2
SAMPLING

Specimen dimensions are influenced by the dimension and the shape of the component to
be tested, in any case, where possible, they shall allow to obtain a 140 mm2 specimen at
least.
Samples shall be cut using a saw or a grinding wheel.
Material shall be properly cooled during cutting by directing a flow of water or oil-water
emulsion over surface.

3
SPECIMEN PREPARATION

Specimens are flattened, polished and cleaned to produce a flat, specular surface.
Surface preparation operations shall be performed in such a way not to cause thermal or
mechanical distortion of metallographic structure.

3.1
Mounting

Degreasing in adequate solvents shall come before mounting in order to remove any oil or
WITHOUT PRIOR WRITTEN CONSENT BY FIAT AUTO S.P.A. IN CASE OF DISPUTE THE ONLY
THIS DOCUMENT MUST NOT BE REPRODUCED OR CIRCULATED TO THE THIRD PARTIES

grease residuals from the specimen walls and to facilitate the specimen/resin adhesion.
Hot mounting can be performed using proper equipment and thermosetting resin; cold
mounting can be carried out in simple molds and two component liquid resin.
Cold mounting is necessary on all samples subject to structural or dimension changes due to
VALID REFERENCE IS THE ORIGINAL ITALIAN EDITION

hot process.

3.2

Grinding and polishing

Flattening operation can be carried out manually or using proper equipment (belt roughing
machine)
CONFIDENTIAL

Manual grinding and polishing is carried out on rotary discs with abrasive papers (silicon
carbide) cooled with water. The grinding papers have grain 120, 500, 1000, 4000 and they
are used progressively starting form the coarsest (grain 120) and finishing with the paper
having grain 4000 (abrasive paper grain size is indicative and is shown for information only).

Specimen shall be rotated 90° each time paper grain is changed so that marks produced by
the new abrasive paper are perpendicular to those produced in the previous stage. Polishing
shall go on until marks left from the previous stage have been completely eliminated.

At this point it is advisable to carry out an intermediate step using a cloth and suspension
containing 6 µm diamond powder, and possibly also another step using a cloth and
suspension containing 3 µm diamond powder.
The final polishing is carried out using a soft cloth and suspension containing 1 µm diamond
powder, or using a soft cloth and alumina.

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Fiat Group Automobiles Change 50210
The polishing with alumina has to be carried out with a gentle pressure, sample rotation and
abundant use of demineralized water in order to prevent surface hardening. If this case
should occur, it is necessary to carry on with final polishing until it totally disappears.
For aluminum or aluminum alloys, the final polishing has to be carried out always with soft
cloth and suspension containing 1 µm diamond powder.

Semiautomatic or automatic grinding and polishing shall be performed according to

indications given by manufacturer.

4
POLISHED SURFACE ETCHING

Specimen surface etching is used to differentiate the several structural components of an

alloy, so that they are evident when performing a microscopic inspection.

4.1
Chemical etching

Chemical etching is performed by dropping from a dropping bottle a reactive quantity

sufficient to cover the whole sample. As soon as the metallographer judges, on his own
experience basis, that the sample has reached the right tone, stop etching by means of a
spout of ethyl alcohol and followed by a warm air blow.

The following table shows the most commonly used chemical etchants. For particular
etchings, refer to metallographic atlas.

THIS DOCUMENT MUST NOT BE REPRODUCED OR CIRCULATED TO THE THIRD PARTIES

WITHOUT PRIOR WRITTEN CONSENT BY FIAT AUTO S.P.A. IN CASE OF DISNPUTE THE
ONLY VALID REFERENCE IS THE ORIGINAL ITALIAN EDITION
CONFIDENTIAL

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 Page 4
50210 Change

Name Composition General use prescriptions

NITAL 1 to 5 ml nitric acid, For carbon steels and cast irons.
100 ml ethanol (95%)
or methanol (95%)
PICRAL 10 g picric acid, For ferritic stainless steels and martensitic stain-
100 ml ethanol (95%) less steels.
or methanol (95%)
MARBLE'S 10 g copper sulphate, For austenitic stainless steels, cast irons with
REAGENT 50 ml hydrogen austenitic matrix (Ni-resist), iron-nichel and
chloride, 50 ml colbalt-base superalloys.
distilled water
VILELLA'S 5 ml hydrogen For martensitic stainless steels and ferritic stain-
REAGENT chloride, less steels.
1 g picric acid, Caution! For preparation and storage use plastic
100 ml ethanol (95%) bottles only (polyethylene).
or methanol (95%)
0.5% hydrogen For aluminum alloys.
--- fluoride (48%) in
Caution! For preparation and storage use plastic
distilled water bottles only (polyethylene).
KELLER'S 2 ml hydrogen fluoride For aluminum and aluminum alloys.
REAGENT (48%), Caution! For preparation and storage use plastic
3 ml hydrogen bottles only (polyethylene).
chloride,
5 ml nitric acid,
190 ml distilled water
5 g ferric chloride, For copper and copper alloys.
WITHOUT PRIOR WRITTEN CONSENT BY FIAT AUTO S.P.A. IN CASE OF DISPUTE THE ONLY
THIS DOCUMENT MUST NOT BE REPRODUCED OR CIRCULATED TO THE THIRD PARTIES

--- 100 ml ethanol (95%),

5-30 ml hydrogen
chloride
VALID REFERENCE IS THE ORIGINAL ITALIAN EDITION

GLYCEREGIA 3 parts glycerol, For iron-base and nickel-base superalloys and

2-3 parts hydrogen austenitic stainless steels.
chloride, Caution! Use the solution immediately after
1 part nitric acid preparation. Do not store.
AQUA REGIA 1 part nitric acid and 3 For iron-base and nickel-base superalloys.
parts hydrogen Caution! Use the solution immediately after
chloride preparation. Do not store.
CONFIDENTIAL

Aqueous saturated For revealing austenitic grains formed during heat

picric acid solution treatment of the specimen, according to the
"Bechet-Beaujard" method described in the UNI
---
EN ISO 643:2006 standard concerning the
micrographic determination of the grain size in
steels.

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 Page 5
Fiat Group Automobiles Change 50210
4.2
Electrolytic etching

The electrolyte used for this kind of etching does not etch the metals of the specimen if
current does not flow.
The advantage of this etching method is the possibility to accurately monitor the etching
process by acting on the electrical parameters of the system, setting the voltage and the
duration of the current flow.

The following table shows the parameters of the most commonly used electrolytic etching
method.

Name Composition General use prescriptions

OXALIC 10 g oxalic acid, 100 ml For austenitic stainless steels and alloys with
ACID distilled water high nickel content.
Voltage: 6 V
Etching time: 5 - 20 sec

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WITHOUT PRIOR WRITTEN CONSENT BY FIAT AUTO S.P.A. IN CASE OF DISNPUTE THE
ONLY VALID REFERENCE IS THE ORIGINAL ITALIAN EDITION
CONFIDENTIAL

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