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Springer Series in Materials Science 295

Anja Weidner

Deformation
Processes in
TRIP/TWIP
Steels
In-Situ Characterization Techniques
Springer Series in Materials Science

Volume 295

Series Editors
Robert Hull, Center for Materials, Devices, and Integrated Systems,
Rensselaer Polytechnic Institute, Troy, NY, USA
Chennupati Jagadish, Research School of Physical, Australian National University,
Canberra, ACT, Australia
Yoshiyuki Kawazoe, Center for Computational Materials, Tohoku University,
Sendai, Japan
Jamie Kruzic, School of Mechanical & Manufacturing Engineering, UNSW
Sydney, Sydney, NSW, Australia
Richard M. Osgood, Department of Electrical Engineering, Columbia University,
New York, USA
Jürgen Parisi, Universität Oldenburg, Oldenburg, Germany
Udo W. Pohl, Institute of Solid State Physics, Technical University of Berlin,
Berlin, Germany
Tae-Yeon Seong, Department of Materials Science & Engineering,
Korea University, Seoul, Korea (Republic of)
Shin-ichi Uchida, Electronics and Manufacturing, National Institute of Advanced
Industrial Science and Technology, Tsukuba, Ibaraki, Japan
Zhiming M. Wang, Institute of Fundamental and Frontier Sciences - Electronic,
University of Electronic Science and Technology of China, Chengdu, China
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Anja Weidner

Deformation Processes
in TRIP/TWIP Steels
In-Situ Characterization Techniques

123
Anja Weidner
Institute of Materials Engineering
TU Bergakademie Freiberg
Freiberg, Germany

ISSN 0933-033X ISSN 2196-2812 (electronic)


Springer Series in Materials Science
ISBN 978-3-030-37148-7 ISBN 978-3-030-37149-4 (eBook)
https://doi.org/10.1007/978-3-030-37149-4
© Springer Nature Switzerland AG 2020
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Dedicated to my parents
Gudrun und Gerd
Preface

There are two things that are necessary to our work: tireless
perseverance and the willingness to throw away something
that you put a lot of time and effort into.
Albert Einstein

It was a long way from the diploma work over the Ph.D. thesis up to the present
habilitation thesis. During these 24 years, many events happened—a lot of them
with positive feelings, but some also, hopefully to minor extent, with negative
feelings. The best thing in the world, which happened to me during these 24 years,
is my family—my two sons Johannes and Jonathan and my husband Stephan.
These 24 years provided a lot of experiences in the research field of Materials
Science and Engineering at different places—Freiberg and Dresden—accompanied
by numerous excellent scientists. My research interests started with X-ray diffrac-
tion analysis on cold-worked, textured metallic materials during Ph.D. time at the
Institute of Materials Science. Later on at Technische Universität Dresden, cyclic
plasticity of NiAl single crystals and nickel polycrystals was in the focus of my
interests followed by crack growth of microstructurally short cracks in stainless
steel. Here it was also where the first contact with the field of in situ testing/
characterization in scanning electron microscope came about.
With the habilitation thesis, the circle closes where everything started—at
the Faculty of Materials Science and Technology of Technische Universität
Bergakademie Freiberg. During these last ten years, the field of my research
interests has been significantly enlarged in terms of materials, characterization
techniques and mechanical loading conditions. Overall, the 24 years were focused
almost on experimental work, and many experiments went wrong. During this time,
the above-mentioned motto was a good companion and advisor. It helped to
overcome difficulties with experimental setups, data evaluation processes and other
unforeseeable challenges.
Finally, I succeeded with results on different in situ testing and characterization
techniques, which are worth to be collected and summarized in the present work
embedded in the scientific background knowledge and state of the art in the field of

vii
viii Preface

Materials Science and Engineering. Nevertheless, the amount of the results pre-
sented here are the consequence of stimulating and fruitful scientific collaborations
with scientists, colleagues and friends all around Germany and other countries.
The present work is based on investigations performed within the framework
of the Collaborative Research Centre 799 (CRC 799) “TRIP matrix composites”,
which have been supported financially by the German Research Foundation at the
Technische Universität Bergakademie Freiberg since 2008. The results presented
were obtained in a period between 2009 and 2018 in subproject B5 “2D in situ
characterization in the scanning electron microscope” at the Institute of Materials
Engineering.

Freiberg, Germany Anja Weidner


Acknowledgements

The present habilitation thesis is the result of a fruitful work within an excellent
research environment with respect to human, technical and financial resources.
Many people contributed to this comprehensive work on in situ investigations on
high-alloy CrMnNi TRIP/TWIP steels. Therefore, it is my utmost concern and need
to acknowledge for support in all respects.
My special thanks go to Prof. Dr.-Ing. habil. Horst Biermann, the Director of the
Institute of Materials Engineering and owner of the Professorship of Materials
Engineering. He continually promoted and supported my scientific interests and
research works. Moreover, he opened the horizon to broader field of materials
research. His motivation, encouragement and support as well as private commu-
nication greatly facilitated my writing this habilitation thesis. Furthermore, I thank
him for fruitful discussions of different parts of the present work. Finally,
I acknowledge his critical and always constructive review on the habilitation thesis.
Prof. Dr. rer. nat. habil. Dr. h. c. Günter Gottstein and Prof. Dr. Ullrich Prahl are
gratefully acknowledged for their reviewing activities on the habilitation thesis and
helpful comments.
Furthermore, I would like to thank Prof. Dr.-Ing. habil. Christos G. Aneziris for
his support and encouragement within the framework of the CRC 920 “Multi-
functional Filters for the Metal Melt Filtration—A Contribution towards Zero Defect
Materials”.
Prof. Dr.-Ing. habil. Ulrich Martin has accompanied my entire scientific career in
Freiberg starting from my first days of study in September 1989 through my Ph.D.
studies at the Institute of Materials Science that finished in 1998, and including my
return to Freiberg and the CRC 799 project in 2009. During this time, he was an
ever-present source of helpful words and deeds, including both friendly advices and
constructive criticism.
Many thanks must also go to Prof. Alexey Vinogradov. We first met in 2009 in
Japan, and he subsequently introduced me to the art of acoustic emission analysis.
Since that time, we have developed a close and fruitful scientific relationship and a
deep friendship.

ix
x Acknowledgements

I would also like to thank my colleagues Dr.-Ing. Peter Trubitz, Dr.-Ing.


Sebastian Henkel, Dr.-Ing. Sania Berg, Dr.-Ing. Stefan Martin, Dr.-Ing. Alexander
Glage, Dr.-Ing. Dominik Krewerth and Dr.-Ing. Dirk Kulawinski for our helpful
and fruitful discussions and the friendly working atmosphere, which contributed in
a substantial manner to the success of the present work.
Diploma students and Ph.D. candidates generated a major share of the experi-
mental results presented in this thesis during their work within the CRC 799 project.
Therefore, I would particularly like to thank Dipl.-Ing. Johannes Solarek and
Dipl.-Ing. Christian Segel for their patient performance of in situ tests in the SEM
and the application of digital image correlation and/or acoustic emission. My sin-
cere thanks also go to Dipl.-Ing. Alexandra Illgen (Müller) for her excellent work
on fully-coupled full-field measurements in studying the Portevin–Le Chatelier
effect in metastable steels undergoing martensitic phase transformation.
At the same time, I would like to express my thanks to Mikhail Linderov, Ph.D.
student of Alexei Vinogradov, who in 2013 carried out a six-month research project
with Prof. Biermann at the Institute of Materials Engineering. Together with
Dipl-Ing. Christian Segel, he performed tensile tests on TRIP/TWIP steels com-
plemented by in situ acoustic emission measurements. With his work, he con-
tributed in a substantial manner to the better understanding of the kinetics of
deformation mechanisms of the steels under investigation, in particular, at higher
temperatures.
Although their results were not included in the present work, the work of other
colleagues must be acknowledged, since these results contributed to a substantial
degree in improving our knowledge of material behaviour itself. Therefore, I would
like to thank Dipl.-Ing. Stephanie Ackermann for her excellent experimental work
in performing high-pressure and biaxial testing as well as for her deep under-
standing of both mechanics and plastic deformation; M.Sc. Matthias Droste for his
cyclic loading experiments and helpful discussions on the results of ultrafine-
grained materials, M.Sc. Desiree Heinze and Dipl.-Ing. Karin Fischer for their
investigations on the reversion behaviour of martensite in the generation of
ultrafine-grained austenite; and Dipl.-Ing. Robert Lehnert for his investigations of
AE emission during scratch tests on steel specimens and compression tests of pure
zirconium dioxide as well as for his nanoindentation experiments and pillar com-
pression tests within SEM.
Mr. Gerd Schade, Mrs. Karin Zuber, Mrs. Angelika Müller, Mrs. Katrin Becker,
Mr. Robby Prang, Mr. Uwe Schönherr, Mrs. Brigitte Bleiber, Mrs. Astrid Leuteritz,
Mrs. Petra Geissler, Mr. Klaus König and Mr. Markus Büttner, Mr. Tim Pieper,
Mr. Thomas Ludewig—all from the Institutes of Materials Science and Materials
Engineering—are gratefully acknowledged for their assistance in various experi-
mental issues such as performing tensile tests, specimen preparation for in situ tests
or SEM investigations, solving electronic problems with the mechanical and ther-
mal loading devices, carbon coating of specimens, preparation of TEM foils or the
manufacture of many specimens by the workshop staff.
Acknowledgements xi

Both of the secretaries of the Institute of Materials Engineering (Mrs. Ramona


Trubitz and Mrs. Ulrike Schramm) as well as the Coordinator of the CRC 799,
Mrs. Antje Beier, and its Manager, Dr. Peter Michel, are gratefully acknowledged
for their assistance in all official and organizational affairs.
My special thanks go also to Mr. Uwe Gubsch for his continuous support as
system administrator handling and solving all problems and issues of computer
engineering.
The students Christian Krancher and Felix Hossang are gratefully acknowledged
for their support preparing significant part of figures of the present work. The proof
reading of the final version by Dipl.-Ing. Alexander Schmiedel, Dipl.-Ing. Johannes
Günther, Dipl.-Ing. Robert Lehnert, M.Sc. Matthias Droste and Dipl.-Ing. Carl
Wolf is also highly appreciated.
Furthermore, I would like to express my sincere thanks to all members of the
Institute of Materials Science and Materials Engineering as well as both collabo-
rative research centres (CRC799 and CRC920) for the inspiring working atmo-
sphere that facilitated fruitful discussions and excellent team work.
I would also like to thank the representatives of the companies that supplied
either the scanning electron microscope or in situ loading devices. Thus, my thanks
go to Mr. Haak, Dr. Neumann and Mr. Gosda from Electron Optic Service (GmbH)
for their continuous support with the SEM MIRA3 XMU from TESCAN Company
(Czech Republic). Similarly, Mr. Kammrath, Mr. Weiss and Mr. Stirba are grate-
fully acknowledged for their support regarding the tension/compression loading
device. The support and assistance from Mrs. Bettina Seiler and Mrs. Elke Noak
from Chemnitzer Werkzeugmechanik GmbH is also highly appreciated for intro-
duction and work with the digital image correlation software VEDDAC and
VEDDAC strain. All three groups are further acknowledged for their contributions
to and support of the DGM/DVM workshop “In situ testing in the scanning electron
microscope”.
This habilitation thesis is dedicated to my parents—Gudrun and Gerd. Without
their support and aid during my entire life, I would never have been able to take the
path of a scientific career. I would also like to thank my parents in law for their
support.
Finally, I would like to express my special thanks to my husband Stephan and to
my two sons—Johannes and Jonathan—for their infinite patience and everlasting
assistance over the last years.

Freiberg, Germany Anja Weidner


Contents

1 Motivation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2 Plastic Deformation and Strain Localizations . . . . . . . . . . . . . . . . . . 7
2.1 Plastic Deformation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.2 Dislocation Glide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.3 Deformation Twinning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.4 Critical Resolved Shear Stress . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
2.5 Strain Hardening . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
2.6 Strain Localizations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
2.6.1 Strain Localizations on Microscopic Scale . . . . . . . . . . . . . 27
2.6.2 Strain Localizations on Macroscopic Scale . . . . . . . . . . . . 33
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
3 Martensitic Phase Transformation . . . . . . . . . . . . . . . . . . . . . . . . . . 47
3.1 General Considerations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
3.2 Thermodynamic Aspects of Martensitic Phase Transformation . . . 50
3.3 Martensite in Ferrous Alloys . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
3.4 Martensitic Phase Transformation in Steels . . . . . . . . . . . . . . . . . 54
3.4.1 Direct c to a′ Transformation . . . . . . . . . . . . . . . . . . . . . . 55
3.4.2 Direct c to ɛ Transformation . . . . . . . . . . . . . . . . . . . . . . . 60
3.4.3 Direct ɛ to a′ Transformation . . . . . . . . . . . . . . . . . . . . . . 61
3.4.4 Indirect c–a′ Transformation via ɛ-Martensite . . . . . . . . . . 62
3.5 Influence of Stacking-Fault Energy . . . . . . . . . . . . . . . . . . . . . . . 63
3.6 Olson–Cohen Model of Martensitic Phase Transformation . . . . . . 66
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
4 Advanced High-Strength Steels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71
4.1 General Considerations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71

xiii
xiv Contents

4.2 Twinning-Induced Plasticity (TWIP) Steels . . . . . . . . . . . . . . . . . 73


4.2.1 Thermodynamic Aspects of TWIP Steels . . . . . . . . . . . . . 73
4.2.2 Deformation Behaviour of TWIP Steels . . . . . . . . . . . . . . 74
4.2.3 Modelling of the TWIP Effect . . . . . . . . . . . . . . . . . . . . . 80
4.3 Transformation-Induced Plasticity (TRIP) Steels . . . . . . . . . . . . . . 83
4.3.1 Thermodynamic Aspects of TRIP Steels . . . . . . . . . . . . . . 84
4.3.2 Deformation Behaviour of TRIP Steels . . . . . . . . . . . . . . . 89
4.3.3 Modelling of the TRIP Effect . . . . . . . . . . . . . . . . . . . . . . 94
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
5 In Situ Techniques for Characterization of Strain Localizations
and Time Sequence of Deformation Processes . . . . . . . . . . . . . . . . . 99
5.1 General Considerations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
5.2 In Situ Imaging Techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102
5.2.1 Optical Microscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102
5.2.2 Scanning Electron Microscopy . . . . . . . . . . . . . . . . . . . . . 108
5.3 In Situ Acoustic Emission Measurements . . . . . . . . . . . . . . . . . . . 115
5.3.1 General Aspects of Acoustic Emission . . . . . . . . . . . . . . . 116
5.3.2 Acoustic Emission—A Multiscale Random Time-Series
Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
5.3.3 Sources of Acoustic Emission . . . . . . . . . . . . . . . . . . . . . 130
5.3.4 Instrumentation and Data Acquisition . . . . . . . . . . . . . . . . 135
5.3.5 Processing of AE Data . . . . . . . . . . . . . . . . . . . . . . . . . . . 140
5.3.6 State of the Art in Materials Engineering . . . . . . . . . . . . . 151
5.4 In Situ Full-Field Measurement Techniques . . . . . . . . . . . . . . . . . 156
5.4.1 Displacement and Strain Fields . . . . . . . . . . . . . . . . . . . . . 157
5.4.2 Temperature Fields . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 179
5.4.3 Fully-Coupled Measurements . . . . . . . . . . . . . . . . . . . . . . 191
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 195
6 Object of Investigations—High-Alloy Fe–16Cr–6Mn–xNi–0.05C
Cast Steels with TRIP/TWIP Effect . . . . . . . . . . . . . . . . . . . . . . . . . 205
6.1 General Considerations on High-Alloy Fe–16Cr–6Mn–xNi–
0.05C TRIP/TWIP Steels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 205
6.2 Applied Methods for Characterization of the Deformation
Behaviour and the Related Microstructures . . . . . . . . . . . . . . . . . 209
6.2.1 Deformation Experiments . . . . . . . . . . . . . . . . . . . . . . . . . 209
6.2.2 Microstructural Characterization Techniques . . . . . . . . . . . 210
6.3 Mechanical Behaviour . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 213
6.3.1 Uniaxial Quasi-static Loading . . . . . . . . . . . . . . . . . . . . . . 213
6.3.2 Uniaxial Cyclic Loading . . . . . . . . . . . . . . . . . . . . . . . . . 217
6.3.3 Planar-Biaxial Loading . . . . . . . . . . . . . . . . . . . . . . . . . . . 219
Contents xv

6.4 Microstructure Evolution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 221


6.4.1 Fe–16Cr–6Mn–6Ni–0.05C Steel . . . . . . . . . . . . . . . . . . . . 221
6.4.2 Fe–16Cr–6Mn–9Ni–0.05C Steel . . . . . . . . . . . . . . . . . . . . 238
6.4.3 Fe–16Cr–6Mn–3Ni–0.05C Steel . . . . . . . . . . . . . . . . . . . . 241
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 243
7 Case Studies on Localized Deformation Processes in High-Alloy
Fe–16Cr–6Mn–xNi–0.05C Cast Steels . . . . . . . . . . . . . . . . . . . . . . . . 245
7.1 Significance of Complementary In Situ Characterization
Techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 245
7.2 Microscopic Strain Localizations During Plastic Deformation . . . . 249
7.2.1 In Situ Deformation in the Scanning Electron
Microscope . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 249
7.2.2 High-Resolution DIC (Sub-lDIC) for Evaluation
of Local Strain Fields . . . . . . . . . . . . . . . . . . . . . . . . . . . 251
7.2.3 Strain Localization During Tensile Deformation . . . . . . . . 254
7.2.4 Orientation-Dependent Magnitude of Shear of Individual
Martensitic Grains . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 273
7.2.5 Magnitude of Shear of Twin Bundles . . . . . . . . . . . . . . . . 277
7.2.6 Strain Localization During Cyclic Deformation . . . . . . . . . 281
7.2.7 Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 307
7.3 Time Sequence of Deformation Processes . . . . . . . . . . . . . . . . . . 313
7.3.1 Acoustic Emission Measurements and Analysis . . . . . . . . . 313
7.3.2 Acoustic Emission During the Deformation Process . . . . . . 315
7.3.3 Influence of Chemical Composition . . . . . . . . . . . . . . . . . 323
7.3.4 Evolution of Martensitic Phase Transformation at Room
Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 330
7.3.5 Influence of Deformation Temperature . . . . . . . . . . . . . . . 331
7.3.6 Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 338
7.4 Macroscopic Strain Localization During Plastic Deformation . . . . . 340
7.4.1 Fully-Coupled Full-Field Measurements . . . . . . . . . . . . . . 341
7.4.2 The Occurrence of Portevin–Le Chatelier (PLC) Effect . . . 342
7.4.3 Temperature and Strain Fields . . . . . . . . . . . . . . . . . . . . . 346
7.4.4 Portevin–Le Chatelier Effect and Acoustic Emission . . . . . 353
7.4.5 Correlation of PLC Effect with Martensitic Volume
Fraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 354
7.4.6 Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 360
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 363
8 Prospects of Complementary In Situ Techniques . . . . . . . . . . . . . . . 365
8.1 General Remarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 365
8.2 Complementary In Situ Techniques and Microstructural-Based
Modelling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 368
xvi Contents

8.3 Example 1: Modelling of Strain-Hardening Behaviour of


CrMnNi TRIP/TWIP Steels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 371
8.3.1 Orientation Dependence of Deformation Mechanisms
Detected by AE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 374
8.3.2 Strain Localizations Across the Length Scale of
Microstructure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 375
8.4 Example 2: Damage Behaviour of TRIP Matrix Composites . . . . . 379
8.5 Example 3: Deformation and Damage Behaviour of Laminated
TRIP/TWIP Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 381
8.6 Example 4: Shape Memory Materials . . . . . . . . . . . . . . . . . . . . . 382
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 383
9 Concluding Remarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 385

Appendix . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 389
Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 435
Abbreviations

AC Alternating current
ACF Auto-correlation function
ACOM Automated crystal orientation mapping
AD Analog–digital
ADC Analog–digital converter
AE Acoustic emission
AFM Atomic force microscopy
AHSS Advanced high-strength steel
AOI Area of interest
APS Active pixel sensor
APT Atom probe tomography
ARB Accumulative roll bonding
ASK Adaptive sequential k-means algorithm
ASTM American Standard for Testing and Materials
BC Band contrast
BCC Body-centred cubic
BCT Body-centred tetragonal
Bs Brass (-type shear band, texture component)
BSE Backscattered electron
C Copper (-type shear band, texture component)
CC Cross-correlation
CCD Charge-coupled device
CL Cathodoluminescence
CLSM Confocal laser scanning microscopy
CM Confocal microscopy
CMOS Complementary metal-oxide semiconductor
COD Crack opening displacement
CP Crystal plasticity
CRC Collaborative research centre

xvii
xviii Abbreviations

CRSS Critical resolved shear stress


c-SEM Classical scanning electron microscope (in sense of the chamber size)
CSL Coincidence site lattice
CSSC Cyclic stress-strain curve
CTOD Crack tip opening displacement
Ctwin Twinned copper (texture component)
DAMASK Düsseldorf Advanced Materials Simulation Kit
DB Deformation band
DDD Discrete dislocation dynamics
DESY Deutsches Synchrotron
DFT Density function theory
DFT Discrete Fourier transformation
DIC Digital image correlation
DSA Dynamic strain ageing
DSP Digital signal processor
DSS Duplex stainless steel
DTT Deformation temperature transition
EBSD Electron backscattered diffraction
ECAP Equal channel angular pressing
ECCI Electron channelling contrast Imaging
EDS Energy-dispersive X-ray spectroscopy
EM Electron microscopy
ESEM Environmental scanning electron microscope
FAST Field-assisted sintering technology
FCC Face-centred cubic
FCT Face-centred tetragonal
FE Field emission
FEM Finite element modelling
FE-SEM Field-emission scanning electron microscope
FF Full field
FFT Fast Fourier transformation
FHP Freiberg High-Pressure Centre
FIB Focused ion beam
FOV Field of view
FPA Focal plane array
fps Frames per second
FT Fourier transformation
G Goss (texture component)
GB Grain boundary
HCF High-cycle fatigue
HCP Hexagonal closed packed
HDDW High dislocation density wall
HIP Hot-isostatic pressing
HPT High-pressure torsion
HR-DIC High-resolution digital image correlation
Abbreviations xix

HRTEM High-resolution transmission electron microscopy


ICD Inter-cluster distance
ICME Integrated computational materials engineering
IFOV Instantaneous field of view
IPF Inverse pole figure
IR Infrared radiation
IRIC Infrared image correlation
IR-TG Infrared thermography
KAM Kernel average misorientation
KS Kurdjumov–Sachs
LA Loading axis
LAGB Large-angle grain boundary
LC Lomer–Cottrell
LCF Low-cycle fatigue
LC-SEM Large-chamber scanning electron microscope
LDC Load–displacement curves
LDM Long-distance microscope
LV Low vacuum
LV-SEM Low-vacuum scanning electron microscope
LWIR Long-wave infrared radiation
LYS Lower yield strength
MBIP Microband-induced plasticity
MD Molecular dynamics
MMC Metal matrix composite
MPT Martensitic phase transformation
MSC Microstructurally short crack
MSE Materials Science and Engineering
MSPS Million samples per second
MSV Mean square values
MWIR Mid-wave infrared radiation
NCC Normalized cross-correlation
ND Normal direction
NDT Non-destructive technique
NETD Noise-equivalent temperature difference
NSSD Normalized sum square difference
NW Nishiyama–Wassermann
OIM Orientation imaging mapping
OM Optical microscopy
OR Orientation relationship
PCA Principal component analysis
PDF Probability density function
PF Phase field
PID Proportional–integral–derivative
PLC Portevin–Le Chatelier
PSB Persistent slip band
xx Abbreviations

PSDF Power spectral density function


PSM Persistent slip marking
PSZ Partially stabilized ZrO2
PT Phase transformation
RAAP Rotation angle/axis pair
RD Rolling direction
RT Room temperature
SB Slip band
SD Slip direction
SDP1 Slip direction leading partial dislocation
SDP2 Slip direction trailing partial dislocation
SDreg Slip direction regular dislocation
SE Secondary electron
SEM Scanning electron microscopy
SEM-DIC Digital image correlation on images of scanning electron microscopy
SF Stacking fault
SFE Stacking-fault energy
SHPB Split Hopkinson pressure bar
SHTB Split Hopkinson tension bar
SIF Stress intensity factor
SMA Shape memory alloy
SME Shape memory effect
SMM Shape memory materials
SP Slip plane
SPD Severe plastic deformation
SRS Strain rate sensitivity
SS Slip system
SSD Sum square difference
SST Stereographic standard triangle
STT Stress temperature transition
SWIR Short-wave infrared radiation
TB Twin boundary
TC Thermo-camera
TD Transverse direction
TE Transmitted electron
TEM Transmission electron microscopy
TG Thermography
TMCP Thermomechanical controlled processing
TRIP Transformation-induced plasticity
t-SEM Transmission scanning electron microscopy
TTFA Thermal thin-film ablation
TWIP Twinning-induced plasticity
UFG Ultrafine-grained
UTS Ultimate tensile strength
VHCF Very high-cycle fatigue
Abbreviations xxi

VP Variable pressure
VP-SEM Variable-pressure scanning electron microscope
XRD X-ray diffraction
YS Yield stress
ZNCC Zero-normalized cross-correlation
ZNSSD Zero-normalized sum square difference
µCT Microcomputer tomography
DCTODpl Plastic portion of the crack tip opening displacement
Symbols

List of symbols is organized according to bullets of the table of content and


separated in Latin and Greek symbols.

Plastic Deformation

A Cross section
A0 Initial cross section
A, B, C, D Notation of lattice points
a, b, c Lattice constants
b Distance between atoms
~ b1 , ~
b, ~ b2 Burgers vector
cB Velocity of PLC band
C1 Coefficient for dislocation generation
C2 Coefficient for reduction of dislocation density
C3 Coefficient for the limitation of the mobility of dislocations
C4 Coefficient for the dynamic recovery rate of forest dislocations
C5 Concentration of the solute atoms at dislocation line
dc Thickness of dislocation free channels
dSF Width of stacking fault
dw Thickness of dislocation dense walls
D Grain size/diameter
Di Thickness of ith slip band
E Young’s modulus
Eel Elastic energy
F Applied load
G Shear modulus
h Strain-hardening rate

xxiii
xxiv Symbols

H Strain-hardening coefficient
k1 Hardening coefficient of forest dislocations
k2 Dynamic recovery rate of dislocations
k Hall–Petch constant
l0 Initial gauge length
l Final gauge length
L Length of pile up (or slip band)
M Taylor factor
n Number of dislocations
S Strain rate sensitivity
Si Instantaneous strain rate sensitivity
Sas Asymptotic strain rate sensitivity
T Temperature
up; i Displacement in the direction of Burgers vector for ith slip band
v Cross-head velocity
wb Width of PLC band
x Displacement
a Factor in Taylor equation describing interaction of dislocations
a, b, c, d Notation of f111g planes of Thompson tetrahedron
e Resolved strain
ea; p Plastic strain amplitude
eel Elastic strain
ep Plastic strain
er Strain to rupture
etrue True strain
eu Uniform strain
de Deviation of strain
DeB Strain increment within PLC band
e_ Strain rate
c Shear strain
cSB; i Shear strain amplitude within ith slip band
cSF Stacking-fault energy
H Strain-hardening coefficient
k Angle between slip direction and load axis
K Mean free path of dislocations
l Schmid factor
. Dislocation density
.f Density of forest (sessile) dislocation
.m Density of mobile dislocation
r Stress, flow stress, normal stress
ra Applied stress
rCRSS Critical resolved shear stress
rtrue True stress
rUTS Ultimate tensile stress
Symbols xxv

ry Yield stress
rr Stress at rupture
s0 Experimentally observed shear stress
sCRSS Critical resolved shear stress
smax Maximum shear stress
sth Theoretical shear stress
/ Angle between slip plane normal direction and load axis

Martensitic Phase Transformation

a, b, c Axis of unit cell


a, b, c Lattice constants
afcc Lattice constant of fcc austenite
abcc , cbct Lattice constant of bcc a-ferrite, d-ferrite, a'-martensite
abct , cbct Lattice constant of bct a'-martensite
Af Austenite finish temperature
As Austenite start temperature
~
b Burgers vector
E str Strain energy
fa
0
Volume fraction of a0 -martensite
G GIBBS free energy
DG Difference of GIBBS free energy
DGA!M Difference of GIBBS free energy for martensitic transformation from
austenite into martensite
0
DGc!a Difference of GIBBS free energy for martensitic transformation from
c-austenite into a0 -martensite
DGc!e Difference of GIBBS free energy for martensitic transformation from
c-austenite into e-martensite
n Geometry factor
N Number of closed-packed planes involved in formation of e-martensite
Md Temperature up to which deformation-induced martensitic
transformation occurs
Mf Martensitic finish temperature
Ms Martensitic start temperature
Msr Martensitic start temperature under external applied load
p Pressure
R Radius of dislocation nodes
s Shear strain
s1 , ~
~ s3 Shear vector
~
s2 Shuffling vector
T, T1 Temperature
xxvi Symbols

T0 Equilibrium temperature
Tc Curie temperature
TL Melting temperature
DT Undercooling
DT Width of the hysteresis loop of martensitic phase transformation
VA Volume of austenite
VM Volume of martensite
a Evolution of deformation bands
a0 a0 -martensite
b Probability of formation of a'-martensite nucleus
c Austenite
cSF Stacking-fault energy
c0SF Stacking-fault energy of pure iron
c Interface energy
e e-martensite
epl Plastic strain
.A Dislocation density austenite
rc!e Surface energy for transformation of c-austenite into e-martensite
us; e Shear angle for formation of e-martensite
us; twin Shear angle for twinning

Advanced High Strength Steels

~
b Burgers vector
B Fit parameter Olson–Cohen model
C1 Coefficient for dislocation generation
C2 Coefficient for reduction of dislocation density
C3 Coefficient for the limitation of the mobility of dislocations
C4 Coefficient for the dynamic recovery rate of forest dislocations
C5 Concentration of the solute atoms at dislocation line
Creq Chrom equivalent
D Grain size
dtw Thickness of twins
F Volume fraction of twins
F0 Maximum volume fraction of twins
k2 Dynamic recovery rate of dislocations
m Fit parameter Olson–Cohen model
M Taylor factor
Mf Martensitic finish temperature
Md Temperature up to which deformation-induced martensitic transforma-
tion occurs
Symbols xxvii

Md30 Temperature up to which 30% of deformation-induced martensite


developed
Ms Martensitic start temperature
Msr Martensitic start temperature under external applied load
Nieq Nickel equivalent
T Temperature
a0 a'-martensite
c c-austenite
cSF Stacking-fault energy
0
DGc!a Difference of GIBBS free energy for the c—a' martensitic transformation
e e-martensite
e Applied strain
ecrit Critical strain
e_ Strain rate
K Mean free path of dislocations
. Dislocation density
.f Density of forest dislocations
.m Density of mobile dislocations
r Stress, flow stress, shear stress
rtw Stress in grains with twins
rtwfree Stress in grains without twins
rDSA Stress due to dynamic strain ageing

In Situ Techniques

Acoustic Emission

a Radius
Að f Þ Transfer function (after Fourier transformation)
~
b Burgers vector
cL Velocity of longitudinal wave
cT Velocity of transversal wave
Ci; j; k; l Elastic stiffness tensor
D Duration of AE event
Dij Force dipoles
D Measure of distance
DEUC Euclidean distance
DMAN Manhattan distance
DMIN Minkowski distance
dAl ðtÞ Time-dependent dislocation loop area
dBAE Decibel of acoustic emission
E AE energy
xxviii Symbols

Eð f Þ Source function (after Fourier transformation)


E ðf1 ; f2 Þ Narrow band energy
f Frequency
fa Averaged frequency
fc Fundamental frequency
feff Effective width of spectrum
fi Observed frequency
fm Median frequency
fN Nyquist frequency (cut-off frequency)
Fi Expected frequency
Gð f Þ Power spectral density function
Gnoise ð f Þ Power spectrum of electrical noise
Gmax Maximum of power spectral density function
Gi ð f Þ Integrated power spectral density function
Gij Green’s function
GH Heaviside Green’s function
gð f Þ Normalized power spectral density function
i, j, k, l Space variables
K Number of class intervals
Ku; PA Gain of used pre-amplifier
^k Space–time variable
k Number of desired clusters
ki , kj Individual clusters
m Activity of acoustic emission (AE)
mi , mj Centroids of individual clusters
ni , nj Number of elements within each individual clusters
N Number of counts, number of observations
N Length of time-series
DN Number of AE hits
Pð xÞ Probability distribution function
p1 , p2 , p3 Point coordinates
q1 , q2 , q3 Point coordinates
qf Kurtosis (frequency domain)
qx Kurtosis (time domain)
r Number of independent variables
r Distance between source and epicentre
r, r 0 Space coordinates
~r0 Centroid position of point-like source
R Rise time
Rxx ðsÞ Auto-correlation function
Ryy ðsÞ Auto-correlation function
Rxy ðsÞ Cross-correlation function
rx ðsÞ Normalized auto-correlation function
r ð sÞ Normalized auto-correlation function of Poisson distribution
Symbols xxix

sf Skewness (frequency domain)


sx Skewness (time domain)
S1 , S2 , S3 Individual clusters
t Time
t, t0 Time coordinates
Dt Unit time, time interval
Dts Sampling time interval
T Displacement threshold
T Transducer response
ui ðr; tÞ Displacement in ith direction depending on space and time coordinates
U ðt Þ Voltage of measured signals at transducer
U2 Mean square voltage
2
Unoise Average background noise
Up Maximum AE amplitude, peak voltage
URMS Root mean square voltage
Uth Threshold value for voltage signal
Uz Maximum displacement in z-direction (surface normal)
v Velocity
x1 , x2 , x3 Elements of data set
X ðt Þ Random data
^ ðt Þ
X Fourier transform of X ðtÞ
^
XT ðtÞ Truncated Fourier transform of X ðtÞ
Y ðt Þ Random data
Zcc Correlation coefficient
a Significance level
cmerged Centroid drift vector
dð t  t 0 Þ Delta function
dmerged Inter-cluster distance
lx Mean value
lðx1Þ First moment
lðx2Þ Second moment
r Source function (time domain)
r Pre-existing vertical stress
rx Standard deviation
r2x Variance (time domain)
r2f Variance (frequency domain)
s Inter-event time interval
s0 Relaxation time
v2 Chi-square function
X2 Goodness-of-fit test
W 2 ðt Þ Mean square value
xxx Symbols

Displacement and Strain Fields

C Cross-correlation coefficient
CZNCC Zero-normalized cross-correlation coefficient
F Deformation gradient tensor
f Reference image
g Image of deformed state
i, j Coordinates of the measuring point
i0 , j0 Coordinates of the displaced measuring point
L Initial length
l Final length
DL Change in length
dl Incremental strain element
nn Subset or facet size (square)
NN Size of the search field
mn Subset or facet size (rectangular)
Pðx0 ; y0Þ Central point subset (or facet) in reference image f
P x00 ; y00 Central point subset (or facet) in image of deformed
state g
Pu;i Point in coordinate system of non-deformed state
Pv;i Point of coordinate system in deformed state

Q xi ; yj Central point subset (or facet) in reference image f
 
Q xi0 ; yj0 Central point subset (or facet) in image of deformed
state g
R Rotation tensor
ui Rigid body translation
ux Displacement in x direction
uy Displacement in y direction
uxy Shear displacement
U, V Shape functions
U Displacement tensor, right-hand displacement
tensor
Ux , Uy , Vx , Vy First-order shape functions
Uxx , Uyy , Vxx , Vyy , Uxy , Vxy Second-order shape functions
V Left-hand deformation tensor
ð x  yÞ Macroscopic coordinate system
ð x0  y0 Þ Local coordinate system in non-deformed state
ðx00  y00 Þ Local deformation-induced coordinate system by
displacement tensor U
x00 Direction of normal strain exx
y00 Direction of normal strain eyy
x0 ; y0 Point coordinates of central point in reference
image f
Symbols xxxi

xi ; yj Point coordinates of individual point in reference


image f
0 0
xi ; yj Point coordinates of individual point in image g of
deformed state after displacement
dX Line element before displacement
dx Line element after displacement
a Part of shear angle according to dux
dy
b du y
Part of shear angle according to dx
cxy Shear angle
eeng Engineering strain
eG Green strain
etrue True strain
de Incremental strain element
exx Normal strain in x direction
eyy Normal strain in y direction
exy Shear strain
evM Equivalent strain according to Von Mises
eT Equivalent strain according to TRESCA
e1 , /1 Major strain
e2 , /2 Minor strain
k Stretch ratio
k1 , k2 Eigenvalues of displacement tensor
/ Logarithmic strain
U a ð xÞ Mechanical transformation function

Temperature Fields

c Specific heat capacity


di Intrinsic dissipation
di Zero-dimensional heat source field
di One-dimensional heat source field
di Two-dimensional heat source field
e Thickness
E el Elastic energy
E int Intrinsic energy
E pl Plastic energy
E stor Stored energy
E tot Total energy
k Heat conduction tensor
L2 Direct view thermogram
L1 , L 3 Reflected thermograms (by mirrors)
xxxii Symbols

L Length
l Width
q Heat flux vector
re External heat supply or loss
s Heat source
sth Thermomechanical coupling
T Absolute temperature
T0 Equilibrium temperature field
vk Internal state variable
Wmech Mechanical work
a Absorption
a Thermal expansion coefficient
e Emissivity
 Strain tensor
e Elastic part of strain tensor
p Plastic part of strain tensor
. Reflection
. Mass density
/ Intensity of infrared radiation measured at thermo-camera
/O Radiation intensity of measuring object
/M Radiation intensity of the measuring section
/e Emitted intensity
/s Transmitted intensity
/. Reflected intensity
HO Temperature measuring object
HBG Temperature background
Hu Temperature environment
HP Temperature measuring section
s Transmission
sp Transmission of measuring section
sth Time constant of heat loss in z direction
seq Local heat loss

Fully-Coupled Measurements

T Temperature
k Radiation path
k1 Transmission
k2 Reflection
Symbols xxxiii

High-alloy CrMnNi TRIP/TWIP Steels

Creq Chrom equivalent


Ms Martensitic start temperature
Nieq Nickel equivalent
N, N1 , N2 Number of cycles
Nf Number of cycles to failure
R Stress ratio
T Temperature
x, y, z Specimen coordinate system, x—loading axis, z—surface normal
direction
a0 a0 -martensite
a01 Deformation-induced a'-martensite
0
a2 High-pressure-induced a'-martensite (decompression path)
c Austenite
cSF Stacking-fault energy
c0SF Stacking-fault energy of pure iron
d d-ferrite
e e-martensite
e1 Deformation-induced e-martensite
e2 High-pressure e-iron phase
e Applied strain
ea; t , Det =2 Total strain amplitude
e_ Strain rate
l Schmid factor
u1 , /, u2 Euler angles

Case Studies

CZXCC Zero-normalized cross-correlation coefficient


CZNCCi0 ; j0 Zero-normalized cross-correlation coefficient at point i0 , j0 in the
deformed state
CZXCCmax Maximum zero-normalized cross-correlation coefficient
dDB Thickness of deformation band
E AE energy
f Frequency
fm Median frequency
F Applied load
gð f Þ Normalized power spectral density function
DG Activation energy of interstitial diffusion
k Boltzmann constant
K Material constant
xxxiv Symbols

L Size of field of view (FOV)


L Length of single-ended slip band
L Length of AOI parallel to the loading axis
l0 Object dimension
l0min Minimum spatial resolution
m Factor describing the dependence of critical strain on dislocation
density
Ms Martensitic start temperature
MT Magnification factor
ndis Number of dislocations
nn Size of subset (or facet)
NN Size of search field
N Number of cycles
NB Number of PLC bands
R Recorded image resolution
s Magnitude of shear
t Time
tin Time, when PLC band entering the AOI
tout Time, when PLC band passed AOI
T Temperature
T0 Initial temperature
Tmax Peak temperature, maximum temperature
DT Temperature increase
DTB Temperature increase within PLC band
U Displacement tensor
vB Average band velocity
a Part of shear angle according to dduyx
a0 a0 -martensite
0
a1 Deformation-induced a'-martensite
0
a2 High-pressure-induced a'-martensite (decompression path)
a0i ; a0ii ; a0iii ; a0iv Martensite variants
a0max ; a0tot Maximum (total) volume fraction of a'-martensite
0
amin Minimum volume fraction of a'-martensite
atrace Angle between the trace of activated slip plane on specimen surface
and x-axis (loading axis)
b du
Part of shear angle according to dxy
b Factor describing dependence of critical strain on vacancy
concentration
bI Image displacement accuracy
btrace Angle between the trace of activated slip plane on side face and
x-axis (loading axis)
c Austenite
cxy Shear angle
Symbols xxxv

cSF Stacking-fault energy


c0SF Stacking-fault energy of pure iron
d d-ferrite
e e-martensite
e Applied strain
exx Normal strain in x direction
eyy Normal strain in y direction
exy Shear strain
evM Equivalent strain according to Von Mises
e1 Major strain
e2 Minor strain
ea;t Total strain amplitude
ec Critical strain
et Total strain
eAEt;c
Critical true strain evaluated by AE
eSSC
t;c
Critical true strain determined from stress-strain curve
eTGt;c
Critical true strain evaluated by TG
et;max Maximum true strain
DeB Strain increase within PLC band
e_ Strain rate
e_ 0 Initial strain rate
gI Image speckle dimension
g0 Object speckle dimension
k1 , k2 Eigenvalues of displacement tensor
l SCHMID factor
r Applied stress
List of Figures

Fig. 2.1 Mechanical behaviour under quasi-static uniaxial loading.


a Typical engineering stress-strain curve of a ductile material.
1—Young’s modulus, 2—yield stress (YS) ry , 3—ultimate
tensile stress (UTS) rUTS , 4—strain to rupture er and 5—work
of deformation. b True stress-strain curve versus engineering
stress-strain curve. c Typical stress-strain curves of materials
with high strength at low ductility, high strength at high
ductility and low strength at high ductility. Modified according
to [1]. Permission of Pearson Education . . . . . . . . . . . . . . . . . .. 8
Fig. 2.2 Permanent deformation by slip of lattice planes. a Rigid slip of
neighbouring lattice planes. b Progress of energy and shear
stress during rigid slip of atoms. Modified according to [1].
Permission of Pearson Education . . . . . . . . . . . . . . . . . . . . . . .. 10
Fig. 2.3 Plastic deformation of a crystal by motion of dislocation along
a slip plane. Modified according to [1]. Permission of
Pearson Education. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 10
Fig. 2.4 Schematic illustration of different types of dislocations in
crystal lattice. a Edge dislocation with Burgers circuit.
b Three-dimensional representation of edge dislocation.
c Screw dislocation. d Part of a dislocation loop with segments
of edge and screw-type dislocation. Modified according to
[1]. Permission of Pearson Education . . . . . . . . . . . . . . . . . . . .. 10
Fig. 2.5 Unit cells of fcc, bcc and hcp crystal lattices with indicated
basis slip systems based on close-packed lattice planes and
lattice directions. a fcc crystal lattice with f111gh110i slip
system. b bcc crystal lattice f110gh111i slip system. c hcp
crystal lattice with f0001gh0001i slip system . . . . . . . . . . . . . .. 12

xxxvii
xxxviii List of Figures

Fig. 2.6 Thompson tetrahedron for description of dislocation reactions


in fcc crystal lattice. a Construction of the tetrahedron.
b Tetrahedron with separation of regular h110i dislocations
into h112i Shockley partials. c Several reactions of Shockley
partials forming Lomer-Cottrell (LC) locks (bold red lines).
Modified according to [4]. Permission of IOP Publishing . . . . .. 13
Fig. 2.7 Stacking faults in fcc crystal lattice. a Dissociation of regular
dislocations forming stacking fault. b Stacking sequence of
atomic layers of the fcc and hcp crystal lattice. c Intrinsic and
extrinsic stacking faults. d SF tetrahedra. e Cross-slip. a,
e Modified according to [3]. Permission of Springer. d,
c Modified according to [5] and [6]. Permission of Elsevier . . .. 14
Fig. 2.8 Deformation twinning in fcc crystal lattice. a Twin system
consisting of twin plane, direction of shear and shear plane.
b Movement of atom positions during deformation twinning.
Modified according to [3]. Permission of Springer . . . . . . . . . .. 16
Fig. 2.9 Description of twin orientation. a Twin boundary with
coincident site lattice places. b Misorientation 60° h111i of a
R3 boundary. Modified according to [1] (a) and [9] (b).
Permission of Pearson Education and Springer, respectively. . .. 17
Fig. 2.10 Deformation twinning of bcc a, b and hcp c, d crystal lattices.
a, c Unit cells with indicated twinning plane, direction of shear
and shear plane. b, d Cooperative movement of atoms along
direction of shear during twinning. TD—twin direction, TP—
twin plane, PoS—plane of shear. Modified according to [3].
Permission of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 17
Fig. 2.11 Critical resolved shear stress for activation of slip system.
a Definition of angles / and k for calculation of Schmid factor
l. b Activation of slip on multiple parallel slip planes leading
to distortion of the single crystal. Modified according to [3].
Permission of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 19
Fig. 2.12 Dependence of critical resolved shear stress on
crystallographic orientation. a Stereographic standard
projection ½001. b Loading path for activation of primary slip
system in fcc crystal lattice. c Schmid factor contour lines
(constant µ value) within stereographic standard triangle
(SST). Modified according to [3]. Permission of Springer . . . .. 20
Fig. 2.13 Stereographic standard triangle with contour lines of Schmid
factors l for the activation of slip (red) and twinning (black) in
fcc crystals. a Tensile loading. b Compressive loading.
Reproduced from [20]. Permission of Elsevier . . . . . . . . . . . . .. 20
List of Figures xxxix

Fig. 2.14 Activation of slip in differently oriented grains of a


polycrystalline specimen during tensile loading. Through
the deformation related to the activated single slip, the
connectivity at the grain boundaries would be lost. Thus, gap
(black) or overlap (dark grey) of material would be the
consequence (a). Therefore, the activation of secondary slip
system (c) is necessary in order to compensate the deformation
caused by the primary slip system (b). In addition, at the grain
boundaries, geometrically necessary dislocations are
introduced. Modified according to [3]. Permission
of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 21
Fig. 2.15 Strain hardening according to Kocks–Mecking model.
a Schematical Kocks–Mecking plot for fcc polycrystal in
comparison to single crystals. Modified according to [27].
b Kocks–Mecking plots of AISI 316LN at different
temperatures. Reproduced after [28]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 24
Fig. 2.16 Schematic overview on strain localizations. a Stationary strain
localizations. b Propagative strain localizations Modified
according to [38]. Permission of Trans Tech Publ . . . . . . . . . .. 25
Fig. 2.17 Typical examples of microscopic strain localizations. a Fine
slip lines in a polycrystalline nickel specimen under tensile
loading interrupted at the yield point. b Slip bands in a
polycrystalline nickel specimen under tensile loading between
yield point and uniform elongation. c Deformation bands in a
polycrystalline steel specimen under tensile loading interrupted
at uniform elongation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 27
Fig. 2.18 Microscopic strain localization during cyclic loading.
a Schematic drawing of cyclic strain localization in a persistent
slip band (PSB) emerging at the specimen surface as persistent
slip marking (PSM). Reproduced from [52]. Permission of
Taylor & Francis. b Schematic drawing of the dislocation wall
and dislocation channel configuration of the ladder-like
structure of PSB. Reproduced from [59]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 29
Fig. 2.19 Microstructural features of cyclic strain localization.
a Persistent slip markings. b Extrusions and intrusions of
persistent slip markings. c Dislocation arrangement of
persistent slip bands. All examples are SEM micrographs
belonging to polycrystalline nickel deformed cyclically at
ea;p ¼ 5  104 up to 30,000 cycles 0:6 Nf . . . . . . . . . . . . . .. 30
xl List of Figures

Fig. 2.20 Dislocation pattering during cyclic loading in fcc materials.


a Influence of dislocation glide behaviour and plastic strain
amplitude on the appearance of PSBs. Modified according to
[60]. Permission of Elsevier. b Influence of grain orientation
(loading axis) on the dislocation patterning of the matrix.
Reproduced from [61]. Permission of Elsevier . . . . . . . . . . . . .. 30
Fig. 2.21 Typical appearances of various kinds of shear bands.
a Macroscopic shear bands in a-brass. b TEM micrograph of
Brass-type shear band (SB) with crossing the lamellar structure
of twin/matrix. c TEM micrograph of Copper-type shear band
in pure copper [65]. d Macroscopic shear bands in austenitic
stainless steel. e Adiabatic shear bands after compression tests
of aluminium alloy 7083 at strain rate 8  103 s−1 [66].
a, b After cold rolling with 95% of thickness reduction. c After
cold rolling up to 97% of thickness reduction. d After cold
rolling with 90% of thickness reduction. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 33
Fig. 2.22 Difference between dislocation lack yield point and
pronounced yield stress due to unpinning of dislocations.
a Dislocation lack yield point caused by dislocation
multiplication and interaction. b Pronounced yield strength as
a consequence of Cottrell effect. Modified according to [78].
Permission of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 34
Fig. 2.23 Stress-strain curve of a material with Lüders effect. Modified
according to [93]. Permission of De Gruyter . . . . . . . . . . . . . .. 35
Fig. 2.24 Example of serrated plastic flow caused by dynamic strain
aging. Stress-strain curves of an Al–3.5% Mg alloy tensile
deformed at RT and two strain rates resulting in different
appearances of serrated plastic flow. Reproduced from [113].
Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 37
Fig. 2.25 Three main types of PLC bands. a Type A bands: Each stress
drop is related to the initiation of a new band. b Type B bands:
Several bands initiate volatile but correlated. c Type C bands:
Several bands initiate in a stochastic way at different places.
Modified according to [112]. Permission of Elsevier . . . . . . . .. 38
Fig. 2.26 Parameters describing the strain jump, the velocity and the
width of PLC bands occurring during serrated plastic flow.
Modified according to [115, 116] . . . . . . . . . . . . . . . . . . . . . . .. 38
Fig. 2.27 PLC effect in different type of alloys. a Ferritic steel.
b Austenitic steel AISI 304. c TWIP steel. d Al–Mg alloy
AA5052. e Ni-base superalloy. Reproduced from [133] (a),
[134] (b), [142] (c), [125] (d), [142] (e). Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 39
List of Figures xli

Fig. 2.28 Strain-rate sensitivity. a Instantaneous and asymptotic


strain-rate sensitivity. Reproduced from [147]. b Interplay
between dynamic strain aging, strain-rate sensitivity and
dislocation interaction. Modified according to [148].
Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 40
Fig. 3.1 Self-accommodation of lattice stress caused by martensitic
phase transformation. a Initial shape of crystal before
martensitic phase transformation. b Shear deformation of the
crystal. c Accommodation of shear deformation by dislocation
glide. d Accommodation of shear deformation by twinning.
Modified according to [3]. Permission of Springer . . . . . . . . . .. 48
Fig. 3.2 Schematic visualization of the orientation relationship between
austenitic and martensitic phases. a Bain, b Kurdjumov–Sachs
and c Nishiyama–Wassermann. Modified according to [4–6].
Permission of Springer and Wiley VCH, respectively . . . . . . . .. 49
Fig. 3.3 Hysteresis loop of martensitic phase transformation. Modified
according to [1]. Permission of Cambridge International
Science Publishing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 50
Fig. 3.4 Thermodynamics of martensitic phase transformation.
a Temperature dependence of GIBBS free energy of the
austenitic and martensitic phases indicating the martensitic
start temperature Ms . Modified according to [7]. Permission of
Taylor and Francis. b Influence of mechanical energy on the
MPT. Modified according to [8]. c Schematic drawing of the
temperature–stress range for stress-assisted and strain-induced
martensitic transformation. Modified according to [9].
Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 51
Fig. 3.5 Allotrope modifications of iron as a function of temperature
T and pressure p. Modified according to [10] . . . . . . . . . . . . . .. 52
Fig. 3.6 Schematic drawing of the complete set of possible
transformations between the three important crystal lattices
occurring in metallic materials: body-centred cubic,
face-centred cubic and hexagonal closed packed. Modified
according to [14]. Permission of Elsevier . . . . . . . . . . . . . . . . .. 54
Fig. 3.7 Martensitic phase transformation according to Bain. a BCT
crystal lattice of the martensitic phase in the fcc crystal lattice
of the austenite. Modified according to [16]. b Three
sub-lattices of octahedral interstitial lattice sites of the bcc
crystal lattice. Modified according to [18]. c Carbon atoms
occupying only one out of the three octahedral interstitial
sublattices leading to a tetragonal distorted bct lattice of Fe–C
martensite. Modified according to [17]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 55
xlii List of Figures

Fig. 3.8 Martensitic phase transformation according to Bain. a Bain—


orientation relationship [4]. b Shear operations of the iron
atoms above and below body-centred iron atom to change from
the ABC stacking sequence of the fcc crystal lattice to the AB
sequence of the bcc crystal lattice shown in c. b, c Modified
according to [19] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 56
Fig. 3.9 Martensitic phase transformation according to Kurdjumov–
Sachs. a Three-dimensional arrangements of atoms in the
austenitic, the tetragonal and the martensitic lattice. b Atom
position in the corresponding two-dimensional planes.
c Individual shear operations. Reproduced from [5].
Permission of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 57
Fig. 3.10 Martensitic phase transformation according to Schumann
following a two-step shear mechanism. a Three-dimensional
representation. b Two-dimensional projection. Modified
according to [22]. Permission of Wiley VCH . . . . . . . . . . . . . .. 58
Fig. 3.11 Variant selection of a′-martensite according to KS-OR.
Reproduced from [23]. Permission of Elsevier . . . . . . . . . . . . .. 58
Fig. 3.12 Martensitic phase transformation according to Nishiyama in
comparison to Kurdjumov–Sachs. a Reproduced from [25].
b Direction of shear in {111} plane of austenite. Nishiyama
(left) and Kurdjumov–Sachs (right). Reproduced from [24].
c Nishiyama (left) and Kurdjumov–Sachs (right) in
combination with C-atoms on three different octahedral
sublattices (small circles). Reproduced from [17]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 59
Fig. 3.13 Shear operations for the formation of e-martensite. According
to [28]. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 61
Fig. 3.14 Six equivalent a′-martensite variants with h111ia0 habitus.
According to Schumann [32]. Permission of Wiley VCH . . . . .. 62
Fig. 3.15 Indirect martensitic phase transformation from austenite into
a′-martensite via e-martensite. a, b Process of dislocation glide
(~
b ¼ a6 ½211). c Shearing (~ s1 ¼ a6 ½1210). d Shuffling
a 
s2 ¼ 6 ½110). e bcc crystal lattice of a′-martensite. Modified
(~
according to [33]. Permission of Wiley VCH . . . . . . . . . . . . . .. 63
Fig. 3.16 Double shear mechanisms on two different f111g planes
yielding the formation of a′-martensite. a Double shear in the
½011 intersection line due to partial dislocation s1 k ½11 2 on
  
ð111Þ and s2 k ½112 on ð111Þ. Modified according to [15].
Permission of Wiley VCH. b Intersecting bands of stacking
faults indicating first and second invariant plane strain and the
stable a′-martensite nucleus at centre. Reproduced from [34].
Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 63
List of Figures xliii

Fig. 3.17 Olson–Cohen model of martensitic phase transformation.


a Temperature dependence of the parameter a—describing the
rate of deformation band formation. b Temperature
dependence of the parameter b—describing the probability of
intersectioning of deformation bands forming a′-martensite.
c Calculated transformation curves based on (3.5) in
comparison with experimental data of Angel [59]. Reproduced
from [51]. Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . .. 67
Fig. 4.1 Relationship between total elongation and ultimate tensile
strength of different categories of advanced high-strength
steels. Reproduced from [1]. Permission of Elsevier . . . . . . . . .. 72
Fig. 4.2 Fe–Mn phase diagram. a Metastable phase diagram. b Fe-rich
corner of the Fe–Mn–C equilibrium phase diagram at 700 °C.
c Superimposition of the 700 °C austenite stability range and
the microstructure observed after quenching from 950 °C to
room temperature. Reproduced from [27]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 74
Fig. 4.3 Stress-strain curves of different high-Mn TWIP steels.
a Fe–Mn–C steels. Reproduced from [29]. b Fe–Mn–Si–Al
steels. Reproduced from [31]. Permission of Elsevier . . . . . . . .. 75
Fig. 4.4 Strain-hardening behaviour. a Comparison of the stress-strain
behaviour and strain-hardening rate for IF, TRIP and TWIP
steels. b Illustration of the mean free path approach (dynamic
Hall–Petch effect). Reproduced from [32]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 75
Fig. 4.5 Schematic representation of strain-hardening curve obtained
for TWIP steels. a Evolution of microstructure with respect to
the different stages (1) to (5) of strain-hardening curve.
b Indicated influence of different parameters on
strain-hardening. Modified according to [38]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 76
Fig. 4.6 Influence of grain size (3 µm and 50 µm) on the
strain-hardening behaviour of high-Mn TWIP steel (Fe–
22Mn–0.6C). a True stress-true strain curves.
b Strain-hardening curves. c Models for microstructure
evolution for grain sizes 3 and 50 µm. Modified according to
[33]. Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . .. 79
Fig. 4.7 Modelling of the stress-strain behaviour of TWIP steels.
a Comparison of the model curves for the twin-free grains and
twinned grains with experimental true stress versus true strain
curves. In addition, the model curve according to the rule of
mixture is plotted. b Strain-hardening curves obtained from the
experimental data and the calculation according to the rule of
mixture. Reproduced from [63]. Permission of Elsevier . . . . . .. 83
xliv List of Figures

Fig. 4.8 Comparison of the temperature course of chemical driving


force DG for different martensitic transformation in both binary
Fe-based alloys with different contents of Ni and Cr and for
ternary Fe-based alloys with 17% Cr. a Direct c ! a′
transformation. b c ! e transformation. c e ! a′
transformation. In addition, the DG  T course for pure iron is
shown (bold black line). Reproduced according to [71]. With
courtesy of A. Weiss and H. Gutte . . . . . . . . . . . . . . . . . . . . . .. 87
Fig. 4.9 Stress-temperature-transition and
deformation-temperature-transition diagrams for Fe–16Cr–
6Mn–6Ni–0.05C steel. a Stress-temperature-transition
(STT) diagram. b Deformation-temperature-transition
(DTT) diagram. c Comparison of the phase field c ! a′ for
three Fe–16Cr–6Mn–xNi–0.05C steels with varying nickel
content x = 3 wt%, 6 wt% and 9 wt%, respectively.
Reproduced from [74]. Permission of Wiley VCH . . . . . . . . . .. 89
Fig. 4.10 Stress-strain behaviour and strain-hardening behaviour of
TRIP steels. a Schematic representation of the TRIP effect on
the stress-strain behaviour. Modified according to [77].
Permission of Wiley VCH. b Strain-hardening behaviour (bold
line) and evolution of the volume fraction of strain-induced
a′-martensite (dashed line). Reproduced from [78]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 90
Fig. 4.11 Strain-hardening behaviour and mechanical properties
of austenitic steels enabling TRIP effect. a Influence
of temperature on strain-hardening behaviour. b Influence
of temperature on mechanical parameters: Yield strength,
ultimate tensile strength, uniform elongation and strain to
failure. Reproduced from [79]. With courtesy of S. Martin.
b Reproduced from [31]. Permission of Elsevier . . . . . . . . . . .. 91
Fig. 4.12 Influence of the strain rate and the stacking-fault energy on the
TRIP/TWIP effect of austenitic stainless steels. Reproduced
from [45]. Permission of Springer. . . . . . . . . . . . . . . . . . . . . . .. 92
Fig. 4.13 Schematic diagram of 610SA steel showing the relationship
between grain size and mechanism of deformation-induced
martensite. Modified according to [91]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 93
Fig. 5.1 Acoustic emission—generation and detection of acoustic
emission signals. a Generation of elastic waves by
spontaneous energy release caused by the formation of a brittle
crack. b Detection of surface displacement by suitable
transducer. Modified according to [131]. Permission of IOP
Publishing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 116
List of Figures xlv

Fig. 5.2 Similarities of seismology and acoustic emission. a Frequency


domain of earthquakes and acoustic emission. b Time domain
of seismic signals. c Time domain of AE signals. Modified
according to [132]. Permission of Taylor and Francis . . . . . . . . . 117
Fig. 5.3 Two different types of AE signals. a Continuous signal.
b Transient (burst) signal. c AE data stream consisting of
continuous and burst-type signals . . . . . . . . . . . . . . . . . . . . . . . . 118
Fig. 5.4 Specific parameters describing acoustic emission signals in the
time. a Burst-type signals. b Continuous-type signals . . . . . . . . . 118
Fig. 5.5 Schematic illustration of the meaning of the “kurtosis” for the
AE amplitude distribution. a q > 0 for transient AE signal.
b q * 0 for continuous AE signal. Reproduced from [136].
Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 122
Fig. 5.6 Schematic illustration of an acoustic emission data set
containing burst signals (a). b Definition of the time interval
Ds between the burst signals shown in (a). c Description of the
AE data by a Poisson’s probability density distribution.
d Significant deviation of the AE data from Poisson’s
distribution (c). Modified according to [136]. Permission of
Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 123
Fig. 5.7 Examples for special auto-correlation functions. a White noise.
b Sine wave. c Exponential according to Poisson’s process
described by (5.18). According to [135] . . . . . . . . . . . . . . . . . . . 126
Fig. 5.8 Different shapes of power spectral density functions. a The AE
energy E is given by the area (green) below the curve of the
PSDF. b Median frequency fm of a PSDF. c PSDFs with
different AE energy E, but the same median frequency.
d PSDFs with different AE energy and median frequencies.
Modified according to [137]. Permission of Elsevier . . . . . . . . . 128
Fig. 5.9 Correlation between AE source (body force) and the
displacement detected at a certain distance and a certain time
within a finite volume. Convolution of each and every time
body force with its Green’s function. Modified according to
[141]. Permission of Taylor and Francis . . . . . . . . . . . . . . . . . . . 130
Fig. 5.10 Detectability threshold of acoustic emission in terms of crack
size (area) and crack velocity. Modified according to [143].
Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 134
Fig. 5.11 AE response according to different fracture behaviour. a Brittle
fracture. b Ductile fracture. According to [131]. Permission of
IOP Publishing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 135
Fig. 5.12 Sensor response of two different types of AE sensors.
a Resonant-type sensor. b Broadband-type sensor (Copies of
calibration sheets of resonant sensor R50 (a) and broadband
sensor WD) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 136
xlvi List of Figures

Fig. 5.13 Two variants of calibration procedures for AE sensors. a Glass


capillary on a steel transfer block (NIST). b Hsu-Nielsen
source or pencil break test on an acryl rod (EN 1330) [148].
With courtesy of A. Vinogradov . . . . . . . . . . . . . . . . . . . . . . . . . 137
Fig. 5.14 Effect of the band-pass filter on the AE waveforms. Modified
according to [129]. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 138
Fig. 5.15 AE data acquisition instrument with N channels for AE data
acquisition with fast analog/digital converter and
one-parametric channel with slow analogue/digital converter
for recording additional parameters such as load, strain,
temperature. According to [148]. With courtesy
of A. Vinogradov . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 138
Fig. 5.16 Scheme of two different approaches for AE data acquisition.
a Narrow-band data acquisition. b Broadband data acquisition.
Modified according to [131]. Permission of IOP Publishing . . . . 140
Fig. 5.17 Threshold-based AE data acquisition. a Record of AE data.
b Suitable single transient signal for determining detection
threshold value above noise level. c More complex AE signals
consisting of several transient signals and continuous signals,
where it is difficult to define appropriate threshold value.
According to [148]. With courtesy of A. Vinogradov . . . . . . . . . 141
Fig. 5.18 Time-series analysis of AE data in terms of probability density
distributions. a Experimental data set of peak amplitude
distribution. b Schematical description of bimodal frequency
distribution consisting of Poisson’s distribution and normal
distribution. According to [148]. With courtesy
of A. Vinogradov . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 142
Fig. 5.19 Description of the time history of AE signals in reduced
parameter space using the median frequency fm and the
kurtosis q showing development of damage in the
fibre-reinforced composite. a Whole process. b 1 < t < 30 s.
c 30 < t < 60 s. d 60 < t < 690 s. e 690 < t < 760 s.
f 760 < t < 830 s. g 830 < t 860 s. According to [160].
Data with courtesy of A. Vinogradov . . . . . . . . . . . . . . . . . . . . . 147
Fig. 5.20 Difference between data categorization and clustering.
a Supervised learning—categorization/classification.
b Non-supervised learning—clustering. Modified according to
[157]. With courtesy of E. Pomponi . . . . . . . . . . . . . . . . . . . . . . 148
Fig. 5.21 Results of clustering process in a bivariate feature space.
a Three clusters with their centroids. b Parameter description
used for the adaptive sequential k-means algorithm (ASK).
a According to [160]. With courtesy of A. Vinogradov.
b Reproduced from [161]. Permission of Elsevier . . . . . . . . . . . 150
List of Figures xlvii

Fig. 5.22 Comparison of three different clustering algorithms applied on


an AE data stream obtained from crack growth experiments on
a CuZr alloy. a Three different types of mean PSDF identified
out by the FFT related to cluster 1, cluster 2 and cluster 3.
b Three different cluster algorithms applied on a
two-dimensional feature space given here by the median
frequency fm and the energy E: (i) adaptive sequential
k-mean algorithm (ASK), (ii) fuzzy c-means algorithm and
(iii) k-means algorithm. c Temporal evolution of the three
identified clusters and their relation to deformation and damage
mechanisms. Reproduced from [161]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153
Fig. 5.23 Speckle paint pattern for digital image correlation. a Poor
contrast. b Good contrast, however, too large regions with
black contrast. c Optimum contrast for DIC. Reproduced from
Aramis [237]. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 160
Fig. 5.24 General principle of digital image correlation. a Definition of
area of interest on the specimen surface with subdivision into
equidistant virtual grids (black squares). b Computed
displacement vectors (blue arrows) for each point of the virtual
grid. Modified according to [242]. Permission of
IOP Publishing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 161
Fig. 5.25 Subset definition and determination of displacement vector.
a Definition of square-shaped subset n  n around a centred
measuring point Pðx0 ; y0 Þ in the reference image characterized
by unique greyscale distribution. b Computed displacement 
vector of subset in the deformed image with P0 x00 ; y00 as the
centred point of the target subset exhibiting the same greyscale
distribution as the reference subset. Reproduced according to
[242]. Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . 162
Fig. 5.26 Definition of subset size n  n and search field size N  N
in the reference image f (a) and in the image of deformed
state g (b) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 163
Fig. 5.27 Displacement of the reference subset (red square, left) as well
as the distortion of the target subset (middle, right), whereas
the greyscale distribution (speckle pattern) remains unchanged.
Reproduced from [244] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 164
Fig. 5.28 Displacement gradients at subset points. a Influence of
zero-order shape functions: (i) rigid body rotation, (ii) rigid
body translation. b Influence of first-order shape functions.
c Influence of second-order shape functions. Reproduced
according to [246] and [242]. Permission of Elsevier . . . . . . . . . 165
Fig. 5.29 Schematical illustration of the subpixel correlation algorithm.
Modified according to [250]. Permission of IOP Publishing . . . . 167
xlviii List of Figures

Fig. 5.30 Definition of strain variables for digital image correlation.


a Translation and strain of a line element
dX. b Two-dimensional deformation of a surface element
(unit square) including shear angle description. c Definition
of the coordinate systems. Modified according to [237] . . . . . . . 169
Fig. 5.31 Results of DIC in combination with optical images.
a Low-resolution DIC—strain field eyy obtained on a single
image of the whole area of interest taken at low magnification
(5 ). b High-resolution DIC—strain field of eyy with overlaid
grain boundary structure of the same AOI shown in (a).
However, here the reference images and images of deformed
states are stitched of 316 individual images of
31  magnification taken ex situ. Note that the subset size in
(b) is much smaller (14 µm) than the one used in (a) (89 µm),
which results in higher resolution fields with subgrain level
accuracy. Reproduced from [288]. Permission of Elsevier . . . . . 175
Fig. 5.32 High-resolution SEM-DIC on dual-phase steel DP800 at two
different average equivalent Von Mises strains. a Band
contrast map of EBSD measurement. b evM = 0.061.
c evM = 0.096. Reproduced from [296]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 179
Fig. 5.33 Schematic illustration of factors influencing the overall
detected IR at the thermo-camera. Modified according to
Infratec [312]. With courtesy of Infratec . . . . . . . . . . . . . . . . . . . 182
Fig. 5.34 Energy aspects of elasto-plastic material behaviour. Modified
according to [317]. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 186
Fig. 5.35 Example for the arrangement of in situ IR–TG measurements
during cyclic loading in the VHCF regime. a Thermo-camera
Vario hr (Infratec, Dresden, Germany) in combination with
ultrasonic fatigue testing machine. b Experimental setup for
full surface view thermography both schematical drawing and
real arrangement. c Three thermograms. L2 —real thermogram.
L1 , L3 —thermograms of the two mirrors. Reproduced from
[326] and [327]. Permission of Elsevier . . . . . . . . . . . . . . . . . . . 189
Fig. 5.36 Different experimental setups for fully-coupled full-field
measurements of kinematic and thermal field. a Two-face
measurement approach with CCD and TC viewing opposite
specimen sides. Reproduced from [336]. Permission of
Wiley VCH. b One-face measurement approach with CCD and
TC on the same area of interest using dichroic mirror for
separating visible and infrared radiation. c One-face
List of Figures xlix

measurement approach with co-planar arrangement of CCD


and TC. d One-face measurement approach with TC only.
b–d Modified according to [227, 203] and [340], respectively.
Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 192
Fig. 5.37 Mode of operation of dichroic mirror. a Radiation path k in
transmission k1 and reflection k2 . b Curve of reflection of
k2 . c Curve of transmission k1 . According to [341] . . . . . . . . . . 193
Fig. 5.38 Suitable patterning for fully-coupled DIC and IR–TG
measurements using two-camera setup for one-face
measurement. a Speckle pattern for DIC. b Same area imaged
by TC. c Greyscale distribution of speckle pattern for DIC.
According to [205]. Permission of Elsevier . . . . . . . . . . . . . . . . 193
Fig. 5.39 Suitable surface pattern for one-face, one-camera fully-coupled
measurements of strain and thermal fields—known as IRIC. IR
image of the specimen surface expressed in digital levels.
Modified and reproduced according to [340]. Permission of
Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 194
Fig. 5.40 One-face, one-camera IRIC measurement. a Experimental
setup for temperature calibration using large cooled
surrounding equipment and back-side reflection.
b Thermograms of the back-side reflection (left) and the front
side (right) of a NiTi-SMA specimen provided in digital levels.
Average temperature is about 53 °C. Reproduced from [340].
Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 195
Fig. 6.1 High-alloy CrMnNi steels. a Phase diagram of Fe–16Cr–7Mn–
xNi–0.05C steels with varying nickel content between 0 and
16 wt%. Modified according to [2]. With courtesy of S.
Martin. b Schaeffler diagram for the three basic steel variants:
Fe–16Cr–6Mn–3Ni–0.05C, Fe–16Cr–6Mn–6Ni–0.05C,
Fe–16Cr–6Mn–9Ni–0.05C . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 206
Fig. 6.2 Three different variants of martensitic phase transformation in
Fe–16Cr–6Mn–6Ni–0.05C steel. a Spontaneous martensite
upon cooling from 20 to −196 °C. b Stress-assisted martensite
during compression at −40 °C. c Strain-induced martensite
during compression at RT. Reproduced according to [2]. With
courtesy of S. Martin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 207
Fig. 6.3 As-cast microstructure of the three basic Fe–16Cr–6Mn–xNi–
0.05C steel variants. a Fe–6Cr–6Mn–3Ni–0.05C. b Fe–16Cr–
6Mn–6Ni–0.05C. c Fe–16Cr–6Mn–9Ni–0.05C . . . . . . . . . . . . . . 209
Fig. 6.4 Temperature dependence of tensile deformation behaviour of
Fe–16Cr–6Mn–6Ni–0.05C steel at a low strain rate of
e_ = 4  10−4 s−1. a Stress-strain curves. b Work hardening
curves. c Mechanical parameters: yield strength, ultimate
l List of Figures

tensile strength, uniform elongation and elongation to failure.


a, b Reproduced from [11]. Permission of Springer
(c) Reproduced from [25]. Permission of Trans Tech Publ . . . . . 214
Fig. 6.5 Temperature and strain rate dependence of the compressive
deformation behaviour of Fe–16Cr–6Mn–6Ni–0.05C steel at a
low strain rate of e_ = 4  10−4 s−1. a Stress-strain curve at
different temperatures. b Stress-strain curves at room
temperature and different strain rates. c Work hardening at RT
and different strain rates. Reproduced from [12]. Permission of
Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 214
Fig. 6.6 Comparison of the tensile deformation behaviour of the
investigated steel variants as a function of the chemical
composition, the deformation temperature and the strain rate.
a Fe–16Cr–6Mn–3Ni–0.05C TRIP steel. b Fe–16Cr–6Mn–
6Ni–0.05C TRIP/TWIP steel. c Fe–16Cr–6Mn–9Ni–0.05C
TWIP steel. a–c Tested at strain rate of 10−3 s−1. d Three Fe–
16Cr–6Mn–xNi–0.05C steel variants tested at RT and different
strain rates. In addition, the volume fractions of a′-martensite
determined by ferritescope measurements are indicated . . . . . . . 216
Fig. 6.7 Cyclic deformation behaviour of investigated steel variants and
evolution of a′-martensite volume fraction. a Fe–16Cr–6Mn–
3Ni–0.05C steel. b Fe–16Cr–6Mn–6Ni–0.05C steel.
c Fe–16Cr–6Mn–9Ni–0.05C steel. Reproduced from [13].
Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 218
Fig. 6.8 Influence of the austenite stability on the fatigue life of
Fe–16Cr–6Mn–xNi–0.05C cast TRIP/TWIP steels.
Reproduced from [13]. Permission of Wiley VCH . . . . . . . . . . . 219
Fig. 6.9 Results of investigations on the biaxial deformation behaviour
of cast Fe–16Cr–6Mn–6Ni–0.05C TRIP steel. a Equivalent
stress versus true equivalent plastic strain curve under biaxial
loading conditions with constant load ratio resulting in biaxial
tension, biaxial compression and biaxial shear in comparison
with uniaxial tensile test. b Evolution of martensitic volume
fraction corresponding to the stress-strain curves shown in (a).
c Results of the biaxial in-phase and out-of-phase cyclic
loading experiments in comparison with results of uniaxial
cyclic deformation. Von Mises equivalent strain versus
number of cycles to failure curve. a, b Reproduced from [29].
c Reproduced from [14]. Permission of Elsevier . . . . . . . . . . . . . 220
Fig. 6.10 Evolution of deformation bands in dependence on the applied
plastic strain observed during in situ tensile test of Fe–16Cr–
List of Figures li

6Mn–6Ni–0.05C steel at RT. a Initial state e = 0%.


b e = 0.9%. c e = 2.8%. d e = 9.8%. SEM micrograph taken in
BSE contrast. Large-angle grain boundaries are indicated by
black lines and activated slip systems by dashed white lines.
1—primary slip system, 2—secondary slip system. Loading
axis horizontal. According to [30] . . . . . . . . . . . . . . . . . . . . . . . 222
Fig. 6.11 Evolution of deformation bands in dependence on the applied
number of cycles N at a total strain amplitude of
ea;t = 5  10−3 observed during in situ cyclic loading test of
Fe–16Cr–6Mn–6Ni–0.05C steel at RT. a First cycle. b 30
cycles. c 50 cycles. d 100 cycles. SEM micrograph taken in
BSE contrast. AOI within one individual grain of the as-cast
microstructure. Loading axis horizontal. Reproduced from
[31]. Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . 222
Fig. 6.12 Individual deformation bands with lentil-like areas (black
arrows) related to a′-martensite. SEM micrographs taken in
BSE contrast. a Fe–16Cr–6Mn–6Ni–0.05C steel after tensile
loading at RT up to e = 8%. b Fe–16Cr–6Mn–6Ni–0.05C steel
after cyclic loading at RT with a total strain amplitude of
ea;t = 5  10−3. White arrows indicate deformation bands on
the secondary slip system, which are less pronounced. Loading
axis horizontal. Reproduced from [31]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 223
Fig. 6.13 Examples for pronounced surface profile caused by formation
of deformation bands along different slip systems and
a′-martensite (marked by arrows). SEM micrographs taken in
SE contrast). a–c Different grains within specimen of
Fe–16Cr–6Mn–6Ni–0.05C steel cyclically deformed with total
strain amplitude of ea;t = 5  10−3 up to 100 cycles.
Reproduced from [31]. Permission of Elsevier . . . . . . . . . . . . . . 223
Fig. 6.14 Appearance of deformation bands in the austenitic matrix
exhibiting hex crystal lattice and containing a′-martensite
nuclei after cyclic loading of Fe–16Cr–6Mn–6Ni–0.05C steel
at RT with total strain amplitude of ea;t = 5  10−3 up to 100
cycles. Results obtained by EBSD measurements. a Phase
map, b Orientation map. c Orientation map bcc phase with
band contrast and indicated characteristic misorientation of
a′-martensite nuclei (red, yellow lines) and Kurdjumov–Sachs
phase orientation relationship (white lines). d Orientation map
hex with band contrast and phase orientation relationships
fcc/hex (white lines) phase and hex/bcc (yellow lines).
Orientation map in inverse pole figure colouring according
to the loading axis. Loading axis horizontal. Reproduced from
[31]. Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . 224
lii List of Figures

Fig. 6.15 Evolution of strain-induced martensitic phase transformation


obtained under tensile loading of Fe–16Cr–6Mn–6Ni–0.05C
steel at RT up to 10% of elongation and at failure (e = 60%).
a, c Phase maps. b, d Band contrast map. Red lines: Twin
boundaries (R3). White arrows indicating d-ferrite. Loading
axis horizontal. a, b Reproduced from [39]. c, d Reproduced
from [40]. Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . 226
Fig. 6.16 Evolution of deformation bands in dependence on the number
of cycles during fatigue loading of Fe–16Cr–6Mn–6Ni–0.05C
steel at RT with a total strain amplitude of ea;t = 3  10−3.
Results of EBSD measurements. Phase maps with grey as
austenite, yellow as e-martensite and blue of a′-martensite and
d-ferrite. a After N1 = 250 cycles. b After N2 = 500 cycles.
Loading axis horizontal. Reproduced from [38]. Permission of
Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 227
Fig. 6.17 Influence of temperature on the evolution of the strain-induced
martensitic phase transformation. Results of EBSD
measurements obtained after tensile loading of Fe–16Cr–6Mn–
6Ni–0.05C steel at 100 °C at 10% of elongation (a, b) and at
elongation to failure (e = 33%) (c, d). a, c Phase maps.
b, d Band contrast maps with indicated twin boundaries
(red lines). a, b Reproduced from [39]. c, d Reproduced
from [40]. Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . 228
Fig. 6.18 Dendritic structure of the as-cast microstructure with opposed
segregation of the elements Ni and Cr of Fe–16Cr–6Mn–6Ni–
0.05C steel. Results of combined EBSD/EDS measurements.
a, e Crystallographic orientation maps. b, f Band contrast maps
with indicated large-angle boundaries. c, g EDS element maps
of nickel and d chromium. e–g Enlarged region marked by
rectangle in (a) with indicated grain 1. Arrows in (g) indicate
regions with enhanced nickel enrichment in grain part 1a . . . . . 229
Fig. 6.19 Two examples of results obtained by post-mortem EBSD
measurements on specimen of Fe–16Cr–6Mn–6Ni–0.05C steel
after quasi-hydrostatic, high-pressure experiment up to 18
GPa. a–f Larger overview on several austenitic mother grains.
g–l Enlarged view at higher magnification within one
individual austenitic mother grain. a, g SEM images using
BSE contrast. b, h Phase maps. c, i Crystallographic
orientation map of fcc phase. d, j Crystallographic orientation
maps of hexagonal phases. e, f, k, l Crystallographic
orientation maps of bcc phase. e, k Colour code of the inverse
pole figure with respect to the normal direction. f, l Colour
code of the inverse pole figure with respect to the transverse
direction. Reproduced from [15]. Permission of Springer . . . . . . 231
List of Figures liii

Fig. 6.20 Schematic summary of the characteristic phase transformation


processes as a function of hydrostatic pressure in combination
with EBSD maps (red: austenite, yellow: hexagonal (e1 , e2 )
and blue: martensite (a01 , a02 ). Open red squares—compression
path. Open black squares—decompression bath. At 14 GPa
during decompression a blow-out occurred terminating the
test. Reproduced from [15]. Permission of Springer . . . . . . . . . . 232
Fig. 6.21 Appearance of individual stacking-faults after plastic
deformation of Fe–16Cr–6Mn–6Ni–0.05C steel in the
austenitic steel matrix concurrently to deformation bands on
primary and secondary slip systems. a After tensile
deformation. b After cyclic deformation. c Onset of the
formation of an individual deformation bands with individual
SF on different slip planes. In addition, individual regular
dislocations are visible (black arrows). d SF on at least three
different slip planes with intersection points, which are
favoured places for the formation of martensite nuclei.
a, b Reproduced from [20]. c Reproduced from [26].
d Reproduced from [47]. Permission of Elsevier and
Taylor&Francis, respectively. . . . . . . . . . . . . . . . . . . . . . . . . . . . 234
Fig. 6.22 Arrangement of stacking-faults in tensile deformed Fe–16Cr–
6Mn–6Ni–0.05C steel obtained on electron transparent foils.
a Bright field image of conventional TEM showing
deformation band consisting of several overlapping
stacking-faults (marked by white lines) and individual
stacking-faults with small width (marked by white arrows).
b, c t-SEM images showing individual stacking-faults on two
different slip systems. d Bright field images of t-SEM showing
reaction between stacking-faults on different slip planes
forming Lomer-Cottrell locks. a Reproduced from [50].
b–d Reproduced from [39]. Permission of Elsevier . . . . . . . . . . 235
Fig. 6.23 Microstructure of Fe–16Cr–6Mn–6Ni–0.05C steel deformed
cyclically at ea;t = 5  10−3 up to two different number of
cycles N1 = 250 (a) and N2 = 500 cycles (b). a, b EBSD phase
maps. c, d inverted ECCI micrographs. a, b Band contrast
image with overlapped phase identification; yellow…hex,
blue… bcc (a′-phase), rest fcc (c-phase), black…zero
solutions. c, d Arrangement of stacking-faults within the same
individual grain as shown in (a, b). Reproduced from [31].
Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 236
Fig. 6.24 Influence of temperature on the microstructure of Fe–16Cr–
6Mn–6Ni–0.05C steel deformed in tension up to 10% of
elongation. a, b Results of EBSD measurements after
deformation at RT. c, d Results of EBSD measurements after
liv List of Figures

deformation at 100 °C. a, c Crystallographic orientation maps


in inverse pole figure colouring according to the loading axis
of the hex stacking-fault areas. b, d Crystallographic
orientation maps of austenite exhibiting twin orientations
inside deformation bands (marked by white arrows). Loading
axis horizontal. Reproduced from [47]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 237
Fig. 6.25 Results of high-resolution transmission electron microscopy
investigations on Fe–16Cr–6Mn–6Ni–0.05C steel after
deformation up to 5% compression strain. a HRTEM image
together with corresponding fast Fourier transformation
(FFT) patterns of characteristic areas consisting of the
e-martensite (hex) and nanotwins (tw) with fcc crystal lattice in
the closest vicinity on the atomic scale within the thin
individual deformation band. Reproduced from [6]. Permission
of Wiley VCH. b SAED pattern taken on a deformation band
in Fe–16Cr–6Mn–9Ni–0.05C specimen after deformation in
compression up to 25%. Diffraction spots assigned to austenite
(black), twinned austenite (red) and e-martensite (hex) are
indicated. Reproduced from [53]. Permission of Elsevier . . . . . . 238
Fig. 6.26 Mechanical twinning occurring during tensile deformation of
Fe–16Cr–6Mn–9Ni–0.05C steel up to elongation of failure.
Results of EBSD measurements. a–c After deformation at RT,
e = 70%. d–e After deformation at 100 °C, e = 55%.
a, d Band contrast maps with indicated twin boundaries (red
lines). b, e Orientation maps with inverse pole figure colouring
according to the loading axis. c, f Kernel average
misorientation maps with maximum misorientation angle
of 5° between the nearest 8 neighbours of each individual
measuring point. Loading axis horizontal. Reproduced from
[40]. Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . 239
Fig. 6.27 Evolution and thickening of microtwins with increasing
applied strain for Fe–16Cr–6Mn–9Ni–0.05C steel during
tensile test at RT. a e = 2.5%. b e = 3.75%. c e = 5.0%.
d e = 7.5%. e e = 8.75%. f e = 10%. Secondary electron
contrast. Loading axis horizontal . . . . . . . . . . . . . . . . . . . . . . . . 240
Fig. 6.28 Twin formation during tensile deformation of Fe–16Cr–6Mn–
9Ni–0.05C steel at RT at different strain levels. Results of
in situ EBSD measurements. Overlay of band contrast map and
crystallographic orientation map in combination with inverse
pole figure with respect to loading axis resembling both twin
orientation and change of the crystallographic orientation
of the austenitic grain due to tensile deformation . . . . . . . . . . . . 241
List of Figures lv

Fig. 6.29 Strain-induced martensitic phase transformation of Fe–16Cr–


6Mn–3Ni–0.05C steel during tensile deformation up to 10% of
elongation. a, b After deformation at RT. c, d After
deformation at 100 °C. Results of EBSD measurements in
terms of phase maps. a, c Initial state. b, d 10% of elongation.
Modified according to [30] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 242
Fig. 6.30 Strain-induced martensitic phase transformation of Fe–16Cr–
6Mn–3Ni–0.05C steel during tensile deformation up to
elongation of failure. a, c After deformation at RT (e = 33%).
d–f After deformation at 100 °C (e = 45%). Results of EBSD
measurements. a, d SEM micrographs in BSE contrast.
b, e Phase maps. Red—austenite, yellow—e-martensite, blue
—a′-martensite + d-ferrite. c, f Orientation maps of the bcc
phases in inverse pole figure colouring according to the
loading axis. Reproduced from [40]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 243
Fig. 7.1 Deformation-induced microstructure of high-alloy Fe–16Cr–
6Mn–6Ni–0.05C cast steel facilitating TRIP effect. Complex
microstructure consisting of a deformed austenitic matrix with
individual dislocations and short SF, deformation bands
formed by the high density of SFs and, locally, microtwinning
(red line) as well as a′-martensite grains with dimensions
 1 µm. Reproduced from [18]. Permission of Springer . . . . . . 246
Fig. 7.2 Schematic overview of applied methods of characterization
and in situ techniques in combination with general information
obtained for the comprehensive description of the deformation
behaviour of Fe–16Cr–6Mn–xNi–0.05C TRIP/TWIP steels.
a Schematic stress-strain curves of steels with TRIP and TWIP
effects in comparison with steel without these effects.
b, c Stress-strain curves of Fe–16Cr–6Mn–xNi–0.05C steels
obtained from tensile tests representing the influence of
chemical composition and strain rate (b) as well as of
deformation temperature on the mechanical properties (c).
d Phase composition determined by EBSD measurements.
e, f Microstructure and defect arrangements obtained by the
electron channelling contrast imaging (ECCI) technique on
bulk specimens (e) and using transmission electron detector in
the SEM (t-SEM) on an electron transparent foil (f).
g Calculated magnitude of shear of individual microstructural
constituents based on combined DIC and EBSD
measurements. h Load–displacement curves of individual
microstructural constituents obtained by in situ
nano-indentation inside SEM. i Kinetic of the martensitic
lvi List of Figures

phase transformation obtained from AE measurements during


tensile testing at room temperature. j Kinetics of all
deformation mechanisms occurring in Fe–16Cr–6Mn–xNi–
0.05C TRIP steels. Reproduced from [18]. Permission
of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 248
Fig. 7.3 In situ tensile and cyclic loading experiments in SEM.
a Specimen geometry. b Stress-strain curve of quasi in situ
tensile test at room temperature. c Stress-strain hysteresis loops
of quasi in situ cyclic loading with a total strain amplitude of
ea;t = 4  10−3 up to 1450 cycles . . . . . . . . . . . . . . . . . . . . . . . . 249
Fig. 7.4 View inside the SEM chamber (Mira3 XMU, Tescan, Brno,
Czech Republic) with tension/compression module (Kammrath
and Weiss, Dortmund, Germany) mounted on the SEM motor
stage. a Total view of the loading stage inside the SEM in
combination with heating and cooling system. b Detailed view
on a deformed specimen with mounted heating device on the
rear of the specimen. c Position of the tension/compression
module for in situ testing in combination
with BSE detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 250
Fig. 7.5 Surface contrast obtained by deposition of Pt nanoparticles on
the vibration-polished specimen surface of a Fe–16Cr–6Mn–
6Ni–0.05C steel. a Initial state before tensile loading. b Same
AOI at a maximum elongation of e = 2.3%. c Result of digital
image correlation in terms of Von Mises equivalent strain
at e = 2.3% . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 252
Fig. 7.6 Examples of etched specimen surfaces for high-resolution
digital image correlation. a Fe–16Cr–6Mn–3Ni–0.05C steel.
b Fe–16Cr–6Mn–6Ni–0.05C steel. c Fe–16Cr–6Mn–9Ni–
0.05C steel. Etch pits are different depending on the specific
grain orientation. a, c Etched after vibration polishing.
b Etched without vibration polishing. Scratches
are visible . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 253
Fig. 7.7 Two-dimensional cross-correlation field CZNCCmax for the quasi
in situ tensile test performed on Fe–16Cr–6Mn–6Ni–0.05C
steel at room temperature up to a maximum elongation
of e = 15%. a SEM image in SE contrast showing the etched
surface in the initial state. b Cross-correlation coefficient
of the DIC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 254
Fig. 7.8 Sequence of six consecutive strain intervals of an in situ
deformation experiment in tension at RT for Fe–16Cr–6Mn–
6Ni–0.05C steel. A comparison of the SEM micrographs
(SE contrast) and the calculated strain fields evM is shown.
Macroscopic strain level is provided in the SEM micrographs.
List of Figures lvii

Loading axis horizontal. Grain orientation with respect to the


loading axis is indicated in the SST in (f) . . . . . . . . . . . . . . . . . 255
Fig. 7.9 Local strain fields and EBSD measurements of Fe–16Cr–
6Mn–6Ni–0.05C steel deformed in tension at RT up to a total
elongation of 15%. a Local strain calculated at 15% of
elongation provided in Von Mises equivalent strain. b Phase
map. c Crystallographic orientation map in inverse pole figure
colouring with respect to the normal direction (ND). Red lines
—twin boundary austenite. Loading axis horizontal.
Reproduced from [22]. Permission of Elsevier . . . . . . . . . . . . . . 256
Fig. 7.10 Evolution of the normal strain exx up to e = 5.30% during
tensile deformation of Fe–16Cr–6Mn–6Ni–0.05C steel at RT.
The black small arrows indicate the direction of the minor
strain. Loading axis horizontal . . . . . . . . . . . . . . . . . . . . . . . . . . 257
Fig. 7.11 Evolution of the minor strain e2 up to an applied strain of
e ¼ 12:2% during tensile deformation of Fe–16Cr–6Mn–6Ni–
0.05C steel at RT. The small black arrows indicate the
direction of the major strain e1 . Black arrows indicate areas
with negative minor strain. Loading axis horizontal . . . . . . . . . . 258
Fig. 7.12 Evolution of the shear strain exy up to an applied strain of
e ¼ 12:2% during tensile deformation of Fe–16Cr–6Mn–6Ni–
0.05C steel at RT. White arrows indicate areas with increased
shear strain, the same areas that exhibit negative minor strain
(cf. Fig. 7.11). Loading axis horizontal . . . . . . . . . . . . . . . . . . . . 259
Fig. 7.13 Local strain fields at an applied strain of e ¼ 12:2% tensile
deformation of Fe–16Cr–6Mn–6Ni–0.05C steel at RT in
combination with crystallographic orientation. a Normal strain
exx . b Minor strain e2 . c Shear strain exy . d Crystallographic
orientation map in inverse pole figure colouring according to
loading axis. Loading axis horizontal. Reproduced from [22].
Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 260
Fig. 7.14 Local strain fields obtained during tensile deformation of Fe–
16Cr–6Mn–6Ni–0.05C steel at RT. a Normal strain in the x-
direction exx . b Normal strain in the y-direction eyy . c Shear
strain exy . d Von Mises equivalent strain evM . Applied strain
e ¼ 18%. Loading axis horizontal. Grain corresponds to grain
1a shown in Sect. 6.4 by Fig. 6.18 . . . . . . . . . . . . . . . . . . . . . . . 260
Fig. 7.15 Results of EBSD measurement on AOI shown in Fig. 6.13 for
Fe–16Cr–6Mn–6Ni–0.05C steel tensile deformed at RT.
Applied strain e = 18%. a Band contrast map. b,
e Crystallographic orientation of austenite and a′-martensite,
respectively. Inverse pole figure colouring with respect to the
loading axis. c, f Kernel average misorientation of austenite
lviii List of Figures

and a′-martensite, respectively. Maximum misorientation


angle is 5°. d Phase map. Loading axis horizontal. Grain
corresponds to grain 1a shown in Sect. 6.4 by Fig. 6.18 . . . . . . 261
Fig. 7.16 Comparison of the evolution of strain localization within
deformation bands in coarse austenitic grain (a) and smaller
austenitic grain (b) for four different applied strain values
(provided in images) during tensile deformation of Fe–16Cr–
6Mn–6Ni–0.05C steel at RT. c, d Evolution of exx over
deformation process followed along the indicated measuring
line in (a) and (b), respectively. Grain shown in (b) and
(d) corresponds to grain 1a shown in Sect. 6.4 by Fig. 6.18 . . . 263
Fig. 7.17 SEM images in secondary electron contrast taken during quasi
in situ tensile tests at 100 °C on Fe–16Cr–6Mn–6Ni–0.05C
steel at an elongation of 6% (a) and 15% (b), respectively.
Inclination angles of slip lines with loading axis are indicated.
Loading axis horizontal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 263
Fig. 7.18 Local strain fields in terms of Von Mises equivalent strains evM
calculated from quasi in situ tensile test of Fe–16Cr–6Mn–
6Ni–0.05C steel at 100 °C. a e = 3%, b e = 6%, c e = 9%
and d e = 15% . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 264
Fig. 7.19 Results of EBSD measurements on AOI shown in Fig. 7.18
obtained after tensile test at 100 °C up to 15% of elongation.
a Band contrast map with indicated twin boundaries (red).
b Phase map with austenite (red) and e-martensite (yellow).
c Crystallographic orientation map in inverse pole figure
colouring with respect to the loading axis. d Kernel average
misorientation map (maximum misorientation angle 5°).
Loading axis horizontal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 265
Fig. 7.20 Results of digital image correlation obtained on SEM
micrographs taken in secondary electron contrast on Fe–16Cr–
6Mn–9Ni–0.05C steel during in situ tensile test at RT. a e =
1%. b e = 3%. c e = 5%. d e = 8%. e e = 15%. Left: Von Mises
equivalent strain evM . Middle: Minor strain e2 . Right: Shear
angle cxy . Loading axis horizontal . . . . . . . . . . . . . . . . . . . . . . . . 267
Fig. 7.21 Results of the determination of local strain fields and EBSD
measurements of Fe–16Cr–6Mn–9Ni–0.05C steel tensile
strained at RT up to total elongation of 15%. a Von Mises
equivalent strain evM . b Band contrast map with indicated twin
boundaries (red lines). c Kernel average misorientation KAM.
d–f Crystallographic orientation in IPF colouring for normal
direction (d), loading axis (e) and transverse direction (f). . . . . . 268
List of Figures lix

Fig. 7.22 Results of the determination of local strain fields and EBSD
measurements of Fe–16Cr–6Mn–9Ni–0.05C steel deformed in
tension at 200 °C up to total elongation of 15%. a, b Von
Mises equivalent strain at e = 2% (a) and e = 15% (b). c Band
contrast map of EBSD measurement at e = 15%. Loading axis
horizontal. d Calculated magnitude of shear at e = 15% . . . . . . . 269
Fig. 7.23 Results of the determination of local strain fields and EBSD
measurements of Fe–16Cr–6Mn–3Ni–0.05C steel tensile
strained at RT up to total elongation of 15% in combination
with results of EBSD measurements. a, b Evolution of local
strain fields at two different applied strain levels during tensile
deformation in terms of Von Mises equivalent strain evM .
c Calculated magnitude of shear after 12% global strain.
d ECCI micrograph of the AOI after re-polishing. e Band
contrast map with highlighted phase distribution (austenitic
phase (fcc)—grey; deformation bands (hex crystal lattice)—
yellow; a′-martensite and d-ferrite (bcc)—blue).
f Crystallographic orientation map of the bcc phase in the
inverse pole figure colouring code according to the loading
direction. Loading axis horizontal . . . . . . . . . . . . . . . . . . . . . . . . 271
Fig. 7.24 Results of the determination of local strain fields and EBSD
measurements of Fe–16Cr–6Mn–3Ni–0.05C steel tensile
strained at 100 °C up to total elongation of 15%. a,
b Evolution of local strain fields at two different applied strain
levels during tensile deformation in terms of Von Mises
equivalent strain evM . c Band contrast map with highlighted
phase distribution (austenitic phase (fcc)—grey; deformation
bands (hex)—yellow; a′-martensite (bcc)—blue) at a global
strain of 15%. d Calculated magnitude of shear after 15%
global strain. Loading axis horizontal . . . . . . . . . . . . . . . . . . . . . 272
Fig. 7.25 Illustration of the activated slip systems of the austenitic grain
under investigation using digital image correlation. a EBSD
band contrast map showing deformation bands parallel to
primary slip plane ð111Þ: b ECC image of the marked area in
(a) at higher magnification with indication of all four f111g
slip planes activated at an applied strain of 15%. c Part of the
Thompson tetrahedron related to slip planes ð111Þ and ð 111Þ:
The cutting edge of ð111Þ and ð111Þ slip planes is the ½0 11
direction. Trace angle of this direction on the specimen surface
is inclined of 107° to the loading axis. Loading axis
horizontal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 274
Fig. 7.26 Different martensite variants occurring in deformation bands in
Fe–16Cr–6Mn–6Ni–0.05C after tensile deformation at RT
lx List of Figures

(cf. Fig. 7.10). a Crystallographic orientation map of the


austenitic matrix, deformation bands with stacking faults and
a′-martensite grains inside deformation bands. b Stereographic
standard triangle reflecting the orientation of the austenite
(c) and the three major a′-martensite variants (a0i , a0ii and a0iii )
with respect to the normal direction . . . . . . . . . . . . . . . . . . . . . . 275
Fig. 7.27 Stereographic projection of the slip plane normal (triangle) and
slip directions (circles) of activated slip systems of austenite
and a′-martensite variants a0i , a0ii and a0iii . Filled circles—regular
dislocations. Open circles—partial dislocations. Red—primary
slip system. Blue secondary slip system. x; y; z—specimen
coordinate system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 276
Fig. 7.28 Influence of the crystallographic orientation of a′-martensite on
the calculated magnitude of shear at 15% applied global strain.
a Shear angle cxy determined by DIC. b Crystallographic
orientation map. c Calculated magnitude of shear s½011 .
Loading axis horizontal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 277
Fig. 7.29 Magnitude of shear for twins formed in Fe–16Cr–6Mn–9Ni–
0.05C TWIP steel deformed in tension at RT (cf. Fig. 7.21).
a Traces of the three possible slip planes (black lines) and the
projections of the slip directions of the corresponding partial
dislocations (red lines) on the specimen surface. Primary SS—
bold lines, secondary SS—dashed lines, third SS—dash-dot
lines. b Crystallographic orientation map of the AOI in IPF
colouring with respect to the loading axis. The twin system is
indicated, and 6 twin bundles are labelled. c Magnitude of
shear calculated in the twin shear direction ½1 21 . . . . . . . . . . . . 279
Fig. 7.30 Magnitude of shear for twins formed in Fe–16Cr–6Mn–9Ni–
0.05C TWIP steel deformed in tension at RT (cf. Fig. 7.19).
a Traces of the three possible slip planes (black lines) and the
projection of the slip directions of the corresponding partial
dislocations (red lines) on the specimen surface. Primary SS—
bold lines, secondary SS—dashed lines, third SS—dash-dot
lines. b Crystallographic orientation of the AOI in IPF
colouring with respect to the normal direction. The activated
twinning system is indicated. c Magnitude of shear calculated
in the twinning shear direction ½211. . . . . . . . . . . . . . . . . . . . . . 280
Fig. 7.31 Mechanical stress-strain hysteresis loops for in situ cyclic
loading of a Fe–16Cr–6Mn–6Ni–0.05C TRIP steel at RT and a
total strain amplitude of ea;t ¼ 4  103 for selected number of
cycles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 281
List of Figures lxi

Fig. 7.32 Etched specimen surface of Fe–16Cr–6Mn–6Ni–0.05C TRIP


steel during cyclic loading at ea;t = 4  10−3 at RT at different
cycles. SEM images taken in SE contrast at F = 0 N after
unloading from maximum tensile load (cf. Fig. 7.29). a Initial
state. b N = 100 cycles. c N = 400 cycles. d N = 800 cycles.
Loading axis horizontal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 282
Fig. 7.33 Evolution of the displacement fields and the calculated strain
fields of the in situ cyclic loading experiment shown in
Fig. 7.29 for different cycles (N = 100, N = 400, N = 850,
N = 1450). From left to the right: SEM image of the specimen
surface. Equivalent Von Mises strain evM . Normal strain exx .
Normal strain eyy . Shear strain exy . Formation of deformation
bands (white dashed lines) along the primary SS and changes
on the specimen surface caused by MPT (red rectangles) are
indicated in the SEM images . . . . . . . . . . . . . . . . . . . . . . . . . . . 283
Fig. 7.34 Results of the EBSD measurements of the AOI of the DIC
calculations (see Fig. 7.33) on a Fe–16Cr–6Mn–6Ni–0.05C
steel specimen after cyclic loading at RT with a total strain
amplitude of ea;t = 4  10−3 up to 1450 numbers of cycles.
a Phase map with indicated orientation of the austenitic mother
grain (loading axis). Red—austenite, yellow—hex crystal
lattice, blue—a′-martensite. b Band contrast map.
c, d Crystallographic orientation map of the a′-martensite and
hex crystal lattice, respectively. Colour code with respect to the
loading direction, which lies horizontal. e Region of
a′-martensite grains at higher magnification where it becomes
obvious that the macro deformation band is composed of
several very thin individual bands (see white arrows) with a
thickness <1 µm (500–750 nm) . . . . . . . . . . . . . . . . . . . . . . . . . 284
Fig. 7.35 Crystallographic orientation of a′-martensite variants formed
during cyclic loading. a Stereographic projection of the slip
plane normal (bars) and slip directions (circles) of the primary
(red) and secondary (blue) slip system in combination with the
trace angles of the slip planes (black lines) and slip directions
(blue lines) on the specimen surface. Red lines correspond to
the projections of the slip directions of the Shockley partial
dislocations. Dotted blue line corresponds to the cutting edge
with a direction of ½011 of the two slip planes (cf. Fig. 7.25c).
b–d Variants of a′-martensite formed within deformation
bands using different IPF colour code maps: loading axis
(b), normal direction (c) and transverse direction (d). Loading
axis horizontal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 286
Fig. 7.36 Combination of results of DIC calculations with results of
EBSD measurements for N = 400. From left to right: normal
lxii List of Figures

strain exx , normal strain eyy , shear strain exy , equivalent Von
Mises strain evM . Middle row: Deformation bands with hex
crystal lattice. Bottom row: Crystallographic orientation of hex
crystal lattice together with orientation of a′-martensite
grains . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 289
Fig. 7.37 Combination of results of DIC calculations with results of
EBSD measurements for N = 1450. From left to right: normal
strain exx , normal strain eyy , shear strain exy , equivalent Von
Mises strain evM . Middle row: Deformation bands with hex
crystal lattice. Bottom row: Crystallographic orientation of hex
crystal lattice together with orientation of a′-martensite
grains . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 290
Fig. 7.38 Stereographic standard triangle containing the crystallographic
orientations of the theoretical possible 24 a′-martensite
variants (a) and the experimentally observed orientations
(c) shown in the IPF colouring mode (loading axis) displayed
in (b). Red cross indicates the orientation of the austenitic
mother grain . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 293
Fig. 7.39 Crystallographic orientations of all grains labelled in Fig. 7.35
and listed in Table 7.7 using the SST both with respect to the
loading axis and with respect to the surface normal direction in
comparison with the calculated theoretical 24 martensite
variants. In addition, IPF colour map of loading axis
is displayed . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 293
Fig. 7.40 Pole figure representation for both the austenitic mother grain
and the cyclic strain-induced a′-martensite formed within
deformation bands. The colouring corresponds to the IPF
colour code with respect to the loading axis x . . . . . . . . . . . . . . 294
Fig. 7.41 a′-martensite formed during cyclic loading of Fe–16Cr–6Mn–
6Ni–0.05C steel at RT within deformation band. a Labelling of
martensite grains. b Twin boundaries between different
martensite types: R3 (white lines) and R11 (green lines) . . . . . . 295
Fig. 7.42 Habit planes and long directions of a′-martensite variants in
combination with invariant shear directions of austenite and
corresponding shear directions of martensite. a Band contrast
map of area with a′-martensite grains. b Traces of habit planes
(black) and projections of long directions (blue) and invariant
shear directions of austenite (red). c Correlation of invariant
shear systems austenite/shear systems martensite with respect
to the martensite variants V1–V6. d Visualization of the
arrangements of slip systems for individual variants V1–V6
List of Figures lxiii

belonging to IPF colour types T1–T6. Traces of slip planes are


given by bold black lines and projection of slip directions by
dashed black lines. Note for V2 and V5 double slip
is indicated . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 302
Fig. 7.43 Interpretation of local strain fields obtained from DIC for
different individual arrangements/combinations of
a′-martensite grains (a–d). IPF colour code with grain labelling
is shown together with the specific alignment of invariant shear
systems for each grain. The specific grain orientations and
a′-martensite variants are indicated in the SST. Furthermore,
the strain tensor components exx , eyy , exy are shown with
indicated specific alignments of slip systems and invariant
shear systems. The colour code of the strain maps is simplified
as follows: green—zero values, red—maximum positive
values, blue—maximum negative values. . . . . . . . . . . . . . . . . . . 304
Fig. 7.44 Normal strain fields exx at different numbers of cycles
(N = 400, 850, 1100 and 1450) in combination with the
arrangement of slip traces and the projections of slip directions
of partial dislocations. Differences between tension and
compression are indicated by T and C, respectively . . . . . . . . . . 306
Fig. 7.45 Resolution of SEM-DIC obtained in the present work. a Etch
pit surface contrast pattern used for SEM-DIC with a FOV 51
 38 µm2, the subset size of 30  30 pixels2 and 10 pixels
distance of measuring points exemplarily shown for a
reference image. b Same FOV after 15% tensile deformation at
200 °C of a Fe–16Cr–6Mn–9Ni–0.05C TWIP steel.
Obviously, identical features in (a) and (b) are marked by
white arrows . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 308
Fig. 7.46 Strain error fields from drift distortion achieved at maximum
load of a tensile test on aluminium alloy used for SEM-DIC.
a exx . b eyy . c exy . Reproduced from [30]. Permission
of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 309
Fig. 7.47 Comparison of the shear strain fields for Fe–16Cr–6Mn–6Ni–
0.05C steel (a, c, d) and Fe–16Cr–6Mn–9Ni–0.05C steel
(b) with different lengths of deformation bands after tensile
loading (a–c) and cyclic loading (d). a Single-ended stacking
fault bands; L = 140 µm. b Single-ended twin bundles; L = 70
µm. c Double-ended stacking fault bands; L = 30 µm.
d Single-ended stacking fault bands; L = 50 µm . . . . . . . . . . . . 312
Fig. 7.48 Experimental setup for in situ AE measurements during tensile
deformation at RT and elevated temperatures. a Geometry of
flat tensile specimens and AE sensor location. b Specimen
mounted for RT experiments on the electromechanical testing
lxiv List of Figures

device of Hegewald & Peschke. c Specimen mounted for


tensile deformation at elevated temperature on the
electromechanical testing device of Zwick in combination
with climate chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 314
Fig. 7.49 Threshold-less and continuously recorded AE data stream.
a AE data stream (green) synchronized with the stress–time
curve (black) for Fe–16Cr–6Mn–3Ni–0.05C steel tested
in tension at room temperature and at a strain rate
of 1  10−2 s−1. b Detail of the marked area in the AE
time-series in (a) showing a very intensive flux of AE bursts
of different amplitudes. Reproduced from [33]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 315
Fig. 7.50 AE data streams (green) synchronized with the stress–time
curves (black) obtained during tensile testing at room
temperature and at a strain rate of 1  10−2 s−1 of the three
investigated high-alloy TRIP/TWIP steels: a Fe–16Cr–6Mn–
9Ni–0.05C, b Fe–16Cr–6Mn–6Ni–0.05C and c Fe–16Cr–
6Mn–3Ni–0.05C. Reproduced from [33]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 316
Fig. 7.51 Time sequence of the parameters AE energy E and median
frequency fm derived from the power spectral density function
obtained by fast Fourier transformation of the AE data in
combination with the stress-strain curves; a 9 wt% nickel, b 6
wt% nickel and c 3 wt% nickel. Room temperature and strain
rate 1  10−2 s−1. Reproduced from [33]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 318
Fig. 7.52 Different types of average normalized power spectral density
functions of AE signals derived from fast Fourier
transformation of AE data streams collected during tensile
testing of Fe–16Cr–6Mn–9Ni–0.05C steel (a), Fe–16Cr–6Mn–
6Ni–0.05C steel (b) and Fe–16Cr–6Mn–3Ni–0.05C steel (c) at
room temperature and at a strain rate of 1  10−2 s−1.
Reproduced from [33]. Permission of Elsevier . . . . . . . . . . . . . . 320
Fig. 7.53 Results of the AE cluster analysis in terms of energy E and
median frequency fm coordinates based on the different types
of PSDFs identified by FFT for Fe–16Cr–6Mn–9Ni–0.05C
steel (a, b), Fe–16Cr–6Mn–6Ni–0.05C steel (c) and Fe–16Cr–
6Mn–3Ni–0.05C steel (d), respectively. b Enlarged detail of
(a). Reproduced from [33]. Permission of Elsevier . . . . . . . . . . . 321
Fig. 7.54 Schematic representation of temporal evolution of cumulated
number of elements (a) and cumulated energy (b) for each
cluster identified by cluster analysis shown in Figs. 7.52 and
7.53, which can be correlated with different sources of AE
associated with different deformation mechanisms . . . . . . . . . . . 323
List of Figures lxv

Fig. 7.55 Time sequence of AE clusters evaluated for Fe–16Cr–6Mn–


9Ni–0.05C steel and correlated with different deformation
mechanisms—dislocation glide and mechanical twinning—
shown in combination with the stress-strain curve obtained
during tensile test a room temperature. a Cumulated AE
energy. b Number of elements per cluster. Reproduced
from [33]. Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . 324
Fig. 7.56 Microstructure of Fe–16Cr–6Mn–9Ni–0.05C steel after tensile
test to strain to failure at e = 42% at room temperature. a SEM
micrograph in BSE contrast. b–d Results of EBSD mapping of
an area of interest marked in (a). b Band contrast map with
indicated R3 twin boundaries (red). c Orientation map in
inverse pole figure colouring with respect to the surface normal
direction. f Kernel average misorientation. Loading axis
horizontal. Reproduced from [33]. Permission of Elsevier . . . . . 325
Fig. 7.57 Time sequence of AE clusters evaluated for Fe–16Cr–6Mn–
6Ni–0.05C steel and correlated with different deformation
mechanisms—dislocation glide, formation of deformation
bands by motion of partial dislocations and formation of
a′-martensite—shown in combination with the stress-strain
curve obtained during tensile test a room temperature.
a Cumulated AE energy. b Number of elements per cluster.
Reproduced from [33]. Permission of Elsevier . . . . . . . . . . . . . . 326
Fig. 7.58 Microstructure of Fe–16Cr–6Mn–6Ni–0.05C steel after tensile
test interrupted at 10% elongation. a SEM micrograph in BSE
contrast. b Inverted ECC image of the region indicated in
(a) showing individual stacking-faults (SF) arranged in
between deformation bands as well as lentil-like a′-martensite
nuclei inside the deformation bands with high SF density.
c, d Results of EBSD measurements of a typical area of
interest. c Phase map: fcc austenite—red, bands with
stacking-faults indicated as hex phase (e-martensite)—yellow,
bcc a′-martensite—blue. d Orientation map in inverse pole
figure colours with respect to the surface normal direction for
the martensitic a′-phase. e Overlay of crystallographic
orientation map of austenite and phase map of martensite
(blue) and stacking-fault band (yellow) corresponding to the
marked area (white rectangle) in (d). Loading axis horizontal.
Reproduced from [33]. Permission of Elsevier . . . . . . . . . . . . . . 327
Fig. 7.59 Time sequence of AE clusters evaluated for Fe–16Cr–6Mn–
3Ni–0.05C steel and correlated with different deformation
mechanisms—formation of deformation bands by motion of
partial dislocations, formation of a′-martensite and occurrence
of PLC bands—shown in combination with the stress-strain
lxvi List of Figures

curve obtained during tensile test a room temperature.


a Cumulated AE energy. b Number of elements per cluster.
Reproduced from [33]. Permission of Elsevier . . . . . . . . . . . . . . 328
Fig. 7.60 Microstructure of Fe–16Cr–6Mn–3Ni–0.05C steel after tensile
test interrupted at 10% of elongation. a SEM micrograph in
BSE contrast. b Inverted ECC image showing individual
stacking-faults arranged in between deformation bands.
c, d Results of EBSD measurements of a typical area of
interest. c Phase map—austenitic phase in red, bands with
stacking-faults indexed as hex phase (e-martensite) in yellow,
martensitic a′-phase in blue. d Orientation map in inverse pole
figure colouring with respect to the surface normal direction
for the martensitic a′-phase. Loading axis horizontal.
Reproduced from [33]. Permission of Elsevier . . . . . . . . . . . . . . 329
Fig. 7.61 Volume fraction of the strain-induced a′ martensite in Fe–
16Cr–6Mn–6Ni–0.05C steel and Fe–16Cr–6Mn–3Ni–0.05C
steel obtained during tensile tests at RT and at a strain rate of
1  10−3 s−1 in combination with the cumulative AE energy
calculated independently of the group of signals belonging to
AE cluster 2 identified and separated from other sources by the
AE cluster analysis. Reproduced from [33]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 330
Fig. 7.62 Temporal evolution of AE energy E and median frequency fm
derived from power spectral density functions obtained by fast
Fourier transformation of AE data streams collected during
tensile tests of TRIP/TWIP cast steels at room temperature
(a, c, e) and 100 °C (b, d, f) at nominal strain rate of
3  10−3 s−1. a, b Fe–16Cr–6Mn–9Ni–0.05C steel.
c, d Fe–16Cr–6Mn–6Ni–0.05C steel. e, f Fe–16Cr–6Mn–3Ni–
0.05C steel. Reproduced from [40]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 332
Fig. 7.63 Scatter plots showing bivariate distributions of AE descriptive
variables—average energy E and median frequency fm—for
austenitic stainless steels with different Ni contents tested at
room temperature and 100 °C. Parameters related to individual
realizations assigned to different AE clusters (i.e. to different
deformation mechanisms). Reproduced from [40]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 334
Fig. 7.64 Results of the AE cluster analysis for Fe–16Cr–6Mn–9Ni–
0.05C steel tested in tension at RT (a, c) and 100 °C (b, d).
Time sequence of the cumulative AE energy (a, b) and of the
number of AE cluster elements (c, d). Reproduced from [40].
Permission of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 335
List of Figures lxvii

Fig. 7.65 Results of the AE cluster analysis for Fe–16Cr–6Mn–6Ni–


0.05C steel tested in tension at RT (a, c) and 100 °C (b, d).
a, b Temporal evolution of the cumulative AE energy.
c, d Temporal evolution of the number of AE cluster elements.
Reproduced from [40]. Permission of Elsevier . . . . . . . . . . . . . . 336
Fig. 7.66 Summary of microstructure observations and EBSD
measurements on Fe–16Cr–6Mn–6Ni–0.05C steel after tensile
test at RT (a–c) and 100 °C (d–f). a, d Phase map with
austenitic phase (fcc) in red, e-martensite (hex) in yellow and
a′-martensite (bcc) in blue colour (b, e). Crystallographic
orientation map in the inverse pole figure colouring code
according to the surface normal direction; (e, f) band contrast
images with indicated twin boundaries (red). Stress axis is
horizontal. Reproduced from [40]. Permission of Elsevier . . . . . 337
Fig. 7.67 Results of the AE cluster analysis for Fe–16Cr–6Mn–3Ni–
0.05C steel tested in tension at RT (a, c) and 100 °C (b, d).
a, b Temporal evolution of the cumulative AE energy.
c, d Temporal evolution of the number of AE cluster elements.
Reproduced from [40]. Permission of Elsevier . . . . . . . . . . . . . . 338
Fig. 7.68 Comparison of cumulated AE energy and volume fraction of
a′-martensite determined from ferritescope measurements with
model description of Olson and Cohen for steel with 6 and 3
wt% nickel. Modified according to [33]. Permission
of Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 339
Fig. 7.69 Two-camera setup for fully-coupled full-field measurements in
combination with AE measurements during tensile tests on
Fe–16Cr–6Mn–3Ni–0.05C TRIP steel in a wide range of
temperatures and strain rates. 1—Thermo-camera. 2—AE
sensor. 3—Digital camera. 4—Gripping system. 5—
Specimen. a Setup in the electromechanical testing device
(Zwick). b Higher magnification with clamped specimen and
AE sensor fixed by a rubber band (blue) to the specimen
surface. According to [41] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 341
Fig. 7.70 Flow curves of the metastable Fe–16Cr–6Mn–3Ni–0.05C
TRIP steel tested in tension at room temperature and different
nominal strain rates (a). Vertical bars indicate the onset of
instability flow. b Details of the flow curves indicated by
rectangles in (a) at higher resolution. Reproduced from to [41].
Permission of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 342
Fig. 7.71 Flow curves of metastable Fe–16Cr–6Mn–3Ni–0.05C TRIP
steel at higher temperatures and the four nominal strain rates:
10−4 s−1, 10−3 s−1, 10−2 s−1 and 10−1 s−1. a 60 °C and b 80 °C.
A vertical bar indicates the onset of serrated plastic flow.
lxviii List of Figures

c Detail of the flow curve marked by the rectangles in (a) at


higher resolution. Reproduced from [41]. Permission
of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 344
Fig. 7.72 Quasi-isothermal stress-strain curves of metastable Fe–16Cr–
6Mn–3Ni–0.05C TRIP steel tested at room temperature and
strain rates of 10−3 s−1 and 10−2 s−1, respectively, with
additional compressed air-cooling device. Reproduced from
[41]. Permission of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . 344
Fig. 7.73 Strain rate sensitivity of the metastable Fe–16Cr–6Mn–3Ni–
0.05C TRIP steel in dependence on the applied strain at
different temperatures. a Room temperature. b 60 °C. c 80 and
140 °C. Reproduced from [41]. Permission of Springer . . . . . . . 346
Fig. 7.74 Infrared thermographic measurements during tensile tests of
Fe–16Cr–6Mn–3Ni–0.05C steel at room temperature and a
nominal strain rate of 10−3 s−1. a True stress-true strain curve
in combination with temperature evolution curves
(T-t) measured at three different points along the gauge length
(green, grey, red) and a sequence of infrared thermograms
of the whole gauge length for low strain levels (e < 0.15).
b Sequence of infrared thermograms of the whole gauge length
for higher strain level (e > 0.289) showing the development
and propagation of two individual macroscopic bands of
localized plastic strain. Reproduced from [50]. Permission of
Elsevier . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 347
Fig. 7.75 Results of the full-field measurements on two opposite sides
of the gauge length of the specimen of Fe–16Cr–6Mn–3Ni–
0.05C steel tested in tension at RT and 10−3 s−1. a Part of the
flow curve and the temperature–time curve. b Thermograms
taken at points indicated in (a). c Corresponding local strain
fields calculated for the opposite side of the gauge length.
According to [51] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 348
Fig. 7.76 Results of in situ thermographic measurements during tensile
tests of Fe–16Cr–6Mn–3Ni–0.05C steel at room temperature
and with two different strain rates: a and c = 10−4 s−1 and
b and d = 10−2 s−1. Each thermographic image corresponds to
a certain true strain, which is noted in the images. Black arrows
mark the direction of the movement of individual PLC bands.
Each sequence is related to the initiation and motion of two
individual bands. Reproduced from [41]. Permission
of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 349
List of Figures lxix

Fig. 7.77 Temperature–time curves evaluated on three distinct points


across the gauge length of specimens of Fe–16Cr–6Mn–3Ni–
0.05C steel during tensile tests at RT and four different strain
rates. a 10−4 s−1. b 10−3 s−1. c 3  10−3 s−1. d 10−2 s−1.
According to [51] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 350
Fig. 7.78 Correlation of stress-strain curves and time-resolved
temperature evolution obtained during tensile tests
of Fe–16Cr–6Mn–3Ni–0.05C steel at room temperature in
combination with six infrared thermograms indicated in the
temperature profile. a Lower strain rate 10−4 s−1. b Higher
strain rate 10−2 s−1. Reproduced from [41]. Permission
of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 350
Fig. 7.79 Local strain fields obtained by the digital image correlation
technique during tensile tests of Fe–16Cr–6Mn–3Ni–0.05C
steel at room temperature and two different strain rates,
10−4 s−1 (a) and 10−2 s−1 (b). The sequences show the
movement of individual PLC band. Reproduced from [41].
Permission of Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 351
Fig. 7.80 Evaluation of band velocity using thermographic
measurements with microscopic objective lens at RT and a
strain rate of 3  10−3 s−1. According to [51] . . . . . . . . . . . . . . 352
Fig. 7.81 Results of the analysis of acoustic emission signals obtained
during tensile test at room temperature and a nominal strain
rate of 10−2 s−1 for Fe–16Cr–6Mn–3Ni–0.05C steel.
Stress-strain curve in combination with development of the
average energy E of the AE signals (green) and the mean
frequency fm (blue) determined from the power spectral
density function. a Complete data set. b Data for t > 20 s . . . . . 354
Fig. 7.82 Results of the AE cluster analysis of Fe–16Cr–6Mn–3Ni–
0.05C steel during tensile tests at a strain rate of 1  10−2 s−1
and different temperatures. a RT. b 40 °C. c 60 °C. Left:
Scatter plots of AE energy E and median frequency fm .
Middle: Time sequence of identified clusters in terms of
cumulated AE energy in combination with stress-strain curve.
Right: Time sequence of identified clusters in terms of number
of cluster elements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 355
Fig. 7.83 Occurrence of the PLC effect in the Fe–16Cr–6Mn–3Ni–0.05C
TRIP steel depending on the strain rate, the temperature at the
beginning of the deformation test (a) and the maximum
temperature reached during the tensile test (b). Black circles
indicate the absence of the PLC effect, while red diamonds
indicate its occurrence. Reproduced from [41]. Permission of
Springer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 357
lxx List of Figures

Fig. 7.84 Calculation of the activation energy for the diffusion of


interstitial atoms. a Double logarithmic plot of the critical
strain versus strain rate at constant temperature (20 °C) for the
calculation of b according to (7.7). b Arrhenius plot of the
critical strain versus the deformation temperature at constant
strain rate (10−4 s−1) for the calculation of DG according to
(7.8). Experimental values are obtained from stress-strain
curve (SSC) and thermography (TG), cf. Table 7.14.
Reproduced from [41]. Permission of Springer . . . . . . . . . . . . . . 359
Fig. 7.85 Fully-coupled full-field measurements of temperature and strain
fields during tensile tests at RT and two different strain rates.
a Strain rate 10−3 s−1. b Strain rate 10−2 s−1. In addition, part of the
stress–time and the temperature–time curves is shown. The
sequence of initiation and propagation of an individual band is
indicated by numbers in the temperature–time curve. Both the
thermograms and the local strain fields show the complete gauge
length of the tensile specimen. Local strain is given in terms of
Von Mises strain. According to [51] . . . . . . . . . . . . . . . . . . . . . . . . . . . . 361
Fig. 7.86 Wavelength windows for transmission and reflection of a
dichroic mirror with long-pass filter and a cut-off wavelength
of 900 nm. Band of transmission: 900–1300 nm. Band of
reflection: 400–850 nm. According to [60] . . . . . . . . . . . . . . . . . 362
Fig. 8.1 Integrated computational materials engineering.
a Four-element paradigm of modern Materials Science and
Engineering, b top-down approach for structure–property
relationship in the field of plasticity of metallic materials.
Modified according to [2, 3], respectively. Permission of
Science and Elsevier, respectively. . . . . . . . . . . . . . . . . . . . . . . . 369
Fig. 8.2 Contributions of complementary in situ characterization
techniques to the microstructural parameter-based modelling
of the strain-hardening behaviour of TRIP/TWIP
steels [10] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 372
Fig. 8.3 Correlation of AE with the grain orientation of a Fe–16Cr–
6Mn–6Ni–0.05C steel during scratch test using Vickers
indenter at 1 N applied load. a Complete AE data stream with
indicated start and finish of the scratch, b scratch together with
microstructure shown in terms of IPF colouring according to
the scratch direction, c correlation with the temporal evolution
of AE clusters identified from AE stream. Grain orientations
are given in IPF colour code with respect to the scratch
direction [13] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 376
Fig. 8.4 Experimental approach for investigations of the influence
of grain size and orientation on temporal evolution of deformation
mechanisms, strain localizations and local hardening . . . . . . . . . . . . . 377
List of Figures lxxi

Fig. 8.5 Strain localizations and MPT in a fine-grained microstructure


of a hot-pressed Fe–16Cr–6Mn–6Ni–0.05C steel after tensile
deformation up to 15% of global applied strain. a Local strain
field in terms of Von Mises equivalent strain with indicated
grain boundaries, b phase map from EBSD measurements
showing stacking fault deformation bands and a’-martensite
grains, c crystallographic orientation map using inverse pole
figure colour code with respect to the loading axis (horizontal)
[17] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 378
Fig. 8.6 Results of SEM-DIC obtained on TRIP matrix composite after
tensile deformation at RT up to 4% global applied strain.
Fe–16Cr–6Mn–6Ni–0.05C with 10% Mg-PSZ [22]. Loading
axis horizontal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 380
List of Tables

Table 2.1 Theoretical and experimental shear stress of selected pure


metals [3] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 10
Table 2.2 Typical stacking-fault energies of pure metals
and alloys [3] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 14
Table 2.3 Twinning systems of fcc, bcc and hcp crystal
lattices [1] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 17
Table 3.1 Variant selection according to Kurdjumov–Sachs orientation
relationship (cf. Fig. 3.11). According to [23] . . . . . . . . . . . .. 59
Table 5.1 In situ experiments under mechanical and thermal
loading . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100
Table 5.2 Overview about various imaging and diffraction techniques
used in combination with in situ experiments. . . . . . . . . . . . . . 101
Table 5.3 Summary on important probability distributions used for
describing acoustic emission signals . . . . . . . . . . . . . . . . . . . . . 123
Table 5.4 Typical parameters obtained from the power spectral density
function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 127
Table 5.5 Statistical parameters describing the normalized power
spectral density function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 129
Table 5.6 Different windows functions for spectral smoothing [149] . . . . 145
Table 5.7 Various parameters in time and frequency domain used
for acoustic emission analysis. Modified according to [157].
With courtesy of E. Pomponi . . . . . . . . . . . . . . . . . . . . . . . . . . 146
Table 6.1 Chemical composition and characteristic properties of the
investigated Fe–16Cr–6Mn–xNi–0.05C steel variants
(with x = 3 wt%, 6 wt% or 9 wt% nickel) . . . . . . . . . . . . . . . . 207
Table 6.2 Activated slip systems for grain ð137Þ½011 investigated
during in situ tensile deformation of Fe–16Cr–6Mn–9Ni–
0.05C steel in combination with EBSD shown in Figs. 6.27
and 6.28 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 241

lxxiii
lxxiv List of Tables

Table 7.1 Minimum, maximum and average values of strain exx , Von
Mises equivalent strain evM and shear strain exy obtained for
Fe–16Cr–6Mn–9Ni–0.05C steel during in situ tensile
test at RT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 268
Table 7.2 Activated slip systems of the investigated austenitic grain
in a Fe–16Cr–6Mn–6Ni–0.05C TRIP steel deformed in
tension at RT (cf. Figs. 7.9 and 7.13) . . . . . . . . . . . . . . . . . . . 273
Table 7.3 Activated slip systems of the martensitic variants formed
in a Fe–16Cr–6Mn–6Ni–0.05C TRIP steel deformed
in tension at RT (cf. Figs. 7.9 and 7.13) . . . . . . . . . . . . . . . . . 276
Table 7.4 Activated slip systems of the investigated austenitic grain in a
Fe–16Cr–6Mn–9Ni–0.05C TWIP steel deformed in tension
at RT (cf. Fig. 7.21) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 278
Table 7.5 Activated slip systems of the investigated austenitic grain in a
Fe–16Cr–6Mn–6Ni–0.05C TRIP steel deformed in tension at
100 °C (cf. Fig. 7.19) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 280
Table 7.6 Activated slip systems in the investigated grain of
a Fe–16Cr–6Mn–6Ni–0.05C TRIP steel cyclically
deformed at RT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 285
Table 7.7 Calculated g-matrices for 24 martensite variants V1–V24
using the g-matrix of the austenitic mother grain and the
transformation matrixes provided by Kitahara et al. [27] . . . . . 291
Table 7.8 Assignment of grain labelling to different types of martensite
according to IPF colour code . . . . . . . . . . . . . . . . . . . . . . . . . . 295
Table 7.9 Activated slip systems of martensitic variants
(primary and secondary) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 296
Table 7.10 Summary of observed variants and their orientation or
misorientation relationships, respectively . . . . . . . . . . . . . . . . . 301
Table 7.11 Habit planes, invariant shear systems in austenite and
corresponding shear systems in a′-martensite according
to variants V1–V6 and IPF colour types T1–T6 . . . . . . . . . . . . 301
Table 7.12 Calculation of the involved number of dislocations in the
formation of stacking fault bands and twin bundles according
to (2.20) and the resulting thickness of the corresponding
bands. The necessary parameters are: lattice constant a =
0.3593 nm; Burgers vector ~ bh112i = 0.1467 nm; lattice
spacing d f111g = 0.2047 nm . . . . . . . . . . . . . . . . . . . . . . . . . . . 312
Table 7.13 Band parameters determined using thermographic
measurements during tensile tests at RT and different strain
rates. T0 —initial temperature, e_ 0 —initial strain rate,
NB —number of bands, DTB —temperature increase inside
PLC band, DeB —local strain increase inside PLC band,
vB —average band velocity . . . . . . . . . . . . . . . . . . . . . . . . . . . . 353
List of Tables lxxv

Table 7.14 Parameters describing the occurrence of the PLC effect in


Fe–16Cr–6Mn–3Ni–0.05C steel. e_ 0 —initial strain rate,
T0 —initial temperature, Tmax —maximum temperature of the
specimen without additional cooling, et;max —maximum true
strain to failure, a0max —maximum content of a′-martensite,
t;c —critical true strain identified by IR-TG, et;c —critical
eTG SSC

true strain identified from stress-strain curves, eAE t;c —critical


true strain identified by acoustic emission . . . . . . . . . . . . . . . . 356
Table A.1 Overview of AE investigations on metallic materials since
2000 classified according to the field of application . . . . . . . . . 390
Table A.2 Chronological overview of investigation of strain
localizations using the digital image correlation in
combination with optical microscopy and scanning electron
microscopy as well as FEM simulations starting
from year 2000. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 400
Table A.3 Chronological overview of the application of infrared
thermography (IR-TG) starting from 2000 including
classification of the research field . . . . . . . . . . . . . . . . . . . . . . . 412
Table A.4 Chronological overview of the application of fully-coupled
full-field measurements starting from 2000 . . . . . . . . . . . . . . . 420
Chapter 1
Motivation

We have for some time labelled civilizations by the main


materials they have used: The Stone Age, The Bronze Age, and
The Iron Age … A civilization is both developed and limited by
the materials at its disposal … Today, man lives in the
boundary between The Iron Age and a New Materials Age.

(Sir George P. Thompson—Nobel Laureate in Physics, 1937)


[1, 2]

Since the time of Sir George P. Thompson, a huge number of new materials have
been designed and developed and have come into focus for industrial application—
such as ceramics, composite materials, and elastomers and polymers. In the field of
metals, new developments included bulk metallic glasses, aluminium-lithium alloys
and new superalloys as well as steels such as dual-phase steels, micro-alloyed steels
and high performance steels that enabled either transformation-induced plasticity
(TRIP) or twinning-induced plasticity (TWIP).
In this context, an important issue in materials research is the prediction, vari-
ation and control of the properties of the newly developed materials for further
improvement of their application behaviour under extreme conditions. Therefore,
comprehensive knowledge of the materials behaviour down to the atomic scale and
well-developed theoretical approaches (computer simulations, models, and statis-
tics) are imperative.
An important contribution to enhance knowledge of materials behaviour under
different loading conditions—especially with respect to their microstructure-
property relationship—can be gained from so-called in situ experiments. The term
in situ (Latin: place of origin) in materials research means the observation of
changes in a material’s behaviour or in its microstructure during exposure to certain
mechanical, thermal, electrical or magnetic loading. In situ experiments can be
performed using complementary imaging techniques (e.g. optical microscopy,
electron microscopy, thermography, atomic force microscopy) or diffraction tech-
niques (e.g. neutron diffraction, X-ray diffraction, electron diffraction). Depending
on the technique used, in situ observations will deliver information either on the

© Springer Nature Switzerland AG 2020 1


A. Weidner, Deformation Processes in TRIP/TWIP Steels,
Springer Series in Materials Science 295,
https://doi.org/10.1007/978-3-030-37149-4_1
2 1 Motivation

nanometre scale (nm) through the microscopic (µm) and mesoscopic (mm) and up
to macroscopic scale (cm, m). Furthermore, in situ observations can provide
information from either a small surface area or even from large volume elements.
In the past, the characterization of structural materials was quite often performed
post-mortem, i.e. after mechanical loading, failure or utilization under service
conditions. In this manner, however, only the result of a dynamic process is
investigated. In some cases, it is possible to draw conclusions on the origin of the
damage process. However, essential information on the temporal evolution of
processes remains hidden and undiscovered. Another possibility would be the
performance of stopped tests, which would, however, require multiple specimens,
and where the consistency with respect to the initial microstructure and chemical
compositions must be guaranteed. In addition, a crucial drawback of post-mortem
investigations is the preparative intervention in the materials state for the visual-
ization of microstructural details, which can ultimately cause preparative changes in
the microstructure leading to misinterpretations.
Therein is the key to answer the question: “Why we should be interested in in situ
testing?” The great potential of in situ observations/experiments is to study and to
analyse the temporal evolution of ongoing deformation and damage processes in
structural materials under defined loading conditions. However, the potential of in situ
observation can be increased even more by combination with powerful complementary
characterization techniques, e.g. electron backscattered diffraction, thermography,
digital image correlation or acoustic emission measurements. The combination of
various methods with their different resolution ranges in terms of lateral, spatial or time
resolution can provide a deeper knowledge and understanding of the time sequence of
microstructural processes. In addition, information gained through in situ experiments
could contribute in a substantial manner to microstructure-based modelling of material
behaviour under different loading conditions.
The aim of the present work is to demonstrate the potential of in situ experiments
performed on a microscopic and macroscopic scale in order to investigate localized
deformation processes in metallic materials, in particular their kinetics, and the
correlated evolution of local strain fields. Consequently, the methods used are
focused on in situ mechanical tests using optical microscopy and scanning electron
microscopy in combination with digital image correlation as well as infrared
thermography and acoustic emission measurements. Whereas the digital image
correlation on images from optical microscopy or scanning electron microscopy
contributes to the evaluation of local strain fields occurring during plastic defor-
mation, the infrared thermography focuses on the evolution of local temperature
fields. In contrast to these two-dimensional surface investigations, the acoustic
emission measurements provide real-time based three-dimensional volume infor-
mation with remarkably high time resolution. Thus, the combination of the chosen
in situ techniques contributes to a better understanding of the time-dependent
course of individual deformation mechanisms.
The material under investigation in the present work is a class of metastable,
low-carbon, high-alloy CrMnNi cast steels, which was developed and designed
within the framework of a collaborative research activity at Technische Universität
1 Motivation 3

Bergakademie Freiberg called “TRIP matrix composites” (CRC 799). These meta-
stable CrMnNi cast steels stand out by virtue of their excellent mechanical properties
such as concurrently high strength and ductility. These extraordinary mechanical
properties are caused by either martensitic phase transformation leading to the TRIP
effect or mechanical twinning resulting in the TWIP effect. The CrMnNi steel alloys
are also used as a matrix for composite materials, which were reinforced by MgO
partially stabilized ZrO2 (Mg-PSZ) particles. The Mg-PSZ particles undergo a
martensitic phase transformation as well, yielding compressive stresses in the sur-
rounding material due to a volume dilation and a shear transformation of the ZrO2
particles. The combination of both effects—martensitic phase transformation of the
CrMnNi steel matrix as well as martensitic phase transformation of the Mg-PSZ—
results in damage tolerant materials with a high capability for the absorption of
mechanical energy. This makes this novel class of metal matrix composites favour-
able candidates for applications such as in crash absorbing components or compo-
nents with a high wear resistance.
The present work is focussed on the metastable CrMnNi cast TRIP/TWIP steels
in order to characterize the time sequence of localized deformation processes on a
microscopic scale such as (i) the formation of deformation bands, (ii) martensitic
phase transformation and (iii) mechanical twinning as a function of the chemical
composition and the deformation temperature. In addition, the macroscopic local-
ization phenomenon of the Portevin-Le Chatelier effect is also discussed.
The work consist of nine chapters. After the motivation, Chap. 2 provides an
introduction to plastic deformation, strain-hardening and strain localization during
plastic deformation on different length scales. Chap. 3 deals with martensitic phase
transformation in general and in steels in particular. The thermodynamics, kinetics
and the influence of stacking fault energy on the martensitic phase transformation
are discussed.
Chapter 4 gives a short summary on advanced high strength steels with excellent
mechanical properties—the high-alloy TRIP and TWIP steels. Each steel class is
described by its thermodynamics, deformation behaviour, microstructure and state
of the art modelling of their strain-hardening behaviour.
In Chap. 5, a literature review is provided on selected in situ techniques suitable for
the investigation of strain localizations on macroscopic and mesoscopic length scales.
However, since the number of publications in these fields are so manifold, the pro-
vided literature review does not claim for completeness. Furthermore, the large field of
in situ micro and nanoscale testing of materials using transmission electron micro-
scopy (e.g. review paper of Gianola and Eberl [3]) as well as the considerable amount
of diffraction techniques are excluded since the focus of the present investigations is on
microscopic and macroscopic material behaviour. Therefore, only in situ experiments
using optical microscopy, scanning electron microscopy, infrared thermography and
acoustic emission measurements are introduced, which are used in the present work
for the investigation of strain localizations and their temporal evolution during plastic
4 1 Motivation

deformation. Each technique is discussed in the context with some historical and
method-related background information. In addition, an overview is provided on the
state of the art of application of these techniques in the field of Materials Engineering.
Chapter 6 is concerned with the material under investigation—high-alloy
CrMnNi TRIP/TWIP steels. The metastable high-alloy CrMnNi TRIP/TWIP cast
steels studied are described with respect to their mechanical and microstructural
properties based on a profound knowledge gained within the framework of the
collaborative research activity at Technische Universität Bergakademie Freiberg
—“TRIP matrix composites”—over the last decade.
In Chap. 7, in situ experiments as well as their combination in terms of
fully-coupled, full-field measurements are used to demonstrate the great potential of
microscopic (scanning electron microscopy) and macroscopic (acoustic emission)
examination by means of three case studies: (1) The in situ scanning electron
microscopy experiments in combination with digital image correlation are used to
evaluate the development of strain localization during tensile and cyclic loading of
TRIP/TWIP steels and reveal the influence of temperature and chemical compo-
sition on the strain localization. (2) In situ acoustic emission measurements during
tensile tests reveal the time sequence of individual deformation mechanisms, such
as dislocation glide, the formation of stacking faults, martensitic phase transfor-
mation, or twinning. In addition, the influences of chemical composition and
temperature on the time sequence of these individual deformation mechanisms are
detected. (3) The combination of optical microscopy, thermography and acoustic
emission measurements during tensile testing is used in order to study the
macroscopic inhomogeneous deformation behaviour of one of the TRIP steel
variants.
Finally, in Chap. 8 it is discussed how the above mentioned in situ methods and
case studies contribute to a better understanding of the deformation and
strain-hardening behaviour of the investigated high-alloy TRIP/TWIP steels and
how the results can be incorporated into existing models describing the TRIP or
TWIP effect. Furthermore, the benefit of the combination of different in situ tech-
niques is discussed. Moreover, the application of in situ techniques to promising
materials and processes is depicted.
Chapter 9 provides concluding remarks on the main achievements obtained by
the complementary in situ characterization techniques—(i) in situ SEM testing in
combination with digital image correlation, (ii) in situ acoustic emission mea-
surements, and (iii) fully-coupled full-field measurements using thermography and
digital image correlation. It is shown that the application of these techniques
facilitates the investigation of both the microscopic strain localization occurring in
high-alloy CrMnNi cast TRIP/TWIP steels on a sub-micrometre resolution and the
time sequence of activated deformation mechanisms. In addition, an outlook is
provided on further developments and applications of these techniques.
References 5

References

1. N.E. Promisiel, Metall. Mate. Trans. B 16, 5–11 (1984)


2. D.L. Cocke, A. Clearfield, Design of New Materials (Springer, Boston, MA, USA, 1987)
3. D.S. Gianola, C. Eberl, JOM 61, 24–35 (2009)
Chapter 2
Plastic Deformation and Strain
Localizations

Abstract This chapter gives an overview of basic knowledge on plastic defor-


mation and strain localizations. The chapter starts with general remarks on plastic
deformation continuing with details on deformation mechanisms such as disloca-
tion glide and twinning were shortly summarized focusing for most common crystal
lattices in metallic materials: (i) face-centred cubic lattice, (ii) body-centred cubic
lattice and (iii) closed-packed hexagonal crystal lattice. In addition, the critical
resolved shear stress is introduced and the mechanisms of strain hardening are
described. Finally, different phenomena of strain localization are described distin-
guishing between strain localizations on microscopic scale (slip bands, deformation
bands, persistent slip band and shear bands) and macroscopic strain localizations
(Lüders effect, Portevin–Le Chatelier effect).

2.1 Plastic Deformation

Frequently, engineering components experience plastic deformation under


mechanical loading, resulting ultimately in damage and failure of the material.
Thus, plastic deformation describes the non-reversible change in the shape of a
solid material in response to forces applied. An elementary way to demonstrate the
plastic deformation behaviour of solid materials is that of uniaxial quasi-static
loading in tension. Thus, recording the applied load F versus the resolved elon-
gation DI on the specimen facilitates calculation of the applied stress r and the
resolved strain e. Figure 2.1 shows a typical stress-strain ðr  eÞ curve of a ductile
material. Clearly, different parts of the stress-strain curve can be distinguished. At
first, there is a linear correlation between stress and strain, which resembles the
elastic part of the material behaviour. The applied stress is proportional to the
resolved strain or elongation according to Hooke’s law [see (2.1)]:

F DI I  I0
r ¼ E  e with r¼ and e¼ ¼ ð2:1Þ
A0 I0 I0

© Springer Nature Switzerland AG 2020 7


A. Weidner, Deformation Processes in TRIP/TWIP Steels,
Springer Series in Materials Science 295,
https://doi.org/10.1007/978-3-030-37149-4_2
8 2 Plastic Deformation and Strain Localizations

Fig. 2.1 Mechanical behaviour under quasi-static uniaxial loading. a Typical engineering
stress-strain curve of a ductile material. 1—Young’s modulus, 2—yield stress (YS) ry , 3—
ultimate tensile stress (UTS) rUTS , 4—strain to rupture er and 5—work of deformation. b True
stress-strain curve versus engineering stress-strain curve. c Typical stress-strain curves of materials
with high strength at low ductility, high strength at high ductility and low strength at high ductility.
Modified according to [1]. Permission of Pearson Education

Here, r is the applied stress and e is the resolved strain. The factor of propor-
tionality is Young’s modulus E. The material does not experience plastic defor-
mation after removal of the applied load.

Upon reaching the yield stress ry , the material starts to deform plastically. The
rise of the stress-strain curve beyond the yield point is caused by strain hardening.
Thus, the linear dependency according to (2.1) transforms to a power law expressed
by the Ramberg–Osgood relationship (2.2) [2]:

r ¼ H  enp ð2:2Þ

which is applied to the plastic strain ep instead of the total strain e. The exponent
n is the strain-hardening exponent and H is the strength coefficient. Since the total
strain e is the sum of elastic strain eel and plastic strain epl , the total strain can be
given in combination with (2.1) as [2]:

r  r 1n
e¼ þ ð2:3Þ
E H

With increasing strain, the material resistance against an externally applied load
increases due to increased hardening. The slope of the stress-strain curve becomes
more gradual until a point of maximum stress is reached, which is related to the
ultimate tensile stress (UTS) rUTS . The tensile strength of materials describes the
ability of a material to resist external applied load before failure. The point of the
maximum stress is related to the uniform elongation eu . At the UTS, the initial cross
section A0 of a tensile specimen starts to decrease significantly due to necking,
which is responsible for decreasing stress levels with further straining of the
material. Finally, the specimen fails at the stress to rupture rr , and er can be
expressed as the strain to rupture. The stress-strain curve shown in Fig. 2.1 is a
2.1 Plastic Deformation 9

so-called engineering stress-strain curve, which takes into account only the initial
cross section of the specimen A0 for stress calculation. For ductile materials, the
applied load F is frequently related to the current cross section A rather than to the
initial cross section A0 resulting in true stress. The true strain etrue and the true stress
rtrue are then calculated according to (2.4):

etrue ¼ lnð1 þ eÞ rtrue ¼ rð1 þ eÞ ð2:4Þ

The true stress-true strain curves differ markedly from engineering stress-strain
curves, as shown in Fig. 2.1b. Thus, the true stress is always higher than the
engineering stress.
The stress-strain behaviour of engineering materials varies in a wide range
depending on chemical composition, material processing, deformation temperature
and strain rate (see Fig. 2.1c). For a given chemical composition and method of
processing technology, the increase in temperature results in most cases in a
decrease in yield stress, UTS and stress to fracture accompanied by an increase in
ductility. However, the increase in strain rate results in a significant increase in yield
stress and UTS.
The plastic deformation of materials is a consequence of the slip of two
neighbouring atomic planes within a crystalline lattice resulting in permanent
deformation of the material. However, the movement of all atoms of one individual
atomic plane during slip would require the theoretical shear stress of the material, as
determined by (2.5) [3]:

Gb
rth ¼ ð2:5Þ
2pd

Here, G is the shear modulus, b the distance between atoms within one lattice
plane and d the distance between two lattice planes as shown in Fig. 2.2. However,
the shear stress observed experimentally is much less as that demonstrated in
Table 2.1, where the theoretical shear stress sth and the experimentally observed
shear stress s0 —also known as critical resolved shear stress sCRSS —are summarized
for selected pure metals.
The discrepancy between the theoretical shear stress and the shear stress observed
experimentally can be explained by the dislocation theory. Thus, the introduction of
one-dimensional lattice defects—the dislocations—facilitates the slip of neigh-
bouring lattice planes. A dislocation can be understood as a half-plane of atoms
additionally introduced to the lattice. Due to stepwise movement of the additional
half-plane as shown in Fig. 2.3, the slip of neighbouring atoms is facilitated.
In general, two dislocation types can be defined: (i) edge dislocations and
(ii) screw dislocations. An edge dislocation can be understood in simple terms as a
half-plane of atoms being introduced. A screw dislocation is characterized by the
displacement of two parts of the crystallographic lattice that are related to the
dislocation line. Figure 2.4 shows schematic illustrations of edge and screw
dislocations.
10 2 Plastic Deformation and Strain Localizations

b)
a)

Fig. 2.2 Permanent deformation by slip of lattice planes. a Rigid slip of neighbouring lattice
planes. b Progress of energy and shear stress during rigid slip of atoms. Modified according to [1].
Permission of Pearson Education

Table 2.1 Theoretical and experimental shear stress of selected pure metals [3]
Material rth ½MPa rCRSS ½MPa rth =rCRSS ð%Þ rUTS ½MPa
Ag 1000 0.37 0.037 20
Al 900 0.78 0.087 30
Cu 1400 0.49 0.035 51
Ni 2600 3.2 0.123 121
a-Fe 2600 27.5 1.058 150

Fig. 2.3 Plastic deformation of a crystal by motion of dislocation along a slip plane. Modified
according to [1]. Permission of Pearson Education

Fig. 2.4 Schematic illustration of different types of dislocations in crystal lattice. a Edge
dislocation with Burgers circuit. b Three-dimensional representation of edge dislocation. c Screw
dislocation. d Part of a dislocation loop with segments of edge and screw-type dislocation.
Modified according to [1]. Permission of Pearson Education
2.1 Plastic Deformation 11

The magnitude and the direction of the distortion resulting from the dislocation is
given by the Burgers vector ~ b, which depends on the crystal lattice. Thus, the direction
of ~b is related to the most densely packed direction within the plane where the dis-
location is located, which is mostly a close-packed plane. The Burgers vector ~ b is,
therefore, often the next neighbour distance. The magnitude of ~ b is determined by the
lattice constant a and the interplanar lattice distance according to (2.6):
  a pffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
~
 b ¼ h2 þ k 2 þ l 2 ð2:6Þ
2

Here, h; k; l are the Miller indices of the respective lattice plane.


For edge dislocations, the Burgers vector ~ b is perpendicular to the dislocation
line (see Fig. 2.4a, b), whereas for screw dislocations ~ b lies parallel to the dislo-
cation line (see Fig. 2.4c). A dislocation line cannot end within a crystal. Thus,
dislocation loops are observed that contain both edge- and screw-type segments
(see Fig. 2.4d). The amount of dislocations present in a material can be described
by the quantity of the dislocation density, which is defined simply as the total length
of dislocations (m) per total volume (m3) or, alternatively, by the number of dis-
location lines n intersecting an area (m2) resulting in the unit m−2. The typical
dislocation density q of non-deformed metals is about 1010 m−2. This amount of
dislocations is already present in metallic materials after their metallurgical pro-
cessing. However, the dislocation density can increase significantly during plastic
deformation up to 1015 m−2 due to activation of dislocation sources (e.g. Frank–
Read sources).

2.2 Dislocation Glide

The dislocation glide behaviour and, consequently, the deformation behaviour of


materials depend significantly on the crystal lattice. The most common crystal
lattices of metals are (i) face-centred cubic (fcc), (ii) body-centred cubic (bcc) and
(iii) hexagonal close-packed (hcp) crystal lattices. Dislocation glide in fcc materials
occurs on f111g planes along h110i directions, which are close-packed planes and
directions (see Fig. 2.5a). Therefore, the fcc crystal lattice possesses 12 slip systems
of type f111gh110i (four f111g planes each containing three h110i directions).
Due to the closed-packed nature of fcc crystal lattice (atomic packing factor of
74%), the critical resolved shear stresses sCRSS on slip systems are quite low (0.35
to 0.7 MPa, Table 2.1) resulting in the good ductility of fcc metals and alloys.
Dislocations in bcc materials glide along closed-packed f110g planes and
directions h111i resulting in 12 slip systems of type f110gh111i (six f110g planes
each containing two h111i directions). In addition, 12 f112g and 24 f123g planes
can be activated with each h111i direction. Thus, at least 48 slip systems are
available in bcc materials. However, with a lower packing density (an atom packing
12 2 Plastic Deformation and Strain Localizations

Fig. 2.5 Unit cells of fcc, bcc and hcp crystal lattices with indicated basis slip systems based on
close-packed lattice planes and lattice directions. a fcc crystal lattice with f111gh110i slip system.
b bcc crystal lattice f110gh111i slip system. c hcp crystal lattice with f0001gh0001i slip system

factor of 68%) compared to the fcc crystal lattice, the critical resolved shear stresses
on slip systems of bcc materials are significantly higher (35–70 MPa, Table 2.1).
Similarly to fcc crystal lattice, the hcp crystal lattice is also a closed-packed
structure (with an atomic packing factor of 74%). The closed-packed plane, and,
therefore, the common slip plane, is the basal plane f0001g containing three slip
directions h1120i (with three slip systems f0001gh11 20i). Although the critical
resolved shear stresses are low (comparable to fcc materials) due to the
closed-packed character of the crystal lattice, the deformation behaviour of hcp
materials is more brittle in several cases. Depending on the c/a ratio of hcp
materials, other slip planes such as prismatic planes f01 10g or pyramidal planes
f0111g, f1122g can be activated [3].
According to Frank’s rule ðEel  aGb2 Þ [3], the elastic energy of a perfect dis-
location is proportional to the square of the magnitude of the Burgers vector, which
is mostly the shortest lattice vectors (e.g. 1=2h110i or h001i in fcc crystal lattice).
Thus, dislocation glide in fcc materials is facilitated by dislocations with the
Burgers vector ~ b ¼ a=2h110i, since the elastic energy ðEel  1=2a2 Þ is half of that
for ~
b ¼ ah001i ðEel  a2 Þ. In terms of energetically aspects, it can be favourable for
a regular dislocation ~b to dissociate into two partial dislocations (i.e. a leading and a
 2  2  2
     
trailing partial dislocation) with ~b1 and ~ b2 if the condition ~b [ ~ b1  þ ~
b2  is
fulfilled. Thus, a regular dislocation with ~
b ¼ a=2h110i in fcc materials will dis-
sociate into two partial dislocations with the Burgers vector ~ b1;2 ¼ a=6h112i
according to (2.7):
a  a a 
½101 ¼ ½112 þ ½2
11 ð2:7Þ
2 6 6

Dislocations with Burgers vectors ~ b1 and ~b2 are so-called Shockley partial
dislocations. The formation of Shockley partials is independent of the character
(edge or screw) of the regular dislocation. The separation of regular dislocations
2.2 Dislocation Glide 13

Fig. 2.6 Thompson tetrahedron for description of dislocation reactions in fcc crystal lattice.
a Construction of the tetrahedron. b Tetrahedron with separation of regular h110i dislocations into
h112i Shockley partials. c Several reactions of Shockley partials forming Lomer-Cottrell
(LC) locks (bold red lines). Modified according to [4]. Permission of IOP Publishing

into Shockley partials can be visualized for all twelve possible slip systems of the
fcc crystal lattice by the Thompson tetrahedron shown in Fig. 2.6.
In addition, Fig. 2.6c illustrates reactions of Shockley partials. Thus, two leading
Shockley partials on two different f111g planes can combine and form a so-called
Lomer-Cottrell-lock according to (2.8):
a a a
½112 þ ½112 ¼ ½110 ð2:8Þ
6 6 3

which is a new dislocation, where the Burgers vector is not in the slip plane
anymore, comparing the reaction ac þ cd ¼ ad (see Fig. 2.6). Therefore, LC-locks
are sessile and act as obstacles on dislocation motion.
The area between two Shockley partial dislocations is called a stacking fault
(SF) (see Fig. 2.7a). The combined defect consisting of Shockley partials and a SF
is called an “extended dislocation”, which can glide on its own slip plane. Due to
the formation of a SF, the sequence of stacking of atomic layers in the crystal lattice
is changed. The stacking sequence of closed-packed f111g planes of the fcc crystal
lattice can be described as a ABCABC sequence, whereas in hcp, the sequence of
closed-packed f0001g planes is described as ABAB (cf. Fig. 2.7b). The dissocia-
tion into partial dislocations leads either to the removal of an atomic layer (intrinsic
stacking fault) or to the introduction of an additional atomic layer due to two
subsequent SFs (extrinsic stacking fault) shown in Fig. 2.7c. Thus, the stacking
sequence of atomic layers caused by an intrinsic SF is of type ABAB, which is
related to the hcp crystal lattice. The stacking sequence of atomic layers caused by
extrinsic SF is the inversion of the local sequence due to two SFs on neighbouring
f111g planes. The interaction (cutting) of SF on several f111g planes leads to the
formation of a SF tetrahedron, where the sides of the tetrahedron are formed by SFs
(see Fig. 2.7d). Thus, SF tetrahedra can be observed in fully or partially closed
states [5].
14 2 Plastic Deformation and Strain Localizations

Fig. 2.7 Stacking faults in fcc crystal lattice. a Dissociation of regular dislocations forming
stacking fault. b Stacking sequence of atomic layers of the fcc and hcp crystal lattice. c Intrinsic
and extrinsic stacking faults. d SF tetrahedra. e Cross-slip. a, e Modified according to [3].
Permission of Springer. d, c Modified according to [5] and [6]. Permission of Elsevier

Between the two partial dislocations, repulsive forces are active until a balance is
achieved between the minimization of elastic energy due to the dissipating dislo-
cations and the increase in stacking-fault energy. Thus, the dissociation distance of
the partial dislocations and, therefore, the width of stacking faults are determined by
the stacking-fault energy (SFE) cSF according to (2.9) [3]:

G ~b1  ~
b2
dSF ¼ ð2:9Þ
2  p  cSF

According to (2.9), the width of the SF dSF is inversely proportional to the SFE.
Table 2.2 gives an overview of stacking-fault energies of common pure metals and
alloys [3]. Thus, the lower the stacking-fault energy (SFE) the larger is the width of
the stacking fault.
Therefore, the stacking-fault energy has a significant influence on the defor-
mation behaviour of materials. The movement of partial dislocations is restricted to

Table 2.2 Typical stacking-fault energies of pure metals and alloys [3]
Pure metals Alloys
Al a-Fe Ni Cu Au Ag Stainless steel a-brass
cSF [mJ/m2] 250 200 200 90 75 25 <20 <10
2.2 Dislocation Glide 15

the activated slip plane. In order to change the slip plane, dissociated screw dis-
locations have to recombine by means of constriction. After recombination, the
dislocation can change the slip plane (cross-slip) and dissociate again in the new
slip plane as shown in Fig. 2.7e. However, with increasing dissociation distance or
width of the stacking fault, the probability for recombination of partial dislocations
decreases. Consequently, cross-slip becomes more and more difficult with
decreasing SFE. Hence, the planarity of dislocation glide increases.
Thus, two primary and distinct dislocation glide behaviours have to be distin-
guished: (i) planar glide of dislocations, where dislocation glide is restricted to the
activated slip plane and (ii) pronounced cross-slip of dislocations, where disloca-
tions can change easily between different slip systems (also known in the literature
as wavy slip behaviour). Which type of dislocation glide behaviour is favoured
depends in particular, as mentioned above, on the crystal lattice and the
stacking-fault energy, but also on short-range order (SRO). Therefore, materials
with a higher stacking-fault energy as well as bcc materials exhibit pronounced
cross-slip behaviour. In contrast, materials with low stacking-fault energy and/or
SRO exhibit planar glide behaviour.
Along with the Shockley partial dislocations, a second type of partial disloca-
tions are known, which are formed in fcc crystal lattice by removing (intrinsic fault)
or inserting (extrinsic fault) a f111g lattice plane. These so-called Frank partials
have a Burgers vector ~ b ¼ a=3h111i and are immobile (sessile) dislocations [6].

2.3 Deformation Twinning

Along with dislocation glide, deformation twinning is a second possible defor-


mation mechanism during plastic deformation of metallic materials. Mostly, it is
observed in hcp materials due to the low number of slip systems or in bcc materials
at low deformation temperatures, when the activation of regular slip systems is
impeded. A typical fcc alloy that exhibits intensive deformation twinning is a-brass.
However, quite recently, deformation twinning has also been observed in austenitic
stainless steels (e.g. TWIP steels) or in pure metals with high or higher SFEs such
as nanocrystalline copper or aluminium (e.g. [7]). This indicates quite clearly that
the activation of deformation twinning depends on numerous parameters such as
(i) crystal lattice, (ii) stacking-fault energy, (iii) grain size, (iv) grain orientation,
(v) loading conditions and (vi) temperature.
In the fcc crystal lattice, mechanical twinning occurs on the f111g plane. As
shown in Fig. 2.8a, the direction of twin shearing is ½11 2, which corresponds to the

intersection line of the ð111Þ plane and the ð110Þ plane. Thus, f110g is the shear
plane, which contains both the f111g twin plane and the h112i twin direction.
Figure 2.8b shows the mechanism of deformation twinning according to [3]. Here,
a view of the lattice planes ð110Þ of several aligned unit cells is shown. Atoms at
the positions A, B and C within the twinned region are shifted along the shear
16 2 Plastic Deformation and Strain Localizations

direction ½112, whereby the atoms A, B and C are shifted by one-third of the
interatomic distance, two-third of the interatomic distance, and by the entire
spacing, respectively. These atom shifts are accompanied by changes in the lattice
shape, since atom shifts at positions A and B end at interatomic spaces. Thus, the
crystallographic orientation within the twinned region differs from the orientation of
the neighbouring matrix. The twinned region appears as a mirror image of the
matrix, where the twin plane ð111Þ is the mirror plane. The twin boundary consists
of atoms that belong to both the matrix and to the twinned region as becomes
obvious from Fig. 2.8b.
This is a so-called coincident site lattice (CSL) boundary. Since each third atom
of the matrix and the twin belongs to the boundary as shown in Fig. 2.9a, it is
referred to a CSL3 or R3 boundary. Such a R3 boundary is characterized by a
specific misorientation of the matrix and the twinned region, which can be expressed
by a rotation of 60° around a h111i direction (see Fig. 2.9b). Thus, the coincident
site character of the boundary is similar to an intrinsic stacking fault. Therefore, the
energies of an intrinsic stacking fault in the fcc crystal lattice, i.e. of the f111g twin
boundary and of the f111gfcc k f0001ghcp interface are quite similar [8].
In the microscopic images, deformation twins appear as band-like structures.
However, the thickness of deformation twins can vary from nanometres up to few
micrometres. In contrast to dislocation glide, deformation twinning is accompanied
by changes in the crystallographic orientation.
The twinning systems of bcc and hcp crystal lattices are summarized in
Table 2.3 and are shown together with the atom displacements in Fig. 2.10.
Several model descriptions are known for twin nucleation and growth and have
long been discussed in literature. However, a consistent theory is still lacking. In
1995, Christian and Mahajan gave a comprehensive overview of different models
related to deformation twinning in bcc, hcp and fcc crystal lattices [8]. In addition,

Fig. 2.8 Deformation twinning in fcc crystal lattice. a Twin system consisting of twin plane,
direction of shear and shear plane. b Movement of atom positions during deformation twinning.
Modified according to [3]. Permission of Springer
2.3 Deformation Twinning 17

Fig. 2.9 Description of twin orientation. a Twin boundary with coincident site lattice places.
b Misorientation 60° h111i of a R3 boundary. Modified according to [1] (a) and [9] (b).
Permission of Pearson Education and Springer, respectively

Table 2.3 Twinning systems of fcc, bcc and hcp crystal lattices [1]
Crystal lattice Twin plane Direction of shear Shear plane Examples
fcc f111g h112i f110g Al, Cu
bcc f112g h111i f110g a-Fe
hcp 
f1012g  i
h1011 
f1121g a-Ti, Zn

Fig. 2.10 Deformation twinning of bcc a, b and hcp c, d crystal lattices. a, c Unit cells with
indicated twinning plane, direction of shear and shear plane. b, d Cooperative movement of atoms
along direction of shear during twinning. TD—twin direction, TP—twin plane, PoS—plane of
shear. Modified according to [3]. Permission of Springer

an excellent graphical description of the models for twin nucleation that have been
discussed in the literature was recently provided by De Cooman et al. [10].
The first description of mechanical twinning dates back to 1961, where Venables
[11] proposed the well-known pole mechanism, which is a prismatic glide mech-
anism. According to this model, a prismatic dislocation glide source dissociates into
a sessile Frank partial dislocation (pole dislocation) with ~ b ¼ a=3h111i and a
mobile Shockley partial dislocation (twinning partial dislocation) with
~
b ¼ a=2h110i. The mobile Shockley partial forms a large extended intrinsic SF,
which is capable of recombining at an underlying f111g plane if a certain unstable
18 2 Plastic Deformation and Strain Localizations

configuration is reached [8]. However, the required dislocation configurations and


dislocation reactions are unfavourable from an energetic point of view. Moreover,
these mechanisms cannot describe the high rate of twin formation [12].
Hirth and Lothe [13] and Venables [14] carried out modifications of the pole
mechanisms. Venables [14] discussed the reaction of Shockley partials with regular
dislocation. Venables [14] also described a possible mechanism that would lead to
immobile Frank dislocations located at the twin interface, which could act as
obstacle for the propagation of twin boundaries and could also explain the stability
of twins after unloading [12].
Later, in 1963, Cohen and Weertman [15] first introduced the idea that so-called
LC-locks serve as sources for partial dislocations. According to Cohen and
Weertman [15], a regular dislocation dissociates into a sessile Frank partial and a
mobile Shockley partial due to interaction with a LC-lock. Thus, the twin is formed
by continuous emission of Shockley partials each creating a sessile Frank
dislocation.
Mori and Fujita [16] proposed a stair-rod cross-slip mechanism for twin for-
mation. This mechanism consists of a glide process of a Shockley partial on the
primary slip plane and a second Shockley partial dislocation gliding on the con-
jugate slip plane, which is emitted by the reaction of the first Shockley partial
gliding into a LC-lock at the intersection of primary and conjugate slip planes.
Multiple slip activity and high stress concentrations are necessary for the activation
of the dislocation dissociation process in the twin plane, as described by the models
of both Cohen and Weertman [15] and Mori and Fujita [16].
The model proposed by Mahajan and Chin [17] describes twin formation as a
reaction of two regular dislocations gliding on the primary and the conjugate slip
plane leading to three Shockley partial dislocations. These three Shockley partials
are located on three consecutive adjacent {111} planes leading to a three-fold
extrinsic SF acting as a nucleus for twinning [12]. The model description by Miura/
Takamura/Narita (cited in: [8]) is more complex and is widely criticized since the
reaction products are rarely observed. According to Miura, Takamura and Narita
(cited in: [8]), twin formation occurs due to the reaction of regular dislocations with
LC-locking located at the intersection of the primary and the cross-slip plane.
Based on experimental investigations on mechanical twinning in Hadfield steels,
Karaman et al. [18] developed a new model in order to describe the formation of
extrinsic SF and twinning processes. The model of Karaman et al. [18] is based on
slip of Shockley partials on the primary and the conjugate f111g slip plane leading
to a LC-lock with a Burgers vector ~ b ¼ a=3h110i. Based on Schmid factor cal-
culations, Bracke et al. [19] asserted that in fcc austenitic stainless steels, twinning
occurs according to the model proposed by Mahajan and Chin [17]. In contrast,
Idrissi et al. [12] came to the conclusion that twin nucleation occurs via the
mechanism proposed by Cohen and Weertmann [15] or Miura/Takamura/Narita
(cited in: [8]), whereas twin growth is controlled by the mechanism proposed by
Venables [14].
2.4 Critical Resolved Shear Stress 19

2.4 Critical Resolved Shear Stress

The activation of dislocation glide on slip systems or twinning is triggered by the


shear stress resolved in the slip plane or twin plane as a function of their crystal-
lographic orientation with respect to the loading axis. The critical resolved shear
stress (CRSS) for an individual slip system can be calculated according to Schmid’s
law illustrated in Fig. 2.11 and expressed by (2.10):

rCRSS ¼ ra ðcos k  cos /Þ ¼ ra  l ð2:10Þ

Here, k corresponds to the angle between the slip direction and the loading axis,
and / is the angle between the slip plane normal direction and the loading axis. ra
is the applied load. The product cosk cos/ is the so-called Schmid factor l, which
reaches maximum value of 0.5 at an inclination angle of 45° of both the slip plane
normal and the slip direction to the loading axis.
Depending on the crystallographic orientation, the critical resolved shear stresses
of individual slip systems are different. The 12 slip systems of the fcc crystal lattice
can be visualized by a stereographic projection shown in Fig. 2.12. The triangle
½001–½011–½111 (shadowed area; see Fig. 2.12a) is the so-called stereographic
standard triangle (SST) that is used to describe the activation of different slip
systems with respect to the crystallographic orientation of single crystals or indi-
vidual grains of a polycrystal. The Schmid factor l for an individual crystallo-
graphic orientation is represented by contour lines of constant l value within the
SST. Thus, the slip system with the highest CRSS has a ð111Þ slip plane with a
½
101 slip direction (indicated by line, see Fig. 2.12b) for a crystal orientation with
loading axis lying within this SST. It becomes obvious that the point within the
SST, which is equidistant to ½101 (45° between loading axis and slip direction) and
ð111Þ (45° between loading axis and slip plane normal direction) is the point with
the highest Schmid factor l = 0.5 (see Fig. 2.12c). The slip system with the highest
Schmid factor l at a given applied load is the so-called primary slip system with the
ð111Þ slip plane and ½101 slip direction. Slip systems with lower resolved shear
stresses are the cross-slip, the conjugate and the critical system. The cross-slip

Fig. 2.11 Critical resolved shear stress for activation of slip system. a Definition of angles / and
k for calculation of Schmid factor l. b Activation of slip on multiple parallel slip planes leading to
distortion of the single crystal. Modified according to [3]. Permission of Springer
20 2 Plastic Deformation and Strain Localizations

Fig. 2.12 Dependence of critical resolved shear stress on crystallographic orientation.


a Stereographic standard projection ½001. b Loading path for activation of primary slip system
in fcc crystal lattice. c Schmid factor contour lines (constant µ value) within stereographic standard
triangle (SST). Modified according to [3]. Permission of Springer

system ð111Þ ½101


 contains the same Burgers vector as the primary system and
allows, therefore, for cross-slip. The conjugate system ð11 1Þ ½101 is the slip system
across the boundary ½001—½111 of the SST. The critical slip system ð
 111Þ ½101 is
the system with the lowest critical resolved shear stress.
The co-planar system is the second system sharing the same primary slip plane
—ð111Þ½011. The boundaries of the SST characterize double slip: (i) ½001–½ 111—
conjugate double slip, (ii) ½011–½111—co-planar double slip, and ½001–½011
critical double slip, respectively. The corners of the SST also represent multiple slip
activities on slip systems with identical Schmid factors: (i) ½011: multiple slip on
two slip systems—primary and co-planar plane: (ii) ½ 111 multiple slip on three slip
systems—primary, conjugate and cross-slip, and (iii) ½001 multiple slip on four slip
systems—primary, conjugate, cross-slip and critical plane.
Similarly, the CRSS can be calculated for the activation of partial dislocations or
twinning systems, and also represented by contour lines in the SST. In addition, it is
crucial to calculate the CRSS according to the type of applied uniaxial load—
tension or compression. Thus, Fig. 2.13 shows the SST with indicated contour lines
of l values separated for (a) tensile and (b) compressive loading. The activation of
dislocation glide is represented by red contour lines, whereas the black lines show
the activation of twinning systems. Clearly, different l values for twinning and

Fig. 2.13 Stereographic standard triangle with contour lines of Schmid factors l for the activation
of slip (red) and twinning (black) in fcc crystals. a Tensile loading. b Compressive loading.
Reproduced from [20]. Permission of Elsevier
2.4 Critical Resolved Shear Stress 21

Fig. 2.14 Activation of slip in differently oriented grains of a polycrystalline specimen during
tensile loading. Through the deformation related to the activated single slip, the connectivity at the
grain boundaries would be lost. Thus, gap (black) or overlap (dark grey) of material would be the
consequence (a). Therefore, the activation of secondary slip system (c) is necessary in order to
compensate the deformation caused by the primary slip system (b). In addition, at the grain
boundaries, geometrically necessary dislocations are introduced. Modified according to [3].
Permission of Springer

dislocation glide can be recognized. In addition, the difference in the activation of


both mechanisms during tensile and compressive loading becomes obvious.
The activation of primary slip system lead to displacement with respect to the
loading axis as demonstrated for single crystalline material in Fig. 2.11b, which has
to be compensated by rotation and bending.
In polycrystalline materials, the deformation of individual grains due to acti-
vation of primary slip systems has to be compensated by the activation of further
slip systems (secondary, tertiary) in order to keep the physical integrity at the grain
boundaries (cf. Fig. 2.14). The compatibility at the grain boundaries can be guar-
anteed for two-dimensional considerations by the activation of two independent slip
systems, while for the three-dimensional case, the activation of five independent
systems is required [3]. This was first postulated by Von Mises in 1928 [21, 22].

2.5 Strain Hardening

Plastic deformation of a polycrystalline material is restricted to individual grains


with different orientations separated by grain boundaries, which all together should
deform in a way that the compound of different grains remains undamaged.
According to Schmid’s law, the slip system with the highest critical resolved shear
22 2 Plastic Deformation and Strain Localizations

stress is activated. Thus, grains with a favourable orientation—high Schmid factor


—will be first deformed plastically followed by grains with less favourable ori-
entations. The activation of slip systems in less favourable oriented grains is trig-
gered by the pile-up of dislocations at the grain boundary. The pile-up of
dislocations within an individual grain yields two different stresses. First one is the
so-called back-stress of the pile-up on following dislocations and acts in a direction
opposite to the applied shear stress. The back-stress increases with an increasing
number of dislocations in the pile-up, which is, however, limited by half of the
grain diameter. Back-stresses are long-range order stresses, which cannot be
accommodated locally. The second stress is a forward stress, which is caused by
repulsive forces between individual dislocations within a pile-up. The forward
stresses also act in neighbouring grains and facilitate there the activation of slip
systems due to the increase in the resolved shear stress on the slip systems.
Therefore, the flow stress of a material is determined by the grain size according to
the (2.11):

k
r ¼ r0 þ pffiffiffiffi ð2:11Þ
D

known as the Hall–Petch relationship, where k is the Hall–Petch constant and D the
grain size. Furthermore, the flow stress of a material can be expressed using the
dislocation density according to the Taylor relation [23] given by (2.12):
pffiffiffi
r ¼ r0 þ M  a  G  b  . ð2:12Þ

Here, M is the Taylor factor, a is a factor describing the strength of dislocation–


dislocation interaction depending on type and arrangement of interacting disloca-
tions, G the shear modulus, ~ b the Burgers vector and q the dislocation density. The
Taylor factor for polycrystalline metallic materials with random crystallographic
orientation is given by M ¼ 3:06. The a factor reaches typically values of 0.3–0.4.
However, values in a range of 0.1  a  0.4 are possible [24]. Along with the
dislocation density, the flow stress of a material is a function of applied strain rate
and deformation temperature, i.e. r ¼ f ð.; e_ ; T Þ: Furthermore, the evolution of
dislocation density is strain dependent leading to strain hardening. The evolution of
the dislocation density as a function of the applied strain can be described according
to the Kocks–Mecking model [25] by a balance of production and annihilation of
dislocations:

d. 1
¼M  k2 . ð2:13Þ
de bK

Here, K is the mean free path of dislocations and k2 is the dynamic recovery rate
of dislocations as a function of strain rate, temperature and stacking-fault energy.
Since the mean free path of dislocations is related to the grain size, (2.13) can be
expressed as follows:
2.5 Strain Hardening 23


d. 1 k1 pffiffiffi
¼M þ .  k2 . ð2:14Þ
de bD b

with D as the grain size and k1 as the hardening coefficient of forest dislocations.
The two coefficients k1 and k2 can be determined from the so-called Kocks–
Mecking plot. According to Kubin and Estrin [26], the evolution of dislocation
density as a function of strain has to be distinguished into two dislocation densities
—mobile dislocations .m and sessile (forest) dislocations .f , which are linked with
each other. The corresponding equations can be expressed as follows [26]:

d.m C1 .f C3 pffiffiffiffi
¼M 2  C 2 .m  .f ð2:15Þ
de b .m b

d.f C3 pffiffiffiffi
¼ M C2 .m  .f  C 4 .f ð2:16Þ
de b

Here, C1 describes the dislocation generation, C2 the reduction of dislocation


density due to interaction of mobile dislocations, C3 the limitation of the mobility of
dislocations due to the mean free path caused by spatial arrangement of forest
dislocations, and C4 the dynamic recovery rate of forest dislocations due to climbing
and cross-slip, which is significantly dependent on temperature and strain rate.
The hardening of a material under applied load can be expressed by [25]:

dr
H¼ ; ð2:17Þ
de

which can be separated into a spontaneous part—the hardening rate—and a


dynamic recovery term (negative). The strain-hardening curves can be plotted as ddre
versus r (Kocks–Mecking plot) or as ddre versus e (Hall–Petch plot). A schematic
Kocks–Mecking plot [27] is shown in Fig. 2.15a for a fcc polycrystal in compar-
ison to a fcc single crystal. Clearly, four different stages can be distinguished for the
strain-hardening behaviour of single crystals. Furthermore, different hardening
behaviours of polycrystals in comparison to single crystals can be recognized. For
single crystals oriented for single slip, the hardening curve can be interpreted as
follows: stage I—easy glide on primary slip system with low hardening, stage II—
linear increase in hardening due to multiple slip activities leading to interaction of
dislocations, and, consequently, to sessile dislocations acting as obstacles on further
dislocation motion, and stage III—dynamic recovery with a decrease in hardening
coefficient due to an increase of the annihilation rate mainly caused by cross-slip of
screw dislocations. In pure polycrystalline materials, stages I and II are missing.
The strain-hardening curve is dominated by stage III with continuously decrease in
hardening. In some cases, a stage IV and even stage V are observed with additional
24 2 Plastic Deformation and Strain Localizations

Fig. 2.15 Strain hardening according to Kocks–Mecking model. a Schematical Kocks–Mecking


plot for fcc polycrystal in comparison to single crystals. Modified according to [27]. b Kocks–
Mecking plots of AISI 316LN at different temperatures. Reproduced after [28]. Permission of
Elsevier

decrease in strain-hardening coefficient H. Strain-hardening curves exhibit different


shapes (see e.g. Fig. 2.15b) as a function of the material and applied mechanical
loading.

2.6 Strain Localizations

Localization of strain is a commonly observed phenomenon during plastic defor-


mation of metallic materials leading to final failure. The spectrum of metallic
materials exhibiting strain localization phenomena includes ductile single crystals
(e.g. [29, 30]), polycrystalline materials with various grain sizes (e.g. [31, 32]),
nanocrystalline materials (e.g. [33, 34]) and metallic glasses (e.g. [35, 36]).
Furthermore, plastic strain localizations occur across a broad spectrum of loading
conditions such as uniaxial tensile or compressive deformation, cyclic loading,
multiaxial loading and high-speed deformation. Moreover, strain localizations are
related to different mechanisms and appear on different length scales ranging from
the macroscale to the meso- and microscale [37]. In addition, localization phe-
nomena can be distinguished into stationary and propagative strain localizations
[38]. The occurrence of plastic strain localization is related to the inhomogeneous
deformation at the dislocation scale [36], and is correlated, therefore, strongly to the
microscopic behaviour of the material. Typical strain localization phenomena are:
(i) formation of slip bands and deformation bands; (ii) formation of persistent slip
bands (PSBs) during cyclic deformation; (iii) development of shear bands;
(iv) formation of plastic zone in front of a crack tip; (v) propagation of Lüders
bands; and (vi) propagation of Portevin–Le Chatelier bands, and, finally,
(vii) necking [38, 39]. Whereas phenomena (i–iv) and (vii) are stationary effects,
phenomena (v) and (vi) are single- or multiple-wave propagating effects,
2.6 Strain Localizations 25

Fig. 2.16 Schematic overview on strain localizations. a Stationary strain localizations.


b Propagative strain localizations Modified according to [38]. Permission of Trans Tech Publ

respectively [38]. Although the formation of slip bands, persistent slip bands or
deformation bands are localized phenomena on the micrometre scale, the macro-
scopic plastic deformation behaviour remains homogenous. In contrast, the local-
ization phenomena of Lüders bands and PLC bands lead to macroscopic
inhomogeneous deformation that results in serrations in the macroscopic
stress-strain curve. Figure 2.16 provides a schematic overview of the different types
of strain localizations according to [38].
Quite often, strain localization phenomena are related to strain softening beha-
viour of the investigated material, i.e. the local strain-hardening coefficient becomes
negative [37]. As softening mechanisms (i) multiplication softening, (ii) structural
softening and (iii) geometrical softening can be distinguished [37], the multipli-
cation softening is related to a rapid increase in the density of mobile dislocations
after yield. Thus, strain softening occurs in materials with poor initial dislocation
density at very low strains such as for dislocation lack yield point. The structural
softening is correlated to the decrease in the dislocation glide resistance. Here,
obstacles on the dislocation motion such as point defect agglomerates (irradiated
materials), shearable precipitates, an enhanced lattice resistance due to SRO or
unstable dislocation arrangements are swept out during further straining.
Geometrical softening is caused by either slip plane rotation, textural softening in
polycrystals or simply by the increase in stress due to decrease in the cross section
of a specimen during a tensile test [37].
However, strain localization can be observed also for materials exhibiting
strain-hardening effects, which was first supposed by Asaro and Rice for ductile
single crystals [40]. Even in numerous polycrystalline materials exhibiting
macroscopically homogenous deformation in combination with pronounced strain
hardening like high-strength steels showing transformation-induced plasticity
(TRIP) or twinning-induced plasticity (TWIP), plastic strain localizations occur on
a microscopic level in terms of the grain size of the material (e.g. [41]).
In general, strain localizations are the consequence of the loss of uniform
deformation causing strain inhomogeneities and plastic instabilities [42]. The most
common macroscopic localization of plastic flow is the onset of necking during
26 2 Plastic Deformation and Strain Localizations

tensile loading of metallic materials. At this point, the cross section of the specimen
is continuously reduced resulting in a significant loss of stress in the stress-strain
curve [36]. The first criterion that described plastic instability is well-known as the
Considére criterion [43]. Here, the criterion of plastic instability is the point, where
the strain-hardening coefficient H becomes equal to the flow stress r at a given
strain rate [36] (2.18):

dr
H ¼r ð2:18Þ
de e_

Here, the deviation of strain de is used as a measure of the local non-uniformity.


Further criterion of plastic instability is the so-called Hart criterion [44], which is
based on the absolute cross-sectional deviation dA as the parameter describing the
non-uniformity [45]. Kubin and Estrin introduced three different types of instability
criterions: (i) h-type criterion; (ii) S-type criterion; and (iii) T-type criterion [42, 45,
46]. In their description, they use the relation between stress and strain and their
time derivatives according to (2.19) [45]:

dr ¼ h de þ S d log e_ ð2:19Þ

Here, h and S are the two intrinsic material parameters known as the
strain-hardening rate h and the strain-rate sensitivity S. Thus, the h-type instability
refers to strain-hardening behaviour of a material, which is, consequently, quite
comparable to the Considère criterion. The S-type criterion is related to the
strain-rate sensitivity, and the most common S-type instability is the occurrence of
PLC effect, which is caused by a negative strain-rate sensitivity due to dynamic
strain ageing. T-type criterion is obtained by coupling (2.19) with the heat equation
and describes the interaction between strain rate and temperature increase. T-type
criterion is the instability criterion particular in case of formation of adiabatic shear
bands [45].
Since the invention of the first criterion of plastic instability by Considère in
1885 [43], the phenomenon of plastic strain localization has been the focus of an
incredibly huge number of investigations. In the past, several review papers are
concerned with summarizing different aspects of strain localizations. Thus, Rice
[31] focused on the localization of plastic deformation in shear bands including
review on experimental observations, presentation of theoretical framework and
calculations of critical conditions for a variety of model materials. The review of
Bréchet and Louchet [38] provides a classification of different strain localization
phenomena. In addition, characteristic lengths of the spatial organization are
defined. Furthermore, some criteria for plastic strain localization are proposed.
Quite recently, Antolovich and Armstrong [47] provided a detailed review that
explains mechanisms and consequences of plastic strain localizations on macro-
scopic and microscopic length scale during tensile stress-strain behaviour, fatigue
loading and fracture.
2.6 Strain Localizations 27

2.6.1 Strain Localizations on Microscopic Scale

Localized plastic deformation on the micrometre scale as a function of the activated


deformation mechanisms (dislocation glide, mechanical twinning) leads to several
inhomogeneities of the deformed microstructure. However, the different
microstructural features of deformed materials are very often confused with each
other and the same term is used to describe quite different features. Most popular
candidate for such confused use is the term “shear band”, which is used for a wide
range of microstructural features including “slip line”, “slip band”, and the classical
shear band after severe plastic deformation. Blicharski et al. [48] provided a clas-
sification of main types of deformation inhomogeneities. Based on [48] and further
literature the following classification is provided.

2.6.1.1 Slip Bands/Deformation Bands

Slip bands (SB). Slip bands indicate regions, which are crystallographically con-
sistent with the traces of slip planes of activated slip systems during plastic
deformation. They appear on a polished specimen surface as slip steps or slip lines
(see Fig. 2.17a, b). Due to their crystallographic nature, they are restricted to the
grain size of the material. Thus, primary slip bands and secondary slip bands can be
distinguished depending on the crystallographic orientation and, consequently, on
the resolved shear strain of individual grains. In addition, bands related to pro-
nounced cross-slip, as in bcc materials, can be distinguished—known as wavy slip
bands [49]. Thus, SB are observed in many metallic materials (fcc, bcc, hcp) under
quasi-static loading conditions.

Fig. 2.17 Typical examples of microscopic strain localizations. a Fine slip lines in a
polycrystalline nickel specimen under tensile loading interrupted at the yield point. b Slip bands
in a polycrystalline nickel specimen under tensile loading between yield point and uniform
elongation. c Deformation bands in a polycrystalline steel specimen under tensile loading
interrupted at uniform elongation
28 2 Plastic Deformation and Strain Localizations

Deformation bands (DB). The term “deformation band” is related to band-like


regions with deviating strain state in comparison to the surrounding material, which
is often accompanied by variation in orientation or dislocation density. Thus, it
includes either regions with fine deformation twins or stacking faults. Since DBs are
correlated also to the crystallographic nature due to deformation mechanisms like
dislocation glide or twinning, DBs are also restricted to the grain size of the
investigated material.
Figure 2.17 summarizes examples for the appearance of slip line, slip bands and
deformation bands on a polished specimen surface.
Slip lines, slip bands as well as deformation bands occur during static monotonic
loading (tension, compression) as well as during heavy plastic deformation like
sheet metal forming. They are the consequence either of dislocation glide (SB),
formation of stacking faults (DB) or micro twinning (DB). The strain localization in
these cases is related to pile-ups of regular dislocations or partial dislocations and is,
consequently, influenced by the grain size of the investigated material. The grain
boundaries of a material act as barriers for the dislocation motion leading to
pile-ups. In addition, dislocation sources in the grain interior (Frank–Read sources)
are active during plastic deformation. Thus, decreasing grain size will lead to
so-called double-ended slip bands by pile-ups on two opposite grain boundaries.
Consequently, stress concentrations arise at grain boundaries leading either to
activation of parallel slip bands in proximity within the same grain or to slip transfer
in neighbouring grains. In case of single-ended slip band or single-ended pile-up
(large grain size), when the slip band does not cross completely the whole grain, the
average shear strain can be expressed by the following (2.20) [47]:

nb
c¼ ð2:20Þ
2L

Here, n is the number of dislocation, ~


b the Burgers vector and L the length of the
slip band or pile-up.

2.6.1.2 Persistent Slip Bands

Strain localizations occur under cyclic loading conditions as well. They play an
important role in the understanding of the phenomenon of fatigue of ductile
materials. Fatigue is a process of degradation of a material under cyclic loading,
which includes crack initiation and crack propagation leading to final fracture.
Fatigue is the result of repetitive cyclic loading below the ultimate tensile stress of a
material and, quite frequently, even below the yield strength. The crack initiation is
correlated directly with the appearance and, even more, with the frequency of strain
localizations, which depends itself on the microstructure and the dislocation glide
behaviour.
Strain localizations occurring during cyclic deformation often form so-called
persistent slip bands (PSBs). The first observation of pronounced localized surface
2.6 Strain Localizations 29

slip marking dates back to investigations of Ewing and Humfrey [50] on poly-
crystalline Swedish iron. The term “persistent” was introduced firstly by Thompson
et al. [51] by investigations of cyclic deformation behaviour of Cu single and
polycrystals and is attributed to the fact that slip markings appeared after
re-polishing and continued cyclic straining at the same places on the specimen
surface. In old literature, these surface slip markings are called slip bands, intense
slip lines, fatigue deformation markings, fatigue bands, slip striations or slip
markings. Today, the term persistent slip markings (PSMs) has been well estab-
lished [52]. The PSMs are characterized by a pronounced surface relief consisting
of extrusions and intrusions. Although it is agreed commonly that the PSMs are
favoured places for crack initiation during cyclic deformation (e.g. [53–55]), “…
the exact mechanism of fatigue crack nucleation has not been totally clarified …”
[56]. TEM investigations by Laufer and Roberts [57, 58] revealed a specific dis-
location arrangement in the region of PSBs, which consists of dislocation dense
walls formed by edge dislocation dipoles and nearly dislocation-free channels
forming a so-called ladder-like structure. However, other appearances of PSBs than
ladder-like structure are also known in the literature depending on the dislocation
glide behaviour.
The schematic drawing in Fig. 2.18 illustrates the appearance both of PSB and
of PSM in combination with typical dislocation arrangements of the matrix and the
PSB. The dislocation arrangement of the matrix represents the so-called “vein”
structure, which consists of bundles of edge multipoles. The dislocation arrange-
ment of PSB contains dislocation dense walls formed by edge dipoles and channels
with few screw dislocations. Figure 2.18b shows that bowed-out screw dislocations
are gliding between the walls. In addition, edge dislocation segments bow-out of the
walls and travers them. Due to these edge segments, the dislocation density is
increased since new screw segments are produced within the channels.

Fig. 2.18 Microscopic strain localization during cyclic loading. a Schematic drawing of cyclic
strain localization in a persistent slip band (PSB) emerging at the specimen surface as persistent
slip marking (PSM). Reproduced from [52]. Permission of Taylor & Francis. b Schematic drawing
of the dislocation wall and dislocation channel configuration of the ladder-like structure of PSB.
Reproduced from [59]. Permission of Elsevier
30 2 Plastic Deformation and Strain Localizations

Fig. 2.19 Microstructural features of cyclic strain localization. a Persistent slip markings.
b Extrusions and intrusions of persistent slip markings. c Dislocation arrangement of persistent slip
bands. All examples are SEM micrographs  belonging
 to polycrystalline nickel deformed cyclically
at ea;p ¼ 5  104 up to 30,000 cycles 0:6 Nf

In general, PSBs are band-like structures having a thickness of few micrometres


up to several tens of micrometres and extending across an entire single crystal or
across grains in polycrystalline material as shown in Fig. 2.19. The formation of
PSBs depends both on several microstructural parameters and on different param-
eters of the cyclic loading. Thus, the stacking-fault energy cSF , the grain size D, the
grain orientation, but also the plastic strain amplitude ea;p , the number of cycles or
the deformation temperature T can influence significantly the cyclic deformation
behaviour and the appearance of PSBs.
Figure 2.20a provides a general overview of the plastic strain amplitude ea;p and
the character of the dislocation glide behaviour on the dislocation arrangements of
the matrix as well as the region of appearance for PSBs [60]. As demonstrated by
Fig. 2.20b the grain orientation, respectively, the orientation of the loading axis

Fig. 2.20 Dislocation pattering during cyclic loading in fcc materials. a Influence of dislocation
glide behaviour and plastic strain amplitude on the appearance of PSBs. Modified according to
[60]. Permission of Elsevier. b Influence of grain orientation (loading axis) on the dislocation
patterning of the matrix. Reproduced from [61]. Permission of Elsevier
2.6 Strain Localizations 31

(LA) has a significant influence on the dislocation patterning in the matrix. Thus,
dislocation arrangements of the matrix can be categorized into four typical struc-
tures: (i) wall structure, which occurs in grains with a LA close to h111i direction;
(ii) labyrinth structure in grains with LA parallel to h001i; and (iii) patch structure
for grains with a h110i LA. Typical bundle structure (iv) is observed for middle
orientated grains (highest Schmid factor, 0.5). PSBs are observed in nearly all grain
orientations, but most frequently within the bundle structure. Increasing plastic
strain amplitude has a significant influence on the wall thickness dw and the channel
width dc (cf. Fig. 2.20b) of the dislocation arrangement both in the matrix and
within the PSB. Thus, the wall thickness becomes smaller whereas the channel
width increases with an increase of the plastic strain amplitude [61].
The localized cyclic shear strain amplitude of an individual SB within a PSB can
be calculated using the crystallographic orientation data of the activated SB as well
as the height of slip steps occurring on a re-polished specimen surface after con-
tinuing half-cycle deformation. Whereas the crystallographic orientation data are
obtained from electron backscattered diffraction (EBSD) measurements, the height
of slip steps within the persistent slip band are measured by atomic force micro-
scopy (AFM). The shear strain amplitude of an individual SB can be then calculated
according to (2.21) [62]:
up;i
cSB;i ¼ ð2:21Þ
2 Di

Here, up;i is the displacement in the direction of the Burgers vector ~b and Di is
the thickness of the activated SB in the direction of the slip plane normal.
According to this procedure, the shear strain amplitudes of slip bands occurring in
cyclically deformed single and polycrystals of nickel were calculated. It was found
that the shear strain amplitudes observed in single and polycrystals are quite similar
in a range between 0.2 and 5% [63]. However, whereas the shear strain is quite
similar, the activated volume fraction of PSBs during re-cycling is quite different
(30% of PSBs in single crystals and 1% in polycrystals, only [63]). Thus, obviously
the grain size has not a significant influence on the absolute value of the strain
localization within the PSBs, however, the activated volume fraction is reduced
significantly.

2.6.1.3 Shear Bands

The term “shear band” is a term used commonly for general microstructural
inhomogeneities, since no clear definition exists. In general, shear bands are a
typical feature of inhomogeneous deformation, which covers microscopic and
macroscopic aspects. The origin of shear bands is related to microstructural inho-
mogeneities. Thus, they occur at large plastic deformations during quasi-static and
dynamic tensile and compressive loading accompanying necking behaviour and at
heavy deformations such as metal forming (rolling). Majority of investigations was
32 2 Plastic Deformation and Strain Localizations

performed on fcc metals and alloys (e.g. [64–66]). Summarizing numerous inves-
tigations, it turned out that a huge number of technical and microstructural
parameters such as loading conditions, grain size, crystal lattice, stacking-fault
energy and microstructure of the investigated materials determine the occurrence of
shear bands as well as their appearance.
Nevertheless, common features of shear bands are (i) their non-crystallographic
appearance and (ii) their different dislocation arrangement and crystallographic
orientation in comparison to the surrounding matrix [65]. The non-crystallographic
nature of shear bands becomes apparent from their arrangement of typical angles
between 35° and 54° with respect to the loading axis. In addition, shear bands
develop across the grain structure. Thus, so-called micro shear bands are running
over a distance of few grain diameters, whereas so-called macro shear bands can
pass the whole cross section of specimens. Furthermore, shear bands are developing
in a characteristic dislocation arrangement of the matrix material, which depends on
the specific microstructure and the SFE of the material. Whereas the orientation
along with the shear bands is unique, the crystallographic orientation within the
band deviates from the surrounding. In addition, they are characterized (iii) by large
amount of carried shear. Therefore, shear bands are favoured places for dynamic
recrystallization leading to a softening and, finally, to degradation of the material
[65].
In combination with shear bands, another form of strain localization has to be
regarded–so-called micro bands [48]. Micro bands are related to the dislocation
arrangement in the microstructure. They appear as straight plate-like areas with a
typical thickness of around 0.1 µm delineated by two sharp parallel dislocation
walls. Micro bands are related to the slip planes and extend across the entire grain
diameter. Due to the localized shear, micro bands form characteristic steps of
intersecting dislocation layers, other micro bands, grain boundaries or deformation
twins. During deformation, the micro bands rotate parallel to the loading direction.
Depending on the SFE, two general types of shear bands can be categorized:
(i) copper (C)-type shear bands and (ii) brass (Bs)-type shear bands as shown in
Figs. 2.21a, b. C-type shear bands occur in materials with higher SFE, where the
plastic deformation is carried by dislocation glide and pronounced cross-slip. In
general, the C-type shear bands are few micrometres thick only and are correlated to
a lamellar arrangement of micro bands. In contrast, Bs-type shear bands develop in
materials with medium and low SFE, where the dislocation glide is restricted to
planar slip without cross-slip. Furthermore, in these materials mechanical twinning
occurs even at lower deformations. The formation of Bs-type shear bands is con-
nected to the formation of a lamellar structure consisting of microtwins arranged
parallel to the loading axis. The Bs-type shear bands consist of dislocation cells,
which are elongated in the direction of the shear band and exhibit a relatively large
misorientation [48].
At dynamic deformation conditions, a third type of shear bands can be identified
—the adiabatic shear bands [48]. Adiabatic shear bands are narrow, nearly planar or
two-dimensional regions of very large shear. A fully developed adiabatic shear
band results in a remarkable displacement of the sheared regions keeping physical
2.6 Strain Localizations 33

Fig. 2.21 Typical appearances of various kinds of shear bands. a Macroscopic shear bands in a-
brass. b TEM micrograph of Brass-type shear band (SB) with crossing the lamellar structure of
twin/matrix. c TEM micrograph of Copper-type shear band in pure copper [65]. d Macroscopic
shear bands in austenitic stainless steel. e Adiabatic shear bands after compression tests of
aluminium alloy 7083 at strain rate 8  103 s−1 [66]. a, b After cold rolling with 95% of thickness
reduction. c After cold rolling up to 97% of thickness reduction. d After cold rolling with 90% of
thickness reduction. Permission of Elsevier

integrity. The thickness of the heavily sheared region is in the order of few tens of
micrometres only or even less, whereas the lateral extent can reach several mil-
limetres up to centimetres as shown in Fig. 2.21e resulting in a high aspect ratio.
General features of adiabatic shear bands can be summarized as follows: (i) thin
layer perpendicular to the direction of maximum shear, (ii) high aspect ratio,
(iii) high external strain, (iv) extreme internal strain, and (v) dynamic generation.
Adiabatic shear bands extend across the specimen independent of the current
microstructure. The origin of adiabatic shear bands is related to inhomogeneities in
the dislocation substructure leading to avalanches of dislocations accompanied by
localized heating and premature failure. Promoting conditions for the formation of
adiabatic shear bands are low thermal conductivity and low heat capacity, high
density, high strain rates as well as low temperatures.

2.6.2 Strain Localizations on Macroscopic Scale

Along with the common localization of plastic deformation during monotonic


tensile deformation in form of necking, further macroscopic localization phenom-
ena are known, leading to characteristic changes in the stress-strain curves—
well-known as serrated plastic flow. The serrated plastic flow manifests in two
effects: (i) Lüders effect and (ii) Portevin–Le Chatelier effect. Both effects are
caused by the microscopic mechanism of dynamic strain aging (DSA). DSA is a
34 2 Plastic Deformation and Strain Localizations

solid solution strengthening mechanism, which occurs in a variety of fcc and bcc
alloys with interstitial or substitutional alloying elements [67].
The explanation accepted commonly for the DSA is related to the Cottrell theory
of kinetics of dislocations [68]. Cottrell and Bilby [68] showed, especially for bcc
iron, that the interaction of interstitially dissolved carbon with dislocations is
responsible for the formation of instabilities in the macroscopic deformation
behaviour—known as the Cottrell effect. Whereas this model assumed
quasi-viscous movement of dislocations, it was shown by Kocks et al. [69] that the
dislocation motion is in principle of jerky manner. During plastic deformation, the
movement of dislocations is hindered and arrested due to their interaction with
immobile dislocations (forest dislocations). Thus, the interaction of solute atoms
with dislocations occurs during the arrest time of mobile dislocations on obstacles
and not directly during the motion of dislocations [67, 70, 71]. At a certain stress,
arrested mobile dislocations will overcome these obstacles and continue moving
until arrested by the next obstacles. Thus, repeated dislocation avalanches occur due
to unpinning of dislocations from solutes with increasing strain [72–75]. However,
the interaction of solute atoms with stacking faults has to be regarded in fcc solid
solutions—known as the Suzuki effect [76]. Here, the impediment of dislocation
motion is caused by solute atoms segregating at stacking-fault ribbons and anchor
these ribbons [77].
Consequently, both the Cottrell effect and the Suzuki effect change the spatially
homogenous deformation into an inhomogeneous and unstable deformation
resulting in strain localizations.
The pronounced yield point occurring due to unpinning of dislocations from
interstitials or solute atoms has to be distinguished from the dislocation lack yield
point. A comparison of both yield point effects is shown in Fig. 2.22. The dislo-
cation lack yield point occurs mainly in materials with a low dislocation density (cf.
Fig. 2.22a). At the beginning of plastic deformation the few dislocations present in
the material are accelerated. At the maximum stress—the upper yield point—dis-
location multiplication occurs, which results in a decrease in stress, and after

Fig. 2.22 Difference between dislocation lack yield point and pronounced yield stress due to
unpinning of dislocations. a Dislocation lack yield point caused by dislocation multiplication and
interaction. b Pronounced yield strength as a consequence of Cottrell effect. Modified according to
[78]. Permission of Springer
2.6 Strain Localizations 35

passing the lower yield point, the stress is increasing again due to strain hardening
caused by interactions of dislocations [78]. As higher as the prior dislocation
density is as lower is the dislocation lack yield point. Thus, for metals with an initial
dislocation density .0 ¼ 1010 m2 and a high dislocation velocity no pronounced
dislocation lack yield point will be observed [78]. In addition, Hahn [79] showed
even for bcc metals that along with interstitial atoms the yield point phenomenon
can be caused as well by rapid multiplication of dislocations.

2.6.2.1 Lüders Effect

The Lüders effect is a well-known phenomenon occurring in materials experiencing


tensile stresses resulting in an instability at the transition from elastic to plastic
deformation behaviour [80]. A typical stress-strain curve is shown in Fig. 2.23. The
stress-strain curve can be classified into four different stages: (i) upper yield point,
(ii) drop of the flow stress, (iii) increase in strain at nearly constant stress level and
(iv) work hardening. At stage (ii) a band of localized strain develops between the
deformed and non-deformed material [81, 82]. The time for the formation of a
Lüders band can be referred to the average time needed for unpinning and mobi-
lization of dislocations [83, 84] or rapid dislocation multiplication.
The individual band propagates with the cross-head velocity along the entire
gauge length. The tilt angle of the Lüders band to the loading axis varies between
40° and 70°—rarely 90° [85–89]. During propagation of a band to the other end of
a specimen, strain is increasing without any significant increase in stress level. If the
band reaches the end of the gauge length, classical strain-hardening occurs.
Main observations of Lüders phenomenon were done in the far and newer past
on various kinds of steels (low-carbon steels: e.g. [84, 85, 90, 91]; TRIP steels: e.g.
[92]).
Lüders bands initiate preferably at the shoulder parts of a tensile specimen since
internal stresses tend to be larger in these parts. Thus, bands can initiate on the two
opposite shoulder parts propagating to the middle of the gauge length or only one
band initiates on one shoulder part moving to the other end of a specimen.

Fig. 2.23 Stress-strain curve


of a material with Lüders
effect. Modified according to
[93]. Permission of De
Gruyter
36 2 Plastic Deformation and Strain Localizations

Furthermore, the macroscopic geometry of specimens has an influence on the


formation of Lüders bands. Thus, specimens with rectangular or square cross
section exhibit a higher tendency for the formation of Lüders bands in comparison
to specimens of identical chemical composition with a circular cross section.
However, along with these macroscopic aspects, the occurrence of Lüders bands is
determined by microstructural features such as crystal lattice, grain size, dislocation
density or content of interstitial atoms.
Thus, the Lüders effect in low-carbon steels is influenced significantly by carbon
content, test temperature and strain rate. The Lüders strain decreases with increase
of ferrite volume fraction [94], test temperature, carbon content [84, 91, 94–96] and
strain rate [85, 92, 94]. In addition, Johnson et al. [84] and Sun et al. [90] reported
an increase in Lüders strain and band velocity with increasing strain rate. Tsuchida
et al. [91] found the following empirical correlation between Lüders strain- and
work-hardening rate at lower yield stress (LYS), which is independent of temper-
ature, strain rate, carbon content and microstructure including ferrite grain size:

eL  ðdr=deÞLYS ¼ 80 MPa ð2:22Þ

Compared to carbon steels, Lüders band effect in high-strength TRIP steels is not
characterized by pronounced stress drop. The band formation is caused by lower
initial strain hardening [92]. The Lüders effect in high-Mn TRIP-assisted steels
depends on mechanical stability of retained austenite. This stability is dedicated to
chemical composition, size and shape of the austenite [97]. In these steels, stress
drop occurs due to formation of stress-assisted martensitic phase transformation due
to metastable character of the austenitic phase with a low stacking-fault energy and
heterogeneous micro plasticity between phases. The generation of stress-assisted
martensite in the range of Lüders strain is connected closely with stress concen-
tration in phases of d-ferrite [92, 98]. Fahr [96] explained the Lüders effect caused
by formation of deformation-induced martensite. Oliver et al. [99], however,
observed formation of martensite after passing Lüders strain plateau.
Furthermore, the Lüders strain increases with an increase in dislocation density
and, consequently, with a decrease in mean free path of dislocations [84, 100].
A decreasing grain size causes an increase in the Lüders strain and yield strength
[83–85, 88, 91, 94, 95, 100, 101]. Therefore, the yield point phenomenon and
inhomogeneous straining of the Lüders band propagation depends on the grain size
[86, 92, 101, 102]. Frequently, the Lüders effect occurs below 2 µm grain size [83,
87, 103, 106]. Tsuji et al. [103] observed the Lüders effect in an ultrafine grained
(ufg) IF-steel with an equiaxed grain structure and an average grain size of about
1 µm, which is nearly free of dislocations. In an ufg aluminium investigated by Yu
[87] the upper range of mean grain diameter was about 4 µm for the occurrence of
Lüders band effect. Cheng [102] observed at an ufg material (Fe–10Cr–5Ni–0.1C)
with a grain size of 200 nm that the Lüders band developed on one end of the gauge
length and propagated to the other end while the specimen was strained.
2.6 Strain Localizations 37

The size of the plateau region in the stress-strain curve attributed to the Lüders
effect depends on the band propagation. The growth of the Lüders band terminates
when the band reaches the other end of the gauge length. Subsequently, the normal
strain-hardening sets in. The decrease in grain size results in a reduction of work
hardening, and in a loss of uniform elongation [104]. Furthermore, smaller grain
sizes favour the development of one single Lüders band, whereas for coarser grain
sizes, the development of multiple or diffuse Lüders bands was observed [85, 107].
Further studies described the Lüders effect as a consequence of shear strain,
which effects macroscopic shaping and activation of new dislocations [86, 87, 108].
As a result, the material creeps below the yield point. The shear strain component is
depending on the grain size, while the shear strain direction is not equal with the
direction of the Lüders slope. Korbel et al. [109] discovered the reason for Lüders
effect in the dynamical formation of dislocation pile-up at grain boundaries. Thus,
an upper yield point and Lüders strain can be observed in every material sufficient
small grain size provided.

2.6.2.2 Portevin–Le Chatelier Effect

The second type of propagating strain localizations during tensile straining of


materials leading to discontinuities in the stress–strain curve caused by DSA is the
so-called Portevin–Le Chatelier (PLC) effect. Here, serrated plastic flow as shown
in Fig. 2.24 is observed for given strain rate and temperature.
The explanation accepted commonly for the occurrence of serrated plastic flow
is DSA comparable to the Lüders effect. The plastic strain localizes as well in
macroscopic bands with thicknesses of few millimetres–so-called PLC bands—
which emerge and propagate along the gauge length. The initiation and propagation
of these bands lead to discontinuities in stress-strain curve, which appear as stress
drops. Three major types of PLC bands were classified [110–112] with different
appearance of discontinuities in the stress-strain curve as shown in Fig. 2.25. Type

Fig. 2.24 Example of serrated plastic flow caused by dynamic strain aging. Stress-strain curves of
an Al–3.5% Mg alloy tensile deformed at RT and two strain rates resulting in different appearances
of serrated plastic flow. Reproduced from [113]. Permission of Elsevier
38 2 Plastic Deformation and Strain Localizations

Fig. 2.25 Three main types of PLC bands. a Type A bands: Each stress drop is related to the
initiation of a new band. b Type B bands: Several bands initiate volatile but correlated. c Type
C bands: Several bands initiate in a stochastic way at different places. Modified according to [112].
Permission of Elsevier

A bands initiate due to stress concentrations on one side of the gauge length and
propagate along the entire gauge length. At the end of the gauge length, either the
band is reflected or a new band initiates moving in opposite direction. Type A bands
lead to smooth stress drops in the stress-strain curve and each individual serration is
related to the initiation of a new band. The smooth part between two successive
serrations is related to the propagation of the band [112, 114]. In contrast, type
B bands propagate in a continuous manner only over short distances. Bands appear
in a volatile, however correlated, way along the gauge length. These bands result in
irregular shaped discontinuities in the stress-strain curve with undefined amplitudes
and frequencies resulting from a discontinuous propagation behaviour [114, 115].
Type C bands appear stochastically and non-correlated at different parts of the
gauge length. The corresponding stress-strain curves show relatively equal dis-
continuities in form of stress drops only with defined amplitudes and frequencies.
All band types propagate along the gauge length and produce undesirable traces at
the surface [114, 115].
The propagating PLC bands can be characterized by following parameters:
(i) the band width of localized strain wB ; (ii) the band velocity cB ; and (iii) the strain
jump caused by the PLC band DeB shown in Fig. 2.26.
For the nucleation of an individual PLC band, the following correlation of band
parameters can be given by (2.23) [112]:

cB  DeB ¼ wB  eB;t ¼ v ð2:23Þ

Fig. 2.26 Parameters


describing the strain jump, the
velocity and the width of PLC
bands occurring during
serrated plastic flow.
Modified according to [115,
116]
2.6 Strain Localizations 39

Here, eB;t is the local strain rate within an individual PLC band and v is the
cross-head velocity. Equation (2.23) is valid for individual band propagation. If two
or more bands are nucleating and propagating, the local strain rate of each band is
contributing to v. Typical band velocities cB are about 4–10 mm/s and are within
individual bands constant. However, the average band velocity is decreasing for
PLC bands propagating subsequently. Furthermore, PLC bands are characterized by
strain localization (e.g. [117, 118]) as well as temperature increase (e.g. [119–121]).
The PLC effect was observed and studied since several decades on different
types of materials such as Cu–Zn alloys (e.g. [122, 123]), Al–Mg alloys (e.g. [119,
124–127]), various types of steels [128] (ferritic steels (e.g. [68, 129–133]), aus-
tenitic steels (e.g. [134–137]), TWIP steels (e.g. [121, 138–143]) or Ni-base
superalloys (e.g. [144, 145]).
The occurrence of PLC effect is associated with either substitutional or inter-
stitial atoms in fcc alloys (e.g. Mg in Al alloys, C in Ni-base superalloys) and with
interstitials (C, N) in bcc alloys. Figure 2.27 shows stress-strain curves for five
typical classes of materials exhibiting PLC effect: (i) ferritic steels (e.g. [133]),
(ii) austenitic steels (e.g. [134]), (iii) TWIP steels (e.g. [142]), (iv) Al–Mg alloys
(e.g. [125]) and (v) Ni-base superalloys (e.g. [145]). Thus, the large spectrum of
occurrence and appearance of the PLC effect becomes obvious. Whereas in Al–Mg
alloys and TWIP steels, the PLC effect occurs already at RT, in ferritic steels,
Ni-base superalloys and austenitic steels the temperature range for occurrence of the
PLC effect is well above RT.

Fig. 2.27 PLC effect in different type of alloys. a Ferritic steel. b Austenitic steel AISI 304.
c TWIP steel. d Al–Mg alloy AA5052. e Ni-base superalloy. Reproduced from [133] (a), [134]
(b), [142] (c), [125] (d), [142] (e). Permission of Elsevier
40 2 Plastic Deformation and Strain Localizations

In ferritic steels, the PLC effect is observed already at 250 °C. In contrast,
temperatures above 400 °C are necessary in austenitic steels. Furthermore, it is
visible that the shape of stress serrations changes significantly with the increase in
temperature. In principle, type A and B PLC bands are observed at lower temper-
atures, whereas type C bands dominate at higher temperatures.
One indicator for the occurrence of the PLC effect is a negative pstrain-rate
sensitivity (SRS). Commonly, positive SRS is observed in pure metals, since stress
is increasing with an increase in strain rate due to higher activation of glide dis-
locations. However, in case of DSA, the interaction of glide dislocations with solute
atoms has to be taken into account. Thus, during time, where dislocation-free
motion is interrupted by obstacles, solute atoms can diffuse to dislocations and pin
them. Consequently, the larger the arrest time of mobile dislocations on obstacles is
the higher is the stress to unpin the dislocations from the obstacles. The SRS S is
defined as the dependence of the stress on the strain rate at a certain strain [146]:

dr
S¼ ð2:24Þ
d_e e

The SRS can be separated into an instantaneous SRS Si and an asymptotic SRS
S1 as shown in Fig. 2.28a. Here, Si is always positive and reflects the spontaneous
stress response at an acute change of the strain rate. Sas is related to the asymptotic
change of flow stress after strain rate jump. Sas can be either positive or negative
[147].
The interplay between DSA, SRS and dislocation interaction is depicted by
Fig. 2.28b. Thus, due to DSA the SRS is lowered. Concurrently, the reduced SRS
results in change of dislocation motion from a disordered mode into a collective
mode. Thus, once a collective mode of dislocation motion is reached, SRS becomes
even negative and plastic deformation is localized within bands [148].
Major factors influencing the occurrence of PLC effect, the stress-strain
response, the type of PLC bands as well as the mechanical properties are (i) tem-
perature, (ii) strain rate and (iii) grain size (e.g. [118, 121]).

Fig. 2.28 Strain-rate sensitivity. a Instantaneous and asymptotic strain-rate sensitivity.


Reproduced from [147]. b Interplay between dynamic strain aging, strain-rate sensitivity and
dislocation interaction. Modified according to [148]. Permission of Elsevier
2.6 Strain Localizations 41

Temperature and strain rate. Both parameters have a significant influence on


the occurrence of PLC effect since they affect the velocity of both mobile dislo-
cations and diffusing solute atoms. Increasing temperature will result in higher
mobility of diffusing solute atoms since the mobility of point defects and the
number of vacancies—both necessary conditions for diffusion—are enlarged. On
the other side, the strain rate influences the velocity of glide dislocations as well as
the number of dislocations nucleating during the plastic deformation. At lower
strain rates, the arrest times of mobile dislocations on obstacles is increasing. Thus,
at low temperatures and high strain rates, the velocity of diffusing solute atoms is
low in comparison to the velocity of gliding dislocations. Likewise, at high tem-
peratures and low strain rates, the velocity of solute atoms is comparable to or
higher as the velocity of mobile dislocation. Under these two conditions, no PLC
effect will occurs. Consequently, the occurrence of PLC effect is limited to medium
temperatures and strain rates. The increase in temperature and a decrease in strain
rate shifts the critical strain for the onset of serrated flow in the stress-strain curve to
lower strain values (e.g. [118, 135, 149]).
Grain size. Along with temperature and strain rate, grain size also influences the
occurrence of PLC effect. Smaller grain sizes have a promoting effect on PLC
effect. Thus, the critical strain for the onset of serrated flow is reduced and the band
velocity is increased due to smaller grain sizes (e.g. [111, 121, 140]).
Further factors influencing the occurrence of PLC effect are (i) dislocation
density, (ii) type of solid solution (SS), i.e. interstitial SS or substitutional SS,
(iii) specimen geometry and (iv) surface roughness of specimens. Korbel and
Pawelek [109] showed that an increase in initial dislocation density results in a
decrease in band velocity and, however, in an increase in localized strain within
individual bands. The increase in vacancy concentration during plastic deformation
has more influence on the diffusion in substitutional SS than in interstitial SS. Chen
et al. [150] found in different fcc alloys an Arrhenius relation between the tem-
perature and the critical strain for the onset of the PLC effect.

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Chapter 3
Martensitic Phase Transformation

Abstract This chapter provides a summary of basic knowledge on martensitic


phase transformation in general and in steels, in particular. Besides the thermo-
dynamic aspects of martensitic phase transformation, the different transformation
path’s (direct c to a’, direct c to e, direct e to a’ and indirect c to e to a’) occurring in
steels are described in detail in combination with the relevant orientation rela-
tionships. In addition, the influence of stacking-fault energy is discussed. Finally,
the kinetics of the martensite transformation process is described according to the
well-known Olson–Cohen model.

3.1 General Considerations

Martensitic phase transformation (MPT) is a diffusionless, solid–solid, first-order


phase transition, in which the initial and final phases differ in their crystal sym-
metry. In general, the high-temperature phase is called austenite and the
low-temperature phase is called martensite [1]. Thus, instead of long-range diffu-
sion, MPT occurs by cooperative, homogeneous, crystallographically oriented
movement of larger groups of atoms relative to their neighbours (<1 interatomic
distance), which is called displacive movement (similar to deformation twinning).
In general, displacive movement is realized by a combination of shear, dilation/
contraction and so-called shuffling of the atoms of the high-temperature phase.
Shear occurs within a shear plane—the so-called invariant plane, in which the
direction and the length of all vectors remain unchanged. The interface between
austenite and martensite, which is identical to the invariant plane, is the so-called
habit plane. Atomic shuffling is described as the relative movement of neighbouring
lattice planes. According to Cohen (as cited in [2]) martensitic transformation is “…
a shear dominant, lattice distortive, diffusionless transformation…”, where the
morphology and the kinetics are determined by the strain energy. Since MPT is a
first-order phase transition, the formation of martensite occurs via nucleation and
growth. Preferred locations for martensite nucleation during cooling are lattice
defects of the austenitic phase. The typical appearance of martensite includes plates,

© Springer Nature Switzerland AG 2020 47


A. Weidner, Deformation Processes in TRIP/TWIP Steels,
Springer Series in Materials Science 295,
https://doi.org/10.1007/978-3-030-37149-4_3
48 3 Martensitic Phase Transformation

Fig. 3.1 Self-accommodation of lattice stress caused by martensitic phase transformation. a Initial
shape of crystal before martensitic phase transformation. b Shear deformation of the crystal.
c Accommodation of shear deformation by dislocation glide. d Accommodation of shear
deformation by twinning. Modified according to [3]. Permission of Springer

laths or lenses [1]. Since both phases exhibit different crystal symmetries, which are
accompanied, in general, by different specific volumes VM and VA , significant
lattice stresses occur during MPT. These lattice stresses are compensated by
so-called lattice invariant deformation (elastic and plastic)—also known as
self-accommodation, which can be the formation of lattice defects, dislocation glide
and mechanical twinning, as shown in Fig. 3.1 [3].
A further characteristic feature of MPT is the appearance of a strong relationship
according to the orientation of the austenitic and martensitic lattices. Thus, distinct
orientation relationships (ORs) exist of the lattice directions and planes of both
phases. The three most common ORs are (i) Bain [4], (ii) Kurdjumov–Sachs
(KS) [5] and (iii) Nishiyama–Wassermann (NW) [6] relationships, which are given
below and are sketched in Fig. 3.2:

ðiÞ Bain-OR : f001gfcc k f001gbcc and h100fcc i k h110bcc i

ðiiÞ KS-OR : f111gfcc k f110gbcc and h110fcc i k h111bcc i

ðiiiÞ NW-OR : f111gfcc k f110gbcc and h112fcc i k h110bcc i:


The type of orientation relationship that occurs provides information about the
transformation process, since different variants of homogeneous lattice distortions
are possible. Furthermore, the ORs occurring restrict the number of possible
alignments between the austenitic and martensitic phases, which are known as
martensite variants. Whereas for the Bain-OR, only three crystallographically
equivalent martensite variants can be formed, the KS-OR allows the formation of
24 crystallographically equivalent martensite variants [6]. The selection of indi-
vidual martensite variants depends on the crystal symmetry and the crystallographic
orientation.
Consequently, the martensitic phase transformation is related to specific features:
(i) an identical chemical composition, but different crystal lattices for the austenitic
and martensitic phases; (ii) a well-defined orientation relationship between the
3.1 General Considerations 49

Fig. 3.2 Schematic visualization of the orientation relationship between austenitic and martensitic
phases. a Bain, b Kurdjumov–Sachs and c Nishiyama–Wassermann. Modified according to [4–6].
Permission of Springer and Wiley VCH, respectively

austenitic and martensitic phases; and (iii) the formation of several crystallo-
graphically and energetically equivalent martensite variants out of one parent
crystal. MPT is (iv) a local deformation of the austenitic crystal lattice and
(v) residual stresses arise due to the local deformation [1]. Among these features
related to the appearance of martensite, a number of kinetic features can also be
formulated: (i) rapid MPT at low temperatures; (ii) the influence of temperature on
the amount of martensitic phase; (iii) the formation of pronounced surface relief;
and (iv) specific appearance of martensite [1].
The kinetics of MPT are significantly dependent on the elastic energy, which
occur due to the nucleation and growth of martensitic crystals, and depend on the
transformation mechanism itself. Thus, the mechanical properties of the alloys
enabling MPT, the initial and martensitic lattice structure determining the trans-
formation mechanism and the degree of coherency at the phase boundary have a
significant influence on both the magnitude and on the accumulation of the elastic
energy [1]. The degree of coherency at the interface boundary between austenitic
and martensitic phases is quite important for the reversibility of the martensitic
phase transformation. A case of total coherency—where the interplanar spacing in
the austenitic and martensitic phases remains equal—is quite rare. More common is
the state of partial coherency, where only some sections have equal interplanar
spacing separated by regions, where lattice defects such as dislocations are built-in,
in order to compensate for coherency strains due to small deviations of the inter-
planar spacing of the austenitic and martensitic phases. Thus, MPT can be fully
reversible when the differences in lattice constants and/or specific volumes between
the initial and martensitic phases are small and the accommodation of the
martensitic phase in the austenitic matrix is not accompanied by plastic deforma-
tion. In this case, the hysteresis between the direct and the reversed transformation
is quite small. Thus, both the structure of the initial phase and the initial shape of
the specimen can be restored—a phenomenon known as the shape memory effect
(SME). However, if the difference in lattice constants and/or specific volumes is
large and/or MPT is accompanied by plastic deformation, energy dissipation and
the formation of lattice defects then the reverse transformation occurs with a larger
50 3 Martensitic Phase Transformation

Fig. 3.3 Hysteresis loop of martensitic phase transformation. Modified according to [1].
Permission of Cambridge International Science Publishing

hysteresis. In this case, the reverse transformation is more likely to occur by the
nucleation and growth of the high-temperature phase (austenite) inside the
martensite crystals than by the gradual reduction of the size of the martensite up to
their disappearance [1]. Figure 3.3 shows a schematic plot of a hysteresis loop for
martensitic phase transformation.
The two effects described above are known as (i) thermoelastic MPT and
(ii) non-thermoelastic MPT. For thermoelastic MPT, the width of the hysteresis loop
DT is small, the mobility of the interface austenite/martensite is high and, therefore,
MPT can occur completely reversible. In contrast, non-thermoelastic MPT results in
a large opening of the hysteresis loop, the mobility of the interface is restricted, and
the reverse transformation occurs through nucleation of the austenitic phase.
Although the nomenclature “martensite” is also related to the specific
microstructure obtained in steels after quenching—named in honour of the scientific
work of the German metallurgist Adolf Martens—martensitic transformation is a
widespread phenomenon and occurs in a large variety of metallic and non-metallic
materials. Thus, along with steels, martensitic transformations occur for instance in
pure metals (e.g. Fe, Co, Ti, Zr), alloys based on these metals and in other alloys
(e.g. b-Titanium alloys: Ti–Mo, Ti–Ni; copper alloys: Cu–Zn, Cu–Al), but also in
ceramics such as ZrO2. In addition, reversible martensitic phase transformations
occurring in shape memory alloys (e.g. Ti–Ni, Co–Ni, Ti–Ta) play an important
role.

3.2 Thermodynamic Aspects of Martensitic Phase


Transformation

The thermodynamic driving force for martensitic transformation is the difference in


Gibbs free energy between the austenitic and martensitic phase DGA!M , favouring
the state of minimum energy. Figure 3.4a shows the temperature dependence in
3.2 Thermodynamic Aspects of Martensitic Phase Transformation 51

Fig. 3.4 Thermodynamics of martensitic phase transformation. a Temperature dependence of


GIBBS free energy of the austenitic and martensitic phases indicating the martensitic start
temperature Ms . Modified according to [7]. Permission of Taylor and Francis. b Influence of
mechanical energy on the MPT. Modified according to [8]. c Schematic drawing of the
temperature–stress range for stress-assisted and strain-induced martensitic transformation.
Modified according to [9]. Permission of Elsevier

terms of Gibbs free energy of the austenitic and martensitic phases. T0 is the
equilibrium temperature, indicating the stability of the martensitic phase at T\T0 .
At T [ T0 , the austenitic phase is thermodynamically stable and no martensitic
phase transformation will occur. Martensitic phase transformation at temperatures
below T0 requires a defined undercooling DT, which is necessary for the formation
of a viable martensitic nuclei. The amount of undercooling has an influence on the
nucleation rate of MPT. DT results in the martensitic start temperature Ms leading to
so-called spontaneous martensite formation.
At the temperature T1 ðMs \T1 \T0 Þ, the thermodynamic driving force is less
than at Ms , thus no spontaneous martensitic phase transformation will occur.
However, the application of external stresses can contribute to the martensite
nucleation energy and, thus, the MPT occurs at T [ Ms as shown in Fig. 3.4b. Two
variants can be distinguished: (i) stress-assisted martensitic phase transformation
and (ii) strain-induced martensitic phase transformation. According to Olson and
Cohen [9], both stresses below the yield point as well as strains beyond the yield
point of the austenitic phase can induce MPT. Figure 3.4c shows the stress and
temperature range for stress-assisted and strain-induced martensitic transformation.
At temperatures of Ms \T\Msr , stresses below the yield point of the material are
sufficient for initiation of martensitic transformation. Nevertheless, the required
stress increases with the increase in temperature due to the concomitant decrease in
the driving force DGA!M . At temperatures of T [ Msr , passing the yield point
causes plastic deformation to occur in the material. Thus, martensite can nucleate at
lower stresses than under stress-assisted transformation, producing so-called
strain-induced martensite. However, the amount of plastic deformation triggering
martensitic transformation increases with the increase in the temperature due to the
further decrease in the driving force DGA!M .
52 3 Martensitic Phase Transformation

Above Md , no martensitic transformation can be induced by plastic deformation.


Along with spontaneous, stress-assisted and strain-induced martensite, isothermal
martensite can occur as well depending on temperature and chemical composition.
Furthermore, martensitic transformations are influenced by both chemical
composition and material properties such as stacking-fault energy and magnetic
properties. In addition, microstructural parameters such as grain size and grain
orientation affect martensitic transformations, as do loading conditions such as
applied stress or strain level and strain rate.

3.3 Martensite in Ferrous Alloys

Pure iron exhibits three allotrope modifications depending on the state variables
temperature T and pressure p as shown in Fig. 3.5. Thus, at ambient pressure and at
T < 911 °C, the stable modification of iron known as the a-phase (or a-ferrite) has a
bcc crystal lattice (with a lattice constant of abcc ¼ 0:2875 nm at RT). In the
temperature range of 911 °C < T < 1392 °C (and ambient pressure), the stable
allotrope modification known as c-phase (or austenite) has fcc crystal lattice with a
lattice constant of afcc ¼ 0:3593 nm. Above 1392 °C up to melting temperature
TL ¼ 1536  C, a further bcc modification occurs: the d-phase (or d-ferrite). At
higher pressures, a third allotrope modification of iron exists: e-iron with a hcp
crystal lattice. Thus, at 10 < p < 15 GPa and temperatures up to 600 °C, a phase
transformation occurs from a-iron (bcc) to e-iron (hcp). A phase transformation
from c iron (fcc) into e-iron (hcp) occurs at higher temperatures (up to TL ), where
the pressure is increasing with increase in temperature.
In addition to the three allotrope modifications, a change in the magnetism of a-
iron occurs at 769 °C—the Curie temperature Tc —from a ferromagnetic (T\Tc ) to
a paramagnetic (T [ Tc ) state, which is, however, not correlated to a change in the
crystal lattice.
The addition of alloying elements has a significant influence on the existence of
the different phase fields. Alloying elements are subdivided into ferrite-stabilizing

Fig. 3.5 Allotrope


modifications of iron as a
function of temperature T and
pressure p. Modified
according to [10]
3.3 Martensite in Ferrous Alloys 53

elements (interstitial: e.g. Al, Be, and substitutional: e.g. Cr, Mo) that broaden the
a-phase field, and austenite-stabilizing elements (interstitial: e.g. C and substitu-
tional: e.g. Mn, Ni) enlarge the c-phase field. Elements such as P act both as ferrite
and austenite stabilizer depending on the content. The interaction with other
alloying elements has also to be taken into account. Thus, Cr can lead to a stabi-
lization of the c-phase field in combination with Mn and Ni.
According to the three allotrope modifications of iron, three different modifi-
cations of martensite can occur in ferrous alloys: (i) a′-martensite (bcc or bct), (ii) e-
martensite (hex crystal lattice) and (iii) c-martensite (fct)—depending on the
chemical composition and the cooling conditions applied. However, the latter one is
quite rare and is observed only in Fe–30Pd and Fe–25Pt [11], and can, therefore, be
neglected for steels.
a′-martensite is the most common martensite in ferrous alloys and its appear-
ance is reported, for example, in Fe–C, Fe–N and Fe–Ni alloys [11]. The crystal
lattice of a′-martensite is either bcc or bct depending on the tetragonality caused by
the content of interstitials such as C or N. Different morphologies are reported for
the occurrence of a′-martensite: (i) lath, (ii) butterfly, (iii) {225}c plate, (iv) lentic-
ular and (v) thin plate. However, the actual appearance of one out of these five
morphologies depends significantly on chemical composition and the Ms temper-
ature. The two most important variants are lath and lenticular martensite. Lath
martensite occurs in Fe–C (<0.6% C), Fe–Ni (<28% Ni) and Fe–Mn (<10% Mn)
alloys, most heat-treatable commercially available steels and in high-strength steels.
Its morphology is characterized by rounded lath tips caused by an interfacial energy
between austenite and a′-martensite of 100 mJ/m2. In general, the dislocation
density of lath-type martensite is quite high in the order of 1014 to 1015 m−2
(comparable to heavily cold-worked alloys). The lenticular morphology appears
mainly in Fe-high C (0.8–1.8% C) and Fe-high Ni (29–33% Ni) alloys. a′-mar-
tensite forms either spontaneous during cooling or due to stress-assisted or
strain-induced deformation (see Sect. 3.2).
e-martensite is mainly reported in Fe-high-Mn alloys (15–27% Mn) and Fe–Cr–
Ni alloys such as austenitic stainless steels and was first described by Schmidt in
1929 in the course of X-ray diffraction experiments [12]. In general, e-martensite is
a plate-type martensite with parallel, planar interfaces caused by an interface energy
austenite/e-martensite of 10 mJ/m2, which is ten times less than for a′-martensite.
The thickness of plates depends on chemical composition and cooling rates. e-
martensite can occur in high-alloy steels as spontaneous martensite (rapid cooling)
or due to deformation [11]. Thus, e-martensite appears in high-Mn steels after rapid
cooling as blocky-type martensite (large thickness of plates up to prior austenitic
grain size) [11], whereas in high-alloy Cr–Mn–Ni steels, it appears as thin plates
with thickness of only a few micrometres. In both cases, it is assumed that the
crystal lattice of the e-martensite is hexagonal. However, in the case of high-alloy
Fe–Cr–Mn–Ni steels, the e-martensite formed due to plastic deformation is char-
acterized by a high density of stacking faults arranged in average on each second
lattice plane—which simulates a hexagonal crystal lattice [13]. However, the c/a
ratio of this e-martensite is far from the ideal c/a ratio of a classical hcp crystal
54 3 Martensitic Phase Transformation

lattice (c/a = 1.633). Therefore, there should be a difference between the


high-pressure e-iron phase with a hcp crystal lattice and the e-martensite observed
after plastic deformation in high-alloy Fe–Cr–Mn–Ni steels (see Sect. 6.4.1).

3.4 Martensitic Phase Transformation in Steels

As early as 1934, Burgers [14] presented a scheme of possible transformations


between the three important crystal lattices occurring in metallic materials:
(i) face-centred cubic lattice; (ii) body-centred cubic lattice; and (iii) hexagonal
closed-packed lattice. This scheme—shown in Fig. 3.6—is based on the works of
Kurdjumov and Sachs [5], Straumanis, Weerths, Mehl and Wassermann (as cited in
[14]). Burgers suggested that “… the transition of a metal such as Zirconium can be
considered as a combination of transition-processes of the iron- and the cobalt-type”
[14]. Here, the iron-type describes the direct transition of fcc austenite into bcc
martensite discussed by Kurdjumov and Sachs [5] and the cobalt-type direct
transition of the fcc b-Co into hcp a-Co (found by Straumanis, Weerth, Mehl and
Wassermann, as cited in: [14]). Furthermore, the scheme of Burgers suggests that
the assumed combined transformation from bcc b-Zr into hcp a-Zr via an inter-
mediate state of fcc Zr can be transferred to other metals and alloys, such as
iron-based alloys, brass alloys or aluminium–silver alloys. Four decades later,
Schumann [15] showed the indirect c-austenite to a′-martensite transition via the
intermediate e-martensite state. In the following, both the direct transformations
(i) c !a′, (ii) c ! e and (iii) e ! a′ as well as the indirect transformation
(iv) c ! e ! a′ will be described for steels.

Fig. 3.6 Schematic drawing


of the complete set of possible
transformations between the
three important crystal lattices
occurring in metallic
materials: body-centred cubic,
face-centred cubic and
hexagonal closed packed.
Modified according to [14].
Permission of Elsevier
3.4 Martensitic Phase Transformation in Steels 55

3.4.1 Direct c to a′ Transformation

Bain transformation. The Bain mechanism was introduced by Bain in 1924 [4]
through suggestion of a tetragonal distortion mechanism, which describes a con-
tinuous fcc–bcc transition path that accounts for the allotropic c- to a-iron transition
in carbon steels [16]. Figure 3.7a illustrates the relationship between the fcc crystal
lattice (black circles) and the body-centred tetragonal crystal lattice (grey circles).
The c-axis is common for both the austenitic (fcc) and martensitic (bct) phases,
where the a′-axis and b′-axis of the martensitic phase are rotated by 45° around
½001 with respect to the a-axis and b-axis of the austenite. Obviously, the axial ratio
pffiffiffiffiffiffiffiffi
of the bct crystal lattice is c=a ¼ 2=1 ¼ 1:414. Therefore, in order to obtain the
bcc crystal lattice with the required axial ratio, both a contraction of 25% along the
c-axis (from cbct ¼ 0:3592 nm to cbcc ¼ 0:286 nm) as well as a dilation of 12%
along the a-axis (from abct ¼ 0:254 nm to abcc ¼ 0:286 nm) is necessary leading to
the well-known Bain strain. Additional shear of the iron atom positions is necessary
in order to transform the atom positions from the ABC stacking sequence of the fcc
crystal lattice into the AB sequence of the bcc crystal lattice as shown in Fig. 3.8.
The tetragonal distortion can be attributed to the solute carbon atoms. The
carbon atoms are placed within the octahedral interstitial lattice sites of the fcc
crystal lattice, which are located on each edge and in the centre of the fcc unit cell.
Octahedral interstitial lattice sites in the bcc crystal lattice are smaller than in the fcc
crystal lattice and are located in the centre of each edge and of each cube face of the
unit cell. However, the bcc octahedral interstitial lattice sites can be divided into
three sublattices as shown in Fig. 3.7b [16]. During martensitic transformation, the
octahedral interstitial sites inherited from the fcc crystal lattice transform to only
one out of the three possible octahedral sublattices in the bcc crystal lattice as
shown in Fig. 3.7c [17]. Since only one sublattice of octahedral interstitial lattice
sites is occupied, the cubic symmetry is destroyed and a tetragonal distortion of the

Fig. 3.7 Martensitic phase transformation according to Bain. a BCT crystal lattice of the
martensitic phase in the fcc crystal lattice of the austenite. Modified according to [16]. b Three
sub-lattices of octahedral interstitial lattice sites of the bcc crystal lattice. Modified according to
[18]. c Carbon atoms occupying only one out of the three octahedral interstitial sublattices leading
to a tetragonal distorted bct lattice of Fe–C martensite. Modified according to [17]. Permission of
Elsevier
56 3 Martensitic Phase Transformation

Fig. 3.8 Martensitic phase transformation according to Bain. a Bain—orientation relationship [4].
b Shear operations of the iron atoms above and below body-centred iron atom to change from the
ABC stacking sequence of the fcc crystal lattice to the AB sequence of the bcc crystal lattice
shown in c. b, c Modified according to [19]

martensite occurs [17]. The degree of tetragonality depends on the carbon content
as shown by Kurdjumov and Kaminski [20, 21] observing a linear relationship
between the carbon concentration and the lattice constants c and a of the martensite.
Based on these studies, the Fe–C martensite can be understood as a supersaturated
solid solution of C, where the C-atoms occupy only one out of three octahedral
sublattices in bcc iron.
Although the Bain transformation is a quite simple and intuitive model, the
Bain-OR (see Sect. 3.1) is not observed experimentally for martensitic phase
transformations in steels. Moreover, significant deviations from tetragonality are
observed experimentally. Here, different interpretations can be found in literature.
Thus, an abnormally low tetragonality is observed for Mn and Cr steels (1.5% C)
that may be attributed to the occupancy of the other two octahedral interstitial lattice
sites by carbon atoms. In contrast, extremely high tetragonality is observed in Al-
and Ni-rich steels that may be explained by the influence of substitutional alloying
elements or the formation of superstructures [16].
Along with the Bain mechanism, several theories based on shear mechanisms are
suggested for the fcc to bcc transformation. Among these theories, the
(i) Kurdjumov–Sachs and the (ii) Nishiyama–Wassermann theories are the most
popular and were developed as early as 1930.
Kurdjumov–Sachs transformation. Kurdjumov and Sachs [5] suggested a
double shear mechanism for the fcc ! bcc (or bct) transformation that is consistent
with their KS-OR (see Sect. 3.1), which was first deduced from X-ray pole figure
analysis of a steel containing 1.4% C. Figure 3.9 illustrates the fcc and bcc (or bct)
crystal lattices during MPT in steels (Fig. 3.9a), their crystallographic relationships
(Fig. 3.9b) and the two steps of shear mechanisms (Fig. 3.9c). Thus, for the
explanation of their OR Kurdjumov and Sachs [5] focussed in both crystal lattices
on unit cells with new symmetries, where the f111g and the f110g planes become
3.4 Martensitic Phase Transformation in Steels 57

Fig. 3.9 Martensitic phase transformation according to Kurdjumov–Sachs. a Three-dimensional


arrangements of atoms in the austenitic, the tetragonal and the martensitic lattice. b Atom position
in the corresponding two-dimensional planes. c Individual shear operations. Reproduced from [5].
Permission of Springer

new base planes of the fcc and bcc (bct) crystal lattice, respectively (see Fig. 3.9a).
Using the projection of the atoms of the new unit cells on the base planes, it
becomes obvious that the fcc crystal lattice can be transformed into the bcc crystal
lattice if: (i) a shear of atom positions on ð111Þ planes occurs on different levels
(differently shaded circles) along a ½211 direction, which is accompanied (ii) by a
change of the angles of the rhombohedral base planes as shown in Fig. 3.9b.
Figure 3.9c demonstrate in detail the two shear operations: (i) shifting of the atoms
of the middle and upper ð111Þ plane to the centre of the base plane leading to a bct
crystal lattice, and (ii) a shear operation on the ð21
1Þ of the final bcc crystal lattice.
58 3 Martensitic Phase Transformation

Fig. 3.10 Martensitic phase transformation according to Schumann following a two-step shear
mechanism. a Three-dimensional representation. b Two-dimensional projection. Modified
according to [22]. Permission of Wiley VCH

Similarly to Kurdjumov [5], Schumann proposed a two-step shear mechanism


in 1975 for direct c ! a′ transition in metastable austenitic stainless steels [22].
Figure 3.10 illustrates the crystallographic shear deformations for the fcc to bcc
transition resulting in a KS-OR. Using the reference system Z || ½112, X || ½10 1 and
Y || ½011 a first homogenous shear with ~ s1 ¼ 16 ½11
2 occurs on the ð111Þ plane. In
this way, the angle of the Z-axis is changed by 19°28′. Due to a second homoge-
nous shear with ~ s3 ¼ 16 ½011, the angle between the X-direction and Y-direction of
the ð111Þfcc base plane is increased from 60° to 70°32′ [22]. The angle between
both shear vectors is about 150°.

Fig. 3.11 Variant selection of a′-martensite according to KS-OR. Reproduced from [23].
Permission of Elsevier
3.4 Martensitic Phase Transformation in Steels 59

Table 3.1 Variant selection according to Kurdjumov–Sachs orientation relationship (cf.


Fig. 3.11). According to [23]
Variant-No. Plane parallelism Direction parallelism Misorientation to V1
(hkl)c || (hkl)a′ [uvw]c || [uvw]a′
V1 ð111Þc k ð011Þa0   k ½111
½101  0 –
c a
V2 ð111Þc k ð011Þa0 ½101c k ½111a0 Twin (R3)
V3 ð111Þc k ð011Þa0 ½011 k ½111
c
 0
a
10.53 from V2
V4 ð111Þc k ð011Þa0 ½011c k ½111a0 10.53
V5 ð111Þc k ð011Þa0 ð111Þc k ð011Þa0 10.53 from V2
V6 ð111Þc k ð011Þa0 ð111Þc k ð011Þa0 21.06 from V2 (R11)

In both transformation path models, the KS-OR allows the formation of 24


martensite variants due to the involvement of four f111g shear planes and six
<110> shear directions (Fig. 3.11) (Table 3.1).
Nishiyama–Wassermann transformation. Nishiyama derived a mechanism
comparable to Kurdjumov–Sachs as shown in Fig. 3.12a that consists of a similar
shear on the f111g planes of the fcc crystal lattice in combination with a second
distortion leading to the NW-OR [24]. The Nishiyama mechanism was first detected
on a single crystal of Fe–30Ni cooled down to the liquid nitrogen temperature.
According to NW-OR, 12 martensite variants can be formed due to possible shear
on four f111g planes with three <112> shear directions per plane (cf. Fig. 3.12b).
However, shear in the opposite direction occurs with difficulty. Moreover, even if it

Fig. 3.12 Martensitic phase transformation according to Nishiyama in comparison to


Kurdjumov–Sachs. a Reproduced from [25]. b Direction of shear in {111} plane of austenite.
Nishiyama (left) and Kurdjumov–Sachs (right). Reproduced from [24]. c Nishiyama (left) and
Kurdjumov–Sachs (right) in combination with C-atoms on three different octahedral sublattices
(small circles). Reproduced from [17]. Permission of Elsevier
60 3 Martensitic Phase Transformation

takes place no variants are generated that exhibit different orientations [24].
However, the martensite variants obtained according to KS-OR differ by only 5°16′
from the variant according to NW-OR. The transformation of the interstitial carbon
atoms into only one out of the three possible octahedral interstitial sublattices of the
bcc crystal lattice mentioned for the Bain mechanism is also valid for the trans-
formation paths based on KS-OR and NW-OR. As shown in Fig. 3.12c (i.e. with a
homogenous shear deformation mechanism that does not involve atomic shuffle),
these paths also transfer all carbon interstitials in austenite onto a single octahedral
sublattice (coloured green) in martensite.
Along with the transformation path described above, further orientation rela-
tionships are found such as (i) the OR according to Greninger and Trojano [26] and
(ii) the OR according to Pitsch [27]:

GT-OR : f111gc k f110ga0 ; h5 12 17ic k h7 17 17ia0 and

P-OR : f100gc k f110ga0 ; h110ic k h111ia0

Both OR are comparable to the NW-OR found mainly after spontaneous or


isothermal martensitic phase transformation.

3.4.2 Direct c to e Transformation

The formation of e-martensite within austenite is comparable to the twinning


mechanism. Thus, likewise to twin planes, the f111g planes are shear planes and
the h112i directions are shear directions. However, the shear angle (with
us;e ¼ 19:47 ) is only half the twinning shear angle (us;twin ¼ 38:94 ). This is due
to the fact that shear does not occur on each f111g plane, but rather on small
packages of two planes (see Fig. 3.13). The transformation process is supported by
partial dislocations a6 h112ic . The OR occurring can be described as follows:
f111ge k f001ge and h112ie k f120ge [28]. However, the lattice deformation
occurring due to the formation of e-martensite is significantly smaller than with
pffiffiffiffiffiffiffiffi
twinning, since the related shear strain s ¼ tan u ¼ tan us;e ¼ 2=4 ¼ 0:35 is half
pffiffiffiffiffiffiffiffi
as much as the twinning shear strain (tan us;twin ¼ 2=2 ¼ 0:7). The resulting
maximum dilatation and compression due to e-martensite is about 19.2% and 16%,
respectively. Since the alternations in length are significantly larger than the
accompanying volume dilation (−0.5%), e-martensite occurs in the form of plates
with a small thickness comparable to twins.
Direct c to e transformation is mainly observed in high-Mn steels during cooling
processes if the chemical driving force is reached. Thus, given the absence of any
external mechanical shear stress on each f111g plane of the austenite three e-
martensite variants are formed with the same crystallographic orientation, since
each f111g plane contains three shear directions with an inclination angle of 120°
3.4 Martensitic Phase Transformation in Steels 61

Fig. 3.13 Shear operations


for the formation of
e-martensite. According
to [28]

between each other. Thus, depending on chemical composition and after cooling
the microstructure consists of e-martensite variants with one typical crystallographic
orientation for each of the four f111g lattice planes of the austenite. If additional
external shear stresses are applied then both the amount of applied stress and the
crystallographic orientation of austenitic grains have a significant influence on the
formation of e-martensite variants. Consequently, anisotropic shear deformation is
observed in analogy to twinning, since under mechanical stresses only martensitic
variants are activated, which lead to elongation under tensile deformation and to
contraction of material under compressive deformation.
The strain-induced c to e transformation was described by Fujita and Ueda [29,
30] on specimens of austenitic stainless steel (AISI 304) and on single crystals with
different orientations of Fe–Mn–C austenitic alloys. It was shown that thin e-plates
are formed by extended stacking-fault bands. A cross-slip mechanism with stair-rod
dislocations is proposed for the growth of the thin e-plates [29]. Furthermore, it was
shown that the formation of e-martensite plates is strongly correlated to the acti-
vated slip systems [30]. Thus, in single-slip-oriented crystals, e-martensite only
occurs along primary slip system, whereas in double-slip-oriented crystals, e-mar-
tensite occurs along both primary and conjugate slip systems.

3.4.3 Direct e to a′ Transformation

The e to a′ transformation is observed mainly in high-Mn steels during cooling


process and is a consequence of the previous c to e transformation. According to
Venables [31], the orientation relationship between e-martensite and a′-martensite
can be described as follows: ð0001Þe k ð011Þa0 ; ½1210e k ½111a0 . The OR is the result
of a three step process consisting of (i) the shuffling of atoms in n + 1th f0001ge
planes, (ii) the displacement of f1010ge plane, and (iii) the shear in h1 210ie
direction. The transformation results in a volume change of about 4% and is
accompanied by dilatation and compression of 13% and 7%, respectively, on two
62 3 Martensitic Phase Transformation

Fig. 3.14 Six equivalent


a′-martensite variants with
h111ia0 habitus. According
to Schumann [32]. Permission
of Wiley VCH

orthogonal axes. These large deformations cannot be compensated elastically nei-


ther by the e-martensite nor by the a′-martensite. Therefore, plastic deformation in
terms of dislocation glide within the martensite needles is necessary as accom-
modation process. Due to the three-fold symmetry of the f0001ge plane three a′-
martensite variants oriented differently can be formed. Finally, due to twinning six
equivalent a′-martensite variants are possible out of one e-martensite orientation as
shown in Fig. 3.14.

3.4.4 Indirect c–a′ Transformation via e-Martensite

Similar to the direct c ! a′ transition, a two-step shear process is required, which


first transfers the fcc crystal lattice into a hex crystal lattice followed by a second
shear on an intersecting plane transfers the hex crystal lattice into the bcc a′-mar-
tensite. Finally, a shuffling process is needed in order to bring the atoms in correct
positions. Figure 3.15 shows the displacement of atoms related to this two-step shear
process according to Schumann [33]. Thus, the first shear is given on a f111gfcc
plane by a partial dislocation with a=6h112i followed by the second shear on a
f0001g plane with a=6h1120i and a final shuffling of a=6h110i on a f110gbcc plane.
In addition, the KS-OR between austenite, e-martensite and a′-martensite becomes
apparent: f111gfcc k f0001ghcp k f110gbcc and h110ifcc k h11 20ihcp k h111ibcc .
As reported in several publications (e.g. [29]), the hex crystal lattice of e-mar-
tensite can be caused by the arrangement of intrinsic stacking faults on each second
f111g plane (see Sect. 2.1.1). Therefore, Schumann [15] mentioned that e-mar-
tensite can be regarded as fcc crystal lattice with stacking-fault parameter of 0.5 (SF
on each second f111g plane). Thus, a=6h112i shear of stacking faults on inter-
secting f111g planes yield the formation of a′-martensite as shown schematically in
Fig. 3.16.
3.5 Influence of Stacking-Fault Energy 63

Fig. 3.15 Indirect martensitic phase transformation from austenite into a′-martensite via e-
martensite. a, b Process of dislocation glide (~
b ¼ a6 ½211). c Shearing (~
s1 ¼ a6 ½1
210). d Shuffling
a 
s2 ¼ 6 ½110). e bcc crystal lattice of a′-martensite. Modified according to [33]. Permission of
(~
Wiley VCH

Fig. 3.16 Double shear mechanisms on two different f111g planes yielding the formation of a′-
martensite. a Double shear in the ½011 intersection line due to partial dislocation s1 k ½11
2 on
ð111Þ and s2 k ½1 12 on ð111Þ. Modified according to [15]. Permission of Wiley VCH.
b Intersecting bands of stacking faults indicating first and second invariant plane strain and the
stable a′-martensite nucleus at centre. Reproduced from [34]. Permission of Elsevier

3.5 Influence of Stacking-Fault Energy

The stacking-fault energy has a significant influence on ongoing deformation


mechanisms such as (i) dislocation glide, (ii) twinning, (iii) formation of e-
martensite/stacking faults and (iv) formation of a′-martensite. Since the SFE itself
depends strongly on chemical composition and temperature, both parameters have a
pronounced influence on deformation mechanisms and MPT, respectively. As a
general trend, it can be stated that with increasing SFE, the tendency for dislocation
glide of regular dislocations is increasing, whereas a decrease in the SFE promotes
the formation of SFs. However, the SFE is an intrinsic material property that can be
either determined experimentally or calculated according to empirical equations and
64 3 Martensitic Phase Transformation

ab initio methods, respectively. A critical review on the SFE of austenitic steels is


provided by Lee et al. [35] summarizing recent progress in studies on SFE.
First of all, the SFE depends significantly on the chemical composition of the
material. For austenitic steels, following main alloying elements have to be taken
into account: Mn, Ni, Cr, Cu, Si, Al, C and N, which can be separated mainly in
elements increasing SFE (C, Al, Ni and Cu) and decreasing SFE (Cr and Si) [35].
Mn has a parabolic influence on the SFE in a range up to 29% Mn in binary Fe–Mn
alloys. Thus, the SFE drops with increasing of Mn content up to 13 wt% Mn and
rises again with further increase in Mn. The parabolic behaviour is also observed for
the Fe–Mn–C system. Nitrogen has a diverse influence on the SFE depending on
the chemical composition of the base material [35]. Thus, whereas in Fe–Mn–Cr–
xN alloys, the SFE decreased with increasing nitrogen content, in Fe–Mn–Cr–Ni–
xN, the SFE increased with the increase in nitrogen [36].
The influence of involved alloying elements on the SFE can be described by
empirical equations. Thus, numerous equations can be found in literature (e.g. [37–
39]). An overview of different approaches was provided by Martin [40]. It becomes
evident that especially main alloying elements such as Cr, Ni and Mn are taken into
account. However, the influence of interstitial atoms such as C or N remains
unattended, although they have a significant influence on the SFE and on MPT,
respectively. However, Dai et al. [41] proposed an empirical equation including
both the SFE energy of pure iron c0SF as well as a large number of alloying elements
including C and N (wt%):

cSF ¼ c0SF þ 1:59Ni  1:34Mn þ 0:06Mn2  1:75Cr þ 0:01Cr2 þ 15:21Mo  5:59Si  60:6ðC þ 1:2NÞ1=2
þ 26:27ðC þ 1:2NÞ  ðCr þ Mn þ MoÞ1=2 þ 0:61½Ni  ðCr þ MnÞ1=2
ð3:1Þ

Here, the SFE of pure iron c0SF is assumed to be about 36–42 mJ/m2 according to
Dai et al. [41].
For the determination of SFE, different experimental techniques [42] are known
such as TEM, XRD or neutron diffraction line broadening analysis. Moreover, the
Calphad-method or ab initio calculations are used. However, most of these tech-
niques have their limitations and drawbacks [42]. The most common techniques for
experimental determination of SFE are related to TEM. Here, at least three different
variants are exercised: (i) measurements of the radius R of dislocation nodes
according to the Whelan equation (cSF ¼ lb2 =R, e.g. [43]); (ii) weak beam analysis
of the distance between dissociated partial dislocations (e.g. [44]); and (iii) direct
measurement of the distance between partial dislocations (e.g. [45]) using HRTEM.
However, the Whelan and the weak beam method are more suitable for materials
with low stacking-fault energy. Especially, the Whelan method tends to overesti-
mate the SFE. Moreover, the measurement of width of dissociated dislocations does
not reflect in any case a thermodynamical equilibrium state, since already at low
stresses regular dislocations tend to dissociate. Thus, the SFE can be
underestimated.
3.5 Influence of Stacking-Fault Energy 65

Other, indirect methods as the X-ray or neutron diffraction use the shift of peak
position and the line broadening due to SFs after plastic deformation (e.g. [13, 46,
47]). However, main drawback of these methods is that interactions between SF and
other defects such as dislocations remain unattended.
Recently, first principle quantum mechanical approaches (e.g. [48, 49]) came
into the focus for the calculation of SFE. Here, electronic, magnetic and volume
moments are taken into account in order to describe the dependence of the SFE on
the chemical composition. The results of these theoretical calculations show that the
influence of an individual alloying element on the SFE of the alloy depends sig-
nificantly on the host composition. Thus, one and the same element can have the
opposite effect. Therefore, a universal empiric equation describing the dependence
of the SFE on the chemical composition cannot be drawn.
Along with chemical composition, the temperature has a significant influence on
SFE. Thus, the SFE is increasing with increasing temperature. According to Remy
[50], above RT, an increase in temperature by 1 K causes an increase in SFE of
about 0.05 up to 0.1 mJ/m2.
According to above-mentioned techniques, for calculation and experimental
evaluation of SFE, a large variety of values obtained for austenitic stainless steels
based on Cr, Ni and Mn as main alloying elements are available in literature. It
turns out that SFE for austenitic stainless steels varies in a range of 17 < cSF <
100 mJ/m2 depending on chemical composition and evaluation method.
The SFE can be calculated using the thermodynamic approach introduced by
Olson and Cohen [51], which takes into account the difference of GIBBS free
energy between austenite and e-martensite Dgc!e , strain energy Estr and surface
energy at the phase boundary between austenite and e-martensite rc!e according to
(3.2):

cSF ¼ N  .A ðDgc!e  Estr Þ þ 2rc!e ðNÞ ð3:2Þ

Here, N is the number of closed-packed planes involved in hcp e-martensite


(according to n = 2) and .A the planar density of atoms. The strain energy E str can
be neglected for the formation of e-martensite [52]. The values accounted for the
surface energy rc!e ranges from 5 to 27 mJ/m2. These simplifications lead to (3.3):

cSF ¼ 2  .A  Dgc!e þ 2rc!e ð3:3Þ

The calculated SFE based on the thermodynamic approach of Olson and Cohen
[51] is used as a base for interpretation of deformation behaviour of metastable
austenitic stainless steels. Thus, in literature [53–56] different threshold values of
SFE are announced for changing between deformation mechanisms such as
(i) formation of e-martensite, (ii) twinning and (iii) dislocation glide. It was stated
by Allain et al. [53] for high-Mn steels that at cSF  18 mJ/m2, the formation of e-
martensite is observed, whereas at cSF  35 mJ/m2, dislocation glide of regular
dislocation takes place. In the range 12  cSF  35 mJ/m2, mechanical twinning
66 3 Martensitic Phase Transformation

is dominating [53]. However, since it is quite difficult to determine experimentally


exact values for SFE by above-mentioned techniques, these “threshold” values can
be used as approaches only. Moreover, different deformation mechanisms run
mostly in parallel, however, with different significance. Along with experimental
determination of values for SFE, another problem arises in terms of description of
deformation mechanisms depending on SFE in terms of metastable austenitic steels.
For austenitic stainless steels, it is assumed that, in case of low SFE (cSF < 18 mJ/
m2), the formation of e-martensite is a favoured deformation mechanism. The SFE
of austenitic steels are comparable to other alloys or pure metals with medium or
low stacking-fault energy such as CuAl 8.5 (*17 mJ/m2), Ag (*16–22 mJ/m2) or
a-brass (*7–12 mJ/m2). However, none of these materials exhibits the formation
of e-martensite [52]. Instead, in these materials pronounced formation of SFs and
twinning is observed. Therefore, a modification of (3.3) was proposed quite
recently by Geissler et al. [52] introducing a volume free energy and a real
GIBBs-like interface energy c for e-martensite instead of using the surface energy
rc!e (5–27 mJ/m2) introduced by Olson and Cohen [51]. The SFE can be then
determined according to (3.4):

cSF ¼ 2  .A  Dgc!e þ c ð3:4Þ

3.6 Olson–Cohen Model of Martensitic Phase


Transformation

The martensitic phase transformation can occur both spontaneously during cooling
(spontaneous and isothermal) or triggered by mechanical load (stress-assisted and
strain-induced); cf. Sect. 3.2. In all cases, kinetics of MPT have to be regarded in
terms of nucleation and growth of martensitic nuclei. In the following, the evolution
of MPT triggered by mechanical load—mainly the strain-induced MPT—will be
discussed. In literature, a huge amount of models and approaches for the description
of the strain-induced MPT in dependence on the plastic deformation is available. In
principle, the numerous models can be separated into macroscopic models and
micromechanics/continuum mechanistic models. An overview of these models is
provided by Wolf [57] and Weiss and Gutte [58], respectively. The most common
and well-adapted model describing the evolution of strain-induced MPT on a
macroscopic point of view was introduced by Olson and Cohen in 1975 [51]. The
Olson–Cohen model [51] describes the evolution of the volume fraction of
strain-induced a′-martensite in dependence on applied plastic strain. It is based on
empirical relations found by experimental investigations of Angel [59] and
Gerberich [60]. As shown before, strain-induced a′-martensite formation occurs
related to the formation of deformation bands, which consist either of e-martensite,
high-density of stacking faults or twin bundles. Favoured nucleation places for
3.6 Olson–Cohen Model of Martensitic Phase Transformation 67

a′-martensite are intersection points of these deformation bands. However, as


shown by Schumann et al. [15] even intersection of individual SFs on different slip
planes can act as nucleation site for a′-martensite. Therefore, the evolution of
volume fraction of strain-induced a′-martensite is correlated strongly with the
volume fraction of deformation bands developing during plastic deformation with
increasing strain. According to Olson and Cohen [51], the evolution of the volume
fraction of a′-martensite with increasing strain can be described by following
equation:

f a ¼ 1  e½bð1 e 
0 aepl n
Þ
ð3:5Þ
0
Here, f a is volume fraction of strain-induced a′-martensite, e is applied plastic
strain, n is a fixed exponent. The parameters a and b are temperature dependent as
shown in Fig. 3.17a, b. Thus, the parameter a describes the evolution of defor-
mation bands with increasing strain. Here, the temperature dependence is given due
to the influence of SFE on formation of e-martensite, SFs or twins. The parameter b
describes the probability of formation of a′-nucleus at intersection of two defor-
mation bands. The temperature dependence of this parameter is caused due to the
influence of chemical driving force. The exponent n is a geometry factor that
includes the orientation dependence of the formation of deformation bands.

Fig. 3.17 Olson–Cohen model of martensitic phase transformation. a Temperature dependence of


the parameter a—describing the rate of deformation band formation. b Temperature dependence of
the parameter b—describing the probability of intersectioning of deformation bands forming a′-
martensite. c Calculated transformation curves based on (3.5) in comparison with experimental
data of Angel [59]. Reproduced from [51]. Permission of Elsevier
68 3 Martensitic Phase Transformation

The exponent n describes, therefore, the number of intersections of deformation


bands acting as nucleation sites for a′-martensite. The number of intersections is
quite low at small strains and is significantly growing with the increase in strain.
0
The transformation curves (volume fraction f a vs. plastic strain epl ) obtained by this
approach have a S shape character as known from classical nuclei formation theory
(cf. Fig. 3.17c for comparison with experimental data of Angel [59]). At high
0
strains, a saturation of f a is observed, which is caused by the b-parameter [51].
Along with the Olson–Cohen model [51] other models exist, which are modifica-
tions of the above-described model. Thus, the model according to Stringfellow et al.
[61] includes additionally the stress state due to developed deformation bands,
which is separated into hydrostatic and deviatoric stress components. Iwamoto et al.
[62] incorporated the influence of the grain size of the austenite on the formation of
a′-martensite into the Olson–Cohen model [51] (see also Sect. 4.2.3).

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Chapter 4
Advanced High-Strength Steels

Abstract This chapter is concerned with the advanced high-strength steels (AHSS).
The focus is on AHSS of second generation—the high-alloy austenitic steels with
twinning-induced plasticity (TWIP) and transformation-induced plasticity (TRIP).
For both groups, the state-of-the-art knowledge regarding the thermodynamic
aspects, the deformation behaviour and the modelling of the deformation and
strain-hardening behaviour is provided. The deformation behaviour is discussed
with respect to the influence of different parameters such as temperature, strain rate
and grain size as well as the appearance of strain localizations.

4.1 General Considerations

For at least two decades, advanced high-strength steels (AHSS) have been the focus
of automotive industry due to their improved formability and crash behaviour.
AHSS of the first generation includes (i) dual-phase steels, (ii) transforma-
tion-induced plasticity-assisted steels (TRIP) (retained austenite), (iii) complex
phase steels and (iv) martensitic steels. The UTS of these steels is well above
300 MPa up to 1 GPa. However, the ductility decreases with increasing strength.
Quite recently, AHSS of the second generation have been under investigation such
as the group of high-alloy austenitic steels with displacive transformations—TRIP
and TWIP steels and the group of nanoparticle hardened advanced maraging TRIP/
TWIP steels. Whereas the TRIP/TWIP steels are characterized by tensile strengths
of between 500 and 900 MPa at concurrently excellent levels of ductility (between
40 and 70% of total elongation), the nanoparticle hardened maraging TRIP/TWIP
steels exhibit tensile strengths of above 900 MPa at moderate ductility. Figure 4.1
illustrates well the spectrum of mechanical properties in terms of ultimate tensile
strength and total elongation for the different categories of AHSS. Future trends in
developing AHSS are ongoing in the direction of nanocrystalline steels such as
reverted nanoaustenitic steels with tensile strengths well above 1 GPa. Benefits of
AHSS for the automotive industry include (i) reductions in car weight, resulting in
reduced fuel consumption and (ii) increased passenger safety due to improved crash
behaviour [1].

© Springer Nature Switzerland AG 2020 71


A. Weidner, Deformation Processes in TRIP/TWIP Steels,
Springer Series in Materials Science 295,
https://doi.org/10.1007/978-3-030-37149-4_4
72 4 Advanced High-Strength Steels

Fig. 4.1 Relationship between total elongation and ultimate tensile strength of different categories
of advanced high-strength steels. Reproduced from [1]. Permission of Elsevier

For several years, modern high-alloy austenitic stainless steels that facilitate
either martensitic phase transformation or twinning during plastic deformation have
been of great scientific interest due to their outstanding mechanical properties of
concurrently high strength and excellent ductility. According to the dominant
deformation mechanisms, these steels are categorized into steels exhibiting
(i) transformation-induced plasticity (TRIP) effect (e.g. [2–4]), (ii) twinning-
induced plasticity (TWIP) effect (e.g. [5–7]), and (iii) microband-induced plasticity
(MBIP) effect (e.g. [8]). The TRIP effect is characterized by a significant increase in
strength and ductility due to martensitic phase transformation from the metastable
face-centred cubic (fcc) c-austenite into body-centred cubic (bcc) a′-martensite
[9–16]. The TWIP effect is based on strain-induced twinning, leading to remarkable
strain-hardening rate and excellent ductility [5–7]. A remarkably good combination
of strength and ductility of MBIP steels (with up to 100% strain to fracture in tensile
deformation) may be achieved as a balance between hardening and softening
effects. While the former is caused by dislocation accumulation in cell structures
and mechanical twinning, the latter is associated with strain localization in
microbands [17, 18].
Possible deformation mechanisms in all these different classes of high-alloy
austenitic steels are (i) dislocation glide, (ii) twinning and (iii) martensitic phase
transformation. Which of these mechanisms are predominant and is influenced
primarily by the stacking-fault energy.
4.2 Twinning-Induced Plasticity (TWIP) Steels 73

4.2 Twinning-Induced Plasticity (TWIP) Steels

The origin of TWIP steels dates back to 1888 when Hadfield discovered “…the
very peculiar properties that manganese in large quantities imports to steel…” such
as “…peculiar hardness and great toughness …and its electrical properties…” [19].
Although Schumann in 1972 [20] and Remy and Pineau in 1977 [21] report on the
excellent mechanical properties of high-manganese steels due to pronounced
mechanical twinning as a function of chemical composition and temperature, their
results remained almost entirely unappreciated [22]. It was in the 1990s that sig-
nificant attention was paid to high-manganese steels that facilitated the TWIP effect.
Thus, Kim and Kim [23] as well as Grässel et al. [24] investigated Fe–Mn–Al–C
and Fe–Mn–Si–Al–C steel alloys, respectively, with an amount of manganese well
above 15% leading to excellent ductility. Grässel et al. [24] reported an elongation
to fracture of up to 82% at room temperature and a tensile strength of up to
600 MPa for the steel variant Fe–25Mn–3Si–3Al–0.3C at moderate strain rates. At
higher strain rates (103 s−1), even higher tensile strengths of up to 1 GPa at a
concurrently high ductility of 80% were observed. Starting from this period, this
group of steels became the focus of intensive scientific research. In particular, the
demand for advanced high-strength steels to replace the extra-low-carbon ferritic
steels—with their property combination of reasonable ductility and low strength—
is an enormous driving force, triggered as it is by demand from the automotive
industry to aid in weight reduction and fuel economy. Today, three different types
of high-manganese TWIP steels are under investigation: (i) Fe–Mn–C (e.g. [25]),
(ii) Fe–Mn–C–Al (e.g. [23]) and (iii) Fe–Mn–Si–Al (e.g. [24]). However, the most
promising candidates for the automotive industry are the Al-alloyed TWIP steel
variants due to the significant weight reduction (up to 6.8–7.3 g/cm3) depending on
the amount of the light-weight metal aluminium.

4.2.1 Thermodynamic Aspects of TWIP Steels

The equilibrium phase diagram of the binary system Fe–Mn that was revisited by
Witusiewicz et al. [26] exhibits a quite simple structure at the iron-rich corner with
an open loop of the c-iron phase field. However, under practical non-equilibrium
conditions such as rapid cooling the metastable phase diagram shown in Fig. 4.2a
reveals more details of the microstructures produced as a function of the manganese
content. Thus, for manganese contents from 5 to 25%, a multiphase microstructure
of Fe–Mn alloys becomes obvious. Whereas at lower Mn contents an a′-martensite
phase with a bcc crystal lattice can be formed in the austenite, higher amounts of
Mn lead to the formation of the e-martensite phase (hcp). Both of these phases are
formed either as stress-assisted or strain-induced variants during plastic deforma-
tion. Thus, in order to achieve stabilization of the austenitic phase up to room
temperature in the binary Fe–Mn system, a Mn content of  27% is necessary.
74 4 Advanced High-Strength Steels

Fig. 4.2 Fe–Mn phase diagram. a Metastable phase diagram. b Fe-rich corner of the Fe–Mn–C
equilibrium phase diagram at 700 °C. c Superimposition of the 700 °C austenite stability range
and the microstructure observed after quenching from 950 °C to room temperature. Reproduced
from [27]. Permission of Elsevier

However, at Mn contents of more than 30–32%, the formation of the brittle b-Mn
phase is observed. For the suppression of the formation of a′-martensite and/or e-
martensite at Mn contents below 25%, further alloying elements such as carbon,
aluminium or nitrogen are needed. All three elements act in a similar manner to Mn
—i.e. as stabilizing elements for the austenitic phase field. Thus, a uniform aus-
tenitic microstructure without any carbides and avoiding the formation of e-mar-
tensite as shown in Fig. 4.2b is obtained for carbon contents below 0.6% and Mn
contents below 12%. A further approach for the formation of single-phase TWIP
steels with suppression of the formation of a′- and e-martensite is the addition of
aluminium (see [27]). A similar effect is achieved at higher Mn contents by
avoiding carbon and by adding Al and Si. Al has a positive influence on density
reduction (up to 3% of Al). Both Al and Si have an influence on the stacking-fault
energy, which is an essential parameter in triggering the ongoing deformation
mechanisms.

4.2.2 Deformation Behaviour of TWIP Steels

High-Mn TWIP steels possess concurrently high strength and superior ductility
leading to excellent formability of these materials (e.g. [28]). The TWIP effect is
caused by pronounced strain-induced twinning leading to an extraordinary
strain-hardening effect (e.g. [29, 30]). Exemplarily, Fig. 4.3 shows typical
stress-strain curves of high-Mn TWIP steels of the type Fe–Mn–C (a) and Fe–Mn–
Si–Al (b) exhibiting pronounced strain hardening.
In comparison to conventional low-alloyed multiphase TRIP steels, high-Mn
TWIP steels have up to double the uniform elongations, significantly higher ultimate
tensile strengths and markedly higher strain-hardening rates (see [22]) as shown in
Fig. 4.4a. The pronounced strain hardening of TWIP steels is caused by the for-
mation of nanometre-thick deformation twins in the austenitic steel matrix.
Commonly, this strain-hardening effect is discussed in terms of the dislocation mean
4.2 Twinning-Induced Plasticity (TWIP) Steels 75

Fig. 4.3 Stress-strain curves of different high-Mn TWIP steels. a Fe–Mn–C steels. Reproduced
from [29]. b Fe–Mn–Si–Al steels. Reproduced from [31]. Permission of Elsevier

Fig. 4.4 Strain-hardening behaviour. a Comparison of the stress-strain behaviour and


strain-hardening rate for IF, TRIP and TWIP steels. b Illustration of the mean free path approach
(dynamic Hall–Petch effect). Reproduced from [32]. Permission of Elsevier

free path approach or so-called dynamic Hall–Petch effect [33, 34] as illustrated by
Fig. 4.4b. Thus, the dominant deformation mechanism is dislocation glide.
However, strain-induced microtwins act as obstacles on dislocation glide. Thus, the
fragmentation of the austenitic grain by increasing numbers of strain-induced twins
leads to a significant reduction in the mean free path for dislocation motion and, in
this manner, to strain hardening. This approach is focused primarily on a single
microstructure-related parameter, i.e. twin spacing [35–37].
However, the strain-hardening effect depends on several parameters such as the
temperature, the strain rate, and the grain size as reported by numerous authors (e.g.
[5, 33, 38]). Figure 4.5 shows a schematic representation of a typical
strain-hardening curve for TWIP steels with different stages of strain hardening
(Fig. 4.5a) and indicates the influence of different parameters such as austenite
grain size, temperature, strain rate and SFE (Fig. 4.5b) [5, 38]. According to
Gutierrez et al. [5], the strain-hardening curve of high-Mn TWIP steels clearly
reveals at least five different stages of strain hardening (see Fig. 4.5a). Thus, the
76 4 Advanced High-Strength Steels

Fig. 4.5 Schematic representation of strain-hardening curve obtained for TWIP steels.
a Evolution of microstructure with respect to the different stages (1) to (5) of strain-hardening
curve. b Indicated influence of different parameters on strain-hardening. Modified according to
[38]. Permission of Elsevier

first stage (1) is characterized by a significant decrease in the strain-hardening rate


and is comparable to stage III of fcc metals with high SFE such as Cu or Al (see
Fig. 2.14, Sect. 2.3). This stage is dominated by dynamic recovery processes
caused by cross-slip and dislocation annihilation. However, it should be noted that
there is a significant difference between the strain-hardening curve described for
single and polycrystalline metallic materials in Sect. 2.3. The “classical”
strain-hardening curve of fcc metals and alloys does not show a minimum of the
strain-hardening rate after passing stage III. Typically, a continuous decay of strain
hardening with increasing stress is observed in structural materials. In region (2),
the strain-hardening rate reaches a minimum value and saturates during small stress
or strain increment. In this state, Gutierrez et al. [5] observe the evolution of
dislocation substructures consisting of dislocation cells. With increasing stress a
pronounced increase in the strain-hardening coefficient is observed in stage (3).
Here, mechanical twinning occurs that cuts the previously formed dislocation cell
structure, leading to further fragmentation of the grain structure and acting as an
obstacle to further dislocation glide. In stage (4), the maximum strain-hardening
rate is reached and remains constant over certain stress/strain increments. Stage
(5) is characterized by a final decrease in the strain-hardening rate until rupture. The
microstructure contains a high dislocation density and a high volume fraction of
twin boundaries, which leads to a reduced capability for trapping more dislocations.
The general trend of influence of different parameters on the shape of the
strain-hardening curve is shown in Fig. 4.5b. It is apparent that a decrease in all
parameters (SFE, grain size, temperature and strain rate) leads to a shift to higher
strain-hardening rates in stage B (including (2) and (3) in Fig. 4.5a). However, an
increase in grain size results in a shift of the inflection point in the strain-hardening
4.2 Twinning-Induced Plasticity (TWIP) Steels 77

curve at A/B to lower strain and strain-hardening values, whereas an extension of


stage C to higher strain values occurs for intermediate grain sizes and higher
temperatures.
Recently, the responsibility of twins for the high degree of strain-hardening was
reviewed in a critical manner by several authors (e.g. [39, 40]). Thus, Huang et al.
[39] stated that the contribution of the mechanical twinning to the work hardening
rate in TWIP steels has been overestimated in recent years. Instead, the contribution
of dislocations on the work hardening is not negligible. Wang et al. [40] provided
experimental results obtained by micropillar compression tests on Fe–Mn–Si–
C TWIP steel single crystals of different orientations. It is demonstrated that
twinning has only a marginal influence on work hardening, whereas the highest
influence may be attributed to the activation of multiple slip mechanisms followed
by the activation of single slip.
Influence of temperature and strain rate. The deformation behaviour of TWIP
steels is influenced significantly by temperature, since twinning as a predominant
deformation mechanism is triggered by the SFE, which in turn depends on both
chemical composition and temperature. Therefore, changes in the deformation
mechanisms are responsible for the temperature-dependent behaviour of mechani-
cal properties. However, since the increase in strain rate is accompanied by an
increase in temperature due to adiabatic heating, the influence of the temperature
and the strain rate cannot be regarded independently of each other. Therefore, the
influence of both parameters on the strain-hardening rate will be discussed together.
Numerous publications report on the influence of both parameters on the defor-
mation behaviour of TWIP steels (e.g. [34, 38, 41–45]).
Thus, Curtze et al. [42] studied the influence of temperature on the deformation
and strain-hardening behaviour of three fully austenitic high-Mn TWIP steels with
different SFE. They showed that the elongation values of all TWIP steels are
reduced significantly at high strain rates, which is attributed to the formation of
adiabatic shear bands. Due to the resulting temperature increase, twinning mech-
anisms are replaced by dislocation glide resulting in lower strain values.
Influence of grain size. Along with the high strain-hardening behaviour, TWIP
steels exhibit a relatively low yield stress (200–600 MPa)—depending on their
chemical composition. According to the Hall–Petch relationship [see (2.11)], the
yield strength of a material can be improved significantly by reduction of the grain
diameter D, which can be obtained either by means of severe plastic deformation
(SPD) processes such as equal channel angular pressing (ECAP), high-pressure
torsion (HPT), accumulative roll bonding (ARB) or by thermomechanical pro-
cessing (TMCP). Quite often, this is accompanied by a certain loss of ductility.
However, information on the influence of grain size on the strength and ductility of
TWIP steels is still quite rare, although the methods of severe plastic deformation
allow the formation of ultrafine-grained structures with grain sizes in the
micrometre and submicrometre range. Ueji et al. [46] reported on a Fe–Mn–Al–
Si TWIP steel regarding the influence of grain size (1.8, 7.4 and 49 µm) on the
stress-strain response at room temperature. The fine-grained austenitic
78 4 Advanced High-Strength Steels

microstructure was obtained by cold rolling with a reduction in thickness up to 83%


and subsequent annealing at different temperatures. The authors showed that for a
TWIP steel with 1.8 µm grain size (0.9 µm including twin boundaries), consider-
able ductility is retained along with the increase in strength of the material in
comparison to other ufg materials such as Al or IF steel [47]. Furthermore, on the
one hand, the authors observed a suppression of strain-induced twin formation. On
the other hand, however, they observed that preferable grain orientation for twin-
ning is close to a h111i direction parallel to the direction of tensile loading. Bracke
et al. [48] showed that formation of fine-grained microstructures in high-Mn TWIP
steels due to cold rolling and annealing is accompanied by a recrystallization tex-
ture that is quite similar to the cold rolling texture of the material, which can be
described mainly by the Goss texture component (G) f110gh001i, the Brass texture
component (Bs) f110gh112i, and the Copper twin texture component (Cutwin)
f552gh115i (see [48]). Thus, along with the grain refinement, the development of a
recrystallization texture has a significant influence on the stress-strain behaviour.
Bouaziz et al. [49] obtained nanostructured Fe–22Mn–0.6C TWIP steel by a
combination of cold rolling and recovery annealing. The material exhibits a very
high yield stress (1500 MPa) and an adequate degree of elongation (8%). The
recovery annealing process decreases the dislocation density significantly, but
retains the very dense nanoscale twin microstructure introduced during the cold
rolling process, leading to these reasonable mechanical properties. Gutierrez and
Raabe [33] investigated the influence of the grain size (3 and 50 µm) on the
strain-hardening behaviour of a Fe–22Mn–0.6C TWIP steel, as shown in Fig. 4.6a,
b. They observed an improved yield strength (380 MPa) and strain hardening at
concurrently good ductility (about 40%).
Detailed microstructural investigations using scanning electron microscopy
(SEM) and the special technique of electron channelling contrast imaging (ECCI)
revealed significant differences in dislocation arrangement at early stages of
deformation in fine-grained (3 µm) and coarse-grained (50 µm) microstructures,
resulting in pronounced differences in mechanical behaviour (see Fig. 4.6c).
Thus, the early dislocation arrangement determines the density of the nucleation
sites for twins per unit grain boundary area that controls the developing twin
substructure. Hence, in the fine-grained microstructure, a loose and homogenous
dislocation arrangement is observed at low strains, whereas either a dislocation cell
structure or cell blocks limited by high dislocation density walls (HDDWs) are
detected in the coarse-grained material for the same strain. Since twinning can be
regarded as a nucleation and growth process (see Sect. 2.2) and taking into account
a dislocation interaction mechanism for twin nucleation (see Sect. 2.2), the
fine-grained microstructure provides a higher number of nucleation sites for twins
per unit grain boundary than the coarse-grained microstructure, where high dislo-
cation density is concentrated into cell walls or HDDWs. Such microstructures
provide lower numbers of twin nucleation sites per unit grain boundary.
Strain localizations. Depending on the chemical composition, high-Mn TWIP
steels (especially Fe–Mn–C steels, e.g. [6, 50–52]), but also Fe–Mn–Al–C steels,
4.2 Twinning-Induced Plasticity (TWIP) Steels 79

Fig. 4.6 Influence of grain size (3 µm and 50 µm) on the strain-hardening behaviour of high-Mn
TWIP steel (Fe–22Mn–0.6C). a True stress-true strain curves. b Strain-hardening curves. c Models
for microstructure evolution for grain sizes 3 and 50 µm. Modified according to [33]. Permission
of Elsevier

e.g. [50, 53], exhibit serrations in the stress-strain response at elevated temperatures
and even at room temperature—known as the PLC effect. As previously described,
the PLC effect is correlated with a negative SRS. Both, the PLC effect and the
negative SRS are caused by a DSA. If an ageing process, related to solute atoms,
occurs fast enough during deformation, then DSA can be observed. Thus, the
dislocation velocity should be similar to the solute mobility. The occurrence of both
effects—DSA and negative SRS—leads to the formation and propagation of PLC
bands that are correlated directly to the presence of serrations in the stress-strain
curve [6, 50–53], which have been investigated by different in situ characterization
techniques such as infrared-thermography (IR-TG) or digital image correlation
(DIC). The in situ techniques are useful for the determination of strain, strain rate,
density of mobile dislocations and temperature increase within these bands.
The origin of DSA in TWIP steels has not been clarified to date. It is even
observed in well-annealed TWIP steels with very low equilibrium vacancy con-
centration. Furthermore, DSA is observed in TWIP steels directly at the beginning
of plastic flow. Consequently, the influence of dislocation-generated vacancies can
be neglected for the occurrence of DSA. Moreover, DSA in TWIP steels also occurs
at RT. However, the diffusivity of carbon atoms at RT is too low even in the case of
a temperature increase during the propagation of PLC bands along the gauge length
[54]. In the case of high-Mn TWIP steels with a considerable concentration of
interstitially dissolved carbon, the pinning of mobile dislocations is caused either by
80 4 Advanced High-Strength Steels

a local ordering process that forms C–Mn octahedral clusters caused by the strong
attractive interactions between Mn and C atoms [55], by C–Mn pairs, by point
defect clusters [56] or by carbon-vacancy pairs [52].

4.2.3 Modelling of the TWIP Effect

Up to now, various models have been proposed that explain the pronounced
strain-hardening behaviour of TWIP steels [57–59]. Thus, Bouaziz and Guelton
[57] and Allain et al. [58] proposed physical models that describe the influence of
strain-induced twinning on the mechanical behaviour of TWIP steels based on the
Kocks–Mecking approach (see 2.13). Bouaziz and Guelton [57] proposed treating
twins as impenetrable obstacles on dislocations. Thus, the term 1/K in (2.13) can be
expressed by:

1 1 1
¼ þ ð4:1Þ
K D t

Here, t is the average twin spacing and D the grain size. According to Bouaziz
and Guelton [57], the average twin spacing can be expressed by (4.2):
1F
t ¼ 2  dtwF ð4:2Þ

with dtw as the average thickness of twins and F as the volume fraction of twins.
The models proposed by Bouaziz and Guelton [57] and Allain et al. [58] led to
isotropic hardening behaviour. Furthermore, their results show that the total volume
fraction of twins is quite small. The plastic deformation is mainly the result of
dislocation glide. Furthermore, twinning is observed on two different, sequentially
activated systems, where twins of the primary system develop across the entire
grain and twins of the second system develop between the primary twins and are,
consequently, significantly shorter and thinner. The importance of the reduction of
the average twin spacing with increasing tensile strain on strain hardening is sup-
ported by results of Jin et al. [60] on a Fe–18Mn–1.5Al–0.6C TWIP steel.
Shiekhelsouk et al. [36] proposed an elastic-viscoplastic polycrystalline model to
describe strain hardening of TWIP steels. The strain rate-dependent constitutive
model takes into account elastic behaviour, thermally activated slip and twinning
mechanism. The results from the model are corroborated by experimental results
[58, 61]. Starting with the consideration of single crystals and polycrystalline
materials and experimental investigations for Fe–Mn–C, Shiekhelsouk et al. [36]
concluded that strain hardening in TWIP steels is related to slip-twin interaction that
can be summarized as follows. For small applied strains (e < 5%), hardening is
caused by dislocation–dislocation interactions due to reduction of mean free path by
forest dislocations. At intermediate strains (5% < e < 20%), dislocation-twin
interaction becomes more important. The mean free path is reduced by the
4.2 Twinning-Induced Plasticity (TWIP) Steels 81

formation of twins on primary system. At strains e > 20%, the interaction of twins
on two activated twin systems becomes important, as it causes a further reduction of
mean free path for dislocations. In summary, the model of Shiekhelsouk et al. [36]
addressed the following aspects regarding strain hardening in TWIP steels:
(i) Thermal activation of dislocation glide determines the yield strength. (ii) The
inelastic strain is carried more by slip than by twinning, since the volume fraction of
twins is quite low in these materials. (iii) The strain generated by twin formation
leads to the relaxation of intergranular stresses. (iv) Slip–twin interactions are the
most important mechanisms for strain hardening. (v) Twin activity is reduced with
increasing twin–twin interactions. Thus, consequently, strain hardening in TWIP
steels is the result of competition between hardening and softening mechanisms
related to twinning. In addition, the formation of C–Mn clusters is also considered
to contribute to the hardening observed in TWIP steels.
Kim et al. [62] and Lee et al. [63] described a constitutive model for describing
strain hardening in a Fe–18Mn–1Al–0.6C TWIP steel caused by mechanical
twinning and dynamic strain ageing. The model is based on tensile tests at different
temperatures (RT  T  400 °C), and detailed microstructural investigations
using TEM and SEM to describe the critical strain for the onset of twinning, the
volume fraction of twins, the twin thickness and the dislocation density. The model
approach is based on the implementation of the Kocks–Mecking model [64] and the
Kubin–Estrin model [65] to the evolution of dislocation density provided by Taylor
[see Sect. 2.3 (2.11)–(2.15)].
For the mechanical twinning found in TWIP steels, the evolution of twin density
given by (4.2) has to be taken into account. The evolution of the storage rate of
dislocations can then be expressed by a combination of (2.14) and (4.2) [62]:
  
d. 1 1 1 F pffiffiffi
¼M þ  þ k2 . ð4:3Þ
de b D dtw 1  F

Regarding the separation into mobile and forest dislocations according to the
Kubin–Estrin model [see (2.15) and (2.16)], the dislocation storage is then
described by (4.4) for mobile dislocations and by (4.5) for forest dislocations [62]:
   
d.m C1 .f C3 pffiffiffiffi 1 1 F
¼M 2  C2 .m  .f    ð4:4Þ
de b .m b b  d b  dtw 1  F
 
d.f C3 pffiffiffiffi 1 1 F
¼ M C2 .m  .f     C 4 .f ð4:5Þ
de b b  d b  dtw 1  F

C1 , C2 , C3 and C4 are constants that are described already in Sect. 2.2 [see (2.15)
and (2.16)].
82 4 Advanced High-Strength Steels

In addition, the evolution of the volume fraction of twins is given by (4.6) [62]:
h im
F ¼ F0 1  ebðdtw ecrit Þ ð4:6Þ

Here, F0 is the maximum volume fraction of twins and ecrit is the critical strain
for the onset of twinning. b and m are fitting parameters. For modelling the
strain-hardening behaviour of TWIP steels, several aspects have to be taken into
account [62]:
(i) Mechanical twinning is not distributed homogenously over the whole
microstructure. Twinning significantly depends on the applied strain and the
grain orientation.
(ii) Therefore, the microstructure has to be separated into (a) twinned grains and
(b) twin-free grains, and can be regarded as a two-phase system.
(iii) Consequently, the stress-strain response of TWIP steels can be described
according to a rule of mixture [62]:

r ¼ f ðeÞ  rtw þ ð1  f Þ  rtwfree ð4:7Þ

Here, f is the fraction of twinned grains, which is a function of applied strain e,


rtw is the stress response of twinned grains and rtwfree of twin-free grains.
(iv) The evolution of the mobile and forest dislocation densities must be described
separately for twin-free grains without the term related to twinning [62]:
   
d.m C1 .f C3 pffiffiffiffi 1
¼M 2  C 2 .m  .f  ð4:8Þ
de b .m b bD
 
d.f C3 pffiffiffiffi 1
¼ M C2 .m  .f   C4 .f ð4:9Þ
de b bd

(v) For twinned grains, the evolution of the dislocation densities has to be
described separately before and after the critical strain for the onset of twin-
ning. Before the onset of twinning the dislocation density evolution is given
by (2.14). After the critical strain, the dislocation density evolution is
expressed by (4.4) and (4.5) for mobile and forest dislocations, respectively.
(vi) Finally, the influence of DSA has to be taken into account by an extension of
(2.12) in the following manner [62]:
pffiffiffi
r ¼ r0 þ M  a  b  . þ rDSA with rDSA ¼ v  C5 ð4:10Þ

Here, C5 describes the concentration of solute atoms at the dislocation line and v
the strength of interaction between the solute atoms and dislocation line.
4.2 Twinning-Induced Plasticity (TWIP) Steels 83

Fig. 4.7 Modelling of the stress-strain behaviour of TWIP steels. a Comparison of the model
curves for the twin-free grains and twinned grains with experimental true stress versus true strain
curves. In addition, the model curve according to the rule of mixture is plotted. b Strain-hardening
curves obtained from the experimental data and the calculation according to the rule of mixture.
Reproduced from [63]. Permission of Elsevier

The results of the model using experimentally determined data for dislocation
densities, twin fraction, critical twin strain, etc., are summarized in Fig. 4.7. Here,
the results of the model applied for twin-free grains, twinned grains and the
two-phase microstructure (rule of mixture) are compared with the experimentally
determined stress-strain curve. It is obvious that the model for twin-free grains
correlates well with the stress-strain curve at small strains, whereas at medium and
higher strains the stress-strain response is underestimated by this model. It is in
agreement with [36] that the hardening at this low degree of deformation is
determined by dislocation–dislocation interaction. However, the model for twinned
grains only fits well with the experimental stress-strain curve at low applied strains.
For higher strains, the stress-strain response is overestimated by this model
approach. Therefore, a reasonably good correlation is achieved using the rule of
mixture for twin-free and twinned grains indicating that the influence of twinning
becomes more dominant at higher strain levels. A further conclusion from this
model approach is that DSA has only a minor effect on actual stress-strain response
and hardening behaviour.

4.3 Transformation-Induced Plasticity (TRIP) Steels

Transformation-induced plasticity can be understood “… as significantly enhanced


plasticity during phase change…” [66]. TRIP is observed in high-strength,
low-alloyed steels such as ferritic-bainitic steels with retained austenite—known as
TRIP-assisted steels (e.g. [67, 68])—or in high-alloy austenitic stainless steels such
as AISI 304 (e.g. [4, 69]). Whereas TRIP-assisted steels exhibit a multiphase
microstructure consisting of retained austenite (>5 vol.%) (due to higher carbon and
84 4 Advanced High-Strength Steels

silicon content) embedded in a ferritic matrix with additional volume fractions of


bainite and martensite, the microstructure of high-alloy TRIP steels with
low-carbon content consists of metastable austenite.
In the present work, high-alloy austenitic steels will be discussed only.

4.3.1 Thermodynamic Aspects of TRIP Steels

The thermodynamics of the transformation-induced plasticity are triggered by the


chemical composition of the material. As shown in Sect. 3.2, Gibbs free energy is
the driving force for MPT that is reasonable for the TRIP effect. The type of MPT
such as (i) spontaneous MPT, (ii) stress-assisted MPT and (iii) strain-induced MPT
is determined by well-defined transition temperatures. The spontaneous MPT
occurs in the temperature range Mf \T\Ms , where Ms is the martensite start
temperature below which first martensite has been formed and Mf is the martensite
finish temperature, where spontaneous MPT is completed. The temperature Msr
describes the temperature where stress-assisted MPT sets in. In the temperature
range Msr \T\Md strain-induced MPT occurs, where Md defines the maximum
temperature where MPT can occur under external stresses. The Md30 temperature is
related to the temperature where up to 50% of strain-induced a′-martensite are
formed due to 30% of plastic deformation [70]. These martensitic temperatures are
depending significantly on the chemical composition. Thus, several empirical
equations are provided in literature for the calculation of the Ms temperature of the
spontaneous c to a′ transition including main interstitial (C and N) and substitu-
tional (Cr, Ni, Mn, Mo, Cu, Si, Al) alloying elements:
0
Msc!a ð CÞ ¼ 1182  1456ð%C þ %NÞ  37%Cr  57%Ni ð4:11Þ
0
Msc!a ð CÞ ¼ 1350  1665ð%C þ %NÞ  28%Si  33%Mn  42%Cr  61%Ni
ð4:12Þ

Msc!a ð C) ¼ 502  820%C  1230%N  13%Mn  30%Ni  12%Cr


0

ð4:13Þ
 54%Cu  6%Mo
0
Msc!a ðKÞ ¼ A3  199:8ð%C þ 1:4%NÞ  17:9%Ni  21:7Mn  6:8%Cr  45%Si
 55:9%Mo  1:9ð%C þ 1:4%NiÞð%Mo þ %Cr þ %MnÞ
 14:4½ð%Ni þ %MnÞð%Cr þ %Mo þ %Al þ %SiÞ1=2 410
ð4:14Þ

It becomes obvious that all alloying elements yield a reduction of the Ms tem-
perature and, therefore, a stabilization of austenite.
4.3 Transformation-Induced Plasticity (TRIP) Steels 85

In analogy to the Ms temperature, empirical equations were developed for the


calculation of the Md30 temperature, which are summarized in [71]. Equation (4.15)
was developed by Angel in 1954 [70] and accounts the main alloying elements C,
N, Si, Mn, Cr, Ni and Mo. The following (4.16) and (4.17) are modifications of
Angel’s (4.15) using different weighting factors for the influence of Ni.
Equation (4.18) takes the grain size into account along with further alloying ele-
ments such as Cu and Nb.
0
Mda ð CÞ ¼ 413  462ð%C þ %NÞ  9:2%Si  8:1%Mn  13:7%Cr  9:5%Ni
 18:5%Mo
ð4:15Þ
0
Mda ð CÞ ¼ 497  462ð%C þ %NÞ  9:2%Si  8:1%Mn  13:7%Cr  20%Ni
 18:5%Mo
ð4:16Þ
0
Mda ð CÞ ¼ 608  515%C  821%N  7:8%Si  12%Mn  13%Cr  34%Ni
 6:5%Mo
ð4:17Þ
0
Mda ð CÞ ¼ 515  462ð%C þ %NÞ  9:2%Si  8:1%Mn  29ð%Ni þ %CuÞ
 13:7%Cr  18:5%Mo  68%Nb  1:42ðGS  8:0Þ
ð4:18Þ

In similar way, the Md temperature is decreasing with an increase in concen-


tration of all alloying elements. Although Cr and Mo are known as ferrite stabi-
lizers, they yield a reduction of both martensitic temperatures. This is caused by the
fact that the stabilizing effect of alloying elements on ferrite or austenite is valid for
binary Fe-systems only.
Once ternary or quaternary systems have to be regarded, the stabilizing princi-
ples of binary systems are no longer valid, since interactions between different
alloying elements have to be taken into account. In order to describe the stabilizing
effect of alloying elements, so-called constitutional diagrams can be drawn. The
most known diagrams belong to Strauss–Maurer [72] and Schaeffler-De Long [73].
These diagrams describe the phase composition of steels where either the weight
per cent of chromium and nickel (Strauss–Maurer) or the nickel and chromium
equivalents (Schaeffler, De Long) are plotted. The Maurer diagram is applicable for
CrNi steels with 0.2 wt% C, which are quenched in water from 1050 °C and
contains the phase boundary lines for austenite, martensite, ferrite, perlite and
troostite. The chromium and nickel equivalents used in the Schaeffler diagram can
be calculated according to the following equations:
86 4 Advanced High-Strength Steels
4.3 Transformation-Induced Plasticity (TRIP) Steels 87

JFig. 4.8 Comparison of the temperature course of chemical driving force DG for different
martensitic transformation in both binary Fe-based alloys with different contents of Ni and Cr and
for ternary Fe-based alloys with 17% Cr. a Direct c ! a′ transformation. b c ! e transformation.
c e ! a′ transformation. In addition, the DG  T course for pure iron is shown (bold black line).
Reproduced according to [71]. With courtesy of A. Weiss and H. Gutte

Nieq ¼ %Ni þ 30%C þ 0:5%Mn ð4:19Þ

Creq ¼ %Cr þ %Mo þ 1:5%Si þ 0:5%Nb ð4:20Þ

Here, the active factor for chromium and nickel is equal to one. Higher active
factors of other alloying elements characterize their more pronounced influence
related to chromium or nickel. In the Schaeffler diagram, the austenite phase field
and the two-phase field of austenite and ferrite are separated by straight lines.
Furthermore, straight iso-lines for different volume fractions of ferrite are included.
The effect of the main alloying elements Cr and Ni on the chemical driving force
for MPT was recently evaluated by Weiss and Gutte [71] both for binary Fe–Ni and
Fe–Cr as well as for ternary Fe–Cr–Ni systems with respect to the different MPT c
! a′, c ! e and e ! a′.
Figure 4.8 shows the influence of the elements chromium and nickel on the
temperature dependence of Gibbs free energy for the c ! a′, c ! e and e ! a′
phase transformations. Thus, the continuous increase in chromium results in a shift
0
of DGc!a to lower temperatures and negative values in the direction of metastable
austenite. In contrast, the increase in nickel content yields a stabilization of the
0
austenite since the DGc!a is shifted to lower temperatures and positive values in
the direction of stable austenite. The same is valid for the ternary Fe–17Cr–xNi
alloy. Finally, at temperature T  200 °C both the binary Fe–xCr and Fe–xNi
alloys as well as the ternary Fe–17Cr–xNi alloy are characterized by metastable
austenite, which is able to undergo either a stress-assisted or a strain-induced MPT.
In similar way, the temperature dependence of DG values for the c ! e and the e !
a′ transitions can be interpreted. However, here, the influence of chromium and
nickel is in the same direction [71].
Recently, thermomechanical modelling of MPT was developed by Weiss and
Gutte [71] for metastable CrNi steels. According to Sect. 3.4, different variants of
MPT (c ! a′, c ! e, c ! e ! a′) can occur individually or overlap each other.
Weiss and Gutte determined the thermodynamical stability factors accounting for
both the martensitic nucleation conditions as well as the relevant mechanical work
of stress-assisted and strain-induced MPT. Based on these results in combination
with detailed microstructure analysis and true stress-true strain curves, specific
stress-temperature-transition (STT) and deformation-temperature-transition
(DTT) diagrams were obtained. These diagrams represent the thermodynamical
stability as well as the nucleation kinetics of the involved phases and allow for the
88 4 Advanced High-Strength Steels
4.3 Transformation-Induced Plasticity (TRIP) Steels 89

JFig. 4.9 Stress-temperature-transition and deformation-temperature-transition diagrams for Fe–


16Cr–6Mn–6Ni–0.05C steel. a Stress-temperature-transition (STT) diagram. b Deformation-
temperature-transition (DTT) diagram. c Comparison of the phase field c ! a′ for three Fe–16Cr–
6Mn–xNi–0.05C steels with varying nickel content x = 3 wt%, 6 wt% and 9 wt%, respectively.
Reproduced from [74]. Permission of Wiley VCH

characterization of the stress-assisted and strain-induced MPT. Furthermore, values


for martensite formation temperatures as well as for strength and plastic strain
regarding MPT can be delivered. Moreover, the influence of the SFE becomes
apparent. Figure 4.9a, b shows an example of STT and DTT diagram, respectively,
for a low-carbon, high-alloy metastable austenitic steel (16 wt% Cr, 7 wt% Mn, 6
wt% Ni) [74], where solid lines are experimentally determined and dashed lines
correspond to approximations. Indicated are the fields of different transformations
such as c ! a′, c ! e, Tw and c ! Tw, specific temperatures Td, different Md, Ms
and specific stress (Rm, r0.2, rA) and strain (Ag, De) parameters. Thus, Md and Td
indicate temperatures below which MPT or twinning occur, respectively. Ms is the
temperature below which spontaneous MPT occurs and rA is the triggering stress
for individual phase transformations or deformation processes.
Figure 4.9c shows the influence of the austenite stability and, consequently, the
stacking-fault energy, on shape and temperatures of the transformation field c ! a′
for three Fe–16Cr–7Mn–xNi–0.05C cast steels with different Ni content. It is
obvious that the Ni content has a significant influence on the austenite stability and,
therefore, on the shape of the phase field c ! a′ as well as on the transition
temperatures. Thus, the Md;c!a0 is shifted to lower temperatures with increasing Ni
content. Moreover, the Md temperature for the steel with 3 wt% Ni is 140 °C,
whereas it decreases up to 50 °C for the steel with 9 wt% Ni.

4.3.2 Deformation Behaviour of TRIP Steels

The mechanical properties of metastable austenitic TRIP steels are characterized by


high strength caused by high strain-hardening rate at concurrently high ductility
(e.g. [75]). The dominating deformation mechanism behind the TRIP effect is the
martensitic phase transformation from the metastable fcc austenite into the bcc a′-
martensite. The pronounced formation of a′-martensite results in sigmoidal course
of the stress-strain curve as shown schematically by Fig. 4.10a. Figure 4.10b shows
the typical strain-hardening behaviour of a steel exhibiting TRIP effect that is
comparable to hardening curves obtained for TWIP steels. However, as shown by
Talonen [76], the evolution of the strain hardening until the second maximum at
higher strain values is caused by the evolution of the volume fraction of
strain-induced a′-martensite. Thus, the first part with the monotonic decrease in
strain-hardening rate until the minimum is common for fcc materials with higher
SFE and steels exhibiting TWIP or TRIP effect. This stage of the hardening curve is
dominated by dislocation–dislocation and dislocation–grain boundary interactions.
90 4 Advanced High-Strength Steels

Fig. 4.10 Stress-strain behaviour and strain-hardening behaviour of TRIP steels. a Schematic
representation of the TRIP effect on the stress-strain behaviour. Modified according to [77].
Permission of Wiley VCH. b Strain-hardening behaviour (bold line) and evolution of the volume
fraction of strain-induced a′-martensite (dashed line). Reproduced from [78]. Permission of
Elsevier

The pronounced increase in strain hardening in stage II is caused by the significant


increase in the volume fraction of strain-induced a′-martensite. Due to the
martensitic grains within deformation bands, the mean free path of dislocations is
reduced as well. At the transition of stage II to stage III, the a′-martensite grains
tend to grow together forming a network of a′-martensite.
At the maximum of the strain-hardening curve stage IV evolves, where the
plastic deformation is carried solely by the martensitic phase.
Since the martensitic phase transformation is determined by austenite stability
and stacking-fault energy, parameters such as (i) temperature, (ii) strain rate and
(iii) grain size have a significant influence on MPT, and therefore, on the TRIP
effect.
Influence of chemical composition. Alloying elements have a significant influence
on the TRIP effect in terms of austenite stability regarding MPT, the morphology of
a′-martensite and difference between Ms and Md temperatures [71] as shown by
thermodynamics of TRIP steels (see Sect. 4.2.2).
Influence of temperature. The influence of temperature on stress-strain behaviour
of classical fcc materials is related to a decrease in hardening with increasing
temperature, whereas the yield strength remains almost unaffected by temperature
increase. However, along with this classical behaviour metastable austenitic steels
exhibit significant changes in mechanical properties depending on deformation
temperature that are related to changes in the dominant deformation mechanisms.
Thus, an anomaly of the uniform elongation and the elongation to rupture is
observed depending on temperature, whereas YS and UTS exhibit a slight and a
pronounced decrease with increasing temperature, respectively. Thus, Fig. 4.11a
provides an example for strain-hardening curves at different temperatures and
Fig. 4.11b shows the temperature dependence of mechanical parameters (YS, UTS,
eun, er) obtained on austenitic steels with TRIP effect. Thus, Fig. 4.11a demonstrates
4.3 Transformation-Induced Plasticity (TRIP) Steels 91

Fig. 4.11 Strain-hardening behaviour and mechanical properties of austenitic steels enabling
TRIP effect. a Influence of temperature on strain-hardening behaviour. b Influence of temperature
on mechanical parameters: Yield strength, ultimate tensile strength, uniform elongation and strain
to failure. Reproduced from [79]. With courtesy of S. Martin. b Reproduced from [31]. Permission
of Elsevier

the influence of temperature on strain-hardening behaviour of metastable austenitic


steel AISI 304. Whereas at RT the classical strain-hardening curve for fcc materials
with a continuous decrease in strain hardening is obtained, pronounced strain
hardening occurring around 10% of elongation is increased with a decrease in
temperature. Thus, at −192 °C a pronounced MPT occurs resulting in a significant
strain hardening. Figure 4.11b shows the effect of temperature on mechanical
properties of a Fe–20Mn–3Si–3Al–0.4C obtained at low strain rate of 10−4 s−1
[31]. Clearly, three different regions can be separated. Region I is characterized by a
moderate increase in both the elongation parameters—uniform elongation eu and
elongation to rupture er —accompanied by a slight increase in UTS, whereas YS
remains nearly unchanged. In this temperature range, neither MPT nor twinning
occurs and the steel deforms by dislocation glide.
In region II, a significant increase in eu and er is observed reaching a maximum at
about 50 °C that is caused by MPT. The rate of transformation is accelerating with
decrease in temperature. The enhanced elongation is not correlated to volume
fraction of formed a′-martensite, but, instead, to the stage when it occurs. The
temperature, where maximum elongation is observed, varies depending on chem-
ical composition. Here, MPT is observed at high strains and contributes, conse-
quently, to the delay of local necking [7, 31, 80]. However, in spite of MPT, the
elongation decreases significantly at temperatures <50 °C since the onset of MPT is
shifted to lower strain values. Both UTS and YS exhibit a pronounced increase in
regions II and III.
Influence of strain rate. The strain-hardening behaviour is influenced significantly
by strain rate depending on austenite stability and, therefore, on chemical com-
position. Most important effect of strain rate on mechanical properties is caused by
adiabatic heating leading to a reduction of rate of phase transformation c ! a′.
92 4 Advanced High-Strength Steels

Fig. 4.12 Influence of the


strain rate and the
stacking-fault energy on the
TRIP/TWIP effect of
austenitic stainless steels.
Reproduced from [45].
Permission of Springer

Thus, for steels with low austenite stability (e.g. AISI 301LN) both strain-hardening
curve as well as martensitic transformation curve evolve over maximum values.
These maxima are shifted to both lower strain hardening and transformation rate,
respectively, as well as to higher strain values. In contrast, in the more stable steel
(AISI 304), the strain rate has a weak influence on the strain-hardening rate [80]
only. Impeding MPT at higher strain rates results in a transition from TRIP to TWIP
effect depending on SFE of the steel as shown in Fig. 4.12. Thus, alloys with a
SFE < 12 mJ/m2 exhibit a martensitic phase transformation from austenite into a′-
martensite via e-martensite independent of strain rate. Likewise, in steel alloys with
SFE > 18 mJ/m2, the dominant deformation mechanism resulting in high ductility
is mechanical twinning independent of strain rate. However, for materials with SFE
in the range 12  cSF  18 mJ/m2, the strain rate has a pronounced influence on
ongoing deformation mechanisms. Whereas at low strain rates MPT yielding TRIP
effect dominates, the temperature increase due to adiabatic heating with increasing
strain rate causes a transition from MPT to twinning yielding TWIP effect. Thus, at
intermediate strain rates both mechanisms are competing. At high strain rates,
TWIP effect is dominant due to the increase in SFE with the increase in the
temperature.
In addition, the different strain rate sensitivities of the CRSS for individual
deformation mechanisms—dislocation glide, twinning, and e-martensite formation
—has to be taken into account. Whereas the CRSS for twinning in fcc materials is
nearly strain rate independent, the CRSS for formation of e-martensite exhibits a
pronounced strain rate sensitivity.
Therefore, the favoured mechanism of strain hardening in the whole range of
strain rates is the mechanism with the lowest CRSS. The transition from TRIP to
TWIP effect is triggered by the difference in CRSS at increasing strain rates [45].
Influence of grain size. The initial grain size of austenite has a significant influence
both on yield strength of material as well as on transformation-induced plasticity.
According to Hall–Petch effect, the reduction of austenitic grain size results in a
significant increase in yield strength of metastable austenitic steel. In the past,
numerous authors investigated the influence of austenitic grain size on MPT and
resulting strain-hardening behaviour for metastable austenitic stainless steels (e.g.
[81–84]). The intensive investigated range of grain size is about 10 µm up to
400 µm. A comprehensive overview of influence of grain size on MPT was pro-
vided by Marechal [85]. Thus, in general, two aspects can be summarized: (i) the
reduction of austenitic grain size results in an increase in austenite stability
regarding spontaneous martensite transformation due to a decrease in Ms
4.3 Transformation-Induced Plasticity (TRIP) Steels 93

temperature (e.g. [86]), (ii) similar effect of reduced grain size was found for
formation of strain-induced a′-martensite. In addition, the reduction of transfor-
mation rate of a′-martensite was observed (e.g. [81]). Quite recently, numerous
investigations were performed on ultrafine-grained austenitic steels and their
mechanical properties (e.g. [87–90]. In general, reduced grain size results in a
reduction of transformation rate yielding a reduction of strain-hardening rate, too.
However, in two-phase materials, such as ufg duplex steels [91] or austenitic
stainless steels with bimodal austenitic grain structure [87] a faster strain-hardening
rate was detected than in coarse-grained counterparts. Furthermore, these investi-
gations turned out that a change in the formation of strain-induced a′-martensite
occurs. Thus, Marechal [85] showed differences in the a′-martensite morphology
depending on the grain size. Whereas in coarse-grained austenite (200 µm), dif-
ferent martensite variants are formed within deformation bands consisting of high
SF density, in ufg material (<1 µm), only one or in maximum two martensite
variants have been formed occupying partly or completely austenitic parent grain.
Recently, Yen et al. [91] supposed a change from strain-induced formation to
stress-assisted formation of a′-martensite in ufg austenitic stainless steels with a
mean grain size <1 µm as shown in Fig. 4.13. Favoured sites for formation of a′-
martensite in ufg austenitic steels are grain and/or twin boundaries instead of
intersection deformation bands in coarse-grained material. In case of ufg austenitic
microstructure often a pronounced Lüders phenomenon is observed similar to other
ufg materials (e.g. [47]).
Influence of deformation mode and stress state. Along with temperature, strain
rate and grain size, applied deformation mode and stress state have a significant
influence both on MPT as well as on strain-hardening behaviour. However, in
literature contradictory statements were found regarding tensile, compressive,
shear, torsion and biaxial loading conditions. Recently, Beese and Mohr [92]
presented an overview of investigations on influence of stress state on martensitic
transformation rate. Thus, Iwamoto et al. [93] showed the influence of deformation
mode and stress state on MPT and the resulting stress-strain response. It was shown
for the steel AISI 304 that the fraction of strain-induced a′-martensite was signif-
icantly higher at small strains during compressive loading than for tensile loading,

Fig. 4.13 Schematic diagram


of 610SA steel showing the
relationship between grain
size and mechanism of
deformation-induced
martensite. Modified
according to [91]. Permission
of Elsevier
94 4 Advanced High-Strength Steels

which results in respective stress-strain responses. At higher strain levels, the


dependence is reversed. This stress-state dependence was incorporated in gener-
alized models of Stringfellow [94] and Tomita and Iwamoto [75] (see Sect. 4.3.2).
The influence of the deformation mode on MPT was also shown by Varma et al.
[81] for investigations on AISI 304L and AISI 316L under tensile loading and
during cold rolling. The steel AISI 316L is known as a stable austenite at RT. Thus,
the steel does not undergo a MPT during tensile loading at RT. However, during
cold rolling a remarkable amount of a′-martensite (10%) is formed. Thus, the
triaxiality of stress state has a positive influence on MPT. Lebedev and Kosarchuk
[95.] investigated two commercially available Fe–18Cr–10Ni steels under uniaxial
tension and compression, torsion and biaxial loading with different principal stress
ratios. From these results, it is concluded that deformation in tension promotes the
formation of a′-martensite in contrast to deformation by torsion or even by com-
pression. Thus, an increase in triaxiality and a reduction of stress deviator—
so-called Lode’s parameter—intensifies MPT from austenite into a′-martensite.
Influence of texture. Alongside with grain size and deformation mode, initial texture
of austenite has to be taken into account regarding martensitic phase transformation
rate. The paper of Creutziger and Foecke [96] was concerned with initial austenite
texture and its influence on MPT. Thus, as known the texture of rolled fcc materials
with low stacking-fault energy (see e.g. [97]) consists of three main texture com-
ponents such as Brass component (Bs) f110gh112i, Goss component
(G) f110gh001i and Copper component (C) f112gh111i. After recrystallization, in
addition, the Cube component (W) f100gh001i can be observed. Creutziger and
Foecke [96] calculated the transformation potential based on work criterion for the
formation of twinned martensite taking into account 16 different stress paths starting
from uniaxial tension along rolling direction (RD) up to deep drawing along RD.
The transformation potentials are drawn in dependence on crystallographic orien-
tation. It turned out that Bs- and C-texture components exhibit lowest transformation
potential, whereas the transformation potential for W-component is significantly
higher at all 16 stress states indicating that both crystallographic orientations are
non-favoured for MPT in contrast to W-orientation. Furthermore, a clear asymmetry
for transformation potential for tensile and compressive stress state was observed.
Unfortunately, G component was not included in these calculations.

4.3.3 Modelling of the TRIP Effect

The stress-strain response of TRIP steels is influenced significantly by the


strain-hardening behaviour caused by formation of strain-induced a′-martensite.
Therefore, the majority of models describing TRIP effect are dealing with kinetics
of MPT (see Sect. 3.6). Furthermore, the models account for influence of strain,
strain rate, temperature and stress state on kinetics of MPT. The most common
model of Olson and Cohen [98] was already described in Sect. 3.6.
4.3 Transformation-Induced Plasticity (TRIP) Steels 95

The model of Ludwigson and Berger (cited in [99]) is based both on the volume
fraction of a′-martensite as well as on the interaction of the evolving strain-induced
a′-martensite and the austenite. Therefore, the model uses a rule of mixture
describing flow stress accounting for strain hardening both of austenite and a′-
martensite related to their volume fractions [100]. Narutani et al. [101] used a rule
of mixture based on stress-strain data of a stable austenite and a pure martensite
accounting for varying volume fractions. However, due to strong overestimation of
experimental stress-strain curves Narutani et al. [101] introduced a term accounting
for strain caused by transformation leading to a strain-corrected rule of mixture
model.
However, these models do not account for the influence of strain rate and
temperature on stress-strain response of TRIP steels. Tomita and Iwamoto [75]
proposed a generalized version of the constitutive equation of Stringfellow’s model
[94] and implemented a heat equation accounting for temperature increase due to
plastic deformation and contribution of latent heating due to MPT. By this model,
the stress-strain response of an austenitic steel AISI 304 under tensile loading is
described qualitatively well in a range of strain rates and temperatures of
5  10−2 s−1  e_  5  102 s−1 and −193 °C  T  72 °C, respectively.
Levitas [102] developed a comprehensive mesoscopic thermomechanical contin-
uum theory for MPT in materials. The model proposed by Yoo et al. [103] uses the
constitutive model of Tomita and Iwamoto [75] in conjunction with a damage
mechanics-based approach accounting for material degradation.
Wolf et al. [100] presented a constitutive model for describing the influence of
strain rate on TRIP effect. The model was developed according to extended
investigations of the influence of strain rate and temperature on stress-strain
response of high-alloy Fe–16Cr–6Mn–xNi–0.05C TRIP steels. Furthermore,
detailed microstructural investigations were performed in order to study the influ-
ence on the ongoing deformation mechanisms. The proposed model is based on the
Ludwik equation for describing flow stress of an austenite with low SFE, a constant
flow stress of martensite based on experiments and a rule of mixture for flow stress
of a two-phase material consisting of austenite and strain-induced martensite.
Finally, adiabatic heating was included into the model. The adiabatic heating
occurring, especially during high strain rate deformation, leads both to a thermal
softening of austenite as well as to a retardation of MPT to higher strain values and
lower volume fraction of strain-induced a′-martensite. The suggested model
describes well experimental data obtained in a wide range of strain rates of 10−4
s−1  e_  103 s−1.
A phenomenological model description was provided by Martin et al. [104]
based on experimental investigations on high-alloy Fe–16Cr–6Mn–xNi–0.05C
TRIP steels with different grain sizes. This approach is based on a Hall–Petch like
effect comparable to TWIP steels that is caused, however, by reduction of mean free
path of dislocations due formation of a′-martensite grains within deformation bands
with high density of SFs. It is shown that resulting strain-hardening behaviour is
influenced significantly by formation of a′-martensite, but is independent of grain
size. However, the grain size has a significant influence on onset of MPT.
96 4 Advanced High-Strength Steels

Along with constitutive models describing TRIP effect, some micromechanical


and mesoscopic models exist (e.g. [102, 105]). A thermomechanical model
describing TRIP effect was proposed by Prüger et al. [106, 107]. This model
incorporates the influence of temperature on martensitic transformation occurring,
especially during high strain rate deformation.

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Chapter 5
In Situ Techniques for Characterization
of Strain Localizations and Time
Sequence of Deformation Processes

Abstract This chapter gives a comprehensive overview on in situ characterization


techniques, which are useful for the characterization of strain localizations and the
temporal evolution of deformation processes. The chapter is divided into four parts
regarding (i) general remarks, (ii) in situ imaging techniques, (iii) in situ acoustic
emission measurements and (iv) in situ full-field measurement techniques. The part
of in situ imaging techniques is divided into (i) optical microscopy and scanning
electron microscopy, whereas the part of full-field measurement techniques is
separated into digital image correlation (measurement of displacement and/or strain
fields) and infrared thermography (measurement of thermal fields). For all in situ
techniques, a short historical overview is given together with a summary of the
basic knowledge and a review of state-of-the-art research (starting from the year
2000 provided in the appendix).

5.1 General Considerations

Both knowledge and understanding of microstructure–property relationships are


essential for the further improvement of materials behaviour and performance. As
shown in the previous sections, strain localizations during plastic deformation of
metals play a significant role, since they are precursors for degradation or damage
of materials. Thus, comprehensive knowledge of these strain localizations is
essential for improvement of mechanical properties of materials. For this purpose,
non-destructive, non-invasive in situ experiments are particularly favourable. In
field of Materials Science and Engineering, in situ experiments are used for direct
observation of processes and reactions of materials at the place of their origin under
defined loading conditions such as (i) mechanical, (ii) thermal and (iii) electrical
loading or combined mechanical/thermal loading. Thus, in situ experiments make it
possible to find answers to the following questions: (i) Which microstructural
processes take place? (ii) Where do these processes occur? (iii) Under which
conditions do processes take place? and/or (iv) How are these processes controlled?
The field of observable microstructural processes during mechanical loading ranges

© Springer Nature Switzerland AG 2020 99


A. Weidner, Deformation Processes in TRIP/TWIP Steels,
Springer Series in Materials Science 295,
https://doi.org/10.1007/978-3-030-37149-4_5
100 5 In Situ Techniques for Characterization …

Table 5.1 In situ experiments under mechanical and thermal loading


In situ experiment Observed reactions Additional parameters
Mechanical loading • Local deformation • Stress, strain
• Tension • Orientation changes • Number of cycles
• Compression • Phase transformation • Number of cracks
• Fatigue • Crack initiation/propagation • Crack propagation rate
• Bending • Crack tip opening displacement (CTOD) • Temperature
• Shear • Fatigue behaviour • Acoustic emission
• Wear • Delamination • Indentation hardness
• Nanoindentation
Thermal loading • Surface reactions • Specimen temperature
• High temperatures • Sintering, solidification
• Low temperatures • Phase transformation

from localized deformation processes such as formation of slip bands (SB), per-
sistent slip bands (PSB), deformation bands (DB) and mechanical twinning via
phase transformations (PT) up to damage mechanisms such as debonding of
particles/inclusions, fracture of particles/inclusions, formation of voids, crack ini-
tiation and crack propagation. Processes like sintering of powder particles, solidi-
fication, phase transformations as well as surface reactions (oxidation) can be
observed during thermal loading. Table 5.1 summarizes typical in situ experiments
under mechanical and thermal loading, including observable reactions as well as
parameters that can be determined additionally.
Therefore, in situ experiments are ideally suited to analyse time sequence of
deformation and damage processes at different length and time scales depending on
method applied. According to methods applied during the in situ experiments, two
main groups can be identified: (i) methods using imaging techniques and
(ii) methods using diffraction techniques. Both—imaging and diffraction techniques
—use radiations of different wavelength. Thus, in situ experiments combined with
imaging techniques are conducted using visible light (0.38—0.78 µm), electrons
(<0.1 nm) or infrared radiation (0.78–12 µm). Moreover, atomic force microscopy
(AFM) in contact or non-contact mode (e.g. [1]) is also used for in situ experiments.
Among imaging techniques, AFM allows the highest lateral resolution (0.1–
10 nm). In situ experiments in combination with diffraction techniques use neutron
(0.1–1 nm), X-ray (1–10 nm) or electron radiation (<0.1 nm). In addition, methods
based on time scales or frequency domains are known such as the analysis of
acoustic waves or harmonic vibrations as well as material properties like mag-
netism. A short overview of imaging and diffraction techniques used for in situ
experiments is given in Table 5.2.
Furthermore, in situ experiments can be separated into (i) real-time, (ii) quasi
in situ and (iii) interrupted monitoring tests. The limiting factor for real-time in situ
experiments is the rate of data acquisition. Thus, and primarily for in situ tests using
both microscopic techniques and diffraction techniques, the real-time observation of
5.1 General Considerations 101

Table 5.2 Overview about various imaging and diffraction techniques used in combination with
in situ experiments
Imaging techniques
Medium Resolution Method Apparatus
Visible light Micrometre Optical microscopy Optical microscope
Electrons Nanometre Electron microscopy Scanning electron microscope
Transmission electron microscope
Infrared Micrometre Thermography Thermo-camera
Atomic force Nanometre Atomic force microscopy Atomic force microscope
Diffraction techniques
Radiation Wavelength Method Apparatus
Neutrons 0.1–1 nm Neutron diffraction Neutron reactor
X-rays 10–1 pm X-ray diffraction Diffractometer, synchrotron,
Computer tomograph,
Electrons <0.1 nm Electron diffraction Scanning electron microscope
Transmission electron microscope
Other techniques
Property Domain Method Apparatus
Acoustic 103–107 Hz Acoustic emission Acoustic emission sensor

ongoing processes is quite complicated and demands a compromise between res-


olution and sampling rate. Thus, thermographic in situ experiments using
thermo-cameras with high sampling rates (50–3000 Hz) are already very close to
real-time experiments (see Sect. 5.3.2). A pure real-time observation is possible
through the detection of acoustic emissions using acoustic emission sensors applied
directly to the material under plastic deformation or on components under operation
(see Sect. 5.2). The majority of in situ experiments is performed as quasi in situ
tests since both imaging and diffraction techniques require at least several seconds
for capturing images or the detection of signals. Here, the in situ tests are stopped at
certain, well-defined loading conditions (e.g. displacement intervals, number of
cycles) for data/image recording. The method of interrupted monitoring is used
when additional techniques have to be applied, which are not part of the in situ
experiment itself.
Finally, different in situ characterization techniques can be combined leading to
so-called fully-coupled, full-field measurements that can also be applied to
large-scale structural components. Thus, infrared measurements that evaluate
thermal fields can be combined with optical measurements that determine kinematic
fields (displacement, strain) during plastic deformation of metallic materials (see
Sect. 5.3.3).
102 5 In Situ Techniques for Characterization …

5.2 In Situ Imaging Techniques

In the following section, the imaging techniques (i) optical microscopy (OM) and
(ii) scanning electron microscopy (SEM) are described in detail under the viewpoint
of their application during in situ experiments under mechanical load. The basic
knowledge of each method as well as the state of the art of its application in field of
Materials Engineering is summarized. The report on the state of the art starts always
with the first in situ experiment. However, no complete literature review is provided
due to enormous amount of literature on in situ optical and SEM investigation. Only
important example with significant outcomes is reported.

5.2.1 Optical Microscopy

The history of optical microscopy dates back to early period of ancient Rome [2].
At this time, Gajus Plinius (23–79 AD) reported on magnifying properties of a
water-filled crystal ball, the Greek astronomer and mathematician Claudius
Ptolomäus (100–178 AD) was concerned with the refraction of light and finally, the
Arab Ibn al-Haitam (965–039) wrote the first book “Treasure of optic” explaining
the refraction and reflection of light. Later on, Snellius (1581–1626) published the
doctrine of refraction [2].
The first optical microscope was invented around 1600. However, progress in
development of optical microscopes was quite slow before beginning of the nine-
teenth century [2]. At that time, the microscope was an instrument that consisted of
curved glasses or mirrors to focus light rays. Optical microscopy experienced great
progress after enunciation of the wave theory of light (1650 Huygens, 1802—
Young and Fresnel). However, such microscopes had significant problems with
optical aberrations, blurred images and poor lens design. After the production of
apochromatic objectives by Ernst Abbe’s collaborative work with Carl Zeiss in
1886, problems of spherical and chromatic aberrations were solved. In 1893,
special illumination path (Köhler illumination) was introduced for optimization of
photomicrography. After World War II (1955), Nomarski introduced another
enhanced powerful contrast-generating optical microscopy theory—so-called
Nomarski interference contrast or differential interference contrast [2]. Further
imaging techniques have been developed such as reflected light microscopy and
enhanced contrast imaging techniques (dark field microscopy, phase contrast
microscopy, polarized light microscopy and fluorescence microscopy). Davidson
and Abramowitz [3] provided a comprehensive overview of fundamentals of image
formation, spherical and chromatic aberrations as well as different enhanced optical
microscopy techniques.
With the early optical microscopes (around 1600), the microscopic images were
drawn by microscopists by hand. With the invention of photography, micrographs
were stored on image plates or photographic films, and development of digital
5.2 In Situ Imaging Techniques 103

cameras spelled genesis of digital photomicrography. With digital cameras,


micrographs are stored directly on a computer chip without any photographic film,
opening up a wide field of image processing including enhancements of brightness
and contrast as well as making permanent storage relatively easy. There are dif-
ferent variants of camera systems available for optical microscopy—(i) tube cam-
eras, (ii) charge-coupled device (CCD) cameras and (iii) active pixel sensor
(APS) complementary metal-oxide semiconductor (CMOS) camera systems. The
selection of type of digital camera should be determined by investigation task and is
restricted by several important camera-specific parameters such as sensitivity of
camera, signal-to-noise ratio, spectral response, dynamic range capability, speed of
image acquisition and readout, geometric accuracy and, finally, resolution. Today,
pixel resolution spans a wide range, from 64  64 pixels (early digital cameras) up
to 15,360  8640 pixels2 (16 k digital camera) [3].

5.2.1.1 In Situ Experiments with Optical Microscopy

In situ observations based on optical microscopy can be exploited during


mechanical or other loading experiments. Here, enhanced contrast techniques such
as differential interference contrast or confocal microscopy are used. For higher
working distances, long-distance microscopy with a wide focus range can be
applied for in situ observations. High-speed cameras are powerful tools for the
observation of highly dynamic experiments.
Differential interference contrast or Nomarski contrast is obtained by splitting a
polarized light beam using a Nomarski prism into two orthogonal polarized
coherent parts that are displaced spatially at specimen plane. The two parts are
recombined before observation by a second Nomarski prism. The interference at
recombination is determined by optical path difference of the beams passed through
the specimen [3].
Confocal microscopy (CM) is an excellent tool for reconstruction of
three-dimensional structures from obtained images. The method is based on elimi-
nation of out-of-focus light by placing a spatial pinhole at confocal plane of the lens.
In this manner, optical resolution and contrast of micrographs are increased. The first
commercial CM became available in the 1960s. The confocal laser scanning
microscope (CLSM) is a special variant of CM, where specimen is illuminated by a
point-source laser, and each volume element is associated with a scattering or
fluorescence intensity. The high resolution of CLSM is comparable to other scanning
techniques such as SEM or AFM. However, working distance of CLSM is more
comparable to conventional optical microscopy, with typical observation spectra of
hundreds of micrometres up to several millimetres. Most applications of CLSM are
related to investigations on biological materials such as colloidal suspensions [4]. In
Materials Engineering, however, CLSM is used for in situ observations of crystal-
lization processes as well as surface changes of materials under mechanical loading
due to plasticity or phase transformation (e.g. [5]).
104 5 In Situ Techniques for Characterization …

Long-distance (or long focus) microscopes (LDM) facilitate the application at large
working distances while maintaining extremely high magnification and resolution.
The special design of these microscopes allows a remarkable depth of view over a
wide field of view (FOV). Thus, it is ideal for use in inspection of production
processes, as well as of mechanical loading experiments. Today, LDMs are
available with working distances between 500 and 1500 mm (Questar, [6]) or even
up to 3000 mm (Infinity, [7]).
High-speed cameras are needed especially for the observation of transient and
dynamic processes, such as impact loading or high-speed plastic deformation.
High-speed cameras are capable of recording video sequences with a frame rate
much in excess of 250 frames per second. Today, high-speed cameras are entirely
electronic and utilize same sensor technology as digital cameras (CCD or
APS-CMOS). Typically, more than 1000 frames per second are recorded over into
DRAM.

5.2.1.2 State of the Art in Materials Engineering

In situ optical microscopy experiments have long been used for in situ surface
investigations over a wide field of materials research on different types of materials.
It is primarily damage mechanisms, damage accumulation and/or surface rough-
ening that are subjects of these in situ investigations using either classical optical
microscopy with enhanced contrast conditions, larger working distances and/or
focus or enhanced depths of focus for three-dimensional observations.
Some of the first in situ optical microscopy experiments were performed by
Basinski et al. [8] in 1983 to study the evolution of persistent slip markings on the
surface of copper single crystals during cyclic loading as a function of the applied
plastic strain amplitude. A so-called Reichert microscope was mounted close to the
specimen and Nomarski contrast (or differential interference contrast) was applied.
In addition to in situ Nomarski contrast imaging, interrupted monitoring was per-
formed after either full tension cycles or full compression cycles regarding mea-
surement of step height using interference microscopy as well as step width using
scanning electron microscopy of revealed surface profile. Peralta and Laird [9]
performed fatigue fracture experiments on copper bicrystals. Crack propagation
starting from notches along interfacial twist boundaries of different orientation was
recorded in combination with in situ optical microscopy and interrupted monitoring
in the SEM. The in situ observations clearly revealed that interfacial crack growth
results in multiple slip in all cases. Depending on the geometry of slip with respect
to the orientation of the twist boundary, multiple slip promotes the interfacial crack
growth. On the other hand, the crack tip was also affected by the presence of
persistent slip bands (PSBs) and impeded crack propagation. Miscow et al. [10]
complemented fatigue experiments on full-scale drill pipes by small-scale experi-
ments in combination with an in situ optical microscope using differential image
contrast. The differential image contrast enhances differences in depth dimension by
5.2 In Situ Imaging Techniques 105

colour contrast. Therefore, it is a powerful technique to monitor the appearance of


slip bands and the evolution of extrusion and intrusion profiles where PSBs emerge
at the specimen surface.
Karaman et al. [11] used a long-distance microscope for in situ observation of
development of surface profiles during tensile or compressive straining of
HADFIELD steel single crystals of different orientations. These in situ optical
microscopy investigations (corroborated by TEM investigations) with a resolution
of a few micrometres revealed that mechanical twinning is dominant deformation
mechanism in ½111- and ½001-oriented single crystals under tensile and com-
pressive load, respectively. Furthermore, activation of twinning on multiple systems
was found to be responsible for higher strain-hardening coefficient than in typical
fcc alloys [11].
In a similar way, Polak and Zezulka [12] studied short crack growth in an
austenitic–ferritic stainless steel using a long-distance microscope. The Questar
long-distance microscope was connected with a high-resolution camera to record
images from specimen surface on the computer for measurements of projected
crack length after finishing fatigue tests. The investigations revealed that crack
propagation rate of individual cracks follows an exponential growth law, while a
number of simultaneous propagating cracks increased with increase in plastic strain
amplitude, the scatter band of crack propagation rate increased with a decrease in
plastic strain amplitude.
The fatigue behaviour of duplex stainless steel has been studied intensively by
Krupp group (e.g. [13–17]). Thus, short fatigue crack growth was observed using
long-distance microscopes in both LCF/HCF [13] and VHCF regime [14–17].
Strubbia et al. [13] performed cyclic loading tests at room temperature on lean
duplex stainless steels (DSS) in order to study preferred crack initiation sites under
LCF and HCF conditions. The surface observations by OM and LDM were cor-
roborated by EBSD measurements for determination of activated slip systems as
well as TEM investigations for analysis of dislocation arrangements occurring
during fatigue tests. It was shown that in lean DSS, crack nucleation sites were
different under LCF and HCF conditions. Thus, in LCF regime, cracks nucleated
along pronounced extrusion/intrusion profiles within the ferritic grains followed by
crack propagation within the austenitic grains by alternating slip and adjacent slip
systems. Phase boundaries were found to act as effective barriers against crack
growth. In the HCF regime, in contrast, cracks started to nucleate at grain
boundaries (GB). While asymmetric slip of screw dislocations was found to be
responsible for crack initiation on ferritic/ferritic grain boundaries, stress localiza-
tions caused crack nucleation on austenitic/austenitic and austenitic/ferritic GBs as
well. Dönges et al. [14, 17] and Krupp et al. [15, 16] continued with investigations
of fatigue behaviour of DSS performing ultrasonic fatigue tests up to 109 cycles
(VHCF regime). An LDM microscope was attached to an ultrasonic fatigue testing
system [18] capturing an image of shallow notch of fatigue specimen every 1000
load cycles [15]. The results corroborated by EBSD, TEM and finite element
modelling (FEM) revealed that low stress amplitudes (close to fatigue limit) led to
nucleation of localized slip bands in only a few austenitic grains without any crack
106 5 In Situ Techniques for Characterization …

initiation in these grains. The cyclic slip activity within these bands decreased
significantly during subsequent cycles (N < 105) indicating pronounced cyclic
hardening within austenitic grains. In this way, slip activity was transferred to
neighbouring regions yielding an increase in number and density of slip bands
(N = 105 − 108). At higher numbers of cycles (N = 108 − 109), the slip band
density remained constant [17]. Furthermore, it was shown that phase boundaries
act as pronounced barriers for slip transfer from the austenitic grains into ferritic
grains. Slip transfer to the harder ferritic phase only occurs under special geometric
relationships of the phase boundary and, if slip transfer occurs, it is often followed
by initiation of microcrack. The impeding effect of phase boundaries on slip transfer
and microstructurally short cracks in DSS seems to be the reason for existence of a
real fatigue limit of rFL  330 MPa up to 109 cycles [16].
The group of Brückner-Foit [19–25] applied long-distance microscopy in their
intensive studies of crack propagation phenomena in various types of materials,
such as steels [19–21], superalloys [24] or gamma titanium aluminides [25]. For the
investigation of crack growth on edge-notched specimens, in particular, a travelling
LDM system composed of two individual long-distance microscopes was mounted
on two three-axis stages to observe the vertical and horizontal crack growth on the
front and the side faces of the tested specimens.
However, the main drawback of these OM and LDM techniques is their
restriction to two-dimensional information. In several cases, however,
three-dimensional information is required. Here, CLSM opens possibility for
optical slicing of specimens and final three-dimensional reconstruction. Thus,
CLSM was applied for in situ investigation of solidification processes of steel melts
with crystal growth of d-ferrite in liquid (e.g. [26, 27]) or nucleation and growth of
austenite along d-ferrite grain boundaries (e.g. [28]). Kim et al. [29] studied mor-
phology of solidification front in a Pd–Cu–Ni–P alloy as a function of undercooling
applied. Recrystallization and oxidation processes in a Mn containing IF steel were
studied by Zhang et al. [30].
Furthermore, investigations are available on the agglomeration process of
non-metallic inclusions formed in steel melt (e.g. [31–34]. In addition, topo-
graphical changes on surface of shape memory alloys due to pseudoelastic defor-
mation (e.g. [35, 36]) as well as phase transformations (e.g. [37]) in steel are of
scientific interest.
In addition, in situ CLSM or OM investigations have been applied to shape
memory alloys (SMA) (e.g. [38, 39]) as well as to ultrafine-grained materials
(ufg) (e.g. [40, 41]). Thus, Niendorf et al. [38] conducted in situ uniaxial and biaxial
(notched specimen) cyclic loading tests on Ni–Ti SMA. The DIC results obtained
on high-resolution optical images taken with a violet laser (480 nm) CLSM
(OLYMPUS OLS 3100) showed that under both conditions, martensitic phase
transformation was traced by evolution of local strain fields. Moreover, it was
shown that under biaxial loading conditions, multiple martensite variants are acti-
vated within individual grains early in deformation process, whereas under uniaxial
loading conditions, single martensite variants were dominant.
5.2 In Situ Imaging Techniques 107

Sangid et al. [41] used in situ CLSM investigations during monotonic and cyclic
experiments for investigations of fatigue crack growth in electrolytically deposited
nanocrystalline Ni–Co alloys. The strain evolution within ufg aluminium alloy
laminates was investigated under tension using CLSM by Kurtovic et al. [40] in
order to study plastic instabilities and the PLC effect on the microscale.
In particular, in situ observation during dynamic tests with high strain rates—
such as impact testing or high-speed plastic deformation—requires rapid image
capturing techniques. Thus, Hopperstad et al. [42] performed investigations on
influence of both stress triaxiality and strain rate on mechanical behaviour of a
structural steel. Tensile tests on notched specimens of ferritic structural steel were
carried out using a split Hopkinson tension bar (SHTB). Various strain rates were
realized by different pre-loading conditions (20 and 40 kN). Some of these
experiments were complemented by in situ recorded optical micrographs using a
high-speed digital camera. The aim of these investigations was to determine the
reduction of the diameter at the notch as a function of time, which required sharp
edge contrast between specimen and background. Therefore, a shadow photography
technique was developed using diffuse light obtained by a light-source placed
behind a translucent screen on opposite side of high-speed camera (Ultranac FS501
image converter camera with frame rates from 2000 to 20,000,000 fps). For direct
correlation of images to actual applied force, the camera was triggered by a strain
gauge placed on input bar of the SHTB. As a result of these investigations, the true
strain at minimum cross section of notched specimens was estimated in relation to
time. However, the cross section became oval-shaped during tensile loading, which
meant that calculated true strain as well as strain rate at notch may have been
unreliable.
Kaiberg et al. [43] developed an image-recording procedure during tearing
process of a double-notched rod-bar with a strain rate of 104–105 s−1.
A combination of an image-converter-type high-speed camera (Ultranac FS 501)
with a CCD unit was used in combination with a long-distance microscope lens and
high-voltage electrical discharge from a capacitor. The high-speed camera facili-
tated recording of 15 frames with an exposure time of 0.4 ms and an interval
between frames of 2 ms. Thanks to the LDM lens, an area of approximately
1.5  1.5 mm2 was studied at a stand-off distance of about 0.1 m. The light from
discharge was focused onto a diffuser just in front of target area using a standard
Köhler illumination system. The results showed that the proposed experimental
setup could be useful for observation of deformation and fracture processes in a
small double-notched specimen of mild steel during tensile deformation at high
strain rates. However, larger aberrations could be introduced in images due to
image converter type, and could, therefore, render the object at slightly different
scales. Moreover, additional application of speckle patterns would improve the
information obtained on deformation fields from such high-speed experiments.
Split Hopkinson pressure bar (SHPB) experiments were performed by Yang
et al. [44] on aluminium foams to study localized deformation at medium strain
rates of 100–300 s−1, while experimental results were compared with numerical
simulations. Shear strain localizations in an AA2219 aluminium alloy were
108 5 In Situ Techniques for Characterization …

investigated by Owolabi et al. [45] using two synchronized ultrahigh-speed cameras


enabling 1 million frames per second (fps). Local strain fields developed in spec-
imen after high strain rate tests using SHPB (1.000–6.000 s−1) were calculated
using digital image correlation (Aramis) based on images captured at 124.000 fps.
The formation of adiabatic shear bands within microstructure was confirmed by
results of digital image correlation.
The application of high-speed camera systems also facilitates the measurement
of displacement fields—and even at moderately high strain rates (e.g. [46, 47])—in
order to study strain-rate-dependent effects such as Lüders behaviour or the PLC
effect.

5.2.2 Scanning Electron Microscopy

The invention of electron microscopy (EM)—i.e. the introduction of transmission


electron microscopy (TEM) in 1932 by Knoll and Ruska [48] and the first com-
mercial scanning electron microscope in 1965 by Cambridge Instruments [49, 50]
following the pioneering work of Knoll 1935 [51] and the theoretical developments
of Ardenne 1938 [52])—helped to overcome the limitations of light microscopy,
which was restricted by the smallest wavelength of visible light (*380 nm). Since
that time, both techniques—TEM and SEM—enjoyed astonishing development in
terms of imaging and analysing tools. Today, high-resolution transmission electron
microscopy (HRTEM) allows resolutions of about 1 Å, while scanning electron
microscopes deliver resolutions of up to few nanometres depending on the used
electron signal—secondary electrons (SE) or backscattered electrons (BSE). In
addition, both types of instruments are equipped with analytical tools such as
energy-dispersive X-ray spectrometry (EDS) and complementary electron diffrac-
tion techniques for crystallographic measurements (automated crystal orientation
mapping—ACOM, EBSD). Thus, the combination of both techniques provides a
great potential for the characterization of various kinds of materials—covering both
the internal structures of solids (from the atomic level up to the nanometre scale) as
well as microstructural properties (microscopic and mesoscopic scale).
A comprehensive review of the progress of studies in Materials Science using TEM
and SEM up to the year 2000 was provided by Newbury and Williams [53],
including both technical developments and pioneering experimental works and
findings.
Since the invention of electron microscopy, in situ experiments have been
performed using both TEM and SEM. The first in situ observation in SEM dates
back to 1976—approximately ten years after the production of the first commercial
SEM. Between 1949 (when Heidenreich introduced the technique of electron
transparent thin foils in TEM [54]) and 1976, numerous in situ investigations were
performed in TEM in order to study plasticity phenomena such as dislocation
motion, the interaction of defects and the behaviour of precipitates [53]. Since that
time, the number of publications on in situ investigations in TEM has increased
5.2 In Situ Imaging Techniques 109

tremendously. In recent decades (after the invention of another modern technique,


namely focused ion beam (FIB) milling), so-called small-scale testing experiments
such as pillar tests or microbending tests—where the specimen geometry lies in the
order of few micrometres—have been developed. However, despite the fact that
small-scale testing is, nowadays, a very hot topic in the field of materials investi-
gations, this type of in situ experiments will not be part of the present work.
Therefore, the focus in the following is on in situ SEM experiments.
Scanning electron microscopy (SEM) is an ideal imaging technique to com-
plement in situ experiments due to high lateral resolution (1 nm) obtained as a
function of energy of electrons used. However, since SEM is a quite common
technique, the setup of a modern field-emission (FE) SEM and its mode of oper-
ation is not repeated here. Further reading on the topic may be found in the
appropriate literature or books (e.g. [55, 56]).

5.2.2.1 In Situ Experiments in Scanning Electron Microscopes

In situ experiments in scanning electron microscopes can be performed under


different loading conditions—mechanical, thermal or electrical load as well as
combined loading,—but also under environmental conditions. For latter case, in
particular, a new type of SEM was developed from the 1970 and became common
around 2000—namely low vacuum (LV), variable pressure (VP) or environmental
(E) SEMs [57]. This type of SEM even facilitates investigations of insulating,
uncoated specimens at higher pressures, which is of importance for investigations
on biological materials, ceramics and composite materials.
Since in situ experiments have to be carried out in vacuum chamber of SEM,
special loading devices are required and their dimensions must be suitable to size of
vacuum chamber. Here, two categories of SEM (in terms of the size of vacuum
chamber) are available: (i) a classical SEM (c-SEM) with dimensions of the vacuum
chamber of around 300  400  500 mm3 and (ii) a large-chamber SEM
(LC-SEM) with a chamber volume of about 2 m3. Whereas for c-SEM miniaturized
loading devices have to be developed, the second category allows observations to
be made on large structural components (e.g. cylinder blocks) including interrupted
monitoring or implementation of complete large-scale testing devices (e.g.
servo-hydraulic push–pull testing machines) inside SEM chamber.
Miniaturized loading devices. Miniaturized loading devices have been commer-
cially available for both mechanical loading and for thermal loading during in situ
experiments for some time—initially from scanning electron microscope producers
themselves (e.g. Jeol [58] or Cambridge Instruments [59]) and later on by com-
panies specializing in in situ loading devices (e.g. Raith, Kammrath & Weiss,
GATAN, Hysitron, Nanomechanics, Klein/Diek). However, along with commer-
cially available systems, a large variety of custom-developed loading devices also
exist. The loading devices can be used as “modules” mounted directly on the
110 5 In Situ Techniques for Characterization …

specimen stage of the SEM or as “tables”, where the loading device is fixed at the
front door of the SEM and the complete unit has to be changed for in situ
experiments.
Mechanical loading devices have been developed for (i) tension/compression or
cyclic tests, (ii) bending tests (three- or four-point bending), (iii) shear tests,
(iv) wear or scratch tests and (v) nanoindentation experiments. The mechanical
loading devices are designed in a way to facilitate coverage of a wide range of
applied loads, from µN up to 10 kN. All mechanical loading devices are equipped
with units for measuring displacement—either as cross-head displacement or by an
extensometer clamped on the rear side of the specimen. Major disadvantages of
mechanical loading devices include their quite low motor velocity, which results in
low strain rates. Thus, depending on the chosen load or strain amplitude, in situ
cyclic loading experiments, in particular, can be quite time-consuming. For
instance, in situ cyclic experiments are often performed on specimens pre-cycled up
to a well-defined ratio of fatigue life ðNf Þ in order to generate a certain number of
microstructurally short cracks for further in situ observation of their propagation.
However, researchers have also introduced some new developments and devices for
in situ cyclic loading using higher deformation frequencies (e.g. [60, 61]. Krupp
et al. developed a piezo-driven miniaturized fatigue testing system for application in
the SEM). A piezo-ceramic actuator is used, resulting in testing frequencies of up to
35 Hz. Quite recently, Geathers et al. [62], Adams et al. [63] and Söker et al. [64]
developed in situ fatigue testing devices for the SEM that allows for 20 kHz testing
frequency.
Tanaka et al. [65] reported on the application of a hydraulic mechanical testing
device from Shimadzu Company (Kyoto, Japan) with a maximum load capacity of
5 kN allowing tensile tests as well as cyclic loading under load control at fre-
quencies of up to 2 Hz.
Thermal loading devices can also be setup as individual modules, which can be
used in combination with mechanical loading devices or as heating/cooling tables.
The temperature range covered by these devices ranges from—100 °C (cooled with
liquid nitrogen) up to 1200 °C. The desired temperature can be adjusted using a
proportional–integral–derivative (PID) control unit, where temperature course is
registered by incorporated thermocouples.
However, in all cases miniaturized specimens are tested with dimensions in
order of a several tens of millimetres in length and up to few millimetres in
thickness. Both mechanical and thermal loading devices can even be used in
combination with analytical detectors in SEM like EBSD, EDS or cathodolumi-
nescence (CL) devices.
Both mechanical and thermal loading devices can be connected to manual as
well as software-based control units, allowing to trigger applied loading process.
Thus, mechanical tests can be performed in an either total displacement controlled
(cross-head displacement or extensometer) or load controlled manner. The com-
bination of mechanical loading modules with heating devices requires additional
cooling of module itself. The heating device is clamped in a similar way to
5.2 In Situ Imaging Techniques 111

extensometer on rear of specimen. In order to guarantee heating of specimen centre


only, mechanical loading module has to be equipped with an additional cooling
system (water or liquid nitrogen).
Large-chamber SEM. In contrast to c-SEM, the LC-SEM allows implementation
of a servo-hydraulic testing machine, which enables investigation of larger speci-
mens or even investigations of certain areas on large construction elements, such as
cylinder blocks for automotive industry. For c-SEM, where small objects/specimens
are investigated, the electron source is usually fixed and object/specimen is moved
(in three dimensions x, y and z), rotated (around z) and tilted (around x or y
depending on SEM). In contrast, in LC-SEMs the object/specimen is fixed and
electron source can be moved around large components, or even around testing
machine. Thus, in LC-SEM the electron gun can be moved in x- and z-direction and
rotated around all three axes (x, y and z). LC-SEMs can be equipped in a similar
fashion to c-SEMs with various kinds of imaging (SE, BSE, InLense-SE) and
analytical detectors (EBSD, EDS).

5.2.2.2 State of the Art in Materials Engineering

The number of published papers dealing with in situ experiments in SEM has been
increased significantly during last five decades, since Roberts and Lehtinen [58]
performed in 1976 the first in situ straining experiment in an SEM (JSM 50A,
JEOL, Japan) on development of voids around inclusions (MnS) in steel under
plastic deformation. This was the first experiment where damage occurring on
inclusions and load–displacement curve were recorded simultaneously by video. In
1977, Grossbeck and Birnbaum [66] published first results on in situ observations
of influence of hydrogen on crack behaviour of coarse-grained pure niobium. More
than 10 years later, Jagannadham et al. [67] mentioned clearly the wish for in situ
SEM investigations for an improvement in knowledge and validation of models
concerning crack initiation associated by hydrogen embrittlement. Starting from
interrupted monitoring of tensile tests on refractory metals at various temperatures
using optical microscopy, they proposed at least four different mechanisms for
influence of hydrogen on fracture behaviour. As a proof for proposed mechanisms,
Jagannadham et al. suggested: [67]: “In situ electron microscopic observations of
nucleation of cracks as a result of slip on different planes in the presence of
hydrogen would be useful in confirming these models inferred from the present
observations.”—not aware obviously of results obtained by Grossbeck and
Birnbaum ten years ago.
Two years after Roberts and Lethinen in 1978, Vehoff and Neumann [59] per-
formed first in situ cyclic loading experiments in SEM in order to study crack
growth mechanisms in ductile materials. The investigations were conducted in an
SEM from Cambridge Instruments (Stereoscan), and the tensile stage developed by
same company was modified for performance of tensile/compressive loading tests.
The results of these in situ experiments confirmed alternating slip at the crack tip on
112 5 In Situ Techniques for Characterization …

two different slip systems as dominating mechanism of ductile crack propagation,


which was proposed in 1974 by Neumann [68] performing interrupted cyclic
loading tests and observation of slip phenomena at the crack tip by optical
microscopy. These investigations can be regarded as a pioneer work for in situ
observation of load-crack tip opening displacement (CTOD) curves in SEM.
Although great success of these first mechanical in situ experiments in SEM, it
took at least more than ten years that the high potential of this experimental
technique was discovered. With beginning of the 1990s, a significant increase in
publications using in situ SEM experiments was documented. On one side, this was
related to improved resolution of SEMs using field emission (FE) for generation of
primary electrons. On the other side, the establishment of new imaging and
diffraction techniques like electron channelling contrast imaging (ECCI) by Joy
[69] (after discover by Coates [70] and Booker [71]) and electron backscatter
diffraction (EBSD) by Dingley and Randle [72] (after discover by Alam et al. [73])
offered great potential for characterization of microstructures of materials at higher
resolution.
The majority of papers published on in situ SEM observations in the 1990s were
concerned with investigations on damage mechanisms in various kind of materials
such as steels (e.g. [74]), aluminium alloys (e.g. [75–80]), titanium aluminides (e.g.
[81–83]), cast iron (e.g. [84]), steels (e.g. [85–88]), shape memory alloys (e.g. [89])
up to brittle ceramic materials (e.g. [90]) or toughened composite materials
(e.g. [91–93]).
Rödel et al. [90] reported the first in situ SEM investigations on crack growth in
brittle materials like alumina ceramics or alumina toughened by SiC whiskers [92].
The development of special loading device for compact tension specimens enabled
direct observation of mechanisms in crack shielding zone on a microscopic scale as
well as quantitative measurements of crack opening displacement (COD).
The main goal of all these investigations was improvement on knowledge and
understanding of crack growth and fracture processes either under monotonic
tensile or cyclic loading. Majority of in situ SEM observation on surface changes
was corroborated by post-mortem TEM investigation to study changes in disloca-
tion structure or arrangement of other lattice defects like twins, stacking faults or
precipitates.
However, since automatization of EBSD data acquisition [94], this technique
became more and more popular for investigation of orientation-dependent proper-
ties. In a variety of published papers, in situ observations were corroborated by
EBSD measurements, which were performed on initial states of specimens before
in situ testing [95] or post-mortem after in situ testing, demonstrating well the
importance of improved knowledge of microstructural deformation and damage
processes gained by this technique. In situ EBSD measurements can be performed
as so-called interrupted monitoring (e.g. [96, 97]), where deformation was per-
formed in situ in SEM. However, for these EBSD measurements specimen was
remounted from loading stage for enabling necessary specimen tilt of 70°. On the
other hand, development of loading devices designed especially for in situ EBSD
measurements or adapters for loading devices accounting for the 70° tilt allowed
5.2 In Situ Imaging Techniques 113

performance of quasi in situ tests (e.g. [98]). In the focus of interest were orientation
changes due to plastic deformation, phase transformations or texture transition path
due to recrystallization using EBSD at higher temperatures (e.g. [99–101]).
Beginning with the twenty-first century, number of papers published about
in situ SEM investigations in field of Materials Engineering raised significantly.
The majority of in situ SEM investigations was related to cyclic experiments on
different types of materials (e.g. metals (e.g. [102, 103]), steels (e.g. [16, 104]),
shape memory alloys (e.g. [105–108]), titanium alloys (e.g. [109]), composites (e.g.
[110]) as well as to investigations within ESEM (e.g. [111]). Therefore, in the
following few examples will be picked out only demonstrating the performance of
mechanical in situ experiments carried out in the SEM in the field of cyclic loading,
as well as in situ experiments in LC-SEM.
Cyclic in situ experiments. The interest in performing cyclic in situ experiments
can be focused on different subjects like (i) slip activity of PSBs occurring in
materials during fatigue (e.g. [112–114]), (ii) influence of load history on the
propagation rate of microstructurally short cracks (MSCs) (e.g. [115–118]) or the
interaction of MSCs with microstructural features like grain boundaries (GB) or
phase boundaries (e.g. [119]), and (iii) martensitic phase transformation (MTP) in
metastable steels (e.g. [120]).
Richter et al. [116] and Blochwitz et al. [115] demonstrated well that direct
observation of propagation of microstructurally short cracks (MSCs) in steel AISI
316L by in situ loading experiments in SEM is a powerful technique gaining a better
knowledge of specific behaviour of MSCs in terms of crack acceleration or crack
arrest. It was shown that plastic range of crack tip opening displacement between
minimum and maximum load (DCTODpl) can be determined by in situ SEM inves-
tigations better and even more precise than by other methods (laser interferometer)
from load–displacement curves (LDC) obtained under symmetrical push–pull load-
ing conditions (R = –1). The CTOD was measured very close to crack tip (few
micrometres ahead of the crack tip being few nanometres wide only), where crack
propagation occurs by plastic blunting/re-sharpening processes. Since DCTODpl of
MSCs determined from COD-load hysteresis loops can be correlated directly to upper
limit of propagation rate of MSCs, this parameter is suitable for investigation of load
hysteresis effects on propagation rate of MSCs. Thus, Weidner et al. [118] demon-
strated that the parameter DCTODpl is very sensitive to overstraining cycles applied
symmetrically in tension/compression or asymmetrically either in tension or com-
pression with varying overstraining ratio and number of overstraining cycles. The
in situ experiments performed on polycrystalline nickel and steel (AISI 316L)
specimens revealed different influence of overstraining on DCTODpl and, therefore,
on the acceleration or deceleration of crack propagation rate.
Similar in situ cyclic loading experiments are presented by Zhang and Liu [121]
investigating fatigue crack growth mechanisms during one individual cycle on an
aluminium alloy (AA7075-T6). However, in contrast to Weidner et al. [118], where
observations were done on cracks grown naturally initiated under symmetric plastic
strain amplitudes, Zhang and Liu studied propagation mechanisms of a pre-crack
114 5 In Situ Techniques for Characterization …

introduced in a single-notched specimen under plane stress conditions. CTOD was


measured during one individual cycle with a stress ration of R = 0.1. Different
crack propagation mechanisms were observed during single cyclic loading: (i) fast,
brittle-like crack growth, (ii) slow crack growth due to crack tip blunting/
re-sharpening, and (iii) accelerated crack growth forming a network of microcracks
linked to final major crack. In addition, crack closure was observed.
Marx and Vehoff [119] studied crack propagation rate of microcracks in single
crystalline nickel-base superalloy (CMSX-4) using CTOD measurements during
in situ cyclic loading experiments in SEM. The in situ tests confirmed physical
model of alternating slip at crack tip. Moreover, it was shown that local crack
opening displacement of microstructurally short cracks cannot be predicted by
elastic–plastic fracture mechanics.
Further example for in situ cyclic loading experiments in SEM is investigation of
slip activity within PSBs occurring during fatigue in polycrystalline specimens
performed by Weidner et al. [113, 114]. Specimens were pre-fatigued in a
servo-hydraulic push–pull machine up to certain part of fatigue life (0.15 Nf , 0.3 Nf
and 0.6 Nf ) so that large number of persistent slip markings (PSMs) occurred at
specimen surface, which were related to typical ladder-like dislocation arrangement
of PSBs in microstructure. The specimen surface was re-polished in order to remove
PSMs. Then, an individual in situ loading cycle was applied to specimen and the
occurrence of fine slip steps on specimen surface was detected in dependence on
registered load–displacement hysteresis loop. From these in situ investigations, three
main findings turned out: (i) a threshold value of about 60% of applied plastic strain
has to be overcome for formation of slip steps; (ii) during an individual loading
cycle, not the whole PSB volume accumulated during cyclic pre-deformation is
active, only a small part of it; (iii) the slip activity depends significantly on number of
cycles of pre-deformation, which indicates that microstructure within PSBs under-
goes an ageing and hardening process due to interaction of dislocations on several
slip systems. In addition, these in situ experiments were complemented by (i) EBSD
measurements determining individual crystallographic orientation and (ii) atomic
force microscopy (AFM) measurements in order to evaluate the height and the width
of individual slip steps as well as formed extrusions. The combination of in situ
observation of slip steps with analysis of grain orientations and slip step profiles is a
classic example for so-called interrupted monitoring as a variant of in situ experi-
ments. By combination of these three methods, both local shear strain amplitude
occurring within PSBs and reversibility/irreversibility of cyclic slip within PSBs
were determined. Furthermore, a quantitative value for irreversibility factor was
determined experimentally for the first time [122].
Interrupted monitoring using in situ cyclic loading up to certain number of
cycles and EBSD measurements were used by Weidner et al. [120] in order to study
MPT in metastable steels exhibiting transformation-induced plasticity (TRIP) effect
in dependence on the number of cycles. The formation of DB is observed very early
in fatigue life and with increasing number of cycles the formation of a-martensite
occurred inside these bands.
5.2 In Situ Imaging Techniques 115

In situ observations in LC-SEM. LC-SEMs used mainly for investigations of


large-scale components [123, 124] were also applied for performing in situ tests
with large-scale loading units [125–127]. Thus, Fried et al. [125] performed in situ
fatigue tests on nickel-base superalloys in order to study the formation of stage I
cracks in dependence on the microstructure. The investigations demonstrated that
initiation of stage I cracks is linked strongly to microplasticity and formation of slip
traces on specimen surface.
Glage [126] performed in situ fatigue tests in LC-SEM on metal matrix com-
posites based on steel matrix reinforced by MgO-partially stabilized ZrO2 (Mg–
PSZ) particles. The material was processed by a powder-metallurgical route fin-
ished by hot-pressing (HP). During cyclic tests, fatigue damage was observed on
specimen surface in a shallow notch acting as stress concentrator for formation of
cracks. It was shown that at a total strain amplitude of ea;t = 4  10−2 damage
occurred directly during first cycle on interface between steel matrix and Mg-PSZ
particle. Further damage occurred by crack propagation along interface steel/
ceramic particle or by fracture of larger Mg–PSZ particles. The formation of
deformation bands in grains of the steel matrix in front of crack tip accompanied by
cyclic hardening led to retardation of crack propagation through steel matrix.
Luo et al. [127] performed wear test in a LC-SEM offering for the first time the
possibility to observe wear process in situ and to study time-dependent wear
mechanisms. For these tests, Luo et al. [127] designed a special vacuum-suitable
pin-on-disc testing device, where Al2O3 ceramic balls were used as wear coun-
terparts testing sprayed coatings of NiCrBSi and WC-12Co. Adhesive and abrasive
wear, surface fatigue as well as tribochemical reactions were observed directly.

5.3 In Situ Acoustic Emission Measurements

The acoustic emission (AE) measurement method is a non-destructive technique


(NDT), which can be applied in situ during different loading conditions. In contrast
to other NDT methods, AE measurements are of passive nature, since signals
identified and analysed are generated by processes or defects evolving under certain
load conditions [128]. In case of active NDT methods such as ultrasonic methods,
artificially generated signals are used to detect shape and location of defects in
investigated material [129]. In comparison to other NDT or in situ characterization
techniques, the AE has some potential advantages such as (i) high sensitivity,
(ii) real-time capability, (iii) total specimen volume sensitivity, (iv) location of
damage regions and (v) sensitivity to any process or mechanism that generates
stress waves [130]. However, due to the random nature of signal sources, individual
particular AE measurement tests are not fully reproducible. Therefore, AE mea-
surements have to be corroborated by other analysing techniques [129].
116 5 In Situ Techniques for Characterization …

5.3.1 General Aspects of Acoustic Emission

According to American Standards for Testing and Materials (ASTM), acoustic


emission is defined as “…a phenomenon whereby transient elastic waves are
generated by the rapid release of energy from localized sources within a material, or
the transient elastic waves so generated…” (ASTM E 610:1977, superseded by
ASTM E1316:2017). Thus, acoustic emission is based on a sudden release of
energy within a solid under certain stimulus (e.g. mechanical load, temperature and
chemical attack) resulting elastic waves propagating through material [131]. The
amount of energy released depends significantly on localization of the source and
velocity of the energy release. Thus, localized, rapid energy releases result in elastic
waves in ultrasonic frequency domain. The waves with sufficient high amplitudes
are detected by transducers attached to specimen surface. Thus, the whole process
—generation as well as detection of elastic waves in ultrasonic frequency domain—
is known as acoustic emission (AE), and each source is called an AE event [131].
Figure 5.1a illustrates generation of elastic waves in a metallic material under
mechanical load leading to formation of a brittle crack. The spontaneous formation
of a crack is connected with a sudden increase in volume due to opening of crack
edges. Thus, this volume increase causes elastic waves that are propagating as
compressive waves through material. At specimen surface, the compressive elastic
wave front causes a normal surface displacement, which is detectable by a suitable
transducer as shown in Fig. 5.1b.
Surface displacements are transformed into electrical signals, which are
pre-processed, analysed and stored for further post-processing. However, wave-
forms measured at surface are influenced not only by nature of the source, but also by
structure of the solid and by wave propagation path. The ultrasonic waves in
materials have different modes: (i) longitudinal (compression), (ii) transversal
(shear), (iii) surface (RAYLEIGH) and (iv) plate waves. These waves propagate with
different velocities that depend, in addition, on materials parameters such as mass
density, elastic moduli or Poisson’s ratio. Thus, in a metallic specimen, the wave
propagation is quite complex and is influenced by different factors: (i) propagation

Fig. 5.1 Acoustic emission—generation and detection of acoustic emission signals. a Generation
of elastic waves by spontaneous energy release caused by the formation of a brittle crack.
b Detection of surface displacement by suitable transducer. Modified according to [131].
Permission of IOP Publishing
5.3 In Situ Acoustic Emission Measurements 117

within material itself, (ii) reflection at specimen boundaries and (iii) overlapping with
elastic waves from multiple sources. Overall, wavefronts detected by transducer
experienced multiple reflections, interferences, mode conversions and damping.
In addition, further influences are exerted by AE recording system through (i) transfer
function of the coupling media, (ii) response function of transducer, (iii) pre-amplifier
and (iv) band-pass filters. Figure 5.1b shows schematics of generation and detection
of AE signals including necessary experimental components.
The appearance of AE signals caused by localized sources activated within a
material under a certain external stimulus bears fundamental similarities with
seismology. Seismic waves are generated due to spontaneous release of elastic
energy caused by sudden stress relaxation at relative movements of tectonic plates
in case of earthquakes, but also by volcanic eruptions, magma movement, large
landslides or even large human-made explosions. In general, the nature of AE
signals and seismic signals from earthquakes is similar. However, as both phe-
nomena are substantially different in scale, they are correspondingly different in
frequency and, consequently, in time-domain waveforms. As shown in Fig. 5.2,
earthquakes occur in the low-frequency domain (  10 Hz), whereas acoustic
emission is attributed to high frequency domain of 103–107 Hz. Further difference
is related to duration of individual signals. Thus, whereas seismic events have
duration of several seconds up to minutes, acoustic emission in materials testing
occurs in range of microseconds.
In general, two different types of AE signals are distinguished by their wave-
forms as shown in Fig. 5.3: (i) continuous signals with longer durations (1–100 ms)
(Fig. 5.3a) and (ii) transient signals with short durations (0.1–10 µs)—the so-called
“bursts” (Fig. 5.3b). The continuously recorded AE data streams are often an
overlap of both individual signal types and occur, in particular, if different signal
sources are activated (Fig. 5.3c) [129].
The AE signals can be characterized by various parameters, a set of which
depends on either a method of signal detection or the strategy of signal processing
adopted. First of all, so-called hits are recorded if the signal exceeds a certain
threshold in either positive or negative direction. The total number of hits N is,
therefore, the simplest parameter describing the dynamic processes within material

Fig. 5.2 Similarities of seismology and acoustic emission. a Frequency domain of earthquakes
and acoustic emission. b Time domain of seismic signals. c Time domain of AE signals. Modified
according to [132]. Permission of Taylor and Francis
118 5 In Situ Techniques for Characterization …

Fig. 5.3 Two different types of AE signals. a Continuous signal. b Transient (burst) signal. c AE
data stream consisting of continuous and burst-type signals

under certain stimulus. Commonly, the activity m of AE of burst-type signals is


described by the ratio of number of AE hits DN detected within a unit time Dt:

DN
m¼ ð5:1Þ
Dt

More specific parameters describing AE are grouped as (i) parameters directly


determined from detected AE waveform and (ii) those calculated from measured
waveforms.
The parameters such as a peak amplitude, duration, and number of counts or rise
time shown in Fig. 5.4a belong to first group. The AE amplitude Up (peak voltage)
is the maximum AE signal during AE event of a burst-type AE or during recorded
realization of a continuous signal. The AE amplitude is measured either in absolute
units (V) referred to input of pre-amplifier or in relative units expressed as dB
according to following relationship [129]:
 
Up
dBAE ¼ 20log  Ku;PA ð5:2Þ
1lV

Here, Ku;PA is the gain of the used pre-amplifier. Thus, an AE signal detected
with an amplitude Up of 0.1 V using pre-amplifier with a gain of 43 dB corre-
sponds to an AE signal with 57 dB.

Fig. 5.4 Specific parameters describing acoustic emission signals in the time. a Burst-type
signals. b Continuous-type signals
5.3 In Situ Acoustic Emission Measurements 119

The number of counts N refers to the number of AE crossing the threshold within
a certain time interval or AE event. The duration D is defined as the time of AE
from first crossing of threshold up to the end of last threshold crossing. The rise
time R is the time interval between first crossing of the threshold and the peak
amplitude. The continuous signals as well as noise level can be characterized by a
root mean square value [129].
The second group contains AE parameters such as energy or average frequency.
These parameters are often based on odd definitions. For example, the energy of AE
was defined by the Physical Acoustic Corp. as “…the integral over the rectified
voltage signal over the duration of the AE hit…” [133], or cited in [129] or [134]).
The average frequency is defined as the ratio of the AE counts versus the duration.
None of these definitions can be considered as a rigorous one and should be
avoided.
In contrast to burst-type signals, not that many parameters are available to
describe the continuous AE signals. The integral characteristics have gained
greatest popularity for this purpose. For example, the rapidly fluctuating signals can
be characterized either by so-called AE envelope:

Z
tþT
1
YðtÞ ¼ jUðt0 Þdt0 j ð5:3Þ
T
t

or, most commonly, by their root mean square voltage URMS ðtÞ:
vffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
u Z
u tþT
u1
URMS ðtÞ ¼ t U 2 ðt0 Þdt0 ð5:4Þ
T
t

with T—the integration time. The root mean square of the mean square voltage
U 2 ðtÞ, which is measure of the power of the electric signal referred to 1 X impe-
2
dance, can be corrected to the average background noise Unoise ðtÞ level as:

Z
tþT
1
U 2 ðtÞ ¼ U 2 ðt0 Þdt0  Unoise
2 ðtÞdt ð5:5Þ
T
t

5.3.2 Acoustic Emission—A Multiscale Random


Time-Series Process

Acoustic emission can be regarded as a natural phenomenon similar to earthquakes


or volcanic eruptions. Those natural processes arise randomly in time and, as such,
120 5 In Situ Techniques for Characterization …

they can be described as random (stochastic) processes fluctuating in time. Thus, it


is very unlikely that two AE experiments repeated with the same object, identical
apparatus settings and identical experimental conditions will result in exactly
identical data sets [129].
Therefore, the AE has to be regarded as a random time-series process of AE
observations Xt registered in evenly distributed time intervals t (t = 1, 2, 3, …
N) with N as the length of the time series.
The basic properties of random data XðtÞ can be described in many ways [135].
Four main types of statistical functions—(i) mean square values (MSVs),
(ii) probability density functions (PDFs), (iii) auto-correlation functions (ACFs) and
(iv) power spectral density functions (PSDFs)—constitute the grounds for quanti-
tative description and comparison of a broad variety of random data sets. While the
MSVs are simple measures of the intensity of the random process, the PDF offer the
most detailed information about the random variable. Note that AE is a multivariate
random process where all descriptive variables are random in nature. This applies to
amplitudes, arrival times, duration, rise time, etc. The ACF and the PSDF are
interrelated by a pair of Fourier transforms according to the Wiener–Khinchin
theorem [135], although they are computed quite differently.
Mean values and variance. The general intensity of random data XðtÞ is expressed
by the mean square values W2 ðtÞ and the RMS value of the intensity by the root
square of W2 ðtÞ [135]:
vffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
ZT u ZT
u
1 u 1
W2 ðtÞ ¼ lim X ðtÞdt and XRMS ðtÞ ¼ t lim
2
X 2 ðtÞdt ð5:6Þ
T!1 T T!1 T
0 0

Moreover, the random data XðtÞ are considered as a combination of quasi-static


(time-independent) component lx and a dynamic fluctuating component. While the
quasi-static component lx is described by its mean value lx , the dynamic fluctu-
ating components are defined by the variance r2x according to (5.7). The square root
of r2x is the standard deviation rx [135].

ZT ZT
1 1
lx ðtÞ ¼ lim XðtÞdt and r2x ðtÞ ¼ lim ½XðtÞ  ux 2 dt ð5:7Þ
T!1 T T!1 T
0 0

Probability density function. The best way to describe the statistical properties of a
random variable X(t) is the application of the probability distribution function or the
probability density function (PDF). The probability distribution function is simply
speaking a mathematical function providing the probabilities of the occurrence of
different possible outcomes in an experiment. The probability distribution functions
are separated into two categories: (i) discrete probability distribution functions and
5.3 In Situ Acoustic Emission Measurements 121

(ii) continuous probability distribution functions. In addition, the probability dis-


tribution function PðxÞ is used to specify the probability of a random variable XðtÞ
falling within a particular range of values (−∞ to +∞). The probability distribution
function is provided by the area under the PDF p(x) but above the horizontal axis
and between the lowest 1 with Pð1Þ ¼ 0 and greatest þ 1 with Pð þ 1Þ ¼
1 values of the range. Thus, the PDF is always positive and its integral is equal to
one [135]:

Z1
pðxÞdx ¼ 1 with pðxÞ  0 ð5:8Þ
1

Commonly, probability density functions are characterized by their moments,


since the first moments play an important role in statistics and physics. Thus, the
n  t central moment of a mean value lx is provided by Bendat and Piersol [135]:

Z1
lðnÞ
xc ¼ ðx  lx Þn pðxÞdx ð5:9Þ
1

ð1Þ
The first moment lx is equal to the mean value, whereas the second moment
ð2Þ
lx accounts for the variance r2x as described above. The third and the fourth
 
ðnÞ ðnÞ
standardized moments lxc =rxc are known as the “skewness” and the “kurtosis”
of the PDF, respectively. They are provided by the following expressions [135]:

l3x l4
sx ¼ 3
and qx ¼ x4  3 ð5:10Þ
rx rx

While the “skewness” describes the asymmetry of the PDF, the “kurtosis” is a
measure of the peakedness of the PDF [135].
The most important distribution describing continuous random variables is the
normal distribution function followed by the Poisson distribution function
describing discrete random variables and the chi-square distribution function used
widely for statistical significance tests [135]. Table 5.3 provides a summary on the
three distributions with respect to their PDSs, their probability distribution functions
and their typical parameters such as the mean value, the variance, the skewness and
the kurtosis. The simplest case of normal distribution is the so-called standard
normal distribution with the first moment (mean value) l equal to zero and the
second moment (variance) r2 equal to unity. Furthermore, for the normal proba-
bility density function, both the third moment (skewness) and the fourth moment
(kurtosis) are zero. That means with respect to the mean value lx , there is no
asymmetry or peakedness of the PDF observable. Regarding the AE signals,
Fig. 5.5 provides an example of normal distributed AE amplitudes and the
122 5 In Situ Techniques for Characterization …

Fig. 5.5 Schematic illustration of the meaning of the “kurtosis” for the AE amplitude distribution.
a q > 0 for transient AE signal. b q * 0 for continuous AE signal. Reproduced from [136].
Permission of Elsevier

illustration of the meaning of “kurtosis”. For both signal types—burst signal (a) and
continuous signal (b)—the AE amplitude distributions are shown. In case of the
continuous signals, the “kurtosis” is close to zero. Therefore, the amplitude dis-
tribution is described nearly perfectly by a normal distribution. In case of the burst
signal, it becomes obvious that the amplitude distribution deviates from the normal
distribution and is characterized by a higher peakedness (q > 0).
The Poisson probability distribution shown in Table 5.3 describes the probability
that exactly k occurrences appear during a time interval of a given length. k is a
non-negative, integer value and k a positive real constant. For the availability of the
Poisson distribution, several requirements have to be fulfilled: (i) the length of the
observation period is fixed in advance, (ii) the analysed process is stationary or
quasi-stationary, and (iii) the number of events occurring in discrete intervals is
statistically independent. The Poisson distribution is one-parametric, since both
mean value and variance equal to each other and equal to k. Figure 5.6 shows an
example for the application of Poisson distribution to AE data. Here, the time
interval s between individual AE events is looked for and s0 is regarded as the
relaxation time, which is inversely proportional to the rate of process. The relaxation
time in AE is defined as the time, required for the amplitude of a damped oscillation
to drop from an initial value to 1=e of that value, where e is the base of natural
logarithms. As long as the AE events belong to statistically independent sources, the
probability density distribution can be described by the Poisson distribution of the
inter-event time intervals s that is provided by an exponential function as [137]:
5.3 In Situ Acoustic Emission Measurements 123

Table 5.3 Summary on important probability distributions used for describing acoustic emission
signals
NORMAL distribution POISSON distribution CHI-SQUARE distribution
Probability density function Probability density function Probability density function

(x − μ )2 λk e− λ
x (k 2) −1e − k
− 1 2
1 p ( x) = p( x ) =
2 k 2 Γ(k 2)
p( x ) = e 2 σ2
2 k!
2πσ

Probability distribution function Probability distribution function Probability distribution function

Mean: µ Mean: λ Mean: k


2
Variance: σ Variance: λ Variance: 2k
Skewness: 0 Skewness: λ−1 2 Skewness: 8 k
Kurtosis: 0
Kurtosis: λ−1 Kurtosis: 12 k

(i) Normal distribution, (ii) Poisson’s distribution and (iii) chi-square distribution. The table
contains graphical and mathematical representation for probability density function and probability
(cumulative) distribution function as well as specific statistical parameters. According to [135],
graphs from [138]

Fig. 5.6 Schematic illustration of an acoustic emission data set containing burst signals (a).
b Definition of the time interval Ds between the burst signals shown in (a). c Description of the AE
data by a Poisson’s probability density distribution. d Significant deviation of the AE data from
Poisson’s distribution (c). Modified according to [136]. Permission of Elsevier
124 5 In Situ Techniques for Characterization …

1 ðs=s0 Þ
pðsÞ ¼ e ð5:11Þ
s0

Figure 5.6a illustrates the definition of the inter-event time interval s between
individual transient AE events. While the experimental data set in Fig. 5.6c can be
described well by the exponential Poisson distribution, the data set shown in
Fig. 5.6d deviates significantly from it. Thus, in the latter case the AE sources
cannot be regarded as independent from each other. The statistical criteria of
hypothesis testing or “goodness of fit” can be applied to verify if the experimentally
observed frequency histogram can be described by the proposed (expected) theo-
retical distribution function. For example, the popular Pearson’s chi-square ðv2 Þ
criterion can be used for this purpose [139].
The chi-square ðv2 Þ distribution is a function that is used for describing the sum
of the squares of k independent standard normal distributed (l = 0, r2 = 1) random
variables Zi ðtÞ [135]:

X
k
v2 ¼ Zi2 ð5:12Þ
i¼1

As seen from Table 5.3, the v2 distribution is one-parametric with k as a positive


integer specified as the degree of freedom, i.e. the number of independent standard
normal distributed random variables.
The v2 distribution is used in the common X2 test or “goodness-of-fit” test for the
description of the probability density function of a recorded data set by some
theoretical density function such as described above. This is done by (5.13) [135]:

X
K
ðfi  Fi Þ2
X2 ¼ ð5:13Þ
i¼1
Fi

Here, K is the number of class intervals in which a random data set of


N observations with N ! ∞ for each class interval is classified. Then, fi denotes
the observed frequency and Fi the expected frequency in the i-th class interval
giving the discrepancy ðfi  Fi Þ between observed and expected data. The X2
function of the goodness-of-fit test follows the above-mentioned v2 function with
the degree of freedom k ¼ Kr1, where r is the number of independent variables.
This results in k ¼ K3 for the case of two-parametric normal distribution (r = 2)
and in k ¼ K2 for the one-parametric Poisson distribution (r = 1). Thus, the
region of acceptance of a hypothesis regarding the equivalence of a probability
density function of a sampled data to some theoretical density function is provided
by the relation shown in (5.14):
5.3 In Situ Acoustic Emission Measurements 125


X 2  v2 k;a ð5:14Þ

with a as the significance level. For the significance level a = 0.05, the minimum
number of class elements K and observation numbers N are proposed by Williams
[140]. Thus, for the example shown in Fig. 5.6c, the expected v2 k;a value for
k = 14 (K = 16; r = 1; k ¼ K2) and the level of significance a = 0.05 is
v2 14;0:05 ¼ 23:68, whereas the calculated value for the observed data set is
v2 ¼ 29:33. Consequently, the recorded AE data set cannot be described by the
Poisson distribution, which means that the AE signals are not related to independent
AE sources.
Finally, the so-called central limit theorem has to be taken into account. It states
that the probability distribution function of a sum of independent variables
approaches that of a normal distribution if the number of variables being summed is
sufficiently large irrespective of which distribution the original individual random
variables follow.
Correlation and auto-correlation function. The AE process can be regarded as a
stationary or quasi-stationary process under the assumption that all possible prob-
ability distribution functions are independent of time translation at least for the
timescale under observation. Thus, considering the AE as a stationary random
process with at least two random variables XðtÞ and YðtÞ, the mean values become
independent of time t [137]:

Z1 Z1
lx ¼ EðXðtÞÞ ¼ X pðXÞdX and ly ¼ E ðYðtÞÞ ¼ Y pðYÞdY ð5:15Þ
1 1

Similarly, the covariance functions are independent of time. Thus, for arbitrary
fixed time t and time interval s, the following covariance functions are obtained
[137]:

Rxx ðsÞ ¼ E ½XðtÞX ðt þ sÞ; Ryy ðsÞ ¼ E½YðtÞY ðt þ sÞ; Rxy ðsÞ ¼ E ½XðtÞY ðt þ sÞ
ð5:16Þ

For the non-stationary process, the mean values as well as the covariance
functions are different at different times, and therefore, these have to be calculated
separately for each time interval of interest. The quantities Rxx ðsÞ and Ryy ðsÞ are
auto-correlation functions of XðtÞ and YðtÞ, respectively, and Rxy ðsÞ is the
cross-correlation function between XðtÞ and YðtÞ. Correlation functions are used as
a measure of correlation between the events in a time series [137]. Thus, the
auto-correlation describes the similarity of individual observations of an individual
random variable as a function of time interval between them, whereas the
126 5 In Situ Techniques for Characterization …

cross-correlation function describes the interaction between time series of two


different random variables. A necessary condition for Rxx ðsÞ being an auto-
correlation function is that Rxx ðsÞ equals Rxx ðsÞ and Rxx ðsÞ is a non-negative
function. Furthermore, Rxx ðsÞ is a continuous function if XðtÞ is in its origin. The
normalized auto-correlation function rx ðsÞ is defined by [137]:

Rxx ðsÞ
rx ðsÞ ¼ ð5:17Þ
Rxx ð0Þ

In the context of the description of random AE data by the Poisson distribution


according to (5.11), the normalized auto-correlation function in (5.17) can be
rewritten as [137]:

RðsÞ
rðsÞ ¼ ¼ eðs=s0 Þ ð5:18Þ
Rð0Þ

Figure 5.7 shows different examples of auto-correlation functions for different


types of random variables. Figure 5.7c represents the specific normalized
auto-correlation function according to (5.18) for different relaxation times s0 . Thus,
for the relaxation time s01 , a high auto-correlation is observed only for very low
time intervals between individual AE events and decreases significantly to zero for
higher time intervals. With increasing relaxation time s0 , the auto-correlation
between time intervals of AE events is increasing, compare the course of r ðs03 Þ that
decreases more or less linearly and reaches values well above zero at high time
intervals indicating a strong auto-correlation [135].
Power spectral density function. The PSDF plays a central role for the analysis of
random processes. Overall, the power spectral density (or power spectrum) applies
to signals existing over all time, or over a large time period such as stationary
processes. The power spectral density describes how the power of a signal or
time-series is distributed over frequency. Here, the term “power” is not used in the
sense of a physical power, but, for convenience with abstract signals, it is simply
identified with the squared value of the signal. In general, the analysis of the

Fig. 5.7 Examples for special auto-correlation functions. a White noise. b Sine wave.
c Exponential according to Poisson’s process described by (5.18). According to [135]
5.3 In Situ Acoustic Emission Measurements 127

frequency content of the random variable XðtÞ can be done via the computation of
the ordinary Fourier transform Xb ðtÞ. However, since for AE a certain periodicity of
a random variable XðtÞ cannot be excluded, the truncated Fourier transform X b T ðtÞ
has to be applied. Thus, in case of individual AE realization, the truncated random
variable XT ðtÞ according to [135]:

XðtÞ; T=2  0  T=2
XT ðtÞ ¼ ð5:19Þ
0 otherwise

is defined. The random variable XT ðtÞ is then expressed as the truncated Fourier
integral:
Z1
XT ðtÞ ¼ b T ðf Þei2pft dt
X ð5:20Þ
1

with
ZT=2
b T ðf Þ ¼
X XT ðtÞei2pft dt ð5:21Þ
T=2

The PSDF is then obtained by the averaging over all realizations of the entire
process leading to
 2
 ZT=2 
2 
i2pft 
Gðf Þ ¼ lim  XðtÞe dt ð5:22Þ
T!1 T  
T=2 

The PSDF used here for AE process is by convention a one-side spectrum since
it is defined only for non-negative frequencies. It is assumed that the frequency
spectrum is symmetrical around f = 0 and the spectrum for f < 0 will deliver no
new information. The double-sided spectrum is given by ðf Þ ¼ 2Gðf Þ.
The integral of the PSDF, i.e. the area under the plot of Gðf Þ versus the fre-
quency, is the energy E (or power) of the AE signals. Furthermore, three other
quantities related to AE signals in terms of PSDF are (i) the narrow-band energy
E ðf1 ; f2 Þ, (ii) the integrated spectrum Gi ðf Þ and (iii) the median frequency fm as
summarized in Table 5.4.

Table 5.4 Typical parameters obtained from the power spectral density function
Energy (power) Narrow-band energy Integrated spectral Median frequency of the
E (power) E ðf1 ; f2 Þ energy (power) Gi ðf Þ spectral density fm
R1 Rf Rf R fm R1
E ¼ 0 Gðf Þdf E ðf1 f2 Þ ¼ f12 Gðf Þdf Gi ðf Þ ¼ f1 Gðf Þdf 0 Gðf Þdf ¼ fm Gðf Þdf
128 5 In Situ Techniques for Characterization …

Fig. 5.8 Different shapes of power spectral density functions. a The AE energy E is given by the
area (green) below the curve of the PSDF. b Median frequency fm of a PSDF. c PSDFs with
different AE energy E, but the same median frequency. d PSDFs with different AE energy and
median frequencies. Modified according to [137]. Permission of Elsevier

An example of a real power spectral density function is shown in Fig. 5.8


representing the energy (Fig. 5.8a) and mean frequency (Fig. 5.8b) together with a
sketch of theoretical PSDFs both with varying shape but identical median frequency
(Fig. 5.8c) as well as varying median frequency (Fig. 5.8d).
The normalized PSDF is given by the PSDF related to the area under the curve
of the spectrum, which equals to the variance according to:

Gðf Þ
gðf Þ ¼ ð5:23Þ
r2x

Furthermore, the total area under a plot gðf Þ versus the frequency f equals to
unity:

Zþ 1
gðf Þdf ¼ 1 ð5:24Þ
0

Therefore, the normalized PSDF gðf Þ can be treated as distribution function with
f as a random variable. Hence, statistical treatment can be applied to the normalized
PSDF, and comparable to (5.7), (5.9), and (5.10), the average frequency, the
variance, the skewness and the kurtosis can be determined, which are summarized
in Table 5.5.
5.3 In Situ Acoustic Emission Measurements 129

Table 5.5 Statistical parameters describing the normalized power spectral density function
Average frequency Variance Skewness Kurtosis
R fmax Rf l3f l4
fa ¼ lf ¼ limfmax!1 fmax
1
0 gðf Þdf r2f ¼ 0max gðf Þ2 df sf ¼ qf ¼ rf4  3
r3f f

Thus, according to these parameters, it is possible to compare different normalized


power spectra to make difference between different types of sources under the
assumption that different sources possess distinct normalized power spectra. This
process of comparison and categorization of normalized PSDF will be discussed in
Sect. 5.3.5. One possible way is the so-called Kolmogorov–Smirnov test, the most
useful and general non-parametric method for comparing two probability functions.
This test is sensitive to differences in both location and shape of the empirical
cumulative distribution functions of the two regarded probability functions.
Relation between auto-correlation function and power spectra. Between the
auto-correlation function and the power spectra, a relation exists that is known as
the Wiener–Khinchin theorem. This theorem indicates that the power spectra of a
wide-sense stationary process equal the Fourier transform of the auto-correlation
function:

Zþ 1 Zþ 1
1
Sðf Þ ¼ RðsÞei2p ds and RðsÞ ¼ 1 Sðf Þei2ps df ð5:25Þ
2p
1

In case of the one-sided power spectral density function of AE signals, (5.25) has
to be written as

Zþ 1 Zþ 1
Gx ðf Þ ¼ 4 Rx ðsÞ cosð2pf sÞds and RðsÞ ¼ Gðf Þ cosð2pf sÞdf ð5:26Þ
0 0

Thus, it turns out that weakly correlated time-series processes exhibiting a


narrow auto-correlation function RðsÞ decreases rapidly with increasing s and is
diminishing for large s show wide spectra. In contrast, strongly correlated processes
with RðsÞ different from zero for large s possess narrow spectra. The white noise as
a fully uncorrelated process is characterized by RðsÞ ¼ adðsÞ, where a is constant
and the Fourier transform of RðsÞ gives Gðf Þ ¼ a. Thus, the PSDF of white noise is
constant over all frequencies 0  f  1. Majority of random process are described
by a normal distribution that is characterized by an exponentially decaying
auto-correlation function ðsÞ ¼ r2x eas . For normal distribution, the PSDF is then
given by:
a
Gðf Þ ¼ 4r2x ð5:27Þ
a2 4p2 f 2
130 5 In Situ Techniques for Characterization …

5.3.3 Sources of Acoustic Emission

The versatile sources of AE encompasses (i) materials degradation (e.g. crack


initiation and growth, fracture of inclusions or particles, surface degradation,
debonding of coatings), (ii) plastic deformation (e.g. dislocation glide, twinning),
(iii) phase transformations (e.g. martensitic phase transformation, solid–liquid
phase transformation), (iv) fabrication processes (e.g. welding, rolling, forging,
machining, grinding) and (iv) leaks [131]. As shown in Fig. 5.1a, the activation of
internal sources under certain stimulus results in elastic waves.
Thus, the wave motion excited by such an impulsive (i.e. delta function
dðt  t0 Þ) so-called body force concentrated at ðr 0 ; t0 Þ and acting in the k-th direction
can be described using the Green’s functions. The displacement ui ðr; tÞ at a certain
distance r and a certain time t within a volume V is given by the following
expression and shown schematically in Fig. 5.9:

Z Zt  
ui ! Gi;j !
r ; r 0 ; t  t 0 fj !r ; t0 dt0 d!
0 0
r ;t ¼ r ð5:28Þ
V 0

This expression involves a convolution of all time-dependent body forces with


their corresponding Green’s functions between all source points and the transducer.
In order to avoid singularities in the Green’s function, the delta function dðt  t0 Þ of
the point source is replaced by the time-dependent Heaviside function 1t H ðt  t0 Þ.
The Green’s function in (5.28) can be substituted by

Gi;j !
d !
r ; r 0 ; t  t 0 ¼ GH r ; r0 ; t  t0 ð5:29Þ
dt i;j

which leads to
Z Zt  
ui !
r ;t ¼ ! 0 0 _ !0 0 0 !0
i;j r ; r ; t  t fj r ; t dt d r
GH ð5:30Þ
V 0

Fig. 5.9 Correlation between AE source (body force) and the displacement detected at a certain
distance and a certain time within a finite volume. Convolution of each and every time body force
with its Green’s function. Modified according to [141]. Permission of Taylor and Francis
5.3 In Situ Acoustic Emission Measurements 131

Furthermore, it is assumed that the sources are randomly distributed point-like


sources described by a centroid position !
r 0 , which can be expressed by the Taylor
series expansion method. In addition, all components of the point source have the
same temporal behaviour. Equation (5.30) can be reformulated as follows:

Z Zt  
ui ! ! ! 0 0
r ;t ¼ GH
i;j;k r ; r 0 ; t  t r_ j;^k ðt0 Þdt0 ð5:31Þ
V 0

 
! !0 0
i;j;k r ; r 0 ; t  t
Here, GH represents the partial derivatives of the Heaviside
D E
elastic Green’s tensor at the point !
r 0 in the ^k-th direction and r_ j;^k ðt0 Þ accounts
for the source function. The subscripts i, j, k = (1, 2, 3 …) are space variables,
whereas subscript ^k = (1, 2, 3 ….) is a space–time variable. Finally, accounting for
the response of the sensor and the AE instrumentation, it is assumed that the
transducer does not disturb the wave at the surface, and therefore, the distortion of
the waveform due to the transducer can be neglected. Thus, in case of a dis-
placement sensitive transducer, the point-to-point response to the delta impulse
excitation can be denoted as T ! r ; t  t0 where r is taken within the transducer
contact area. This assumption leads to the final equation for the acoustic emission
describing the measured electric signal at the transducer UðtÞ as a convolution of
the transducer response T, the wave propagation described by the Green’s function
GH and the source function r:

Z Zt  
UðtÞ ¼ r; t  t0 ÞGH
T ð~ !
r ; !
r
0
; t  t 0
r_ bðt0 Þd!
r dt0 ð5:32Þ
i;j;k 0 j; k
V 0

The application of the Fourier transformation results in a deconvolution of the


so-called transfer function Aðf Þ including transducer response and Green’s function
and the source function Eðf Þ:
D E
uðf Þ ¼ Aj;^k ðf Þ  Eðf Þ with Eðf Þ ¼ rj;^k ðf Þ ð5:33Þ
D E
The source function Eðf Þ ¼ rj;^k ðf Þ can be modelled for different defect
sources. Thus, Scruby et al. [142] used different combinations of force dipoles Dij to
model the body force representation of point-like sources. Under the assumption
that the displacement of a source is represented by a combination of dislocations,
the dipole tensor is given by
132 5 In Situ Techniques for Characterization …

Dij ðtÞ ¼ Ci;j;k;l  bk  dAl ðtÞ ð5:34Þ


!
Here b k is the Burgers vector component in k-direction, and dAl ðtÞ is the
time-dependent dislocation loop area with its normal in the l-direction. Ci;j;k;l is the
elastic stiffness tensor. Scruby et al. [142] calculated the waveforms and the power
spectra for four different source types: (i) single dipole, (ii) horizontal crack,
(iii) pure dilatation and (iv) inclined shear loop. In addition, the effects of the source
orientation, the temporal behaviour and the distance between source and transducer
are analysed. All source types are located 0.025 m from the epicentre, and the rise
time at the transducer is 30 ns. It turned out that in general in the far field, the
calculated waveforms at the epicentre are dominated by the longitudinal waves,
whereas the waveforms caused by the transversal waves depend on the configu-
ration. Thus, for pure dilatation, no displacement caused by transversal wave
occurs. The AE power spectra of all four configurations exhibit a very
low-frequency component. However, the amplitude of the low-frequency compo-
nent is varying from source to source. In addition, the spectra contain harmonic
oscillations with fundamental at 250 kHz corresponding to the delay in the arrival
of longitudinal and transversal waves (absent for case (iii)—pure dilation).
Moreover, a frequency component with slow decrease exceeding the 30 MHz
dominated by the arrival pulse of the longitudinal waves is observed. Furthermore,
both the rise time and the source location have a significant effect on the calculated
AE power spectrum.
Finally, its following conclusions can be drawn from the modelling of AE
sources:
• The detected AE response is capable to reflect the differences between dynamic
sources.
• Especially, the AE power spectrum is sensitive to source types.
• Source rise time and source location have a significant influence on the AE
response.
• Broadband transducers are strictly required to be able to distinguish different
sources.
Detectability of AE. Along with the different source types, orientations, locations
and rise times, the detectability of AE depends significantly on the size and the
velocity of the source. However, here the further explanations are separated
according to sources activated during (i) plastic deformation, (ii) fracture and
(iii) phase transformations.
Plastic deformation. The simplest case for the description of the detectability of AE
during plastic deformation is the assumption of straining of a fcc single crystal
oriented for single slip leading to dislocation formation and propagation on slip
planes inclined 45° with respect to the loading axis. By this process, dislocation
loops are formed causing acoustic emission. According to Scruby et al. [142] and
Wadley and Mehrabian [143] the maximum displacement Uz in z-direction (surface
5.3 In Situ Acoustic Emission Measurements 133

normal) caused by a single dislocation loop expanding with the instant velocity v to
a final radius a can be calculated according to:
!
c2T b  a  v
Uz ¼  ð5:35Þ
c3L r

Here, cL and cT are the velocities of the longitudinal and the transversal wave,
respectively, and r is the distance between the source and the epicentre. Thus,
!
for aluminium with b = 2.9 10−10 m, cL = 6400 ms−1, cT = 3250 ms−1 and
r = 10 mm, the maximum displacement accounts to [143]:

UZ ¼ 1:1613 mða  vÞ ð5:36Þ

Using today’s piezo-electric transducers with a sensitivity of 10−14 m, detectable


AE source during plastic deformation should fulfil the following condition under
the assumption that slip involves cooperative motion of n closely spaced disloca-
tions [143]:

ðn  a  vÞ  0:086 m2 s1 ð5:37Þ

with a as the size of the loop expansion before arrested at pinning points and v the
radial velocity. Equation (5.37) is known as the detectability criterion. In general,
a and v are statistically distributed for AE events during plastic deformation caused
by dislocation motion. However, only these events fulfilling (5.37) can be detected.
Consequently, work hardening occurring during plastic deformation has a signifi-
cant influence on the detectable AE activity. While at the beginning of plastic
deformation a substantial fraction of slip events propagates over larger distances
before getting pinned, the work hardening reduces significantly the mean free path
of mobile dislocations resulting in less events that radiate detectable elastic, and
consequently, the detectable AE activity decreases. Furthermore, it becomes
obvious that the quantities a and v also depend significantly on the grain size of the
material. Here, two different counteracting effects have to be taken into account:
(i) the parameter a is decreasing with decrease in grain size and (ii) the velocity v is
significantly increasing with decrease in grain size. Consequently, the detectable
AE activity is decreasing with the reduction of grain size as shown by Vinogradov
et al. [144].
In addition, precipitations may influence as well the acoustic emission [143].
Here, two different mechanisms have to be distinguished: (i) the Orowan mecha-
nism for incoherent precipitates and (ii) the cutting mechanism for coherent parti-
cles. While the first mechanism results in moderate detectable AE activity only, the
second mechanism causes strong acoustic signals due to intense slip band formation
[143].
134 5 In Situ Techniques for Characterization …

Fracture. In analogy to the detectability criterion provided in (5.37), a detectability


criterion for the formation of a horizontal, circular crack can be given [143]:

r  a2  v  5  1014 WðT  r Þ ð5:38Þ

Here, r is the distance between source and the epicentre, T is the displacement
threshold above which a signal exceeds the noise level and r is the pre-existing
vertical stress. Under the assumption that r = 0.02 m and T = 10−14 (5.38) can be
written as the criterion for detectability of fracture as [143]:

r  a2  v  0:1 W ð5:39Þ

In case of cleavage fracture in a ferritic steel with a = 10 µm (half of the grain


size), v = 1000 ms−1 and r = 500 MPa AE signals are generated, which exceeds
the detectability threshold by 500 times and are, therefore, easily detectable. Since
in analogy to plastic deformation a and v are distributed statistically, some AE
signals are detectable and others not depending on the noise level. The influence of
a and v on the detectability threshold was summarized by Wadley and Mehrabian
[143] in a plot of crack velocity versus crack size as shown in Fig. 5.10. However,
even so a and v are distributed, only those events right of the detectability threshold
in Fig. 5.10 result in detectable AE events.
Thus, brittle intergranular fracture and cleavage fracture in steels are easily to be
detected (see Fig. 5.11a, while microvoid coalescence will be difficult to detect
since the amplitude of the signals will be less and most probably hidden by the
noise level as demonstrated by Fig. 5.11b.
Phase transformation. Phase transformations are also known to generate acoustic
emission [143, 145–147]. However, here it has to be distinguished between diffusion-
controlled and diffusionless processes. While AE caused by diffusion-controlled
process such as the simultaneous growth of ferrite and cementite lamellae forming
pearlite or the growth of small carbides (<1 µm) and lath ferrite forming bainite will
be non-detectable, the martensitic phase transformation generates strong AE signals
and can, therefore, be detectable. For the martensitic phase transformation, two

Fig. 5.10 Detectability


threshold of acoustic emission
in terms of crack size (area)
and crack velocity. Modified
according to [143].
Permission of Elsevier
5.3 In Situ Acoustic Emission Measurements 135

Fig. 5.11 AE response according to different fracture behaviour. a Brittle fracture. b Ductile
fracture. According to [131]. Permission of IOP Publishing

aspects have to be taken into account: (i) the volumetric changes resulting in a dilation
caused by the transformation from fcc to bcc crystal lattice and (ii) the deformation
caused by shear deformation. Both aspects contribute to strong signals several times
larger than the detectability threshold. However, in case of the shear contribution, the
source orientation has to be included. Thus, the maximum displacement occurs at
shear under 45° and temporal waveform of pure shear is added to the dilation signal.
These signals are even stronger than those for pure dilation.

5.3.4 Instrumentation and Data Acquisition

In general, the instrumentation for the AE measurements consists of (i) the AE


sensor, (ii) the pre-amplifier, (iii) the AE instrument including data acquisition and
monitoring and (iv) oscilloscope and cables.
For the AE measurements, AE sensors are needed detecting elastic waves caused
by the spontaneous release of stored strain energy on localized sources within a
material under mechanical, thermal or chemical loading. Thus, the propagating
elastic waves result in very small surface movements (range of displacement in the
order of 10−14 − 10−11 m). The displacement is detected by so-called AE sensors
mounted on the surface [129]. Here, contactless (optical sensors) and contact-type
sensors have to be distinguished. Majority of AE measurements are conducted
using the latter ones. The group of contact-type sensors is formed by capacitive
and piezo-electric sensors. The piezo-electric transducers convert mechanical
movement into an electrical voltage signal. Typically, a displacement of 1 pm is
136 5 In Situ Techniques for Characterization …

transformed into electrical signals of 1 µV. The piezo-electric crystal used is almost
always made from a ceramic (e.g. lead zirconate titanate (PZT)). Among all types of
AE transducers, the piezo-electric sensors provide the best combination of high
sensitivity, selective frequency response, easy handling and low cost [129].
As shown above in (5.32), the transducer response is given by a convolution of
the transfer function of the transducer T, the Green’s function of the wave propa-
gation GH and the source function r. The transducers are selected based on operating
frequency, sensitivity and environmental characteristics, and are grouped into two
classes: (i) resonant and (ii) broadband sensors [129]. The transducer response in the
frequency domain is exemplarily shown in Fig. 5.12 for these two main types of
sensors. The sensitivity of the sensor is given either in dB (according to (5.2) without
the term for the pre-amplifier) or in voltage output per vertical velocity (1 Vs/m) and
is plotted versus the frequency range usually 0.1 MHz  f  2 MHz. The dif-
ference between resonant and broadband sensor becomes obvious. The broadband
sensor has a high sensitivity over a wide range of frequencies, whereas the resonant
sensor has high sensitivity for restricted frequency range only.
The sensor response is crucial for the data analysis and has to be determined for
each sensor individually by calibration procedures. There are two types of cali-
bration procedures. The first one is a so-called primary step force calibration or
absolute calibration provided by the National Institute of Standards and Technology
(NIST), which is shown in Fig. 5.13a. Here a steel block is used with a diameter of
∅ 90 cm and a height of 43 cm. The break of a glass capillary is used as a
step-function impulse, and the elastic waves are detected by a capacitive sensor in
comparison to the sensor under test. The second step force calibration is the pencil
break test (Hsu-Nielsen source). Here, an acryl rod of 790 mm length and 38 mm
height is used for the break of the lead (2H, ∅ 0.5 mm, length 3 mm) of a pencil.
The AE transducer under test is mounted at one front end, and the lead will be
broken 102 mm far from this front end. The pencil break test is also a good measure
for the optimal setup of AE experiments and is, therefore, often used before the
actual AE testing.

Fig. 5.12 Sensor response of two different types of AE sensors. a Resonant-type sensor.
b Broadband-type sensor (Copies of calibration sheets of resonant sensor R50 (a) and broadband
sensor WD)
5.3 In Situ Acoustic Emission Measurements 137

Fig. 5.13 Two variants of calibration procedures for AE sensors. a Glass capillary on a steel
transfer block (NIST). b Hsu-Nielsen source or pencil break test on an acryl rod (EN 1330) [148].
With courtesy of A. Vinogradov

A large variety of transducers regarding size and applicable temperature range is


commercially available. In general, the sensitivity of the transducer is increasing
with the increase in the detector cross-sectional area. For piezo-electric sensors, the
applicable temperature range is quite limited –40 °C  T  177 °C. Resonant
transducers can be used in a wider temperature range. Special AE transducer is also
available for high-temperature applications up to 500 °C.
For good acoustic coupling, the sensor has to be fixed at the surface of the object
under test. Maximum coupling adhesion is achieved with a smooth and clean
transducer’s surface on a smooth and clean object’s surface. Surface roughness and
air gaps can be eliminated by a coupling layer. As coupling media vacuum greases,
water-soluble glycols or solvent-soluble resins can be used. In addition, the
transducer should be stationary. This could be reached by glue or holding devices
such as tapes, elastic bands, springs or magnetic hold-downs. In some cases, it can
be necessary to use AE waveguides. However, it should be noted that the appli-
cation of waveguides introduces further complexity to the frequency response of
AE waves [129].
Pre-amplifier. Pre-amplifiers can be either part of the AE transducer itself or are
available as stand-alone devices. Pre-amplifiers are employed for two purposes:
(i) the amplification of the AE signals and (ii) the conversion of the high-impedance
alternating current (AC) signals of the AE sensor into low-impedance signal, which
leads to a reduction of the loss of signals transmitted over long cables. Thus,
commercially available pre-amplifiers are carefully designed for an optimum
signal-to-noise ratio. The gain of the amplifier is given in dB (see 5.2) and can be
varied depending on the pre-amplifier in a range between 0 dB and 60 dB. In
addition, pre-amplifiers are usually equipped with plug-in filters, which provide the
flexibility to optimize the transducer selectivity and the noise rejection. The filters
operate in the low pass (signals with a frequency lower than a cut-off frequency are
138 5 In Situ Techniques for Characterization …

Fig. 5.14 Effect of the band-pass filter on the AE waveforms. Modified according to [129]

passed, whereas signals with higher frequencies are attenuated), high-pass (vice
versa of the low pass) and band-pass (signals with frequencies of a certain range are
passed whereas signals with frequencies outside this range are attenuated) config-
uration. Band-pass filters are generally employed in a bandwidth from 1 kHz to
2 MHz. The choice of the frequency range depends on the noise level and the
attenuation properties of the material under consideration. However, it should be
noted that the application of a band-pass filter can change drastically the AE
waveforms as shown in Fig. 5.14 [129].
AE instrument. The principal component of the AE measurement setup is the AE
data acquisition board. Here different variants as multiple channel or dual-channel
acquisition boards are commercially available depending on the producer and the
application task. Figure 5.15 shows a typical scheme of a AE acquisition board
with N channels for AE data acquisition and an additional parametric channel.

Fig. 5.15 AE data acquisition instrument with N channels for AE data acquisition with fast
analog/digital converter and one-parametric channel with slow analogue/digital converter for
recording additional parameters such as load, strain, temperature. According to [148]. With
courtesy of A. Vinogradov
5.3 In Situ Acoustic Emission Measurements 139

For channel 1, the signal flow from the AE sensor and the pre-amplifier over the
low-pass and high-pass filter as well as a main amplifier until the analog–digital
converter (ADC) and the detection by the digital signal processor (DSP) is illus-
trated. The data collection can be performed with 1–50 Msamples/s. Therefore, fast
AD converter in the AE channel is necessary. Multiple channels n = 1–N are
constructed in similar way. The parametric channel accounts for lower data
acquisition rate and is used for the detection of additional signals such as
stress-strain data, temperature or vibrations alongside with the AE experiment.
A monitoring system is used in combination with the AE data acquisition board for
the visualization of the AE data and the analysis of parameters such as counts, rise
time, duration, waveforms and frequency spectrum. Furthermore, the AE instru-
mentation can be complemented by oscilloscope for direct observation of AE
events.
AE data acquisition. For the AE data acquisition, two different approaches are
available: (i) the narrow-band detection system [131] or so-called threshold-based
AE data acquisition, and (ii) the broadband detection system [131] or so-called
continuous AE data acquisition. Figure 5.16 provides a short overview of the dif-
ferences between both acquisition techniques. The narrow-band data acquisition
uses a threshold value for the voltage signal Uth detected by the transducer, which is
customer defined lying well above the noise level Unoise depending on the used
experimental setup. In general, one threshold is used. However, multiple thresholds
could be set as well.
Using this method, AE data are recorded as hit detections by crossing the
threshold value as shown in Fig. 5.17a. Parameters, which can be determined via
this approach, are (i) the number of hits crossing the threshold, (ii) the hit rate,
(iii) the number of events, (iv) the arrival time, (v) the amplitudes, (vi) the durations
and (vii) the RMS and the envelope of the hit distribution as a measure for the
“power” and the “energy” of AE signals. However, these terms should not be mixed
with the power spectrum and the determined energy obtained via the Fourier
transformation.
In principal, the threshold-based data acquisition is useful in case of individual
burst signals as shown in Fig. 5.17b (such as sudden cleavage crack formation or
leakage of a pressure vessel). In case of multiple burst events with different
amplitudes or AE data consisting of both burst and continuous signals, the deter-
mination of the threshold value becomes a difficult task (cf. Fig. 5.17c). In contrast,
the broadband data acquisition works without any threshold. Here the complete AE
data stream is recorded. The AE data stream is analysed via Fourier transformation,
and the resulting frequency spectrum is then analysed by different statistical pro-
cedures regarding probability density functions, mean values and variances or the
power spectrum, the energy and the median frequency.
140 5 In Situ Techniques for Characterization …

Fig. 5.16 Scheme of two different approaches for AE data acquisition. a Narrow-band data
acquisition. b Broadband data acquisition. Modified according to [131]. Permission of IOP
Publishing

5.3.5 Processing of AE Data

According to the description of the AE as multivariate random time-series process,


the data analysis has to be performed both on the time and on the frequency
domain. Thus, processing of AE data has to be separated into different steps [149]:
(1) General description of AE time series in time domain (type of AE, set of
time-domain parameters).
(2) Descriptive statistics and time-series analysis (test of stationarity, distribution of
AE parameters, type of time series, auto-correlations).
5.3 In Situ Acoustic Emission Measurements 141

Fig. 5.17 Threshold-based AE data acquisition. a Record of AE data. b Suitable single transient
signal for determining detection threshold value above noise level. c More complex AE signals
consisting of several transient signals and continuous signals, where it is difficult to define
appropriate threshold value. According to [148]. With courtesy of A. Vinogradov

(3) Spectral analysis of AE in frequency domain (fast Fourier transformation,


PSDF, noise subtraction, calculation of spectral parameters, typical shapes of
power spectra, evolution of PSDF).
(4) Data reduction and factor analysis (factor loadings for all AE parameters,
minimized set of descriptive variables).
(5) Data categorization and cluster analysis (parametric clustering, non-parametric
clustering, classification of signals in K groups, noise identification and
filtering).
(6) Descriptive statistics for individual clusters (distribution of AE parameters
corresponding to each cluster, multivariate statistical characterization of AE
sources of different types).
(7) AE kinetics for each cluster (temporal evolution of AE parameters corre-
sponding to each cluster, evolution of individual clusters).
General description of AE time series in time domain. The first step is the visual
evaluation of the recorded AE data stream and the determination of the AE type:
continuous AE or burst-type AE. Commonly, both AE types will occur simulta-
neously during plastic deformation of metallic materials—the continuous AE as a
result of dislocation glide processes and the burst-type AE signals as a result of,
e.g., brittle fracture. Separation between both types of AE signals is done either by
the amplitude distribution [150], the time of arrival (phase picking) [151] or the
kurtosis of the AE waveform in time domain [136]. Vinogradov et al. [136] showed
that the kurtosis of continuous AE signals equals q  0 and the AE waveform can
be described by normal distribution, whereas for burst-type signals, the AE
waveform deviates from normal distribution and the kurtosis equals q > 0 indi-
cating a certain peakedness of the AE distribution (cf. Sect. 5.3.2).
142 5 In Situ Techniques for Characterization …

Descriptive statistics and time-series analysis. Before applying descriptive


statistics and time-series analysis, the most recommended step is the proof of
stationarity of the AE process. This can be done by the non-parametric runs test.
Here, a “run” is defined as “…a succession of one or more identical symbols, which
are followed and preceded by a different symbol or no symbol at all…” [152]. As an
example for a “run” the series of identical flips of a coin can be regarded, where P
and T represent pitch-and-toss of a coin, respectively. Such a run could be
“PTTTTTTPPTPP”, where the number of long run of “toss-T” is 6. Thus, a runs
test is a counting of the number of runs in a series, and comparing the number found
to what one would expect if the observations are independent of one another. In
case of too many or also of too few runs, a dependence of the observations is
evidenced, and therefore, the process is non-stationary. Therefore, for proofing the
stationarity of the AE data, the following steps have to be performed: (i) dividing an
AE realization with 2n data points (usually 211 = 2048 or 212 = 4096) into N time
intervals of equal lengths, where N = 16 or 32 is recommended, (ii) computation of
mean value (or other parameters such as variance, standard deviation) for each
interval and align these obtained results in a new time sequence, (iii) counting the
number of runs of mean values, which are above (A) and below (B) the median
value of the series and (iv) compare the number of counts found to known prob-
abilities rn;a of runs for random data. In case of AE data with a confidence index
a = 0.95 and n ¼ N=2 ¼ 8, the number for runs in the series must be at least
5  Nruns \12 in order to accept the process as stationary such as the sequence
AAABBABBBBAAAABBB contains six runs. However, a sequence having just three
runs such as AAAAAABBAAAAAA can be regarded as a non-stationary process.
In case the stationary test is positive, then the AE data can be described by a set
of probability distribution functions of peak amplitudes U P or time intervals
between pulses s as shown in Fig. 5.18. Based on the probability distribution
function of the time intervals between pulses t, the decision can be done by
comparing the AE process with the Poisson inter-arrival time distribution,

Fig. 5.18 Time-series analysis of AE data in terms of probability density distributions.


a Experimental data set of peak amplitude distribution. b Schematical description of bimodal
frequency distribution consisting of Poisson’s distribution and normal distribution. According to
[148]. With courtesy of A. Vinogradov
5.3 In Situ Acoustic Emission Measurements 143

indicating that AE signals are independent or not. Mostly, bimodal distributions are
found indicating that the AE signals are not independent from each other.
For non-stationary processes, other specially developed methods have to be
applied, which are, however, not in the focus of this work.
Spectral analysis. For the analysis of the AE process in the frequency domain,
different well-elaborated methods are available such as (i) short time Fourier
transformation, (ii) wavelet transformation, (iii) S-transformation or (iv) Hilbert–
Huang transformation. The admittedly most commonly used is the Fourier trans-
formation (FT). It is a one-dimensional transformation, and no time information
will be available since it assumes stationarity. The FT is well suited for the char-
acterization of periodic or pseudoperiodic signals and is simple to interpret. Thus,
the FT will be always the first choice in order to understand the general property of
the system under inspection.
However, in case of transient signals, the short-time Fourier or wavelet trans-
formations will be more suitable. These are two-dimensional transformations, and
time-domain information will be retained. Both transformations provide researchers
and practitioners with well-established tools, which are helpful in many applica-
tions (such as dynamic processes). The wavelet transformation (e.g. [153, 154])
should be preferred every time if it is feasible to work with 2D data in the suc-
cessive steps (i.e. parameters extraction, classification, clustering), and mostly every
time AE wave propagation details are of concern [155].
The spectral analysis via the Fourier transformation will be considered now in
more detail. PSDFs described in Sect. 5.3.2 are related to continuous data.
However, as shown in Sect. 5.3.4, the digital AE data acquisition results (due to the
analogue-digital converter, even if it is a fast one to record as much as possible data)
in discrete AE records evenly spaced in time. Thus, the AE time series collected
depending on the sampling rate results in a sampling time interval Dts , which
defines the maximum resolvable frequency—the so-called Nyquist frequency fN (or
cut-off frequency) [149]:

1
fN ¼ ð5:40Þ
2Dts

Since the AE data are sampled at discrete intervals for a certain period of time,
N readings per realizations of the length T ¼ N  Dts are obtained and the frequen-
cies, at which the Fourier transformation is calculated, are restricted to N frequencies
according to fn ¼ n=NDts . Thus, using the discrete Fourier transformation (DFT), a
discrete periodic time-series AE record is displayed into a discrete periodic fre-
quency spectrum. Thus, a digital signal can be decomposed in its frequency com-
ponents. An algorithm for the efficient calculation of the DFT is the fast Fourier
transformation (FFT). However, due to the discrete nature of the AE records,
so-called leakage effect has to be taken into account in energy (power) calculations.
This effect describes the fact that due to the finite observation time interval of AE
record, the frequency spectrum also contains frequency components, which would
144 5 In Situ Techniques for Characterization …

be not observed only at theoretical infinite time intervals for observation. Due to the
limited number of discrete recorded data for the DFT, the leakage effect leads to
periodic continuations of the time-limited records. The impact of the leakage effect
on the FFT can be minimized either by large observation intervals or by the appli-
cation of so-called windows functions [149]. The application of windows functions
can be either done on recorded original data in the time domain or in the frequency
domain on the power spectra. In the time domain, the data records are multiplied by a
discrete windows function and the DFT (FFT) performed afterwards. For the discrete
window function, different types are known from the literature, such as
(i) Rectangular (Daniel), (ii) Barlett, (iii) Hann or (iv) Welch. These four window
tapering functions are summarized together with their main properties in Table 5.6
[149].
In the time domain, the Welch function can be used for smoothing the peri-
odograms of AE records [156]. Thus, the periodogram is divided in K sections, and
the periodogram of each section is averaged, e.g. a 4096 point realization of AE
records is split into eight segments of 512 points without overlap. Overlap of the
tapering windows is also possible; however, it requires more computing resources.
The smoothed spectrum will have 256 frequencies, whereas the initial spectrum will
have 2048 frequencies. However, applying this technique will result in a loss of
resolution at low frequencies. Second approach is to apply the tapering windows
after the FFT or to combine the tapering window technique both in time domain
first (e.g. Welch) and afterwards in frequency domain (Welch or Barlett) [156].
In a next step, the PSDF of i-th AE record has to be noise-corrected. Therefore,
the power spectrum of the “electrical” noise Gnoise ðf Þ has to be determined from the
prior-to-test measurements of the laboratory background noise. Thus, the Gnoise i ðf Þ
for i = 1 to N (at least N = 30–50) noise records have to be calculated and averaged
over all N [156]:

1X N X
Gnoise ðf Þ ¼ Gnoise
i ðf Þ: ð5:41Þ
N i¼1

This averaged noise spectrum Gnoise ðf Þ is subtracted from each Gk ðf Þ giving the
noise-corrected estimate of the PSDF of AE data [156]:

Gðf Þ ¼ Gk ðf Þ  Gnoise ðf Þ: ð5:42Þ

This kind of simple yet efficient noise correction can be considered as one of the
most obvious advantages of spectral decomposition. Finally, from the
noise-corrected AE power spectrum, the following AE parameters can be deter-
mined: (i) the energy E, (ii) the median frequency fm as well as (iii) the fundamental
frequency fc (frequency corresponding to Gmax of the PSDF), (iv) the spectral
maximum (magnitude of spectral density at fc ) and (v) the effective width of
spectrum feff (cf. also Table 5.4).
Table 5.6 Different windows functions for spectral smoothing [149]
Rectangular Barlett Hann Welch
5.3 In Situ Acoustic Emission Measurements

2 N1
  2ðn  2
W(n) = 1 WðnÞ ¼ N1  n  N1 WðnÞ ¼ 0:5 1  cos n0:5ðN1Þ
2 2 N1 WðnÞ ¼ 1  0:5ðN þ 1Þ

Transient signals Random signals Random signals Random signals


Best frequency resolution Good frequency resolution Good frequency resolution Good frequency resolution
Good amplitude resolution Fair amplitude resolution Fair amplitude resolution Fair amplitude resolution
Poor spectral leakage Fair spectral leakage Good spectral leakage Good spectral leakage
145
146 5 In Situ Techniques for Characterization …

Table 5.7 Various parameters in time and frequency domain used for acoustic emission analysis.
Modified according to [157]. With courtesy of E. Pomponi
AE parameters
Time domain Frequency domain

Up Peak amplitude E Energy


URMS Root mean square voltage Gmax Magnitude of power spectra
trise Rise time fm Median frequency
d Duration fc Fundamental frequency
c Counts feff Effective bandwidth

The normalized PSDF calculated according to (5.23) (power spectra divided by


the energy E) [156]:
Gðf Þ
gðf Þ ¼ ð5:43Þ
E

is used for comparison of different PSDF allowing the distinction between different
sources aiming that different activated AE sources result in different power spectra.
Statistical features describing the normalized PSDF are provided in Table 5.5.
Data reduction and factor analysis. As seen from the previous Sect. 5.3, there is a
high number of parameters, which can be determined from AE data records both in
time and frequency domains as summarized in Table 5.7. However, these different
parameters are not independent from each other. Some of them exhibit strong
correlation and the others do not. Therefore, a next step in the data analyses is to
reduce the number of available parameters describing the AE process.
This is done by the so-called principal components analysis or factor analysis
[158], which is a method of the multivariate statistics aiming at squeezing infor-
mation while maintaining the most important part of it. The aim of the factor analysis
is to suggest a few latent variables (factors) out of manifold different manifested
variables of empirical observations. Thus, the factor analysis allows for a dimen-
sionality reduction. Among different approaches for the factor analysis, the principal
component analysis (PCA) is rather efficient in AE studies as demonstrated by
Vinogradov [159]. It is shown that for AE data, at least two factors covering most of
the variance of experimental data have to be chosen since all determined AE vari-
ables differ substantially in two respects—associated with the time and frequency
5.3 In Situ Acoustic Emission Measurements 147

Fig. 5.19 Description of the time history of AE signals in reduced parameter space using the
median frequency fm and the kurtosis q showing development of damage in the fibre-reinforced
composite. a Whole process. b 1 < t < 30 s. c 30 < t < 60 s. d 60 < t < 690 s. e 690 < t < 760 s.
f 760 < t < 830 s. g 830 < t 860 s. According to [160]. Data with courtesy of A. Vinogradov

domains. Thus, the description of AE data records in a reduced feature space can be
sufficient as illustrated in Fig. 5.19 for data presented by Vinogradov [160]. Here the
behaviour of the two variables “median frequency” and “kurtosis” is regarded over
the entire recorded AE process (Fig. 5.19a). Figure 5.19b–g shows the
time-dependent behaviour of these two variables. Figure 5.19b, c shows the data
group with “median frequency” around 400 kHz and “kurtosis” around zero.
According to aforesaid statements, these data are described by a normal distribution
function and, therefore, belong to continuous-like signals attributed here to noise. In
Fig. 5.19d, data points are characterized by the “kurtosis”, which is well above zero,
signifying thereby that data points cannot be attributed to noise anymore since their
amplitude distribution has a notably higher peakedness than that the normal distri-
bution function, thus indicating the occurrence of burst-type signals. With ongoing
recorded AE process, the “median frequency” is shifted to lower values and the
“kurtosis” to higher values caused by higher amount of burst signals that are results
of damage development and final failure.
In case the AE process cannot be described by a reduced feature space, other
powerful tools with high potential for describing AE results such as the data cate-
gorization or cluster analysis can be applied. The cluster analysis is not an alternative
to data reduction schemes, but it can be an efficient complementary addition to them.
Data categorization and cluster analysis. The data categorization is done either by
cluster analysis or data classification [161]. The term “cluster” describes a con-
glomerate of objects that are similar in some respects. Thus, the aim of a clustering
process is to determine the intrinsic features in a set of unlabelled data grouping,
148 5 In Situ Techniques for Characterization …

Fig. 5.20 Difference between data categorization and clustering. a Supervised learning—
categorization/classification. b Non-supervised learning—clustering. Modified according to [157].
With courtesy of E. Pomponi

finally, similar objects into clusters and disjoining dissimilar objects. Characteristic
feature of the cluster analysis is the absence of patterns or descriptions of clusters.
Thus, the results are defined by the nature of the data themselves [161]. This is in
contrast to what is understood from classification, where patterns or descriptions of
classes are present, and thus, the results are defined by the user. The number of
classes of the classification process is known already in advance (compare grain
size distribution). In the clustering process, the expected number of clusters is
known only approximately or completely unknown. Therefore, the clustering
process is called a “non-supervised” learning process without any knowledge about
the data structure, whereas the classification is a “supervised” learning process since
the structure of the data is known [161]. The difference between classification and
clustering is shown by Fig. 5.20.
Typically, the global criteria for clustering process involve minimizing some
measure of dissimilarity between data points within each cluster, while maximizing
the dissimilarity of different clusters. However, the key issue of cluster analysis is to
find a reasonable measure for (dis)similarity of data points. Thus, the cluster
analysis can be separated into three steps [161]: (i) defining a measure of (dis)
similarity, (ii) defining a criterion function for clustering and (iii) defining an
algorithm to minimize (or maximize) the criterion function. Defining a measure of
(dis)similarity is to find a reasonable feature space (as a result of the factor analysis
—such as median frequency fm , kurtosis q or energy E) and distance measure
between individual data points for the problem under study. Thus, D is a measure of
distance between two points p ðp1 ; p2 ; p3 ; . . .; pn Þ and q ðq1 ; q2 ; q3 ; . . .; qn Þ in a n–
dimensional data space which satisfies the following properties [161]:
(1) Symmetry of two data points:

Dðp; qÞ ¼ Dðq; pÞ ð5:44Þ


5.3 In Situ Acoustic Emission Measurements 149

(2) Positivity:
Dðp; qÞ  0 ð5:45Þ

(3) Self-similarity of two data points:

Dðp; qÞ ¼ 0 with p ¼ q ð5:46Þ

Different variants can be chosen for the measure of distance D such as the
Minkowski distance DMIN , which is a generalization of the Euclidean distance
DEUC , or the Manhattan distance DMAN :
!1=s sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
X
n X n X
n
DMIN ¼ j pi  qi j s
; DEUC ¼ jpi  qi j2 ; DMAN ¼ jpi  qi j
i¼1 i¼1 i¼1

ð5:47Þ

These measures describe the dissimilarity between two points. Describing the
similarity, the correlation coefficient ZCC could be used (see Sect. 5.4.1.2).
The most commonly used criterion function for clustering is the sum-of-square
error for a given data set with n elements ðx1 ; x2 ; x3 ; . . .; xn Þ:

k X
X 2
FCC ¼ xi  mj ð5:48Þ
j¼1 xi 2Sj

Here, k is the number of desired clusters ðS1 ; S2 ; S3 ; . . .; Sk Þ with k\n. The term
xi  mj is the chosen distance measure between the points xi 2 Sj and the
respective centroid mj of the cluster [161].
As an example, the results of the clustering process of a data set in bivariate
coordinate system are shown in Fig. 5.21a revealing three clusters with different
features A and B together with their centroids mj . Different variables of the AE
process could be chosen as the coordinates for the cluster space such as the energy
E, the median frequency fm or the kurtosis q.
The algorithm to minimize (or maximize) the criterion function can be either
parametric or non-parametric, whereas for the first one, the evaluation of a measure
of (dis)similarity is made between a fixed set of parameters specified a priori (e.g. k-
means, nearest-neighbours, fuzzy c-means), for the latter one parameters may be
used (or may be not), and they are, however, flexible and not fixed in advance (e.g.
Kullback–Leibler divergence) [161]. In centroid clustering, clusters are represented
by a central vector, which may not necessarily be a member of the data set. When
the number of clusters is fixed to k, k-means clustering is a centroid-based clustering
with the task to find k cluster centres and assign the objects to the nearest cluster
centre, such that the squared distances from the cluster are minimized. The fuzzy
150 5 In Situ Techniques for Characterization …

Fig. 5.21 Results of clustering process in a bivariate feature space. a Three clusters with their
centroids. b Parameter description used for the adaptive sequential k-means algorithm (ASK).
a According to [160]. With courtesy of A. Vinogradov. b Reproduced from [161]. Permission of
Elsevier

c-means is a variation of k-means allowing a fuzzy cluster assignment. Both, the k-


means and the fuzzy c-means algorithm try to minimize the criterion function given
by (5.48) iteratively [161].
In contrast to this parametric clustering, the non-parametric clustering operates
mainly with the normalized mean PSDF—also known as spectral shape catego-
rization. Thus, Vinogradov et al. [136] introduced a statistical characterization
technique to classify the AE power spectra with respect to their shapes. Vinogradov
et al. [136] showed on Cu-Ge alloys with different solid solution strengthening that
two different AE sources—dislocation glide and twinning—are discriminated due
to their distinct features in the AE power spectra and waveforms and a data cate-
gorization technique based on the power spectra.
Quite recently, Pomponi and Vinogradov [161] developed a new non-parametric
clustering approach—so-called adaptive sequential k-means (ASK) algorithm,
which is an evolutionary algorithm and, therefore, applicable to real-time appli-
cations. Similar to the k-means algorithm, for each cluster ki the mean centroid mi
and the number of elements ni per cluster are determined. In addition, the evolu-
tionary intra-cluster distance (ICD) dki and the point-wise centroid drift vector cki
are estimated, which are the major differences to the k-means algorithm.
Figure 5.21b demonstrates the definition of the main parameters determined for
each cluster and used for merging process during clustering analysis. Thus, xa and
xb are two data points in a bivariate feature space. Dðxa ; mk Þ is the measure of
distance between point xa and the centroid mk of cluster k, wki is the intra-cluster
distance and rki its standard deviation. R is used as an inter-cluster distance between
clusters i and j, and a is a constant. According to these parameters, the intersection
of two clusters is evaluated by comparing the distance between each pair of cen-
troids R with the corresponding cluster diameter (the weighted intra-cluster dis-
tance). Thus, so-called coarsening parameters Ci and Cj for each cluster of the
5.3 In Situ Acoustic Emission Measurements 151

cluster pair ki ; kj are defined and, finally, a merging criterion for two clusters is
defined. According to this, the two clusters ki and kj will be merged if the distance
between their centroids mi and mj , respectively, becomes less or at least equal to
their coarsening parameters Cij assuming that the drift of the centroids is small
compared to the dispersion of data points belonging to the cluster. Thus, the drift of
the centroids of clusters is reducing while the number of elements within each
clusters increases. The merging procedure of two clusters ki and kj with ni and nj
number of elements and mi and mj as centroids results in a new cluster kmerged with
nmerged number of elements and the centroid mmerged according to [161]:
ni nj
nmerged ¼ ni þ nj and mmerged ¼ mi þ mj ð5:49Þ
ni þ nj ni þ nj

The ICD dmerged as well as the centroid drift vector cmerged of the merged cluster
depends on the values of the individual clusters ki and kj dmerged ¼ f dki  dkj and
cmerged ¼ f cki  ckj [161].
Figure 5.22 shows a comparison of the three different clustering algorithms:
ASK, k-means and c-means performed by Pomponi and Vinogradov [161] on an
AE data stream obtained during cyclic crack growth experiments on a CuZr alloy.
Clearly, three different normalized mean PSDFs are identified related to cluster 1,
cluster 2 and cluster 3 (see Fig. 5.22a). Figure 5.22b–d shows the results of the
clustering analysis using the two-dimensional feature space of median frequency fm
and energy E. It is obvious from the cluster representation that a good agreement
between the ASK and the k-means algorithm exists (regarding both shape and
number of cluster elements). Larger difference occurs with respect to the c-means
algorithm.
Finally, each cluster can be described both by the distribution of the AE
parameters in terms of descriptive statistics for individual clusters and by the
temporal evolution of AE parameters in terms of evolution of individual clusters.
The last step is the identification of AE sources based on the descriptive statistics
and the temporal evolution of individual clusters. The last step has to be corrob-
orated by microstructural investigations in order to determine possible deformation
and damage mechanisms. The example shown in Fig. 5.22e shows the evolution of
the three clusters related now to dislocation motion (CL1), to particle fracture (CL2)
and ductile crack growth (CL3). Here, the AE cluster analysis is corroborated by
TEM and SEM investigations.

5.3.6 State of the Art in Materials Engineering

The first introduction of the technology of acoustic emission measurements on


Materials Engineering dates back to the beginning of 1950 with the PhD thesis of
Joseph Kaisers, who performed tensile test on a metallic material recording for the
152 5 In Situ Techniques for Characterization …
5.3 In Situ Acoustic Emission Measurements 153

JFig. 5.22 Comparison of three different clustering algorithms applied on an AE data stream
obtained from crack growth experiments on a CuZr alloy. a Three different types of mean PSDF
identified out by the FFT related to cluster 1, cluster 2 and cluster 3. b Three different cluster
algorithms applied on a two-dimensional feature space given here by the median frequency fm and
the energy E: (i) adaptive sequential k-mean algorithm (ASK), (ii) fuzzy c-means algorithm and
(iii) k-means algorithm. c Temporal evolution of the three identified clusters and their relation to
deformation and damage mechanisms. Reproduced from [161]. Permission of Elsevier

first time acoustic emission signals [162]. Along with the effect that AE signals
generated under different loading patterns can provide valuable information con-
cerning the structural integrity of a material, Kaisers discovered the phenomenon—
known as Kaiser effect—that load levels that have been previously exerted on a
material do not produce any AE activity until former stress is exceeded [163]. Few
years later, in 1961 the experiments of Kaisers are repeated by Schofield and
published under the title “Acoustic Emission under applied stress” [164] that was
the invention of the terminology of AE.
However, already before Kaisers and Schofield, the audible noise—known as tin
cry—accompanying mechanical tests on various kinds of metals as an incidental
observation was known and recorded. The term “tin cry” describes audible emis-
sions produced by the mechanical twinning of pure tin during plastic deformation
and was “… first documented in the eighth century by Arabian alchemist Jabir Ibn
Hayyan. In a book, Hayyan wrote that Jupiter (tin) gives off a ‘harsh sound’ when
worked, while Mars (iron) ‘sounds much’ during forging…” [165].
According to Drouillard [162] the history of AE could be grouped into three
periods until the mid of the 1990s: (i) the enlightenment of AE (1950–1967), (ii) the
Golden Age of AE (1967–1980) and (iii) the period of transition (1980–mid of
1990s). From today’s viewpoint, more than 20 years after Drouillard, a fourth
period can be added: (iv) the renaissance of AE.
The first period—the enlightenment of AE—started in 1950 in Germany with the
work of Kaisers effect and in the English speaking world in 1956 with the publi-
cation of Schofield. Pioneering works among huge amount of research in the field
of acoustic emission were: (i) the discovery of the relationship between AE and
fracture mechanics by Srawley and Brown in 1964 [166], (ii) the introduction of the
concept for elimination of noise due to narrow-band instrumentation using fre-
quency range well above the audio range by Dunegan in 1964 (cited in: [167])
and (iii) the successful source location in a vessel by Srawley and Esgar in 1965
[168].
The second period—the Golden Age of AE—starting from 1967 was charac-
terized by intensive investigations on dislocations being a source of acoustic
emission. One of the most cited publications of this area is the paper on
“Relationship between acoustic emission and dislocation kinetics in crystalline
solids” by James and Carpenter [169] in 1971. By these authors, it was shown that
acoustic emission emitted from single crystals of irradiated LiF, annealed LiF,
NaCl, and zinc under compressive deformation at constant strain rates consisted of
discrete signals of varying amplitudes. Furthermore, the rate of these signals was
154 5 In Situ Techniques for Characterization …

dependent on the total strain applied during the compression tests. It was concluded
by James and Carpenter [169] that a correlation of the activity of acoustic emission
and the rate of the change of mobile dislocation density exists, and that, finally, AE
signals were generated by dislocation breakaway from pinning points.
In the third period—the transition of AE—a change of the application of acoustic
emission for inspection towards the field of process control and total quality
management—so-called structural health monitoring—occurred. At the same time,
the application of AE to concrete and civil structures had increasing activities (e.g.
[170]).
Today, the application of acoustic emission measurements is wide spread from
structural health monitoring of civil structures (e.g. bridges, buildings), pressure
vessels (chemical industry) or aerospace components over machining process
controlling (e.g. drilling, milling, turning [171]), metal forming (e.g. rolling,
forging) and joining technologies (e.g. welding) as well as tribological processes
(e.g. wear, friction, scribing) up to applications to geological materials (e.g. rocks,
salt, sandstone) and the large field of Materials Science and Engineering (MSE).
In MSE, the application of AE encompasses a wide spectrum of materials (pure
metals, alloys, metal matrix composites, ceramics, ceramic matrix composites,
plastics, reinforced plastics, concrete, etc.). The AE experienced a renaissance in
MSE since the powerful tools available together with high performance of com-
puting technologies allow for real-time investigations on the temporal evolution of
various kinds of deformation and damage mechanisms.
The following section is, however, focusing only on application of AE technique
in field of Materials Engineering and metallic materials. Thus, a huge number of
investigations on different metallic materials—single crystals (e.g. [172–174]),
bicrystals (e.g. [175, 176]) and/or polycrystals (e.g. [177–179])—and different
loading conditions (e.g. [180–183]) have been performed in order to characterize the
occurring AE signals and to clarify their correlation with individual mechanisms.
Since not all investigations can be referred here in detail, a comprehensive
overview of investigations of acoustic emission in field of plasticity, fatigue, cor-
rosion and fracture mechanics in the latest years (since 2000) is provided in
Appendix in Table A1. However, the majority of investigations were performed in
the field of plasticity regarding different deformation mechanisms as well as phase
transformations followed by fatigue investigations in order to improve the under-
standing on fatigue behaviour. Investigations are also available for fatigue crack
growth experiments and fracture behaviour as well as pit corrosion is in focus of
acoustic emission.
However, in many studies summarized in Table A1, distinction between dif-
ferent AE sources is done mostly qualitatively. Moreover, the main drawback of
majorities of AE studies performed in the past is the threshold-determined regis-
tration of AE signals. In this way, the AE waveform is reduced to a set of
time-dependent parameters such as peak amplitude, number of counts, rise time,
duration (e.g. review of Skal’s’kyi of AE and plastic deformation [184]). However,
most of these parameters are related hardly to the source mechanism or are strongly
dependent on each other. In addition, significant amount of useful information is
5.3 In Situ Acoustic Emission Measurements 155

hidden below the threshold like continuous signals due to dislocation motion. Since
acoustic emission is a random process, an alternative to a parameter-based
description is the spectrum-based analysis in a frequency domain after a Fourier
transformation. As described in previous section, the PSDF serves as a compre-
hensive characteristic of the AE time-series [128]. The real-time approach devel-
oped recently by Pomponi and Vinogradov [161] concerning AE clustering analysis
based on continuously recorded AE signals is inspired by the sequential k-means
algorithm, which allows the separation of different emitting sources on the basis of
different normalized PSDFs. This special clustering algorithm allows to attribute
different acoustic signals to various deformation and damage mechanisms like
dislocation glide, twinning, martensitic phase transformation as well as crack ini-
tiation and propagation occurring under plastic deformation of materials [156].
Therefore, the following detailed description of different fields of investigations
is focused on experiments using continuously streamed AE data sets.
Plastic deformation. Huge amount of AE investigations were performed in field of
plasticity regarding activation and temporal evolution of different deformation
mechanisms. Thus, Vinogradov et al. [136] showed on Cu-Ge alloys that appli-
cation of a clustering algorithm based on normalized mean PSDFs allows careful
separation of two deformation mechanisms—twinning and dislocation glide.
Majority of newer investigations were performed on magnesium and its alloys (e.g.
[185–189]) mainly in order to understand the mechanism of twinning under dif-
ferent loading conditions (tensile, compressive) as well as the mechanisms of
detwinning (e.g. [190]). Thus, Mathis et al. [188] observed a strong tension/
compression asymmetry in acoustic emission behaviour in Mg alloy in the tem-
perature range RT < T < 200 °C that can be related to the mechanical twinning. At
temperatures T > 300 °C, the asymmetry vanishes, which is related to dislocation
glide as predominant deformation mechanism. Moreover, Vinogradov et al. [190]
were capable to recover kinetics of twin accumulation with strain. They found a
direct correlation between the activity of twinning process and the resulting median
frequency of corresponding PSDFs. Since the twinning activity has a significant
influence on the time interval s between individual transient signals, the median
frequency fm is increasing with a reduction of time interval s due to higher twinning
activity, whereas a reduced twinning activity results in a decrease in median fre-
quency fm . Furthermore, a good agreement between AE results and video obser-
vation regarding twinning and detwinning mechanism was observed.
Macroscopic strain localizations such as serrated plastic flow were also studied by
acoustic emission. Vinogradov and Lazarev [191] showed on tensile tests of a-brass
at RT that occurring intermittent plastic flow in terms of PLC bands of type A
correlates well with results from acoustic emission. This type of instability causes a
continuous AE signals with increased amplitudes when bands are initiated. In
addition, band initiation is accompanied by a decrease in median frequency fm and
an increase in energy E. This seems to be a common signature of plastic instabilities
and is understood as an indicator of increasing correlation in collective dislocation
dynamics.
156 5 In Situ Techniques for Characterization …

Martensitic phase transformation. In the past, in some investigations in field of


plasticity, the correlation of AE and martensitic phase transformation (e.g. [145])
was of special interest in different kinds of materials like b-brass (e.g. [192–194]) or
steels (e.g. [141, 147, 195–198]). Takashima et al. [141, 195] studied intensively
martensitic phase transformation in austenitic stainless steel AISI 304 in combi-
nation with AE and optical microscopy. They showed that martensite transforma-
tion in a band running completely through a grain gave rise to a single AE event.
However, a discrimination of AE emissions of individual martensite laths within the
band or a distinction between two different types of martensite involved—a′-
martensite or e-martensite—was impossible. By Manosa et al. [196], the acoustic
emission analysis was performed on carbon steels with varying carbon content in
order to study kinetics of spontaneous martensitic phase transformation during
cooling process with 150 K/s after an austenitization at 1000 °C for 10 s. Manosa
et al. [196] showed that detected acoustic emission energy generated per unit
volume of martensite correlates with change in dislocation density in martensite
formed as carbon content is varied. Recently, Barat et al. [197] published AE results
during low-temperature tensile deformation of austenitic stainless steel (AISI
304LN). It was shown that AE signals increased rapidly in terms of counts with
decreasing temperature up to −50 °C, which is attributed to higher amount of
formed martensite at lower temperature. In addition, the authors stated that
burst-type AE signals before and after yield strength represent rapid formation of
martensite and interface crack initiation along the austenite/martensite boundary.
Quite recently, Bohemen et al. [198] published results on application of AE mea-
surements on quenched martensite.
Fatigue. Vinogradov et al. [199, 200] performed AE investigations during cyclic
loading of both copper single crystals and ufg copper (after ECAP) on continuously
recorded AE data. It was shown in [199] that spectral analysis (PSDF) of AE is
sensitive to many features of dislocation dynamics during cyclic loading. Thus, all
microstructural changes regarding dislocation arrangements such as matrix hard-
ening, Bauschinger effect, local softening caused by formation of PSBs, cyclic
hardening, and crack initiation are well reflected by AE parameters such as energy
E or median frequency fm . For fatigue of ufg copper [200], spectral analysis of AE
data revealed three main mechanisms: (i) large-scale shear banding, (ii) mode I
tensile crack opening and (iii) mode II crack growth. However, no AE source
related to dislocation glide was found in ufg copper.

5.4 In Situ Full-Field Measurement Techniques

In the past, the classical way to measure displacements or strains was the appli-
cation of strain gauges, extensometers or other mechanical and electrical devices.
Likewise, temperature measurements were performed by applying thermocouples at
the surface of specimens. However, these devices provide integral information of
5.4 In Situ Full-Field Measurement Techniques 157

regions only where they were applied (gauge length, contact point of thermocou-
ple), and their resolution is limited by the used devices. The evolution and spatial
distribution of local strain fields or temperature fields due to strain localization and/
or damage remains disregarded [201]. However, on one side it is well known since
Boas and Hargreves in 1948 [202] that deformation of polycrystalline materials is
very heterogeneous, which is caused by microstructural features such as grain
orientation, grain size and grain morphology [203]. On the other side, it is further
known since Farren and Taylor in 1925 [204] that some part of mechanical energy
introduced to material during plastic deformation is dissipated as heat causing
temperature increase [205].
In the following, digital image correlation (DIC) and infrared–thermography
(IR–TG) are described as contactless and visual full-field measurement techniques.
In contrast to application of strain gauges, extensometers or thermocouples, these
techniques provide spatial distribution of physical quantities such as displacement,
strain and temperature on surface or even in bulk of specimens under external load
[201]. In the last decades, full-field measurements experienced a large improvement
due to enormous development in both the field of camera technology and the
microcomputer technology enabling automated image processing within reasonable
time [206]. Thus, the application of these full-field measurement techniques is very
attractive for investigation of localized deformation processes and plastic instabil-
ities occurring during plastic deformation of various kinds of materials.
Fully-coupled full-field measurements are new developments in this field using
simultaneous recording of kinematic displacement or strain fields and thermal fields
for getting answers in topic of thermomechanics coupling during plastic deforma-
tion at microscopic scale.
In addition, obtained displacements, strain and/or temperature fields can be used
after post-processing for identification of parameters for micromechanical material
models [201].

5.4.1 Displacement and Strain Fields

According to Grediac and Hild [201], for measurement of displacement fields,


various techniques are known since the beginning of the 1970s such as speckle,
speckle interferometry, geometric moiré, moiré interferometry, holographic inter-
ferometry, image correlation or grid method. Strain fields can be either obtained by
numerical differentiation of the recorded displacement fields using above-mentioned
techniques or using directly shearography, speckle shearing photography or moiré
fringes shifting as mentioned by Grediac in [206]. In addition, these techniques can
be classified into non-interferometric (speckle, grid method) and interferometric
(speckle interferometry, moiré interferometry) techniques.
158 5 In Situ Techniques for Characterization …

However, in the following the method of digital image correlation will be


regarded only, since it is the most commonly used method in field of Materials
Engineering.
The method of digital image correlation (DIC) dates back to the beginning of the
1980s and was introduced by researchers of the University of South Carolina (e.g.
[207, 208]). Since that time, DIC was subjected to a spectacular development,
which is still under progress [201]. It had a significant impact in field of experi-
mental mechanics of solids and structures.

5.4.1.1 General Aspects of Digital Image Correlation

The digital image correlation (DIC) is an optical, contactless, non-invasive full-


field measurement technique. The aim of DIC is to calculate both surface
(two-dimensional) and volume (three-dimensional) displacement fields of speci-
mens, structures or components under several loading conditions (mechanical,
thermal) such as motion sequences, deformation stages, heating conditions or stress
relaxations. It is fairly tolerant to several experimental conditions (high tempera-
tures, chemical environment) and is based on numerical images provided usually by
microscopic techniques. Thus, digital images from sources providing greyscale
images can be used for DIC such as (i) video sequences digitized by frame grabber,
(ii) commercial digital cameras, (iii) electron microscopes (SEM, TEM, FIB),
(iv) atomic force microscopes, (v) confocal laser scanning microscopes and
(vi) thermo-cameras. This opens a wide field of application of DIC, which ranges
from materials science and engineering over safety engineering (e.g. trajectory
analysis of dummies during crash tests [209]) to geological science (e.g. emergency
management—micromotion analysis of glaciers) [209].
In experimental mechanics, DIC is meanwhile a very popular and powerful
method for measuring surface displacements in a wide range of applications from
the macroscale down to the submicroscale. In materials research, DIC is an
appropriate method for combination with any other microscopic technique used for
in situ characterization experiments such as OM (e.g. [210]), SEM (e.g. [211–215],
focused ion beam (FIB) technique (e.g. [216–218]) or atomic force microscopy
(AFM) (e.g. [219–224]). Together with IR–TG, it can be applied as so-called
fully-coupled, full-field measurements (e.g. [205, 225–228]).
The application of multicamera systems allows even the determination of
three-dimensional displacement fields. 3D images obtained from computer tomo-
graphic experiments (e.g. [229–231]) can be used for measurements of 3D dis-
placements by digital volume correlation.
Image pattern contrast. The method of DIC provides for the ability to measure
full-field displacements with subpixel accuracy from digital images by finding the
correspondence between matching subsets in images of non-deformed and
deformed states. However, one condition precedent for successful application of
this technique for local strain analysis is the contrast of digital images used for
displacement measurement.
5.4 In Situ Full-Field Measurement Techniques 159

The input data for image analysis are grey levels or positive integers of the
reference image fl and the image of deformed state gl , where the subscript I refers to
a pair of integers (column, line) of the image. The integer values vary between zero
and maximum values of dynamic range of image sensor (e.g. 256 levels for 8-bit
images and 4096 for 16-bit images). The principle of DIC is to evaluate the sought
mechanical transformation Ua between the reference image f and the image of
deformed state g, which can be expressed by following [201]:

gðUa ðxÞÞ ¼ f ðxÞ ð5:50Þ

An essential prerequisite for a successful correlation of reference image f and


image of deformed state g is a suitable contrast pattern at the surface of investigated
specimen. This contrast pattern must be a characteristic signature of each surface
element, which is transported simply by displacement field (equal to mechanical
transformation function Ua in (5.50)) without any other deterioration [201]. In
addition, the grey levels of images should exhibit a broad dynamic range. Thus, the
grey levels should cover as much as possible of available range of encoding depth
of the images (from 8 to 16 bit), however, without exhibiting any saturation [201].
Moreover, a strong contrast between two neighbouring pixels would result in a
good sensitivity for small displacement amplitudes.
In some cases, the natural structure of studied material seems to be sufficient for
sensitive correlation results. Good examples for this are lattice structures of TiAl6V4
alloy produced by selective laser melting [232], or two-phase microstructure of such
as dual-phase steels [233], and Ni-based-superalloys [234–236], or layered
microstructure of ultrafine-grained Al laminates produced by accumulative roll
bonding (ARB) [40]. However, natural pattering of specimen surface can also have
some restrictions with respect to sensitivity of obtained displacement results
depending on preferred direction of natural pattern (such as layered arrangements of
two phases in a duplex stainless steel). If no natural contrast pattern can be used or in
order to circumvent difficulties with natural pattern, an artificial contrast pattern
should be applied to specimen surface. Artificial contrast patterns can be applied by
different approaches: (i) airbrush technology, (ii) grid technology, (iii) deposition of
particles and (iv) etching technique.
(i) Airbrush technology. Here, fine pulverized particles of a black paint where
sprayed on a white background or vice versa—so-called speckle paint pat-
tern. Using airbrush, a fine aerosol of the paint is obtained, where size of
paint droplets can be adjusted by a nozzle. Figure 5.23 shows an example for
black/white speckle paint patterns, and while the patterns of Fig. 5.23a, b are
unfavourable for DIC, Fig. 5.23c shows an optimal speckle paint pattern. In
Fig. 5.23a, the contrast between individual pixels/droplets is too low. The
contrast in Fig. 5.23b is appropriate; however, the image contains too largely
connected areas of black paint. In Fig. 5.23c, the black droplets are arranged
randomly, the contrast covers a wide dynamic range, and there are sharp
contrast changes between individual pixels. The speckle paint pattern is well
160 5 In Situ Techniques for Characterization …

Fig. 5.23 Speckle paint pattern for digital image correlation. a Poor contrast. b Good contrast,
however, too large regions with black contrast. c Optimum contrast for DIC. Reproduced from
Aramis [237]

suitable for wide range of specimen dimensions up to large-scale components


in combination with all optical microscopic image-recording techniques
(digital camera, high-speed camera, LDM, CLSM). However, the application
of paint deposit is restricted by the deformation behaviour of the investigated
material. Large deformation amplitudes can provoke damage and failure of
the paint layer leading, consequently, to a loss of correlation between ref-
erence image f and image of deformed state g. For larger deformation
amplitudes, the application of metal powder can be useful, since it has a
better stability.
However, for DIC analysis based on SEM images, the speckle paint pattern
technology is unfavourable and the other three techniques (ii) to (iv) are more
convenient.
(ii) Grid technology. Microgrids can be obtained on specimen surface either by
electron beam lithography [238] or by gluing nickel grids on specimen surface
deposited with gold (or other precious metal) [239]. The challenge of grid
technology is to find a compromise between line width and mesh size of the
grid regarding accuracy of measurements and size of observed field [238].
(iii) Deposition of particles. Luo et al. [240] developed a technology for
vapour-assisted remodelling of thin gold films. Ultrathin gold films (<20 nm)
are exposed to condensable vapours of volatile solvents at relatively low
temperatures (60–120 °C). Circular gold nanoparticles with diameters
between about 100–500 nm are formed depending on the initial thickness of
the gold layer and the vapour exposure. Scrivens et al. [241] improved and
enhanced the method developed by Luo et al. [240] on a wide variety of
substrate materials (e.g. glass, silicone rubber, epoxy resin, aluminium, sil-
icon, stainless steel) as well as different patterned metal films (e.g. chromium,
copper, silver, combined gold and silver) were tested successfully. Scrivens
et al. [241] obtained the application of this remodelling technique of thin
metal films particles’ sizes between 25 and 500 nm. Thus, the small particle
sizes in combination with a low subset size of about 20  20 pixels2 could
be reliable for spatial resolution of local deformation fields in the
sub-micrometre range (<500 nm). However, drawbacks of this technology
5.4 In Situ Full-Field Measurement Techniques 161

are obviously the connectivity of these nanoparticles to specimen surface


depending on evolution of a pronounced surface profile during mechanical
tests as well as the pattern stability during tests at elevated temperatures.
(iv) Etching technique. One of the best techniques to produce a randomly dis-
tributed and small-sized contrast pattern on the specimen surface is the
application of etching technique. Here, depending on the materials under
investigation, the applied etching solvent produces fine-etch pits on the
specimen surface, which are persistent during the entire plastic deformation
process even at higher temperatures.

5.4.1.2 Principles of Digital Image Correlation

As mentioned already above, the goal of DIC is to evaluate the apparent trans-
formation Ua of a certain area of interest (AOI) on a specimen during specific
loading conditions based on greyscale levels of reference image f and image of
deformed state g. Thus, at first the AOI has to be defined on specimen surface,
which is divided subsequently into an equidistant grid of measuring points (number
of points, distance of points) shown exemplarily in Fig. 5.24a. For each point of
virtual grid, the displacement between reference image f and image of deformed
state g is then computed yielding a full-field deformation measurement within AOI
(see Fig. 5.24b). The basic principle of DIC is tracking of greyscale distribution of
contrast pattern in both images.
Therefore, in reference image f a reference subset (also called as facet or ref-
erence matrix depending on applied software) with dimension of n  n pixels is
defined around a centred measuring point Pðx0 ; y0 Þ as demonstrated in Fig. 5.25.
The subset n  n (red square) is characterized by a specific greyscale distribution of
contrast pattern. The shape of reference subset can be either square ðn  nÞ or
rectangular ðm  nÞ depending on the applied deformation process. For large-scale
deformation, it seems suitable to use rectangular reference subsets m  n with
m [ n, the longer side m parallel to direction of large deformation. However, it is

Fig. 5.24 General principle of digital image correlation. a Definition of area of interest on the
specimen surface with subdivision into equidistant virtual grids (black squares). b Computed
displacement vectors (blue arrows) for each point of the virtual grid. Modified according to [242].
Permission of IOP Publishing
162 5 In Situ Techniques for Characterization …

Fig. 5.25 Subset definition and determination of displacement vector. a Definition of


square-shaped subset n  n around a centred measuring point Pðx0 ; y0 Þ in the reference image
characterized by unique greyscale distribution. b Computed displacement vector of subset in the
deformed image with P0 x00 ; y00 as the centred point of the target subset exhibiting the same
greyscale distribution as the reference subset. Reproduced according to [242]. Permission of
Elsevier

better to use a square or rectangular subset rather than an individual pixel, since a
subset of size n  n (or m  n with m [ n) is characterized by a more specific
arrangement of points of contrast pattern. This makes it better distinguishable from
other subsets. Therefore, a more unique identification in deformed image can be
achieved [242].
In the next step, in the image of deformed state, an analysed image region—
so-called search field—with dimensions N  N is defined. Using mathematical
correlation algorithm (see paragraph 5.3.1.3), the reference subset n  n with
characteristic contrast pattern of reference image is tracked within search field
N  N in image of deformed state. The subset n  n is then shifted to region with
most similar greyscale distribution. The coordinates of measuring point of target
subset are then P0 x00 ; y00 . Consequently, a corresponding displacement vector (blue
arrow) between reference subset and target subset is obtained. The procedure is
described in more detail by Sutton et al. [207, 242] or by Grediac and Hild [201].
Figure 5.25 illustrates both definition of reference subset and displacement of target
subset introduced by Pan et al. [242]. Figure 5.26 illustrates the greyscale distri-
bution as well as the definition of reference subset n  n and search matrix N  N
used by commercially available DIC software [243].
It becomes obvious—both from Fig. 5.25 as well as Fig. 5.26—that contrast
pattern within reference subset remains unchanged. For good correlation results, the
following conditions should be considered: (i) the search field N  N must be larger
than subset size n  n and should be large enough with respect to expected dis-
placements. Outside ðN  nÞ=2 no displacements Di and Dj can be registered. (ii) A
compromise has to be made on subset size with respect to resolution and
5.4 In Situ Full-Field Measurement Techniques 163

Fig. 5.26 Definition of


subset size n  n and search
field size N  N in the
reference image f (a) and in
the image of deformed state
g (b)

miscorrelations. As smaller the subset size as higher the resolution of calculated


strain field is. However, with decreasing subset size the contained lateral infor-
mation decreases as well.
Displacement mapping. Depending on deformation behaviour of investigated
material, a change of the shape of the reference subset in the image of deformed
state is supposable. Figure 5.27 shows another example [244], where not only the
reference subset displacement becomes obvious, but also the distortion of the target
subset, comparable to Fig. 5.25. However, neighbouring points in a reference
subset remain as neighbouring points in target subset assuming continuous defor-
mation of solid material. Thus, the coordinates of point Q xi ; yj in the reference
 
subset (cf. Fig. 5.25) can be tracked to point Q0 x0i ; y0j in the target subset [242].
The new positions x0i and y0i can be described according to (5.51) by so-called
shape functions or displacement mapping functions, U and V, respectively [242,
245–247].

x0i ¼ xi þ U xi yj and y0i ¼ yi þ V xi yj with ði; j ¼ M : M Þ ð5:51Þ

The shape functions U and V can be subdivided into (i) zero-order shape
functions, (ii) first-order shape functions and (iii) second-order shape functions.
Zero-order shape function is applied in case of rigid body translation [245] of the
reference subset and the target subset. That means the displacements are the same
on each point in the subset. However, the deformations of the target subset cannot
be explained by zero-order shape functions, solely. Therefore, first-order shape
functions [247] allowing translation, rotation, shear as well as normal strains
Ux ; Uy ; Vx ; Vy should be applied. Lu and Cary [246] introduced so-called
second-order shape functions Uxx ; Uyy ; Vxx ; Vyy ; Uxy ; Vxy . An overview of dis-
placement gradients at subset points caused by the components of first-order and
second-order shape functions was provided by Lu and Cary [246] and is summa-
rized in Fig. 5.28a. Special attention has to be paid on so-called large-scale
deformations, where easily large rigid body rotations and/or large deformations can
be present between reference and target subset, cf. Fig. 5.28b. In these cases, some
164 5 In Situ Techniques for Characterization …

Fig. 5.27 Displacement of the reference subset (red square, left) as well as the distortion of the
target subset (middle, right), whereas the greyscale distribution (speckle pattern) remains
unchanged. Reproduced from [244]

pixels of the reference subset can run out of the search area within the image of
deformed state leading, consequently, to a substantial decrease in the similarity
between the reference subset and the target subset.
Correlation algorithm. The basic idea of DIC is to evaluate similarity between a
reference subset and a target or deformed subset. This evaluation of similarity is
based on a correlation algorithm, which has to be defined in advance [242]. In
literature, different definitions of correlation algorithm can be found, which were
improved over years and are still under further development [242]. In general, the
correlation algorithm can be categorized into two groups of (i) cross-correlation
(CC) algorithm and (ii) sum of squared difference (SSD) algorithm (e.g. [248,
249]). The SSD algorithm is based on the minimization of the differences between
reference subset at point x, y in the image f and the point xi , yi shifted by i, j in the
image g [248]. The cross-correlation algorithm is based on the maximization of the
similarity between greyscale distribution in images f and g [248]. Pan et al. [242]
provide a comprehensive overview of available correlation algorithms. Thus, in
both categories standard CC, normalized CC (NCC) and zero-normalized CC
(ZNCC) as well as standard SSD, normalized SSD (NSSD) and zero-normalized
SSD (ZNSSD) can be distinguished. While SSD and CC use absolute values of
differences or similarities between greyscale levels, the ZNSSD and ZNCC algo-
rithms account for the global variation in the greyscale setting the average greyscale
difference or similarity to zero [248]. It should be noted that the CC criteria are
related closely to the SSD criteria and their derivation was described by Pan et al.
[242]. These authors concluded that ZNCC (or ZNSSD) correlation criterion
5.4 In Situ Full-Field Measurement Techniques 165

Fig. 5.28 Displacement gradients at subset points. a Influence of zero-order shape functions:
(i) rigid body rotation, (ii) rigid body translation. b Influence of first-order shape functions.
c Influence of second-order shape functions. Reproduced according to [246] and [242]. Permission
of Elsevier

provides the most robust noise-proof performance. Furthermore, this algorithm is


insensitive to offset and linear scale in illumination lighting. Therefore, the ZNCC
algorithm (or ZNSSD) is most commonly used criterion in commercially available
software packages. The algorithm can be expressed by the following complex
(5.52) [242]:
166 5 In Situ Techniques for Characterization …

8 h   i9
X
M M < f x i y j  f m  g x 0 y 0  gm =
X i j
CZNCC ¼ ð5:52Þ
i¼M j¼M
: Df  Dg ;

In (5.52), the parameters fm , gm , Df and Dg can be expressed as follows:

1 X
M X
M
fm ¼ 2
f xi yj ð5:53Þ
ð2M þ 1Þ i¼M j¼M

1 X
M X
M  
gm ¼ f x0i y0j ð5:54Þ
ð2M þ 1Þ2 i¼M j¼M
vffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
u M M
uX X
Df ¼ t
2
f xi yj  f m ð5:55Þ
i¼M j¼M

vffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
u M M h   i2
uX X
Dg ¼ t f x0i y0j  gm ð5:56Þ
i¼M j¼M

However, the other correlation criteria are either insensitive to linear scale in
illumination lighting, but sensitive to offset of lighting (NCC or NSSD) or sensitive
to all lighting fluctuations (CC and SSD).
Subpixel accuracy. Due to the fact that the smallest unit of a digital image is a pixel, the
calculated displacement of (5.52) will be an integer multiple pixel. Further
improvement of accuracy of calculated displacements can be achieved by (i) en-
hancement of resolution of CCD camera (or other imaging devices), (ii) employment
of a large magnification imaging system; and (iii) implementation of a subpixel reg-
istration algorithm into the calculation. Thus, variant (i) is a direct method and suitable
for a fixed measuring area. Variant (ii), however, is accompanied by a reduction of
measured area. Method (iii) is the best choice to improve measurement accuracy since
it is very effective [250]. Pan et al. [250] provide an overview of three different
methods available for subpixel registration algorithm: (i) correlation coefficient curve
fitting method, (ii) Newton-Raphson method and (iii) gradient-based methods. Here,
only the first subpixel registration algorithm will be described in more detail. The
Newton-Raphson method was firstly described in 1989 by Bruck et al. [251] and was
reviewed in [245, 247, 250]. The gradient-based method was firstly introduced by
Davis and Freemann [252] as a method of optical flow.
The correlation coefficient curve fitting method [250] uses a two-dimensional
quadratic function of correlation coefficients C xi ; yj to describe the fitting surface
of a pixel P with the coordinates ðx; yÞ and its eight neighbours Pij with coordinates
xi ; yj as shown in Fig. 5.29 [250]:
5.4 In Situ Full-Field Measurement Techniques 167

Fig. 5.29 Schematical


illustration of the subpixel
correlation algorithm.
Modified according to [250].
Permission of IOP Publishing

C xi yj ¼ a0 þ a1 xi þ a2 yj þ a3 x2i þ a4 xi yj þ a5 y2j ð5:57Þ

In order to evaluate the displacement u and v, a set of linear equations has to be


solved [250]:

@C ðx; yÞ
¼ a1 þ 2a3 x þ a4 y ¼ 0 ð5:58Þ
@x
@C ðx; yÞ
¼ a2 þ 2a5 y þ a4 x ¼ 0 ð5:59Þ
@y

With (5.58) and (5.59), the maximum correlation coefficient can be determined:

2a1 a5  a2 a4 2a2 a3  a1 a4
x¼ y¼ ð5:60Þ
a24  4a3 a5 a24  4a3 a5

The displacement is then calculated:

u ¼ x  x0 and v ¼ y  y0 ð5:61Þ

Here, x0 and y0 are the subset centres and u and v the displacements in x and
y directions, respectively.

5.4.1.3 Computation of 2D Strain Values

Before going into detail, how two-dimensional strain values can be calculated from
measured displacements, some general remarks concerning strain are provided.
First of all, it has to be distinguished between rigid body translations and strains
resulting from deformation. A rigid body translation or displacement occurs if the
distance between all points belonging to the surface element under investigation
remains unchanged. As soon as the distance between individual points has changed,
a deformation occurred leading to strain values [253].
168 5 In Situ Techniques for Characterization …

The term “strain” describes the displacement of individual points belonging to a


line with respect to a reference length (cf. Fig. 5.30a) and can be, therefore, used as
a measure of deformation. According to amount of resolved strains, different strain
(or deformation) theories can be applied: (i) small strain (or deformation) theory,
(ii) large strain theory and (iii) large rotation theory. The small strain theory allows
both small strains and rotations occurring in the material. Thus, the continuum
configurations of the non-deformed and deformed material can be interpreted to be
identical. The large strain theory is applied to large strain deformations such as
elastomers, fluids, biological soft issues and plastically deforming materials. Here,
the configurations of non-deformed and deformed material have to be regarded
separately. The large rotation theory is used for deformations with small strains but
large rotations. According to these theories, different strain measures can be
regarded: (i) stretch (extension) ratio, (ii) engineering strain, (iii) logarithmic (or
true) strain and (iv) Green’s strain [253].
(i) The stretch ratio k is given by elongation of a line element dX to dx and is
expressed by the ratio of the final length l to the initial length L of dX (see
Fig. 5.30a):
ldx
k¼ ð5:62Þ
LdX

(ii) The engineering strain eeng is given by the ratio of change of length DL per
unit of original length L:

DL l  L
eeng ¼ ¼ ð5:63Þ
L L

The relation between stretch ratio k and engineering strain eeng is given by

lL
eeng ¼ ¼k1 ð5:64Þ
L

(iii) Logarithmic strain / (or true strain etrue ) is obtained by integrating incre-
mental strain element de ¼ dl=l:

Z Zl
@e
@e ¼ leading to / ¼ etrue ¼ lnð1 þ eeng Þ ð5:65Þ
l
L
5.4 In Situ Full-Field Measurement Techniques

Fig. 5.30 Definition of strain variables for digital image correlation. a Translation and strain of a line element dX. b Two-dimensional deformation of a
surface element (unit square) including shear angle description. c Definition of the coordinate systems. Modified according to [237]
169
170 5 In Situ Techniques for Characterization …

(iv) Green strain eG is used in the small strain theory and is defined as follows:
 
1 l 2  L2 1
eG ¼ 2
¼ k2  1 ð5:66Þ
2 L 2

The quantitative description of deformation of a surface element of a specimen


needs introduction of deformation gradient tensor F:

dx ¼ F  dX ð5:67Þ

The deformation gradient tensor F describes the transformation of a line element


dX into a line element dx (see Fig. 5.30a), where both line elements connect same
material coordinates. However, the deformation gradient tensor F includes both
rotation and displacement (stretch) components of deformation of a surface ele-
ment. Hence, the deformation gradient tensor can be split into rotation tensor R and
right-hand displacement tensor U (or left-hand displacement tensor V) [237]:

F ¼ R U or F ¼ V R ð5:68Þ

The displacement tensor U of a surface element can be given as follows [237]:


0 1
  du x du x þ du y
U11 U12
U¼ ¼ @ du dþxdu dx A
duy ð5:69Þ
U21 U22 x y
dy dy

Analogue to the displacement tensor, the strain tensor can be determined [237]:
    @ux þ @uy
!
@ux
e11 e12 exx exy @x @x
e¼ ¼ ¼ @ux þ @uy @uy ð5:70Þ
e21 e22 eyx eyy
@y @y

Here, exx and eyy are normal strain, and exy and eyx are shear strain components.
Consistent to the definition of normal and shear stress, the normal strain is per-
pendicular to the face element and shear strain parallel to it.
Consequently, the normal strain in x and y directions—exx and eyy —is deter-
mined in agreement with Fig. 5.30b as follows [237]:

DL l  L length ab  length AB @ux @uy


exx ¼ ¼ ¼ ¼ and eyy ¼ ð5:71Þ
L L length AB @x @y

The changes in the shape of a surface element are described by the shear strain
exy . For the geometric interpretation of the shear strain exy , the shear angle cxy is
used. According to Fig. 5.30b, cxy is defined by the change of the angle between AB
and AC. Thus, the shear angle consists of two parts a and b. The values for a and b
can be different.
5.4 In Situ Full-Field Measurement Techniques 171

@uy @ux
cxy ¼ a þ b ¼ þ ð5:72Þ
@x @y

For small strains, the strain tensor can be written as follows:


   1

exx exy exx 2 cxy
e¼ ¼ 1 ð5:73Þ
eyx eyy 2 cyx eyy

However, the assumption exy ¼ 2cxy is valid in the elastic strain (small strain)
theory only and cannot be applied to strain calculations during plastic deformation.
According to the above-provided arguments, it becomes obvious that (i) a sym-
metric displacement tensor realizes only a parallelogram in the local deformation
field (cf. Fig. 5.30b) and (ii) the orientation of the parallelogram to the original
coordinate system (X, Y) is fixed, and, consequently, rotation of points cannot be
described by the displacement tensor.
Both the rotation and the direction of the rotation of points of the surface element
are described by the rotation tensor, which is part of the transformation gradient
tensor F as shown in (5.68). In order to interpret rotations and directions, therefore,
two coordinate systems have to be introduced: (i) coordinate system of the
non-deformed (initial) point Pu;i and (ii) coordinate system of the deformed point
Pv;i (i is an index for different points). The correlation between these two coordinate
systems can be described as follows [237]:

Pv;i ¼ ui þ F Pu;i ð5:74Þ

with ui as rigid body translation. Figure 5.30c shows the correlation between both
coordinate systems. Thus, finally three coordinate systems have been taken into
account: (i) global (macroscopic) coordinate system ðx  yÞ, which is used for the
definition of coordinates for all points Pi , (ii) local coordinate system of points in
non-deformed state ðx0  y0 Þ, which is placed parallel to the global coordinate
system ðx  yÞ, and (iii) the local coordinate system of points in deformed state
ðx00  y00 Þ, which indicates the direction of strains. The coordinate system ðx00  y00 Þ
is independent of rigid body rotations and translations and reflects the deformation
introduced by the displacement tensor U. Thus, the x00 -direction is the direction of
strain exx and the y00 -direction the direction of strain eyy .
According to this, the calculated strain values exx and eyy are dependent on
chosen coordinate system. In order to eliminate this disadvantage, major and minor
strains can be calculated. Therefore, the symmetric matrix of the displacement
tensor U is transformed to the main diagonal form, and the eigenvalues k1 and k2 of
the main diagonal can be calculated as follows:
rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
exx þ eyy e þ e 2  
xx yy
k1;2 ¼ 1þ   exx  eyy  e2xy ð5:75Þ
2 2
172 5 In Situ Techniques for Characterization …

According to the chosen strain measure, the calculated stretch ratios k1 and k2
can be transformed into corresponding strain values. The major strain (e1 or /1 ) is
then defined as the larger eigenvalue and the minor strain (e2 or /2 ) as the smaller
eigenvalue. The corresponding vectors of the eigenvalues define the direction of
major and minor strain. These calculated strain values are independent of the
coordinate system and can be used universally.
Along with the coordinate independent values of major and minor strain,
effective strains could be of interest as well. Effective strains can be calculated
according to Von Mises or Tresca using the following equations based on true
strain etrue eigenvalues of the displacement tensor U [237]: (i) equivalent strain
according to Von Mises by (5.76)
rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
2 2
evM ¼ e þ e22 þ e23 ð5:76Þ
3 1
rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
 
exx þ eyy exx þ eyy 2
with e1;2 ¼ 2 2  e xx  e yy  e 2
xy

and (ii) equivalent strain according to Tresca by (5.77):

evT ¼ jejmax ð5:77Þ

5.4.1.4 State of the Art in Materials Engineering

In field of materials research, a series of optical methods was established in the


1970s and 1980s for measurements of macroscopic properties such as displace-
ments and strains. These methods included holographic (e.g. [254]), speckle (e.g.
[255]) and Moiré interferometry (e.g. [256, 257]), respectively, allowing both
in-plane and out-of-plane displacements. The holographic interferometry is based
on analysis of interference fringes produced by superimposing reference hologram
image on specimens subjected to subsequent deformation, which is used by
Dudderar et al. [254] for investigation of size of plastic zone in front of a stress
concentration (notch) during cyclic loading. Leendertz et al. [255] showed that
speckle interferometry, which is based on relative phase changes due to interference
of two coherent light fields of random phase and amplitude, is capable to visualize
normal displacement component or one component of in-plane surface displace-
ment with high sensitivity over a large scale of the specimen surface. The Moiré
interferometry is based on grating structures on specimen surface, where super-
position of reference pattern of non-deformed state to pattern in deformed state
resulting in so-called Moiré fringe patterns [256, 258] is used. All methods—
holographic, speckle and Moiré interferometry—can also be applied for out-
of-plane strain measurements using a multicamera setup. However, for accurate
in-plane and out-of-plane measurements of small local surface strains, a highly
temporally and thermally stable optical setup is necessary, which is one of the main
5.4 In Situ Full-Field Measurement Techniques 173

disadvantages of these techniques. In addition, all these techniques have their own
restrictions and limitations. One of the important drawbacks of all interferometric
techniques is the laborious and time-consuming analysis of the fringe patterns
resulting in a high demand for automated pattern recognition and analysis.
In field of photogrammetry (e.g. [259, 260]), significant progresses were
obtained developing similar technique to digital image correlation (DIC), which
dates back to the mid-1970s. Thus, Ackermann et al. [261] described for the first
time a method based on matching of least squares windows aiming high-precision
parallax assessment, point transfer as well as point measurement. Furthermore, the
first online application of digital image correlation for conventional photogram-
metric measuring tasks was reported by implementation of a CCD video camera in
an analytical plotter.
At the end of the 1980s and the beginning of the 1990s, a large number of
automated, non-contacting optical methods were developed for measurements of
displacements and strains—the invention of the digital image correlation (DIC) in
materials research. Thus, in 1983, Sutton et al. [207] and Chu et al. [208] developed
digital image correlation as a technique with subpixel accuracy [251] to measure
displacements of objects under loading conditions. The coarse-fine search technique
developed by Sutton et al. [207] was refined by Bruck et al. [251] introducing a
special method of partial differential corrections, which resulted in shorter com-
putation time. Furthermore, not only displacements can be calculated, but also
displacement gradients.
At same time, automated grid technologies (e.g. [262, 263]) were established.
The grid was either a regular array of well-defined equidistant spots [262] or
crossed grating pattern [263]. Amar et al. [238] introduced a special microgrid
technology developed for in situ testing in SEM in combination with local strain
field measurements using DIC. The microgrid was created on the specimen surface
by electron beam lithography. The width of the grid lines was about 0.25 µm, and
distance between grid lines is about ten times the line width. The microgrid tech-
nology was even improved by Biery et al. [239] using gold deposition on a glued
nickel grid at specimen surface for in situ SEM investigations, which was much
faster and less expensive than electron beam lithography. Biery et al. [239] tested
differences between grids well-aligned with the scanning direction of the electron
beam and non-aligned grids. It was shown that the best resolution was obtained
when the boundaries of the grid markers were aligned by 45° with respect to the
scanning direction. Although a high accuracy of strain measurements can be
guaranteed by the application of a grid pattern on the specimen surface, the distance
between grid lines or other markers restricts the resolution of strain measurements
[239].
In the following years up to now, both digital image correlation and grid tech-
nology were subjected to large development and improvement. In particular, the
correlation algorithm was improved with regard to accuracy and detection speed;
see Hung et al. [264]. Efstathiou et al. [265] gave a short overview of evolution and
application of both techniques in the years from the end of the 1990s up to 2010.
Thus, grid technology was applied in combination with SEM imaging on different
174 5 In Situ Techniques for Characterization …

types of materials varying from steel (e.g. [266–270]) via copper and (e.g. [271,
272] and iron polycrystals (e.g. [273]), respectively, up to zirconium and titanium
aluminides (e.g. [274]. Digital image correlation technique was applied either in
combination with optical (e.g. [40, 41, 232, 265, 275–283]) or SEM-based imaging
technologies (e.g. [210, 213, 215, 284–287]) on various kinds of materials (alu-
minium alloys, copper, various kinds of steel, cast iron, titanium and titanium
alloys, metal matrix composites, ultrafine-grained materials, additive manufactured
materials). In Appendix, Table A5.2 provides a chronological overview of appli-
cation of DIC in combination with OM and SEM in field of Material Science and
Engineering since beginning of the year 2000. The overview is separated in the
different research fields such as (i) plasticity, (ii) fatigue, (iii) fracture mechanics
and (iv) modelling. In addition, applications of DIC in combination with AFM and
FIB as well as application of digital volume correlation using µCT are included.
Numerous investigations in field of plasticity have been performed to study
heterogeneous deformation at grain scale measuring in-plane strain distribution in
mainly cubic materials—except [265] and [274]—with average grain sizes varying
from 10 µm [277] up to 1 cm [271]. Thus, heterogeneity of deformation is a
microstructure-related problem since microstructural features such as grain orien-
tation, grain size, grain shape, grain boundaries and grain–grain interactions are
responsible for strain localizations. The major results can be summarized as
follows:
• The heterogeneity of plastic deformation on grain scale originates mainly from
two types of grain deformation behaviour: Type I are individual grains, which
deform homogenously according to their crystallographic orientation, whereas
type II are related to a cluster of grains exhibiting homogenous strain.
• Strain localization seemed to start at grain boundary triple points or at grain
boundaries inclined at 45° with respect to the loading axis.
• Microbands are found in narrow portion of grains, and macrobands encom-
passing several grains are observed at larger deformation.
• Both grain shape and microtexture have significant influence on strain hetero-
geneity. Thus, large grain size is conducive for strain localization since less
grain boundaries act as barriers for dislocation glide.
• In metal matrix composites (MMCs) based on aluminium reinforced with Al2O3
[284], it was found that the deformation is localized in narrow bands in ductile
matrix and bands are inclined to loading axis by about 45°. Bands initiated
preferentially in the Al matrix at the interface of large Al2O3 particles lead to
local strain maxima.
The DIC method in combination with optical registration of images based on
speckle patterns has been further improved from macroscopic investigations to
studies on a multiscale level. Caroll et al. [288] provided a so-called high-resolution
ex situ DIC with optical microscopy. Caroll et al. [288] argued that a fundamental
restriction of all in situ techniques is their limitation to a single field of view. Thus,
aiming on a spatial resolution of the DIC measurements on subgrain level in situ
5.4 In Situ Full-Field Measurement Techniques 175

Fig. 5.31 Results of DIC in combination with optical images. a Low-resolution DIC—strain field
eyy obtained on a single image of the whole area of interest taken at low magnification (5 ).
b High-resolution DIC—strain field of eyy with overlaid grain boundary structure of the same AOI
shown in (a). However, here the reference images and images of deformed states are stitched of
316 individual images of 31  magnification taken ex situ. Note that the subset size in (b) is much
smaller (14 µm) than the one used in (a) (89 µm), which results in higher resolution fields with
subgrain level accuracy. Reproduced from [288]. Permission of Elsevier

techniques are limited to observations of small number of grains only. Thus, Caroll
et al. [288] proposed a method of so-called interrupted monitoring, where specimen
was imaged before and after mechanical test allowing the capture of multiple image
regions at desired magnification. The individual image regions can be stitched
together to provide high-resolution DIC data over a larger number of grains. The
stitching procedure was applied either to images before DIC or to DIC strain field
images as shown in Fig. 5.31. In the first case, the DIC resulted in artificial bands of
high and low strain due to stitching inaccuracies. Furthermore, ex situ DIC strain
measurements were linked to microstructure and crystallographic orientation by
EBSD measurements on identical area of interest marked by Vickers indentations in
all four corners of the AOI yielding an excellent alignment of both fields.
Efstathiou et al. [265] proposed an analogous method for determination the size
of a representative volume element of plastic strain accumulation in Ti. Since DIC
does not possess an inherent length scale, Efstathiou et al. [265] developed a
technique allowing multiscale strain investigations using DIC measurements based
on different optical magnifications. By assembling numerous images at higher
magnifications, the same field of view is encompassed as observed for lower
magnifications. It was demonstrated impressively on polycrystalline titanium that
the application of this technique provides the possibility to describe the strain
distribution on a grain level for a large number of grains and enables so-called
full-field measurements.
Abuzaid et al. [289, 290] reported the application of this technique for
description of plastic strain localization and fatigue microcrack formation in a
nickel-base superalloy (Hastelloy). Here, slip transmission and plastic strain
accumulation at grain boundaries were studied on high-resolution level for an
aggregate of 600 grains and annealing twins. It was an inverse relation shown
between the determined residual Burgers vector (residual dislocation left in the
176 5 In Situ Techniques for Characterization …

grain boundary due to slip transmission) and the magnitude of strain crossing the
grain boundary.
Quite recently, Eskandari et al. [291] described application of DIC using speckle
pattern in combination with macroscopic tensile tests at different temperatures and
strain rates on a TWIP steel. It is shown that band-like strain localizations occurred
on a macroscopic scale along the gauge length attributing them to stress-assisted
e-martensite formation or stress-assisted twinning.
SEM-DIC. The combination of DIC with in situ deformation in scanning electron
microscope—further called SEM-DIC—provides a powerful tool for measurement
of in-plane displacement fields in combination with characterization of
microstructural processes at high lateral resolution [271, 292]. The combination of
SEM-DIC with electron backscatter diffraction (EBSD) measurements opens pos-
sibility to correlate directly in situ deformation behaviour on scale of microstructure
with underlying crystallography of material [292]. However, it also holds some
challenging tasks regarding both technical requirements (stability of electron beam,
image drift, specimen charging, image distortion, dwell time) and high require-
ments on contrast pattern at specimen surface. Sutton et al. [215] presented a
detailed imaging study using several SEM systems investigating the image errors
occurring in scanning electron microscopy. It was confirmed that image errors are a
generic feature of SEM since image shifts occur at random positions during
imaging process [293]. Due to random nature of image shifts, these authors report
that image drifts have an influence on accuracy of image-based deformation mea-
surements. However, the effect can be minimized through implementation of an
image integration procedure without increasing overall scan time. Thus, Kammers
et al. [292], [294] and Gioacchino et al. [295] stated that SEM image noise can be
reduced by special settings of electron microscope: (i) large spot size or beam
current, (ii) longer dwell time and (iii) multiple image integrations. Although these
suggestions were obtained on a SEM with tungsten cathode, they are also valid for
FE-SEM, since here, due to field-emission cathode, overall noise is already smaller
than for tungsten cathode [295].
In some cases, SEM-DIC is also performed as a type of interrupted monitoring,
which means stepwise deformation outside SEM in a classical material testing
machine and capturing high-resolution images of deformed states using SEM.
The above-described technique of speckle pattern as contrasting method on the
specimen surface for the macroscopic or multiscale DIC is not applicable in the
SEM [239]. Moreover, other useful information (e.g. changes in the microstructure)
may be covered or even hidden by the speckle pattern [239]. The grid technology
has disadvantage that grid step should be large enough in order to visualize
underlying microstructural features.
The scanning electron microscope itself provides micrographs with greyscale
information both applying secondary electron (SE) and backscattered electron
(BSE) contrast. However, the application of the SE contrast is very limited due to
the high sensitivity of secondary electrons for surface topography leading to pro-
nounced changes in greyscale contrast during deformation. The application of BSE
5.4 In Situ Full-Field Measurement Techniques 177

contrast is limited as well, since orientation changes, which may occur during
plastic deformation, provoke significant changes in the greyscale intensities. Thus,
application of DIC to SEM micrographs is a challenging task since a randomly
distributed, high-contrast pattern on specimen surface is necessary for a good
correlation of SEM micrographs. In the past, different methods were tested already
for high-quality and high-resolution correlation results. Such methods are, for
instance, the microlithography [274], etching methods [213] or the application of
colloidal, fine-dispersed, nanosized particles (SiO2 [296], Au [295], Pt [218, 297])
onto specimen surface. Kammers and Daly [298] gave an overview of different
patterning techniques applied for SEM-DIC ranging from focused ion beam
(FIB) technique over nanoparticle patterning up to electron beam lithography
accounting for both advantages and drawbacks of individual techniques. Thus, FIB
patterning allows an accurate control of pattern localization, has a good repro-
ducibility and is independent of substrate. However, it is time-consuming and quite
expensive, and beam damage can be caused on the surface. In contrast, the
nanoparticle patterning is fast and inexpensive. However, the control of pattern
localization as well as reproducibility of results is difficult.
In the last years, several investigations have been performed using in situ
deformation tests using SEM-DIC. It was shown that local strain fields can be
calculated with a lateral resolution in the range of several micrometres. Materials
under investigation were mostly various types of steel (e.g. low-carbon martensitic
steels [299], austenitic stainless steel [295, 300], duplex steels [269, 277],
dual-phase steels [233, 296, 301–305], cast iron (e.g. [306]) or other materials like
aluminium (e.g. [307]), Ni–Ti (e.g. [308]) or nickel-base superalloys (e.g. [236,
309, 310]).
Low-carbon martensitic steels. Na et al. [299] studied the evolution of strain fields
in lath-type martensitic steel under tensile loading up to 10% of elongation. Etched
specimen surfaces (2% Nital) were used for the DIC calculations providing good
greyscale contrast. The results revealed strain localizations due to grain interactions.
Thus, pronounced subgrain formation within lath blocks was observed and cor-
roborated by local misorientation measurements using EBSD.
Dual-phase steels. Ghadbeigi et al. [233, 301] reported on in situ tensile tests in the
SEM using DIC to study initiation and evolution of damage in high-strength
low-alloyed DP600 and DP1000 steels. DIC has been performed on polished and
etched specimen surfaces without any additional patterning by using microstruc-
tural features appearing as dark ferritic phase with embedded martensitic islands.
The investigations showed strain localization within bands inclined at 45° with
respect to loading direction. In addition, martensitic regions exhibited a large strain
and damage occurred by fracture of martensitic islands. Furthermore, it was found
that damage occurred due to both coalescence of voids and formation of microc-
racks. The nucleation of microvoids was caused in large ferritic grains due to
decohesion of submicron carbides as well as MnS inclusions from ferritic matrix.
Decohesion at ferrite/martensite interface was never observed.
178 5 In Situ Techniques for Characterization …

Joo et al. [302] described the evaluation of local strain at nanometre scale using
nanosized silver dot patterns for SEM-DIC using tensile tests. The silver spot
patterns of different dot sizes and distances are obtained by deposition of thin silver
layers with different thickness (25, 50, 75 and 150 Å) and subsequent annealing in
vacuum at 300 °C for 5 min (comparable to the techniques developed by Luo et al.
[240] and Scrivens et al. [241]). Size and spacing of nanodots varied from 23 nm to
189 nm and from 20 nm to 135 nm, respectively, and can be controlled easily by
parameters of heat treatment. Moreover, silver nanodots showed an excellent
connectivity to specimen surface over whole deformation process leading to good
correlation results for martensitic islands with dimensions of 1–3 µm within
dual-phase steels.
Marteau et al. [304] performed DIC investigations based on microlithographic
grid technology on ferritic and dual-phase steels for better understanding of evo-
lution of strain heterogeneities between ferritic and ferritic/martensitic grains,
respectively. The average grain size of ferritic phase of investigated steels was about
20 µm for ferritic steel and 10 µm in dual-phase steel with a mean grain size of the
martensitic islands between 2 and 3 µm. Thus, the used size of the Au grid was
chosen with 1 µm according to the average grain sizes and the grid width was
varied between 0.25 and 0.5 µm. The results of the microtensile tests revealed good
correlation for lower strain values (<4% of elongation). At higher strain values,
pronounced surface topography variations, crack initiation as well as variations in
contrast and brightness caused by the deformed Au grid disturbed correlation
algorithm. Nevertheless, calculated strain fields in ferritic as well as dual-phase
steels revealed formation of slip bands with an angle of 45° with respect to tensile
loading axis with onset of plastic deformation, which becomes more intense with
ongoing deformation. The ferritic grains exhibited pronounced plastic strain values
varying between 50 and 150% of average local strain values. In addition, these high
strain values were independent of individual grain size, shape or orientation and
were correlated more closely to surrounding grain arrangement. Moreover, these
investigations revealed that martensitic islands undergo a pronounced plastic
deformation, which was, however, less than that of ferritic grains.
Tasan et al. [305] also investigated microstructural banding effects in dual-phase
steels during in situ tensile tests using DIC based on natural features of
microstructure. Two different banding structures were analysed: (i) ferritic grains
surrounded by banded martensitic structure and (ii) martensitic bands replaced by
pearlitic bands after special heat treatment. Similar to Ghadbeigi et al. [233, 301]
and Marteau et al. [304], the intragranular formation of slip bands under 45°
inclination was observed early in deformation process. Furthermore, it was shown
that continuously banded martensitic structure surrounding ferritic grains acts as
obstacle on further propagation of these slip bands leading to crack initiation at
interphase boundaries ferrite/martensite. Similar behaviour was found for banded
pearlitic microstructure. However, strain heterogeneities started to develop at dis-
continuities in pearlitic bands. Moreover, in [296, 311] it was observed that strain
localization was affected strongly by specific characteristics of individually banded
microstructure of dual-phase steel. Thus, strain heterogeneity varied significantly
5.4 In Situ Full-Field Measurement Techniques 179

Fig. 5.32 High-resolution SEM-DIC on dual-phase steel DP800 at two different average
equivalent Von Mises strains. a Band contrast map of EBSD measurement. b evM = 0.061.
c evM = 0.096. Reproduced from [296]. Permission of Elsevier

depending on distribution of martensitic phase. To resolve local strain fields even


within very thin martensitic islands, DIC was performed based on contrasting the
specimen surface by nanometre-sized (11 nm ± 4 nm) SiO2 particles (see
Fig. 5.32) [296, 311].
Nickel-base superalloys. SEM-DIC during tensile tests was also performed on
polycrystalline Ni-base superalloys (e.g. Rene 88TD [234, 235]) or single crystals
[236]. Tschopp et al. [234] used Pt nanoparticles deposited on specimen surface by
a laser ablation process called as “through thin film ablation” (TTFA). Stinville
et al. [235] further improved resolution of SEM-DIC using the big advantage of this
type of material—the natural contrast pattern provided by the intrinsic
microstructure consisting of two populations of c′-precipitates—secondary and
tertiary precipitates. While the secondary precipitates are the larger ones with 100—
200 nm, the tertiary are several nanometres in diameter only. These intrinsic
microstructural features were revealed by chemical–mechanical polishing at sub-
sequent heating at 350 °C for several minutes. The obtained pattern was stable
during entire deformation process even up to test temperatures up to 650 °C due to
stability of c′-precipitates. Using this natural contrast pattern, a subgrain resolution
of DIC calculations was obtained. Significant strain localization in this alloy was
observed near twin boundaries during plastic deformation [235].

5.4.2 Temperature Fields

The measurement, analysis and interpretation of temperature fields are of strong


interest in different areas of technology such as (i) medicine, (ii) civil engineering,
(iii) military and (iv) Materials Science and Engineering. In the field of Materials
Science and Engineering, temperature fields are, among others, of interest during
mechanical loading of different kinds of materials. Thus, physical phenomena such
as dynamic strain ageing (e.g. PLC bands in various kinds of metallic materials) or
phase transformation (e.g. in SMA) under monotonic mechanical loading are
related strongly to local changes in temperature field. In addition, deformation
180 5 In Situ Techniques for Characterization …

processes and crack initiation and propagation occurring during cyclic loading yield
local temperature increases. Hence, the infrared thermography is a powerful tool for
full-field measurements of local temperature changes occurring during different
kinds of mechanical loading of metallic materials. In the following, fundamentals of
infrared thermography, reconstruction of heat sources and energy dissipation as
well as application of infrared thermography in field of Materials Science and
Engineering are discussed.

5.4.2.1 General Aspects of Infrared Thermography

The infrared thermography (IR–TG) is a contactless, visual method for temperature


measurement of various kinds of objects, for instance, well known in civil engi-
neering as building thermography. However, IR–TG can also be used as an in situ
characterization technique in field of research and development in material sciences.
Thus, both microstructural and damage processes can be followed by IR–TG since
local changes in microstructure like plasticity or crack initiation and crack propa-
gation are related to local temperature increase and evolution of temperature fields.
Thermographic measurements use infrared radiation (IR), which is among vis-
ible light, radio waves or X-rays part of electromagnetic radiation with wavelength
in range between 0.78 and 14 µm. According to the wavelength, three different
ranges of IR can be separated: (i) short wave infrared (SWIR: 0.78–2 µm),
(ii) middle wave infrared (MWIR: 2–5 µm) and (iii) long wave infrared (LWIR: 5–
14 µm). IR is emitted by all objects at temperatures above absolute zero due to
vibrational movement of molecules/atoms. Thus, surface temperature of a body is
correlated directly with intensity of emitted radiation and its spectral composition.
This is described well by Planck’s radiation law. Thus, (i) amount of emitted IR is
increasing, (ii) spectral composition of IR is changing, and (iii) IR is shifted to
smaller wavelength with an increase in object temperature. The capability of a body
to emit IR is so-called emissivity e. However, IR has similar properties as visible
light (except wavelength)—(i) propagation in all directions, (ii) propagation with
velocity of light, and (iii) all optical laws as reflection, refraction and transmission
are valid. Therefore, in addition to emissivity e, objects can be characterized by
further properties regarding incident radiation like absorption a, reflection . and
transmission s. Each of these properties can have a value between zero and unity
resultant in total radiation law:

1 ¼ aþ.þs ð5:78Þ

The ideal case is a perfect black body, which has an emissivity of 100%.
According to the Kirchhoff’s law, the amount of radiation emitted and absorbed by
an object is the same. That means, a perfect blackbody emits and absorbs 100% of
radiation and there is no reflected (. = 0) and transmitted (s = 0) radiation. Thus, a
good emitter (e = 1) is a poor reflector and vice versa a good reflector (. = 1) is a
poor emitter. The human skin has a very high emissivity, which is with e = 0.98
5.4 In Situ Full-Field Measurement Techniques 181

very close to the perfect blackbody and makes it, therefore, a perfect measuring
object for IR–TG. All other materials have much less emissivity. In addition,
parameters like chemical composition, surface roughness, field of view as well as
the temperature of the measuring object itself have a significant influence on the
emissivity value of the object under investigation. Thus, the emissivity of
non-metallic materials has a relatively high (0.5–0.9) and constant value over a
wide range of wavelength and is independent of the surface roughness. In contrast,
the emissivity of metallic materials is quite low: it decreases significantly with
increase in wavelength and depends strongly on the surface roughness. As higher
the surface roughness as higher the emissivity is. Contrary, a polished surface of
metallic specimen has a quite low emissivity due to directional reflection of IR.
Thus, for exact determination of surface temperature of metallic materials, the
emissivity should be increased by black thermo-lack or graphite spray.
The infrared radiation of a measuring object detected by thermo-camera is
influenced not only by its own properties. Moreover, the detected intensity of
radiation significantly depends on properties of atmosphere and other environ-
mental conditions in surrounding of the object. Thus, IR can be attenuated in
atmosphere due to absorption by gases or scattering at particles. Therefore, IR–TG
is applied in so-called atmospheric windows enabling highest transmission for IR.
Two atmospheric windows are separated according to the wavelength: (i) middle
wave infrared and (ii) long wave infrared. Other environmental conditions
influencing IR–TG measurements are emitted IR from background, emitted IR from
additional sources in surrounding as well as emitted IR from atmosphere. Thus, the
overall radiation intensity U detected by thermo-camera is the sum of radiation
intensities of measuring object UO and measuring section UM [312]:

U ¼ UO þ UM ð5:79Þ

The radiation intensity of measuring object UO consists of three parts: (i) emitted
intensity Ue , (ii) transmitted radiation Us and (iii) reflected radiation U. . The three
radiation parts can be calculated according to the following equation [312]:

ði) Ue ¼ e  UðHO Þ; ðiiÞ Us ¼ s  UðHBG Þ; and ðiii) U. ¼ .  UðHU Þ ð5:80Þ

Here, HO is the temperature of measuring object, HBG the temperature of


background and HU the temperature of environment. Assuming that the measured
object is a non-transparent body with s ¼ 0 and e þ . ¼ 1, the radiation intensity of
the object can be calculated as follows (Fig. 5.33) [312]:

UO ¼ e  UðHO Þ þ ð1  eÞUðHU Þ ð5:81Þ

The radiation of measuring section UM is the sum of attenuated radiation of the


object UO and the radiation of the measuring section itself. Thus, UM is calculated
analogous to (5.81) [312]:
182 5 In Situ Techniques for Characterization …

Fig. 5.33 Schematic illustration of factors influencing the overall detected IR at the thermo-
camera. Modified according to Infratec [312]. With courtesy of Infratec

UM ¼ sp  UO þ 1  sp UðHP Þ ð5:82Þ

Using (5.81) and (5.82), the detected infrared radiation intensity at the
thermo-camera can be described by the following expression, which is known as
the basic equation of thermography [312]:

UM ¼ sp  e  UðHO Þ þ ð1  eÞ  UðHU Þ þ 1  sp  UðHP Þ ð5:83Þ

According to (5.83), the temperature of the measuring object is determined by


 
1 UM  ð1  eÞ  UðHU Þ
HO ¼ U ð5:84Þ
e

Thus, necessary requirements for an exact temperature measurement using IR–


TG are the determination of the emissivity value of the object as well as the
knowledge of the environmental conditions.
Contact-free temperature measurements based on detection of infrared radiation
require special detectors, which are capable to transform heat radiation into an
electric signal. Here, several types of detectors are known—e.g. (i) uncooled
microbolometers as thermal detectors and (ii) quantum detectors made of materials
like InSb, InGaAs or PtSi. The microbolometers are based on measurement of
changes in electrical resistivity caused by temperature increase due to IR.
Therefore, materials with a strong temperature-dependent electric resistivity as well
as an optimum ratio of heat capacity to heat conduction are chosen for
5.4 In Situ Full-Field Measurement Techniques 183

microbolometers. This detector type is less expensive, however, also slower and
less sensitive than quantum detectors. The operation of quantum detectors is based
on the change of electronic states in a crystal structure due to incident photons. In
contrast to microbolometers, the quantum detectors have to be cooled, which make
them much more expensive.
In general, thermo-cameras can be separated into two categories: (i) scanner
cameras and (ii) focal plane array (FPA) cameras. Scanner cameras are based on a
single detector element, and the measuring object is scanned line by line using on
optical–mechanical system of horizontal and vertical deflection mirrors. FPA
cameras consist of a matrix arrangement of individual detector elements.
Disadvantage of the FPA cameras is the fact that each image point is related to an
individual detector element and each detector element has its own transducer
characteristic, which leads to higher deviation between individual measuring points
in contrast to scanner cameras with only a single detector element. Thus, each
imaging point is caused by the same detector element with one single transducer
characteristic. However, scanner cameras are much slower due to the line-by-line
scanning process, which results in geometric distortion mainly during observation
of dynamic processes. Further parameters of thermo-cameras, which have to be
taken into account for IR–TG measurements, are (i) the spectral measuring range,
(ii) the thermal sensitivity, (iii) the geometrical resolution, (iv) the acquisition frame
rate and (v) the pixel resolution of the IR–TG images. The spectral measuring range
is related to the atmospheric windows (see above). The thermal sensitivity of a
thermo-camera describes it ability to distinguished objects with very little tem-
perature difference between them. Therefore, the sensitivity is a parameter repre-
senting the noise level in the IR image—the so-called noise equivalent temperature
difference (NETD). The NETD value should be quite small and is in general in the
order of mK (e.g. 0.03 K). The geometric resolution of a thermo-camera depends
on the field of view (FOV) and the instantaneous field of view (IFOV) both
determined by the size of the FPA detector. Whereas the FOV describes the total
surface area imaged by the camera depending on the distance between object and
camera, the IFOV describes the value of the solid angle captured by an individual
image point [312]. The pixel resolution of IR–TG images is provided by the used
FPA detector. FPA detectors have two-dimensional arrangement of pixels (detec-
tors), where each pixel is in the size of micrometres. The pixel resolution can range
from 160  120 pixels2 (19,200 image points) up to 1280  1024 pixels2
(1310,720 image points). The acquisition frame rate is an essential parameter
especially for the investigation of dynamic processes using IR–TG. Acquisition
frame rates vary in a wide range between 9 and 3 kHz. The frame rate is determined
by the method of “read-out” information, which can be done either by a line-by-line
read-out method or by so-called snap-shot technology. The line-by-line read-out
method is used mainly for detectors based on microbolometers and results in
integration times of about 8 ms, whereas the snap-shot technology is applied in
quantum detector with integration times in the order of a few µs.
184 5 In Situ Techniques for Characterization …

5.4.2.2 Heat Sources and Dissipated Energy

Two different types of heat sources can be distinguished: (i) sources induced by
dissipated energy, which are related to irreversibility of plastic deformation, and
(ii) sources induced by thermomechanical coupling, which are caused by interde-
pendence of mechanical, microstructural and thermal states (e.g. [313–316]).
Furthermore, temperature increase or temperature variations during mechanical
loading are results of (i) location, intensity and distribution of heat sources, (ii) heat
conduction parameters and (iii) heat exchange with surrounding [315], and are,
consequently, not purely intrinsic [316]. Therefore, a set of constitutive equations in
a thermodynamic framework is needed to separate two-dimensional heat source
fields from accompanying phenomena (heat conduction, heat exchange) [316].
To obtain the heat source field from IR–TG measurements, the heat conduction
equation given by (5.85) has to be solved (e.g. [313–316]):

.  c  T_ þ divðqÞ ¼ s ð5:85Þ

Here, q is mass density, c is specific heat capacity, q heat flux vector, T is the
absolute temperature, and s is the overall heat source. The heat capacity c is defined
by (5.86) [315, 316]:
@2W
c ¼ T ð5:86Þ
@2T

with W as the specific Helmholtz free energy. The heat flux vector q is given by
!
q ¼ k  grad T ð5:87Þ

with k as heat conduction tensor.


_
Thus, (5.85) describes the relation between absorption of heat capacity .  c  T,
heat losses by conduction divðqÞ and heat source s. The heat source s is composed
of three parts: (i) intrinsic dissipation di , (ii) thermomechanical coupling sth and
(iii) external heat supply or loss re .
The heat conduction (5.85) can be now rewritten as follows:
 ! 
.  c  T_ þ div k  grad T ¼ di þ sth þ re ð5:88Þ

Several general hypotheses can be used for simplification of local heat con-
duction equation (see 5.88), which results in (5.89):
• The parameters q and c are material constants independent of state variables.
• The isotropic conduction tensor k is also a material constant and independent of
state variables.
• The external heat supply is time independent. The equilibrium temperature field
T0 verifies kDT0 ¼ re . The temperature variations are noted as h ¼ T  T0 .
5.4 In Situ Full-Field Measurement Techniques 185

@h
.c  k  Dh ¼ di þ sth ð5:89Þ
@t

The values di and sth can be expressed by following [315, 316]:

@W : e @W _
di ¼ .  : .  Vk ð5:90Þ
@ 2e @V k

@2W _ @2W :e
sth ¼ .  T  Vk þ .  T  : ð5:91Þ
@Vk @T @ 2e @T

with Vk as internal state variable that depends on operating mechanism. e as the


elastic part of the strain tensor  according to the Hooke’s law  ¼ e þ p .
In addition, (5.85) receives specific formulations depending on material beha-
viour. Thus, in case of perfect elastic material behaviour, the thermomechanical
coupling is the only remaining heat source (under the assumption that no external
heat supply occurs and strain rate is high enough to avoid heat conduction) and
(5.85) obtains the following shape [317]:
 
@h @2W :e
.c  k  Dh ¼ .T : ð5:92Þ
@t @ 2 @T
e

Under the assumption that resulting temperature variations are quite small in
region of elasticity and application of Hooke’s law, the conventional equation of
thermoelasticity is obtained, where a is the thermal expansion coefficient and tr ðr_ Þ
the time derivative of the stress tensor [317].
 
@h a
 kDh ¼ T trðr_ Þ ð5:93Þ
@t .c

Equation (5.93) shows that pure elastic behaviour results in a temperature


decrease during tensile loading and in a temperature increase during compressive
loading [317].
In case of elasto-plastic material behaviour, the situation becomes more com-
plex. The plastic deformation of a material is characterized by a permanent
deformation after removing stress and a work hardening caused by introduction or
multiplication of lattice defects of different kinds and leads, therefore, to a rise of
internal energy stored to material—the so-called stored energy [318]. The release of
this stored energy is known to occur by three microstructural processes at elevated
temperatures: (i) recovery, (ii) recrystallization and (iii) grain growth. Figure 5.37
explains energy aspects involved into elasto-plastic deformation behaviour. Thus,
contribution of energy caused by plastic deformation to total energy of a system is
composed by stored energy and intrinsic dissipation energy (Fig. 5.34).
186 5 In Situ Techniques for Characterization …

Fig. 5.34 Energy aspects of


elasto-plastic material
behaviour. Modified
according to [317]

In this case, both the term for dissipated energy and the term for thermome-
chanical coupling are included to the heat conduction equation:
   
@h @W : e @W _ @2W _ @2W :e
.c  k  Dh ¼ . :   .   V k þ .  T  Vk þ .  T : 
@t @ 2e @V k @Vk @T @ 2e @T
ð5:94Þ

Thus, both the intrinsic dissipation di and the thermomechanical coupling sth
depend on the elastic strain tensor as well as on the variation of internal state
variables.
Especially, for cyclic plasticity, further assumption can be done leading to
simplification of the heat conduction equation:
• During cyclic loading, temperature variations induced have no significant
influence on the microstructural state (except temperature rise at end of fatigue
life when damage occurs). Therefore, the thermomechanical coupling source sth
can be neglected. Hence, fatigue is considered as a purely dissipative mecha-
nism (see 5.95).

@h
.c  k  Dh ¼ d i
@t   ð5:95Þ
@h @W : e @W _
.c  k  Dh ¼ .  : .  Vk
@t @ 2e @V k

The determination of three-dimensional heat source field over the cross section
along the whole gauge part of a specimen can be concerned as an “…ill-posed
problem ….” [319]. However, for thin flat specimens under cyclic loading condi-
tions especially in the regime of high cycle fatigue (HCF) or even very high cycle
fatigue (VHCF), several models have been proposed in the past [320]:
(i) a two-dimensional model connected to the heat diffusion problem over the
thickness of a specimen,
(ii) a one-dimensional model related to the heat diffusion problem over the cross
section of a specimen,
(iii) a zero-dimensional model describing the local thermal diffusion problem.
Boulanger et al. [319] gave a comprehensive overview of these three different
approaches proposed for the application to heat source calculation on thin flat
5.4 In Situ Full-Field Measurement Techniques 187

specimens under cyclic loading in the HCF and VHCF regimes. The following
descriptions are based on their description.
Two-dimensional model. In this approach, it is assumed that the heat source
averaged over the thickness e of a specimen (with length L and the width l) is
representative for the whole thickness of the specimen. Thus, the heat exchanges of
the front and rear of a specimen with surroundings are symmetric and linear. The
2D heat equation model is obtained by integration of (5.96) over the thickness e of
the specimen leading to the following expression:
   2 
@h h @ h @2h
.c þ 1D  k þ 2 ¼ di ð5:96Þ
@t sth @x2 @y

sth is a time constant characterizing heat loss through specimen surfaces in z-


direction (The coordinate system x-y-z is placed according to the specimen
dimensions as follows: with xjjL, yjjl and zjje.).
One-dimensional model. In this approach, the mean heat source of a cross
section of a specimen is regarded. Therefore, the integration of the heat conduction
(5.94) leads to following expression:
! !
@h h @2h
.c þ 2D k ¼ di ð5:97Þ
@t sth @x2

The one-dimensional model is useful to analyse strain localizations occurring in


material under mechanical load such as PLC bands.
Zero-dimensional model. This approach is based on the assumption that the
heat source is uniformly distributed in a specimen gauge part at any time. This
corres-ponds to classical monotonic load before strain localizations occur within
material. Therefore, (5.85) can be simplified as follows:
 
dh h
.c þ  di ð5:98Þ
dt seq

Here, h is temperature variation at the centre of a specimen and seq the local heat
loss.
In addition, the calculation of heat source fields can also be applied to investi-
gations on fatigue crack growth under cyclic loading. The cyclic plastic strain per
cycle is confined within cyclic plastic zone, and a part of plastic strain energy is
dissipated in heat causing temperature variations. Since the size of cyclic plastic
zone is usually quite small, the thermal problem of fatigue crack propagation can be
associated with a linear heat source centred in cyclic plastic zone along the crack tip
in an infinitely thick body [321].
188 5 In Situ Techniques for Characterization …

Independent of the model used for determination of the heat source field, the
dimensions of d i ; di or di are given either in kW/m3 or if divided by the product c in
K/s or °C/s.
The determination of heat source fields is based on IR thermographic mea-
surements of temperature fields. Thus, quantitatively reliable thermal fields are
necessary. Today, the advent of infrared focal plane array (FPA) cameras is a great
progress compared to single liquid nitrogen cooled detector with a scanning system,
since FPA cameras are certainly faster and more sensitive. However, one of the
main drawbacks is non-uniform response of each individual FPA detector element
to thermal field. Therefore, since these temperature fields are usually noisy, some
suitable filtering process has to be applied prior to processing temperature fields,
which can have an influence on spatial resolution of heat source fields [322]. In
addition, for any quantitative use of thermal data obtained from IR camera, several
precautions have to be fulfilled [315] such as (i) thermal stability of the thermo-
graphic system, (ii) calibration of the complete measurement chain with camera and
optics being thermally stable, (iii) pixel calibration, (iv) determination of the
emissivity of studied material surface, (v) determination of spatial resolution of the
camera in optical conditions of use and (vi) proper choice of frame rate and number
of recorded images.

5.4.2.3 State of the Art in Materials Engineering

During the last decades, IR–TG has been established in field of Materials Science
and Engineering as a suitable method for investigation of deformation and damage
processes in metallic materials mainly under mechanical load such as cyclic
deformation (e.g. [323–325],) uniform tensile deformation (e.g. [225–227]) or
dynamic tests. Plastic deformation of metallic materials leads to an increase in
temperature because part of mechanical energy introduced into material is dissi-
pated as heat [204]. Although this fact has been known for long time, it is con-
sidered only for metallic specimens as a whole [225]. Today, it becomes possible to
analyse heat dissipation phenomena during plastic deformation down to the
microstructural level, e.g. grain size of a polycrystalline specimen or discontinuities
like pores or non-metallic inclusions. This is caused mainly by an excellent
development of infrared detectors used in thermo-cameras and due to further
development of additional analysing techniques—like digital image correlation or
full-field measurements as a combination of IR–TG and DIC—during the last years.
Xue et al. [323], Wagner et al. [325] and Krewerth et al. [326, 327] showed that
IR–TG is applied during cyclic deformation, especially in the region of high
number of cycles (N)—so-called very high cycle fatigue (VHCF) regime—in order
to analyse crack initiation as well as crack propagation. In the VHCF regime,
applied stress levels are in an order of magnitude where confined plasticity or even
microplasticity occurs only. However, also in case of microplasticity dissipated heat
is not negligible and is indeed an excellent parameter for studies on local damage
5.4 In Situ Full-Field Measurement Techniques 189

behaviour. In 2006, Xue et al. [323] reported on different temperature increase


during cyclic loading in the VHCF regime depending both on applied strain level
and on applied loading frequency. Using ultrasonic fatigue testing [18], high
loading frequencies up to 20 kHz are applied in order to reach 109 cycles in a
reasonable period. These high loading frequencies lead due to damping behaviour
of the material to significant increase in temperature during fatigue tests. However,
along with this global temperature increase, Xue et al. [323] have shown for two
different high-strength steels as well as cast iron that IR–TG is even capable to
detect fatigue crack initiation due to pronounced increase in temperature in locally
limited areas of several tens of micrometres within a specimen—so-called hot spots.
Crack propagation and damage accumulation are studied by in situ thermography.
Furthermore, studies of Wagner et al. [325] on different aluminium alloys and
steels revealed that overall temperature evolution during ultrasonic fatigue testing
can be characterized by three individual stages: (i) increase in temperature directly
at beginning of cyclic deformation related to applied stress level, (ii) stabilization of
temperature over a wide range of number of cycles due to balancing dissipated
mechanical energy and energy loss due to convection and radiation at specimen
surface as well as heat conduction within material, and (iii) sudden increase in
temperature related to failure of material by crack initiation and propagation
(Fig. 5.35).
Quite recently, Krewerth et al. [326] showed that even multiple crack initiation
within one specimen caused either from interior defects (pores, inclusions) or from
surface roughening or inclusions in touch with specimen surface can be detected
due to IR–TG. Moreover, IR–TG enables to monitor crack paths during cyclic
deformation as well as better interpretation of crack origin on fracture surfaces due
to a lateral correlation of thermal images with fractographic analysis—so-called
correlated fractography. In addition, Krewerth et al. [327] established a method for
full surface view, which enables monitoring whole circumference of cylindrical
specimens by placement of two mirrors arranged behind specimen on opposite side
of thermo-camera. Thus, three infrared images are recorded simultaneously—(i)
direct view of TC and (ii) + (iii) IR images of mirror planes.

Fig. 5.35 Example for the arrangement of in situ IR–TG measurements during cyclic loading in
the VHCF regime. a Thermo-camera Vario hr (Infratec, Dresden, Germany) in combination with
ultrasonic fatigue testing machine. b Experimental setup for full surface view thermography both
schematical drawing and real arrangement. c Three thermograms. L2 —real thermogram. L1 , L3 —
thermograms of the two mirrors. Reproduced from [326] and [327]. Permission of Elsevier
190 5 In Situ Techniques for Characterization …

However, in the past IR–TG has been also applied in situ during mechanical
tests where larger plastic deformation occurs in materials such as static tests in
tension or compression as well as for dynamic tests. Thus, localized plastic
deformation behaviour during tensile tests [225, 226], dynamic tests [328, 329], as
well as macroscopic inhomogeneous deformation like jerky flow [330] can be
characterized by IR–TG. Saeed-Akbari et al. [330] studied jerky flow occurring in a
high-manganese twinning-induced plasticity (TWIP) steel (Fe–Mn–C) during ten-
sile deformation in a wide range of temperature and strain rate applying IR–TG.
Serrations are consequence of strain localization in bands (PLC bands) moving
along gauge length. Using IR–TG, it is possible to determine local temperature
increase within each band, global temperature increase by passing individual bands
as well as velocity of propagating bands. Thus, the influence of applied strain on the
effect of PLC bands was investigated.
In addition, Seghir et al. [225, 227] and Bodelot et al. [205, 226] performed
experimental studies on steel AISI 316L in order to quantify the heterogeneity of
strain and thermal fields caused by plastic deformation on the level of
microstructure of polycrystalline material with a grain size of about 240 µm
neglecting twin boundaries. Here, IR–TG measurements were complemented by
strain field measurements using digital image correlation (see Sect. 5.3.1) resulting
in fully-coupled, full-field measurements (see Sect. 5.4.3). Thus, it was demon-
strated by Bodelot et al. [226] that thermal fields could be detected at higher
deformation levels. However, due to heat dissipation the localization of these
thermal fields is not that strong as observed for strain localization. Thus, thermal
fields were detected on the level of clusters of several grains and not within indi-
vidual grains.
Quite recently, several papers [320, 331, 332] were published concerning cal-
culation of dissipated energy from IR–TG measurements. Thus, Blanche et al. [320]
proposed several heat diffusion models to calculate dissipated energy from infrared
images recorded during cyclic deformation in the VHCF regime of copper poly-
crystals. While the two-dimensional heat diffusion model describes the heat dissi-
pation along the gauge length and the thickness of the specimen, the
one-dimensional heat diffusion model is used in order to evaluate the temperature
evolution over each cross section of the specimen. Using these two models, it was
shown that heat dissipation occurs even at very low stress levels where nearly
elastic behaviour of material is assumed. Furthermore, it was found that the
intensity of dissipated energy increases with stress amplitude as well as number of
cycles.
Federova et al. [331] and Plekhov et al. [333] used IR–TG for calculation of
dissipated energy in front of a crack tip during cyclic deformation. Plekhov et al.
showed that infrared images allow after special data processing algorithm described
in [331] the calculation of the field of heat dissipation at a crack tip, which can be
correlated with the area of localized plastic deformation—the size of the plastic
zone. Furthermore, Federova et al. [331] developed a method to calculate the
J-integral as well as the stress intensity factor (SIF) from the dissipated heat energy
in front of a crack tip.
5.4 In Situ Full-Field Measurement Techniques 191

A chronological overview of application of in situ thermography during


mechanical loading tests under different conditions within the last years (from 2000
on) is summarized in Appendix Table A3.

5.4.3 Fully-Coupled Measurements

Both DIC and IR–TG are non-contact and full-field measurements with high pre-
cision. Thus, DIC technique is capable to resolve strain localizations occurring
during plastic deformation with submicron resolution called HR–DIC or µDIC.
Similar, IR–TG allows to detect thermal fields and to calculate heat sources and
heat dissipation. However, under thermomechanical point of view, the coupling
between both complementary techniques is of strong interest [334].
Thus, each technique holds its own advantages and drawbacks. Among them,
the contrast techniques providing ideal circumstances for the application of each
technique are quite conflictive, and while DIC technique requires a heterogeneous,
high-contrast, randomly distributed speckle pattern, IR–TG needs to have a
homogenous black contrast giving high emissivity factor (e  0.96). Furthermore,
the spatial and temporal coupling of both measurement techniques creates high
demands on lateral resolution of both imaging techniques as well as on synchro-
nization of image acquisition.
In principal, two different approaches of fully-coupled, full-field measurements
of kinematic and thermal fields are possible [334]: (i) two-face measurements (e.g.
[335–337]) and (ii) one-face measurement with either two cameras (e.g. [203, 205,
338]) or one-camera setup (e.g. [339, 340]). Figure 5.36 shows typical arrange-
ments for two-face (a) and one-face measurements (b–d).
Among these three approaches, the first one is the simplest one to realize, since
both specimen surfaces can be prepared according to the optimum requirements for
each individual technique (e.g. [336]). In case of approach (ii), the surface prepa-
ration has to solve the requirements for both techniques. For approach (ii), the
coupling of both measurement techniques on one specimen surface can be realized
either by the application of a dichroic mirror (e.g. [227]) or by a co-planar
arrangement of the thermo-camera and the CCD camera (e.g. [203]).
Performing full-field measurements on polycrystalline specimens with grain size
below the dimension of the specimen thickness, the microstructure especially with
respect to the grain orientations is different on opposite sides of a specimen under
deformation in contrast to experiments using single crystals or oligocrystals.
Therefore, strain fields and thermal fields cannot be correlated directly with each
other. In such cases, it is necessary to collect both information on the same AOI.
The one-face measurement setup operating with two cameras was first introduced
by Bodelot et al. [341]. Here, a dichroic mirror is placed in front of the specimen
inclined at an angle of 45° to the surface normal direction. The working principle of
a dichroic mirror is a selective filtering of radiation. Thus, the infrared radiation is
transmitted, whereas the visible light is reflected by the mirror. Therefore, the two
192 5 In Situ Techniques for Characterization …

Fig. 5.36 Different experimental setups for fully-coupled full-field measurements of kinematic
and thermal field. a Two-face measurement approach with CCD and TC viewing opposite
specimen sides. Reproduced from [336]. Permission of Wiley VCH. b One-face measurement
approach with CCD and TC on the same area of interest using dichroic mirror for separating
visible and infrared radiation. c One-face measurement approach with co-planar arrangement of
CCD and TC. d One-face measurement approach with TC only. b–d Modified according to [227,
203] and [340], respectively. Permission of Elsevier

cameras are placed at an angle of 90° to each other. The thermo-camera is placed
behind the dichroic mirror, whereas the digital camera is placed at 90° to the surface
normal direction. Thus, both detector areas are placed parallel to the specimen
surface and any distortion between the recorded thermal and kinematic fields is
avoided [342]. The dichroic mirror used in these investigations transmits the
infrared radiation of 2–6 µm (MWIR). Wavelength below 2 µm will be reflected by
the mirror including visible light. Figure 5.37 shows typical transmission and
reflection curves of such dichroic mirror. The application of dichroic mirror was
used already in earlier studies for splitting the radiation for thermographic mea-
surements during high strain loading of titanium alloy Ti6Al4V [343].
However, the most challenging task using one-face measurements with the
above-mentioned camera setup is the proper preparation of specimen surfaces
according to the different measurement requirements for DIC and IR–TG.
Therefore, special patterning had to be generated, which fulfil both the requirement
for DIC with a random, high-contrast, finely dispersed speckle pattern as well as for
IR–TG with a uniform black painting realizing a high emissivity factor.
The patterning used finally by Bodelot et al. [341] was micrometre-sized powder
of talc containing in addition titanium oxide, iron and zinc. The powder was solute
5.4 In Situ Full-Field Measurement Techniques 193

Fig. 5.37 Mode of operation of dichroic mirror. a Radiation path k in transmission k1 and
reflection k2 . b Curve of reflection of k2 . c Curve of transmission k1 . According to [341]

Fig. 5.38 Suitable patterning for fully-coupled DIC and IR–TG measurements using two-camera
setup for one-face measurement. a Speckle pattern for DIC. b Same area imaged by TC.
c Greyscale distribution of speckle pattern for DIC. According to [205]. Permission of Elsevier

in ethanol and then sprayed on the specimen surface using airbrush piston. The
quality of pattern used for coupled DIC and IR–TG is shown in Fig. 5.38.
Another way to realize one-face measurements with two-camera setup is the
co-planar arrangement of digital camera and TC in either vertical arrangement as
proposed by Saai et al. [203] or horizontal arrangement as used by Dumoulin et al.
[338]. In both cases, the digital camera is placed directly in front of the specimen
perpendicular to the specimen surface normal and the view plane exactly parallel to
the specimen surface. By this, the error for DIC measurements caused by image
distortions due to misalignment will be reduced. However, a tilt angle between the
digital camera and the TC has to be introduced depending on the geometrical
dimensions of both cameras either in horizontal or vertical direction. Thus, the field
of view (FOV) of thermo-cameras is inclined slightly to the specimen surface,
which can result in some error in temperature determination. The tolerable angle
between thermo-camera and surface normal depends on used camera itself and,
here, especially on depth of view [342]. Using a camera with a depth of view of
about 100 µm, the maximum tolerable angle is about 1°. Therefore, this arrange-
ment is more reliable for coarse-grained materials than for fine-grained
microstructures [342].
Along with the one-face, two-camera setup for fully-coupled full-field mea-
surements, an excellent technique was developed using one camera, only—intro-
duced as infrared image correlation (IRIC). Thus, Maynadier et al. [340] described
194 5 In Situ Techniques for Characterization …

in detail an experimental setup using solely thermo-camera for IRIC. Here, a


specific surface patterning was developed and, in addition, the surrounding tem-
perature was controlled. Again, since DIC needs a non-homogenous, high-contrast
pattern for tracking the displacement, a non-uniform emissivity pattern was created
at the specimen surface. The material under investigation in the studies of
Maynadier et al. [340] was NiTi-SMA, which was used in electrochemical polished
conditions with a low emissivity as usual for polished metallic surfaces (e * 0.1).
The AOI was covered by a mist of black paint giving a heterogeneous pattern of
black dots with high emissivity (e * 0.97). The remaining part of the specimen
is fully covered by black paint for allowing exact temperature determination. Thus,
the resulting image captured by the thermo-camera contains two areas: (i) fully
black for exact temperature determination and (ii) non-uniform emissivity pattern at
the AOI for DIC as shown in Fig. 5.39. Here, the colour code of the IR image is
provided by digital levels in a total range of 214 = 16,000 digits related to a tem-
perature range of 5 °C  T  60 °C. As seen in Fig. 5.39, the localized strain
caused by martensitic phase transformation of the single crystalline NiTi specimen
during loading is related to temperature increase. Thus, both strain fields and
temperature fields can be recorded simultaneously using this excellent arrangement.
However, special care has to be taken on exact temperature measurement.
Therefore, using this arrangement, both the control and the determination of sur-
rounding temperature are essential.
For this, Maynadier et al. [340] developed a specific arrangement of cooled
black body in the surrounding of the specimen as well as a mirror for the infrared
radiation behind the AOI of the specimen as shown in Fig. 5.40.
First fully-coupled full-field measurements were performed in 2001 by Guduru
et al. [328] on maraging steel during impact tests using the two-face measurement
approach. Since that time, several fully-coupled kinematic and thermal field
investigations were performed with continuous improvement of the technical setup
as well as the data acquisition and the data analysis. Table A5.4 in Appendix
provides a chronological overview of recent investigations and important outcomes
(from 2000 on) in this field. It becomes obvious that fields of applications range

Fig. 5.39 Suitable surface pattern for one-face, one-camera fully-coupled measurements of strain
and thermal fields—known as IRIC. IR image of the specimen surface expressed in digital levels.
Modified and reproduced according to [340]. Permission of Elsevier
5.4 In Situ Full-Field Measurement Techniques 195

Fig. 5.40 One-face, one-camera IRIC measurement. a Experimental setup for temperature
calibration using large cooled surrounding equipment and back-side reflection. b Thermograms of
the back-side reflection (left) and the front side (right) of a NiTi-SMA specimen provided in digital
levels. Average temperature is about 53 °C. Reproduced from [340]. Permission of Elsevier

from plasticity over fatigue and fracture mechanics up to thermomechanics.


Materials under investigation are mostly metallic materials of polycrystalline or
single crystalline microstructure. However, the fully-coupled full-field measure-
ments are used as well for materials undergoing large plastic deformations such as
carbon-filled natural rubber (see [344] or [345]).

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Chapter 6
Object of Investigations—High-Alloy
Fe–16Cr–6Mn–xNi–0.05C Cast Steels
with TRIP/TWIP Effect

Abstract This chapter concerns with the material used for the characterization of
strain localizations and the temporal evolution of deformation processes—the group
of low-carbon, high-alloy austenitic CrMnNi TRIP/TWIP steels. This chapter
focuses on a comprehensive description of both the mechanical behaviour and the
microstructural evolution of these steels. The results on mechanical behaviour are
divided into (i) uniaxial monotonic loading, (ii) uniaxial cyclic loading and
(iii) planar-biaxial loading. The description of the microstructural evolution is
separated according to the different austenite stabilities of these steels resulting from
varying nickel contents. The used methods for mechanical testing and
microstructure characterization are shortly summarized. Detailed descriptions are
provided by references.

In the following section, the high-alloy Fe–16Cr–6Mn–xNi–0.05C cast TRIP/TWIP


steels [1] developed within the framework of CRC799 project will be described
with respect to their chemical composition, their mechanical properties and their
microstructural features. Investigations were carried out on these steels to examine
localized deformation processes such as strain-induced martensitic phase transfor-
mation, mechanical twinning and the PLC effect.

6.1 General Considerations on High-Alloy Fe–16Cr–


6Mn–xNi–0.05C TRIP/TWIP Steels

The chemical composition of high-alloy Fe–16Cr–6Mn–xNi–0.05C steels is based


on low carbon contents (  0.05%) and high amounts of chromium, nickel and
manganese. Whereas chromium acts as a stabilizer of ferritic phase, nickel and
manganese stabilize austenitic phase. The chemical composition of the steels was
designed to trigger deformation behaviour involving either TRIP or TWIP effect by
variation of the nickel content. The other two main alloying elements—chromium
and manganese—were kept constant at 16 wt% and 6 wt%, respectively. Further

© Springer Nature Switzerland AG 2020 205


A. Weidner, Deformation Processes in TRIP/TWIP Steels,
Springer Series in Materials Science 295,
https://doi.org/10.1007/978-3-030-37149-4_6
206 6 Object of Investigations—High-Alloy …

Fig. 6.1 High-alloy CrMnNi steels. a Phase diagram of Fe–16Cr–7Mn–xNi–0.05C steels with
varying nickel content between 0 and 16 wt%. Modified according to [2]. With courtesy of
S. Martin. b Schaeffler diagram for the three basic steel variants: Fe–16Cr–6Mn–3Ni–0.05C,
Fe–16Cr–6Mn–6Ni–0.05C, Fe–16Cr–6Mn–9Ni–0.05C

minor alloying elements were carbon, nitrogen, aluminium and silicon. The content
of nitrogen was kept as low as the carbon content. Figure 6.1a shows the phase
diagram for Fe–16Cr–6Mn–xNi–0.05C steel with variation of the nickel content
between 0 and 16%. The largely extended single-phase field of the austenite can be
recognized clearly. The steel variant with 3 wt% nickel (Fe–16Cr–6Mn–3Ni–0.05C
steel) exhibit a ferritic solidification, whereas variants with 6 wt% and 9 wt% nickel
(Fe–16Cr–6Mn–6Ni–0.05C steel, Fe–16Cr–6Mn–9Ni–0.05C steel) exhibit an
austenitic solidification. Depending on content of alloying elements, the phase
composition of the microstructure after solidification can be evaluated according to
the Schaeffler diagram shown in Fig. 6.1b, which describes the occurrence of
individual phase fields as a function of the chromium and nickel equivalent and
which is calculated in analogy to (4.21) and (4.22) by (6.1) and (6.2), which are
given by Weiss and Gutte for austenitic Fe–16–Cr–6Mn–xNi–0.05C steels [3]:

Nieq ¼ %Ni þ 30%C þ 18%Ni þ 0:5%Mn þ 0:3%Co þ 0:2%Cu  0:2%Al ð6:1Þ

Creq ¼ %Cr þ %Mo þ 1:5%Si þ 0:5%W


ð6:2Þ
þ 0:9%Nb þ 1:5%V  0:9%Ta þ 4%Al þ 4%Ti

The chemical composition of the three basic steel variants is summarized in


Table 6.1 together with other characteristic properties describing the austenite
stability. Thus, the martensitic start temperature was calculated based on a model of
Jahn et al. [4] according to (6.3):

Ms ¼ 685  108Nieq þ 4Ni2eq ð6:3Þ

Regarding the Ms temperature, it becomes obvious that for Fe–16Cr–6Mn–6Ni–


0.05C and Fe–16Cr–6Mn–9Ni–0.05C steels, the Ms temperature is well below RT.
6.1 General Considerations on High-Alloy Fe–16Cr–6Mn–xNi–0.05C TRIP/TWIP Steels 207

Table 6.1 Chemical composition and characteristic properties of the investigated Fe–16Cr–6Mn–
xNi–0.05C steel variants (with x = 3 wt%, 6 wt% or 9 wt% nickel)
x (wt% Ni) Chemical composition (wt%) Characteristic properties
C Cr Mn Ni Si Al N Creq Nieq MS (°C) cSF (mJ/m2)
3 0.05 16.0 6.4 3.2 0.8 0.06 0.06 17.4 8.9 38 4.2–10.2
6 0.08 16.0 6.0 6.1 1.0 0.05 0.05 17.7 12.4 −39 10.4–16.4
9 0.04 15.3 5.8 8.6 0.9 0.07 0.05 16.9 13.6 −44 15.5–21.5

Thus, a spontaneous martensitic phase transformation will only occur at T < RT.
However, the required thermodynamic Gibbs free energy can be substituted by
mechanical energy from externally applied load, leading to either stress-assisted or
strain-induced martensitic phase transformation (see Sect. 3.2). In contrast, the Ms
temperature for Fe–16Cr–6Mn–3Ni–0.05C steel is above RT. Thus, a certain
amount of spontaneous MPT will be present in the initial microstructure due to
cooling process. This is in good agreement with the representation shown in the
Schaeffler diagram. The Fe–16Cr–6Mn–3Ni–0.05C steel exhibits about 10% d-
ferrite and 10% martensite in the initial microstructure. The Fe–16Cr–6Mn–6Ni–
0.05C steel contains about 1% of d-ferrite, whereas the Fe–16Cr–6Mn–9Ni–0.05C
steel is purely austenitic. Figure 6.2 shows three possible variants of MPT for Fe–
16Cr–6Mn–6Ni–0.05C steel—(i) spontaneous at T < RT (−196 °C),
(ii) stress-assisted at T < RT (−40 °C) and (iii) strain-induced at T = RT.
Significant differences become obvious between the three variants of MPT.
Whereas the spontaneous (Fig. 6.2a) and the stress-assisted MPT (Fig. 6.2b) are
direct transformations of fcc austenite into bcc a′-martensite (c ! a′) without any
intermediate phase, the strain-induced MPT (Fig. 6.2c) occurs via the intermediate
e-martensite phase (c ! e ! a′).

Fig. 6.2 Three different variants of martensitic phase transformation in Fe–16Cr–6Mn–6Ni–


0.05C steel. a Spontaneous martensite upon cooling from 20 to −196 °C. b Stress-assisted
martensite during compression at −40 °C. c Strain-induced martensite during compression at RT.
Reproduced according to [2]. With courtesy of S. Martin
208 6 Object of Investigations—High-Alloy …

As mentioned above, the activation of deformation mechanisms and the char-


acter of dislocation glide are influenced significantly by the stacking-fault energy
(cf. Fig. 4.5), which itself is a function of chemical composition and temperature.
The SFE was calculated for investigated steel variants according to Dai et al. [5]
using (6.4):

cSF ¼ c0SF  1:34%Mn þ 0:06%Mn2  1:75%Cr þ 0:01%Cr2 þ 15:21%Mo þ 1:59%Ni


 5:59%Si  60:69ð%C þ 1:2%NiÞ1=2 26:27ð%C  1:2%NÞ  ð%Cr þ %Mn
þ %MoÞ1=2 þ 0:61ð%Ni þ %Cr þ %MnÞ2
ð6:4Þ

Here, c0SF is the SFE of pure fcc c-iron and is assumed (according to Dai et al. [5])
to lie between 36 and 42 mJ/m2. The influence of alloying elements is taken into
account by their concentrations in wt%. The calculated SFE summarized in
Table 6.1 provides a range of SFE for each steel variant as a function of c0SF .
Table 6.1 illustrates well that with decreasing nickel content, the SFE decreases as
well. Therefore, a change in the dominant deformation mechanism from dislocation
glide and mechanical twinning (9% nickel) to pronounced martensitic phase trans-
formation (3% nickel) is expected. In addition, the SFE was determined experi-
mentally by TEM investigations [6, 7] as well as by X-ray diffraction measurements
[8, 9]. At 29–43 mJ/m2, the cSF estimated from measurements of dislocation nodes
[6, 7] for Fe–16Cr–6Mn–6Ni–0.05C steel was well above values calculated
according to (6.4). In contrast, cSF determined by in situ XRD bending experiments
was about 17.5 ± 1.4 mJ/m2 for Fe–16Cr–6Mn–6Ni–0.05C steel and 8.1 ± 0.9 mJ/
m2 for Fe–16Cr–6Mn–3Ni–0.05C steel. Thus, values determined by XRD mea-
surements are in good agreement with values calculated according to (6.4).
The three basic steel variants were manufactured as plates with the dimensions
340  340  20 mm3 or 200  200  16 mm3, respectively, by ACTech GmbH
(Freiberg, Germany) using dead mould casting. The cast plates were solution
annealed at 1050 °C for 30 min followed by N2 quenching. The steel variants
showed typical as-cast microstructure, which was characterized by segregations of
alloying elements such as Cr, Ni or Mn due to dendritic solidification as well as
large grain size (50 µm up to 2000 µm) due to solidification process.
The initial microstructure of steels predicted by the Schaeffler diagram (cf.
Fig. 6.1b) was verified by optical microscopy (see Fig. 6.3). Whereas the Fe–16Cr–
6Mn–9Ni–0.05C steel was located well within the single-phase region, the Fe–
16Cr–6Mn–6Ni–0.05C steel was located directly at the border between the
two-phase region austenite and d-ferrite. Only the Fe–16Cr–6Mn–3Ni–0.05C steel
exhibited a three-phase microstructure consisting of austenite (c), d-ferrite and
cooling martensite, which is in good agreement with the calculated martensitic start
temperature Ms = 60 °C. The amount of d-ferrite and cooling martensite was
determined using optical microscopy on binarized micrographs after etching with
6.1 General Considerations on High-Alloy Fe–16Cr–6Mn–xNi–0.05C TRIP/TWIP Steels 209

Fig. 6.3 As-cast microstructure of the three basic Fe–16Cr–6Mn–xNi–0.05C steel variants. a Fe–
6Cr–6Mn–3Ni–0.05C. b Fe–16Cr–6Mn–6Ni–0.05C. c Fe–16Cr–6Mn–9Ni–0.05C

Murakami etching solvent [10]. Thus, the Fe–16Cr–6Mn–3Ni–0.05C and Fe–


16Cr–6Mn–6Ni–0.05C steel steels contained from 8% to 11% and 2% d-ferrite,
respectively. The amount of cooling martensite in Fe–16Cr–6Mn–3Ni–0.05C steel
is also about 10%.

6.2 Applied Methods for Characterization


of the Deformation Behaviour and the Related
Microstructures

6.2.1 Deformation Experiments

The mechanical behaviour of the three basic steel variants was intensively studied
under different loading conditions over a wide range of temperature, strain rate and
load path.
Uniaxial monotonic loading. The mechanical behaviour under uniaxial loading
was investigated quasi-static in tension in a temperature range of −60 °C  T 
200 °C at a strain rate of 4  10−4 s−1 using an electromechanical testing device
(ZWICK 1476) equipped with a temperature chamber [11]. Uniaxial compression
tests were performed in a temperature range of 20 °C  T  300 °C up to strain
rate of 100 s−1 on an MTS 810 servo-hydraulic testing machine [12]. For dynamic
loading of specimens at high strain rates of 102 s−1 or 103 s−1, an instrumented drop
weight tower with a calibrated tube for determination of force and a
Split-Hopkinson-Pressure-Bar (SHPB) were used [12]. Specimens from interrupted
mechanical tests were cut parallel to the loading axis and prepared for further
investigations by SEM and XRD.
Cyclic loading. Uniaxial cyclic loading was carried out using servo-hydraulic
testing systems MTS 810 (100 kN) and MTS Landmark 250 (250 kN). Low cycle
210 6 Object of Investigations—High-Alloy …

fatigue (LCF) tests were performed under symmetric push–pull loading conditions
(R = −1) under total strain control in a total strain amplitude range of 1  10−3 
ea;t  3  10−2 [13]. The resulting strain rates were kept constant at 4  10−3 s−1.
A ferritescope sensor (Helmut Fischer GmbH, Fischerscope MMS PC) was applied
to follow the evolution of ferromagnetic phase fraction [13]. At the end of fatigue
life ðNf Þ, the gauge lengths of specimens were cut parallel to loading axis and were,
finally, prepared by grinding and electropolishing for investigations by optical
microscopy and SEM.
Biaxial loading. Biaxial planar deformation experiments were carried out under
static and cyclic loading conditions using a servo-hydraulic biaxial planar testing
machine (Instron 8000) with four actuators (each having 250 kN of nominal force),
water-cooled grips and cruciform specimens. Different load paths were realized
resulting in biaxial tension, biaxial compression and biaxial shear as well as biaxial
in-phase and out-of-phase cyclic loading [14].
Quasi-hydrostatic high-pressure deformation. The quasi-hydrostatic high-pressure
experiments were performed at room temperature using a multi-anvil system at the
high-pressure laboratory of the Freiberg High-Pressure Research Centre (FHP) in
Germany and a multi-anvil system in combination with in situ synchrotron X-ray
diffraction measurements at Deutsches Elektronen Synchrotron (DESY, Hamburg,
Germany). The maximum pressure achieved for a specimen with ∅ 900 µm and a
height of 500 µm was about 18 GPa [15].

6.2.2 Microstructural Characterization Techniques

The deformation behaviour of high-alloy Fe–16Cr–6Mn–xNi–0.05C cast steels


related to TRIP and TWIP effect was studied intensively under different mechanical
loading conditions such as quasi-static, cyclic, dynamic and biaxial loading. In
addition, mechanical behaviour was tested for alloys with different nickel contents
(x = 3 wt%, 6 wt% or 9 wt%) over a wide range of temperature and strain rates (see
Sect. 6.3). The underlying microstructural processes were characterized as a
function of applied strain or number of cycles. The microstructural characterizations
were performed using a broad spectrum of experimental techniques ranging from
classical optical microscopy via X-ray and synchrotron diffraction up to scanning
and transmission electron microscopy.
Scanning electron microscopy. Using scanning electron microscopy, techniques
such as electron backscattered diffraction (EBSD) and electron channelling contrast
imaging (ECCI) were applied, in particular, alongside with classical secondary
electron (SE) and backscattered electron (BSE) contrast. Through detection and
indexing of Kikuchi patterns [16], EBSD technique facilitated the determination of
both phase composition of deformed material and crystallographic orientation of
individual austenitic grains or martensitic variants. Thus, for interpretation of
6.2 Applied Methods for Characterization … 211

martensitic phase transformation in deformed microstructure, it was primarily


coloured phase maps that were used in combination with band contrast maps.
The band contrast (BC) maps represented the contrast conditions of Kikuchi
patterns detected. The BC is provided in grey values between 0 and 255, whereas 0
is related to lowest level of contrast (black) and 255 to highest level of contrast
(white). The BC maps reflect deformed microstructure perfectly, since regions with
higher defect densities (dislocations, stacking-faults) such as deformation bands
appear in darker contrast than undistorted regions.
In a phase map, in general, all indexed points of the measuring area with same
crystal lattice (fcc, hex, bcc) are represented by same colour. The phase maps
presented in this work are related to the following colour code: (i) austenite (fcc)—
red or grey colour (BC), (ii) e-martensite or deformation bands with SF (hex)—
yellow colour, and (iii) a′-martensite (bcc)—blue colour. Non-indexed patterns or
patterns with a confidence index (CI) less than 0.1 appear in black. The CI reflects
the ratio of identified Kikuchi bands to the maximum number of bands, which were
detectable. CI = 0.1 means that one band out of nine possible ones was detected.
The crystallographic orientation is also provided in colour-coded maps. Here, all
indexed points of the measuring field exhibiting same crystallographic orientation
are represented by the same colour. The colour code used is related to inverse pole
figure colouring of stereographic standard triangle. The inverse pole figure
colouring could be applied for the three axes related to specimen coordinate system
—normal direction (ND), rolling direction (RD; here loading axis), and transverse
direction (TD). Furthermore, specific orientation relationships such as grain
boundaries could be evaluated. Thus, large-angle grain boundaries (LAGB) with a
misorientation angle of  15° between neighbouring grains could be separated
from special grain boundaries such as twin boundaries (TB), which are character-
ized by a misorientation angle/axis pair of 60° h111i. In the present paper, LAGB
and TB are shown by blue (or black) and red lines, respectively. Special phase
orientation relationships between fcc and bcc phases and fcc/hex and hex/bcc
phases can also be recognized by special colour-coded lines. A measurement
quantity for lattice distortion due to a high content of lattice defects such as dis-
locations or stacking-faults is so-called kernel average misorientation
(KAM) factor. The KAM is the local misorientation calculated for each measuring
point and the eight nearest neighbours. The KAM is also shown in colour-coded
maps with a maximum misorientation angle of 5°.
The orientation data obtained from EBSD measurements were saved as average
orientation per grain in terms of the three Euler angles /1 , U and /2 . The Euler
angles were transformed into g-matrix according to equations provided by Randle
[17]. For detailed slip system analysis, the g-matrices of all investigated grains
were transformed into the SST ½001–½011–½111 (cf. Sect. 2.4, Fig. 2.12). These
orientation matrices were used for calculation of activated slip systems including
Schmid factors l, the coordinates of slip planes and slip directions with respect to
specimen coordinate system x  y  z, where x is loading axis and z surface normal.
Here, the angles atrace and btrace were calculated describing the angle between the
212 6 Object of Investigations—High-Alloy …

trace of slip plane on the surface and the x-axis ðatrace Þ and the angle of the trace of
the slip plane on the side face (cut parallel to the x- and z-axis, perpendicular to the
surface) to the x-axis ðbtrace Þ, respectively. Both angles atrace and btrace are given in
positive values counterclockwise with respect to the loading axis (cf. [18]). These
calculations were done using a self-written EXCEL macro [19].
The second powerful SEM method was the electron channelling contrast
imaging (ECCI) technique [20], which allows the imaging of defect arrangements
such as dislocations or stacking-faults in deformed materials. Thus, lattice distor-
tions caused by presence of lattice defects led to changes in backscattering and
channelling conditions as a function of the deviation parameter x [21]. Thus, lattice
defects can be imaged in crystal regions, which are in perfect channelling condi-
tions. The defect should then appear as a bright contrast on a dark background. In
the present paper, so-called inverted ECCI micrographs are shown, where the
above-described contrast conditions are inverted.
Along with these two powerful techniques for applications on bulk specimens,
the SEM also facilitates the detection of transmitted electrons (TE) in combination
with electron transparent thin foils in analogy to classical TEM and a special TE
detector. In the present paper, in order to avoid confusion with the scanning modus
used during TEM investigations—known as scanning transmission electron
microscopy (STEM)—the term transmission scanning electron microscopy
(t-SEM) is used (cf., e.g., [22]). The t-SEM modus facilitates imaging of defect
arrangements such as dislocations, stacking-faults and martensitic islands in elec-
tron transparent foils in both bright field and dark field conditions. In addition,
transmission Kikuchi diffraction (TKD) or transmission EBSD (t-EBSD) can be
performed on TEM foils (cf., e.g., [23]).
Transmission electron microscopy. TEM investigations were performed on
deformed materials states using both the classical bright field and dark field imaging
techniques in combination with diffraction patterns in order to characterize different
phases or lattice defects. High-resolution TEM (HRTEM) was performed as well in
order to study defect arrangements or defect interaction at high resolution. TEM/
HRTEM was performed using transmission electron microscope JEM 2200 FS
(JEOL) operating at an acceleration voltage of 200 kV. Fast Fourier transformations
(FFT) using the programme Gatan Digital Micrograph and stereographic standard
projections were used for interpretation of HRTEM micrographs [6].
X-ray diffraction. X-ray diffraction experiments were used in order to quantify
phase compositions after mechanical loading and to study evolution of martensitic
phase transformation. Thus, volume fraction of e-martensite (hex) and a′-martensite
was evaluated via quantitative phase analysis using the Rietfeld method. Moreover,
XRD measurements were performed in order to study content of defects such as
stacking-fault arrangement within deformation bands as well as to evaluate
stacking-fault energy itself. XRD experiments were carried out on a conventional
diffractometer (URD-65, Seifert/Freiberger Praezisionsmechanik) in Bragg–
Brentano geometry using Cu Ka radiation [24].
6.2 Applied Methods for Characterization … 213

Magnetic measurements. In addition to XRD, SEM and TEM investigations, the


evolution of volume fraction of strain-induced a′-martensite during plastic defor-
mation was investigated by measurement of the ferromagnetic phase fraction.
Whereas metastable austenite (fcc) is paramagnetic, a′-martensite (bcc) is ferro-
magnetic. Thus, it was possible to use a so-called ferritescope to measure ferro-
magnetic phase fraction either post-mortem, at stopped tensile or compression tests,
or in situ during cyclic uniaxial or biaxial loading [13].

6.3 Mechanical Behaviour

The following sections will summarize main aspects of deformation behaviour


under different loading conditions such as monotonic loading in tension or com-
pression, cyclic loading and multiaxial deformation. The specific loading conditions
including specimen geometries and additional techniques are documented in
specified references.

6.3.1 Uniaxial Quasi-static Loading

The deformation behaviour of Fe–16Cr–6Mn–6Ni–0.05C steel was studied inten-


sively by Martin et al. (e.g. [11]) under tensile loading conditions as well as by Wolf
et al. (e.g. [12]) under compressive loading conditions in a wide range of temper-
atures (–60 °C < T < 300 °C) and strain rates (4  10−4 s−1 < e_ < 102 s−1).
Figure 6.4 summarizes results of temperature dependence of tensile and com-
pressive deformation behaviour at a low strain rate e_ = 4  10−4 s−1 [11, 25].
Figure 6.5 provides an overview of temperature and strain rate dependent results
obtained during compressive loading [12].
The stress-strain curves obtained under tensile and compressive loading
demonstrated clearly the influence of temperature on deformation behaviour. In
addition, strain rate had significant influence, though lower than that of temperature.
As Fig. 6.4 shows, increase in deformation temperature led to significant change in
shape of stress-strain curve (a), calculated work hardening (b) as well as mechanical
properties such as uniform elongation and elongation to rupture (c). The
stress-strain curves at −60 °C and room temperature (20 °C) clearly exhibit sig-
moidal shapes, which were caused by pronounced strain hardening due to formation
of a′-martensite during plastic deformation (cf. Fig. 6.4a, b). With increasing
temperature, strain-hardening effect becomes less pronounced and an extended
region of nearly constant strain hardening occurs, which can be attributed to
intensive mechanical twinning. Whereas YS and UTS decreased as expected with
an increase in temperature, uniform elongation as well as elongation to failure
evolved to a maximum value between 60 and 100 °C (cf. Fig. 6.4c). Thus, the
maximum value of uniform elongation between 60 and 100 °C can be understood
214 6 Object of Investigations—High-Alloy …

Fig. 6.4 Temperature dependence of tensile deformation behaviour of Fe–16Cr–6Mn–6Ni–0.05C


steel at a low strain rate of e_ = 4  10−4 s−1. a Stress-strain curves. b Work hardening curves.
c Mechanical parameters: yield strength, ultimate tensile strength, uniform elongation and
elongation to failure. a, b Reproduced from [11]. Permission of Springer (c) Reproduced from
[25]. Permission of Trans Tech Publ

Fig. 6.5 Temperature and strain rate dependence of the compressive deformation behaviour of
Fe–16Cr–6Mn–6Ni–0.05C steel at a low strain rate of e_ = 4  10−4 s−1. a Stress-strain curve at
different temperatures. b Stress-strain curves at room temperature and different strain rates. c Work
hardening at RT and different strain rates. Reproduced from [12]. Permission of Elsevier
6.3 Mechanical Behaviour 215

as a transition from TRIP to TWIP effect. Below this transition temperature, pro-
nounced martensitic phase transformation occurs, whereas above transition tem-
perature, mechanical twinning resulting in TWIP effect is dominating deformation
mechanism.
Similar behaviour was observed during compressive loading at a low strain rate
of e_ = 4  10−4 s−1 as shown in Fig. 6.5a. The indicated values of a′-martensite
volume fraction demonstrated well that with increasing deformation temperature,
volume fraction of a′-martensite decreases significantly. Thus, although at room
temperature a′-martensite volume fraction of about 70% was measured by magnetic
balance, no martensite could be detected at temperatures  100 °C.
A similar but less pronounced effect was that of increase in strain rate, which led
(in a similar way) to a decrease in the volume fraction of a′-martensite. As expected,
yield stresses and flow stresses increased with an increase in strain rate. However, at
a certain strain level a crossover of loading curves obtained at lower and higher
strain rates was observed. The crossover was again caused by a change in
strain-hardening behaviour. The significant reduction of a′-martensite formation
above strain rates of 10−1 s−1 was due to adiabatic heating under dynamic loading
conditions. The temperature increase due to adiabatic heating, which was deter-
mined by Wolf et al. [12] to be 100 K at a strain rate of e_ = 100 s−1, resulted in a
reduction in the thermodynamic driving force for a′-martensite formation.
Consequently, strain-induced martensitic phase transformation was suppressed and
a transition occurred to mechanical twinning and dislocation glide as the dominant
deformation mechanisms.
The deformation behaviour of Fe–16Cr–6Mn–xNi–0.05C steels (x = 3 wt%, 6
wt%, 9 wt% nickel) was studied by Vinogradov et al. [26] under tensile loading
conditions in a temperature range of 20 °C  T  100 °C and at moderate strain
rates of 1  10−3 s−1  e_  1  10−2 s−1. The comparison of stress-strain curves
as a function of chemical composition and strain rate are summarized in Fig. 6.6.
Whereas Fig. 6.6a–c shows tensile deformation behaviour of Fe–16Cr–6Mn–3Ni–
0.05C steel (a) and Fe–16Cr–6Mn–9Ni–0.05C steel (c) in comparison with Fe–
16Cr–6Mn–6Ni–0.05C steel (b) as a function of temperature, Fig. 6.6d shows the
influence of the strain rate at room temperature.
The Fe–16Cr–6Mn–3Ni–0.05C steel exhibited a well-developed sigmoidal
shape of stress-strain curve at all deformation temperatures indicating that a pro-
nounced martensitic phase transformation occurred in this steel up to a temperature
of 80 °C. Whereas at RT about 68% of a′-martensite was formed, about 7% of a′-
martensite was still detected at 80 °C. The change of strain rate between 10−3 s−1
and 10−2 s−1 had only a minor influence on deformation behaviour and the a′-
martensite content formed. However, for all strain rates at room temperature and
even at temperatures of up to 60 °C discontinuities were observed in stress-strain
curves. The serrated flow of this steel observed in a certain range of temperatures
and strain values was caused by PLC effect, which was introduced already in
Sect. 2.4.2.2 and which will be discussed for Fe–16Cr–6Mn–3Ni–0.05C TRIP steel
in detail later in Sect. 7.3, which deals with macroscopic strain localizations. An
increase in temperature between RT and 80 °C has no significant influence on
216 6 Object of Investigations—High-Alloy …

Fig. 6.6 Comparison of the tensile deformation behaviour of the investigated steel variants as a
function of the chemical composition, the deformation temperature and the strain rate. a Fe–16Cr–
6Mn–3Ni–0.05C TRIP steel. b Fe–16Cr–6Mn–6Ni–0.05C TRIP/TWIP steel. c Fe–16Cr–6Mn–
9Ni–0.05C TWIP steel. a–c Tested at strain rate of 10−3 s−1. d Three Fe–16Cr–6Mn–xNi–0.05C
steel variants tested at RT and different strain rates. In addition, the volume fractions of a′-
martensite determined by ferritescope measurements are indicated

deformation behaviour of steel with highest austenite stability. A marginal decrease


in yield strength and UTS is observed (see Fig. 6.6c). The Fe–16Cr–6Mn–6Ni–
0.05C steel exhibited stress-strain behaviour somewhere between those of steels
with lowest and highest austenite stability. As demonstrated already in Fig. 6.4a, an
increase in temperature results in a decrease in volume fraction of martensitic phase.
Whereas stress-strain curves at RT < T < 60° still exhibited a sigmoidal shape, this
shape changed at temperatures of 80 °C. This is in agreement with calculated
volume fraction of a′-martensite, which decreased from 40% at RT down to 0% at
80 °C. Thus, the transition temperature from a pronounced martensitic phase
transformation to a pronounced mechanical twinning is between 60 and 80 °C. The
strain rate in range of 10−3 s−1 < e_ < 10−2 s−1 has a moderate influence on
stress-strain behaviour of all three steel variants (see Fig. 6.6d). As expected, yield
stress and UTS decreased. A decrease in elongation to failure is detected as well.
This is caused by reduced formation of a′-martensite for Fe–16Cr–6Mn–6Ni–0.05C
steel as shown by indicated volume fractions of a′-martensite. In Fe–16Cr–6Mn–
9Ni–0.05C steel, reduced twinning activity is responsible for decrease in ductility.
6.3 Mechanical Behaviour 217

6.3.2 Uniaxial Cyclic Loading

Glage et al. [13, 27] studied intensively the deformation behaviour of the three steel
variants under cyclic loading at room temperature under total strain control. The
cyclic deformation tests were carried out at constant strain ratio of R = −1 in a total
strain range of 1  10−3 < ea;t < 3  10−2 at a constant strain rate of 4  10−3 s−1.
The cyclic loading experiments were accompanied by in situ measurement of fer-
romagnetic phase fraction using Fisher-ferritescope.
Figure 6.7 summarizes cyclic deformation curves as well as evolution of
a′-martensite content, which is obtained from ferromagnetic phase fraction recorded
during cyclic loading tests. It becomes obvious that chemical composition resulting
in different austenite stabilities has a significant influence on cyclic stress-strain
curves (CSSC). Thus, Fe–16Cr–6Mn–3Ni–0.05C steel (Fig. 6.7a) exhibits a sig-
nificant cyclic hardening in the whole range of investigated total strain amplitudes.
In addition, the onset of cyclic strain hardening is shifted to lower number of cycles
and martensite fraction increases with an increase in total strain amplitude. The
pronounced cyclic hardening is followed by a region of stress saturation until final
failure of specimens. The Fe–16Cr–6Mn–6Ni–0.05C steel shows CSSCs
(Fig. 6.7b), which can be subdivided into three different regions. First, a primary
hardening is observed, which is followed by a region of saturation or at low strain
amplitudes even of cyclic softening continuing with a pronounced secondary cyclic
hardening behaviour.
The onset of secondary cyclic hardening is shifted as well to lower number of
cycles and becomes more pronounced with an increase in total strain amplitude.
The CSSCs of Fe–16Cr–6Mn–9Ni–0.05C steel (Fig. 6.7c) exhibit a primary
hardening at low strain amplitudes, which becomes more pronounced with
increasing strain amplitude followed by cyclic softening or moderate increase in
stress close to fatigue failure. At high strain amplitudes, pronounced hardening is
observed without any saturation of stress until fatigue failure. The differences in
CSSCs can be explained by activation of different dominant deformation mecha-
nisms. As seen in Fig. 6.7a, b, cyclic deformation behaviour of steel variants Fe–
16Cr–6Mn–3Ni–0.05C and Fe–16Cr–6Mn–6Ni–0.05C is accompanied by a sig-
nificant increase in ferromagnetic phase fraction, which is attributed to formation of
a′-martensite (after correction for initial amount of d-ferrite and spontaneous
martensite). Thus, the evolution of a′-martensite is obviously different in Fe–16Cr–
6Mn–3Ni–0.05C and Fe–16Cr–6Mn–6Ni–0.05C steels, whereas in Fe–16Cr–6Mn–
9Ni–0.05C steel no a′-martensite is detected at all. The Fe–16Cr–6Mn–3Ni–0.05C
steel exhibits higher a′-martensite fraction compared to Fe–16Cr–6Mn–6Ni–0.05C
steel. For all investigated strain amplitudes, the formation of a′-martensite starts
directly at beginning of cyclic deformation. However, a′-martensite formation
becomes more intense with an increase in strain amplitude. In Fe–16Cr–6Mn–6Ni–
0.05C steel, an incubation period for a′-martensite nucleation is observed, which is
decreasing with an increase in strain amplitude. The incubation period is deter-
mined by necessary threshold of cumulative plastic strain [28].
218 6 Object of Investigations—High-Alloy …

Fig. 6.7 Cyclic deformation behaviour of investigated steel variants and evolution of a′-
martensite volume fraction. a Fe–16Cr–6Mn–3Ni–0.05C steel. b Fe–16Cr–6Mn–6Ni–0.05C steel.
c Fe–16Cr–6Mn–9Ni–0.05C steel. Reproduced from [13]. Permission of Elsevier

Thus, with increasing total strain amplitude threshold of cumulative plastic strain
is decreasing and the incubation period shortened. Consequently, different defor-
mation mechanisms than a′-martensite formation should be activated in Fe–16Cr–
6Mn–9Ni–0.05C steel, which is mechanical twinning similar to quasi-static load-
ing. More detailed description of resulting microstructures will be provided in
Sect. 6.4.
The activation of different deformation mechanisms depending on the austenite
stability and the stacking-fault energy under cyclic loading has a significant
influence on the fatigue life as shown in Fig. 6.8. In the region of low cycle fatigue
6.3 Mechanical Behaviour 219

Fig. 6.8 Influence of the


austenite stability on the
fatigue life of Fe–16Cr–6Mn–
xNi–0.05C cast TRIP/TWIP
steels. Reproduced from [13].
Permission of Wiley VCH

(LCF), an increase in austenite stability yields an improvement of fatigue life. In


contrast, in the high cycle fatigue (HCF) regime, lower austenite stability results in
an increase in fatigue life.
According to monotonic tests under tensile and compressive load, the influence
of deformation temperature on cyclic deformation behaviour was investigated in a
temperature range 10 °C < T < 200 °C [28]. Thus, Biermann et al. [28] showed
that with an increase in temperature, the onset of strain-induced martensitic phase
transformation is shifted depending on applied total strain amplitude to higher
number of cycles and is suppressed nearly completely at T = 50 °C even at highest
strain amplitude of ea;t = 12  10−3. In addition, at a given total strain amplitude
stress amplitude as well as secondary cyclic hardening decreases significantly with
an increase in temperature. At T > 50 °C, a remarkable reduction of fatigue life
occurs, which is in agreement with the fact that the formation of strain-induced
a′-martensite is suppressed completely.

6.3.3 Planar-Biaxial Loading

Kulawinski et al. [29] and Ackermann et al. [14] investigated the deformation
behaviour of Fe–16Cr–6Mn–6Ni–0.05C steel under biaxial monotonic and cyclic
loading conditions, respectively. The biaxial monotonic deformation behaviour was
studied under constant load levels yielding in biaxial tension, biaxial compression
and biaxial shear experiments. Figure 6.9a shows a comparison of results obtained
for three biaxial loading conditions regarding equivalent stress versus true equiv-
alent plastic strain curves with results obtained from uniaxial tensile test. For biaxial
tests, equivalent stress values were determined according to the partial unloading
method described in [29]. Comparable to uniaxial tensile tests, biaxial tests yield a
strong strain hardening, which is caused by a pronounced martensitic phase
220 6 Object of Investigations—High-Alloy …

Fig. 6.9 Results of investigations on the biaxial deformation behaviour of cast Fe–16Cr–6Mn–
6Ni–0.05C TRIP steel. a Equivalent stress versus true equivalent plastic strain curve under biaxial
loading conditions with constant load ratio resulting in biaxial tension, biaxial compression and
biaxial shear in comparison with uniaxial tensile test. b Evolution of martensitic volume fraction
corresponding to the stress-strain curves shown in (a). c Results of the biaxial in-phase and
out-of-phase cyclic loading experiments in comparison with results of uniaxial cyclic deformation.
Von Mises equivalent strain versus number of cycles to failure curve. a, b Reproduced from [29].
c Reproduced from [14]. Permission of Elsevier

transformation. The strain-induced martensitic phase transformation starts directly


after reaching yield point (cf. Fig. 6.9b).
Comparing the three different biaxial loading conditions and the uniaxial tensile
test, it becomes obvious that under biaxial loading conditions, strain-induced
martensitic phase transformation is enhanced significantly. Among the three biaxial
loading conditions, biaxial loading under pure shear conditions revealed the highest
tendency for martensitic phase transformation. It should be noted that absolute
values of volume fractions of a′-martensite cannot be compared directly with results
from uniaxial tensile or compressive loading tests due to influence of grain size and
segregations of alloying elements within as-cast microstructure.
The biaxial fatigue behaviour was studied under biaxial in-phase and
out-of-phase cyclic loading conditions using cruciform specimens [14]. Different
6.3 Mechanical Behaviour 221

phase shifts of the principal strains in the range between equibiaxial push–pull and
equibiaxial shear were investigated. Comparable to uniaxial cyclic loading exper-
iments, a strain-induced martensitic phase transformation is observed after an
incubation time, which is dependent on the resolved plastic strain amplitude
causing pronounced cyclic hardening. However, no significant correlation between
phase shift and martensite formation rate or cyclic hardening rate is found.
Moreover, tests under pure biaxial shear conditions yielded increased number of
cycles to failure, which is accompanied by slowest martensite formation rate.

6.4 Microstructure Evolution

6.4.1 Fe–16Cr–6Mn–6Ni–0.05C Steel

The chemical composition of Fe–16Cr–6Mn–6Ni–0.05 steel yields in an austenite


stability, where Ms temperature is well below room temperature (see Table 6.1) and
MPT can be triggered by additional plastic deformation. As learned from investi-
gations on the stress-strain behaviour under tensile and compressive loading at RT,
a pronounced martensitic phase transformation is responsible for sigmoidal shape of
stress-strain curve and pronounced strain hardening.
The strain-induced martensitic phase transformation during mechanical loading
at RT occurs via formation of deformation bands. The formation of deformation
bands starts locally very early in deformation process during quasi-static tensile
loading directly after passing yield strength. First deformation bands are initiated in
well-oriented grains exhibiting high Schmid factor l (close to l = 0.5) for acti-
vation of slip on f111g planes. With an increase in plastic strain, both the number
of these deformation bands and their thickness are increasing. In addition, the
number of grains containing deformation bands increases as well since dislocation
slip on f111g planes with lower Schmid factor is also activated. Figure 6.10 shows
a sequence of SEM micrographs taken in backscattered electron (BSE) contrast at
different levels of applied plastic strain.
Similar observations were made during cyclic loading experiments. However,
here the formation of deformation bands depends significantly on the applied total
strain amplitude. In agreement with the investigations of Glage et al. [13], for a high
total strain amplitude ea;t  5  10−3 the formation of a′-martensite starts already
below 100 cycles (cf. Fig. 6.7d). Again, the grain orientation has a significant
influence on onset of formation of deformation bands. Figure 6.11 shows a
sequence of BSE micrographs taken at different number of cycles. It is obvious that
for austenitic grain studied, the formation of deformation bands starts within the
first loading cycle. Already at five cycles, pronounced slip is activated on two
different slip systems. With an increase in number of cycles, the number of
deformation bands and their thickness increase as well. In addition, a third slip
system is activated at N > 30 cycles.
222 6 Object of Investigations—High-Alloy …

Fig. 6.10 Evolution of deformation bands in dependence on the applied plastic strain observed
during in situ tensile test of Fe–16Cr–6Mn–6Ni–0.05C steel at RT. a Initial state e = 0%.
b e = 0.9%. c e = 2.8%. d e = 9.8%. SEM micrograph taken in BSE contrast. Large-angle grain
boundaries are indicated by black lines and activated slip systems by dashed white lines. 1—
primary slip system, 2—secondary slip system. Loading axis horizontal. According to [30]

Fig. 6.11 Evolution of deformation bands in dependence on the applied number of cycles N at a
total strain amplitude of ea;t = 5  10−3 observed during in situ cyclic loading test of Fe–16Cr–
6Mn–6Ni–0.05C steel at RT. a First cycle. b 30 cycles. c 50 cycles. d 100 cycles. SEM
micrograph taken in BSE contrast. AOI within one individual grain of the as-cast microstructure.
Loading axis horizontal. Reproduced from [31]. Permission of Elsevier

Under both tensile and cyclic loading conditions, the deformation bands at a
whole do not develop across entire large austenitic grains. Quite often, individual
deformation bands end inside grains.
At higher strain values, lentil-like areas with different orientation contrast
(marked by black arrows) appear inside these deformation bands as shown in
Fig. 6.12 after tensile loading up to 8% of elongation (a) and after cyclic loading up
to 500 cycles at ea;t = 5  10−3 (b). Similar to the deformation bands, their size and
number are increasing with an increase in plastic strain as well as increase in
number of cycles. These lentil-like areas can be attributed to strain-induced
a′-martensite as shown later.
In addition, formation of deformation bands is accompanied by formation of
pronounced surface relief. Depending on inclination angle of Burgers vector with
respect to specimen surface, more or less pronounced surface displacement is
observed. However, due to volume dilation accompanying formation of a′-mar-
tensite, the areas related to a′-martensite appear still on top of surface profile of
6.4 Microstructure Evolution 223

Fig. 6.12 Individual deformation bands with lentil-like areas (black arrows) related to
a′-martensite. SEM micrographs taken in BSE contrast. a Fe–16Cr–6Mn–6Ni–0.05C steel after
tensile loading at RT up to e = 8%. b Fe–16Cr–6Mn–6Ni–0.05C steel after cyclic loading at RT
with a total strain amplitude of ea;t = 5  10−3. White arrows indicate deformation bands on the
secondary slip system, which are less pronounced. Loading axis horizontal. Reproduced from [31].
Permission of Elsevier

Fig. 6.13 Examples for pronounced surface profile caused by formation of deformation bands
along different slip systems and a′-martensite (marked by arrows). SEM micrographs taken in SE
contrast). a–c Different grains within specimen of Fe–16Cr–6Mn–6Ni–0.05C steel cyclically
deformed with total strain amplitude of ea;t = 5  10−3 up to 100 cycles. Reproduced from [31].
Permission of Elsevier

deformation bands and, thus, can be identified clearly even in secondary electron
(SE) contrast images. Figure 6.13 shows three examples obtained after cyclic
loading at ea;t = 5  10−3 up to 100 cycles.
The performance of EBSD measurements revealed clearly the bcc crystal lattice
of formed lentil-like islands within the deformation bands. In addition, the
microstructure of the deformation bands is identified to be hex crystal lattice, which
is in agreement with the nature of e-martensite known from literature (cf. Sect. 4.2).
The formation of a′-martensite is observed solely within deformation bands. In
some cases, a′-martensite nuclei are observed at intersection points of deformation
bands developed according to different activated slip systems. However, quite often
a′-martensite is detected in single deformation band without intersection of a
deformation band related to a secondary slip system (cf. Fig. 6.12). Figure 6.14
224 6 Object of Investigations—High-Alloy …

Fig. 6.14 Appearance of deformation bands in the austenitic matrix exhibiting hex crystal lattice
and containing a′-martensite nuclei after cyclic loading of Fe–16Cr–6Mn–6Ni–0.05C steel at RT
with total strain amplitude of ea;t = 5  10−3 up to 100 cycles. Results obtained by EBSD
measurements. a Phase map, b Orientation map. c Orientation map bcc phase with band contrast
and indicated characteristic misorientation of a′-martensite nuclei (red, yellow lines) and
Kurdjumov–Sachs phase orientation relationship (white lines). d Orientation map hex with band
contrast and phase orientation relationships fcc/hex (white lines) phase and hex/bcc (yellow lines).
Orientation map in inverse pole figure colouring according to the loading axis. Loading axis
horizontal. Reproduced from [31]. Permission of Elsevier

summarizes results obtained from EBSD measurements on deformation bands


developed after cyclic loading with ea;t = 5  10−3 up to 100 cycles at RT.
Figure 6.14a documents phase composition of investigated area. Clearly, formation
of deformation bands on two different slip systems is visible. Whereas the thicker
ones correspond to the primary slip system, the few thinner ones are related to the
secondary system. The deformation bands formed in austenitic matrix
6.4 Microstructure Evolution 225

(red) exhibiting a hex crystal lattice (yellow) contain numerous areas with bcc
crystal lattice—the a′-martensite.
The various crystallographic orientations of three different constituents of the
microstructure—austenite, e-martensite and a′-martensite—become obvious from
Fig. 6.14b. The austenitic matrix exhibits a unique crystallographic orientation,
which is a h111i direction parallel to the loading axis. It becomes obvious that also
deformation bands with hex crystal lattice reveal a unique crystallographic orien-
tation. However, areas of a′-martensite appear with quite different crystallographic
orientations. Two characteristic misorientations occurring between neighbouring a′-
martensite areas are detected.
The first one corresponds to a twin boundary (R3 boundary), which is charac-
terized by a misorientation axis/angle pair of 60° h111i indicated by red lines in
Fig. 6.14c. The second misorientation—less often detected—corresponds to a R11
boundary with a rotation axis/angle pair of 50° h001i (yellow lines in Fig. 6.14c).
In addition, characteristic orientation relationships between austenite and e-mar-
tensite, austenite and a′-martensite, and e-martensite and a′-martensite are detected.
According to Kurdjumov and Sachs [32], fcc/bcc phase orientation relationship
f111fcc k f110gbcc and h110ifcc k h111ibcc is observed indicated by white lines in
Fig. 6.14c. Figure 6.14d documents the fcc/hex orientation relationship f111gfcc k
f001ghcp (white lines) and the hex/bcc orientation relationship f001ghcp k f110gbcc
(yellow lines) according to Schumann [33].
Influence of plastic strain. The martensitic phase transformation is influenced
significantly by applied plastic strain turning out from EBSD and XRD investi-
gations on interrupted in situ testing as well as stopped tensile and compressive
tests. Thus, strain-induced martensitic phase transformation starts passing yield
point with formation of deformation bands followed by formation of a′-martensite
within these bands. Consequently, the amount of a′-martensite formed by an
increase in plastic strain is increasing continuously, whereas the amount of hex e-
martensite evolves via a maximum at intermediate plastic strain, which is proofed
by both EBSD and XRD measurements on stopped tensile (e.g. [11]) and com-
pressive tests (e.g. [34]). In addition, Martin et al. [35] showed a difference for the
evolution of e-martensite and a′-martensite during tensile and compressive loading.
Thus, the formation of e-martensite is favoured under compressive loading due to
small volume contraction between 0.5 and 1.5 vol. % [36]. However, the formation
of a′-martensite, which is accompanied by a volume dilation of about 2 (to 5) vol.
% [36] occurs preferred under tensile loading conditions. Thus, the amount of e-
martensite is increased slightly during compressive deformation, whereas the
amount of strain-induced a′-martensite is higher under tensile loading conditions.
According to Martin et al. [35], maximum of volume fraction of e-martensite occurs
at about 10% of elongation. However, it is shifted to smaller strain values with
decreasing grain size [37]. Exemplarily, Fig. 6.15 shows the microstructure
developed during tensile test at 10% of elongation and at elongation to rupture. It
should be noted that EBSD results are obtained on different specimens. However, it
is visible that both the amount of e-martensite and a′-martensite is increased
226 6 Object of Investigations—High-Alloy …

significantly at elongation to failure (cf. Fig. 6.15a, c). But, it is also observed that
not whole volume fraction of deformation bands transforms into a′-martensite. An
additional microstructural feature becomes apparent from these investigations.
Already at 10% of elongation, microtwins (red lines, black arrows Fig. 6.15b, d) are
visible in proximity to deformation bands with hex crystal lattice. At elongation to
failure, the amount of microtwins is even enlarged. In addition, an increase in
number of cycles during fatigue leads to both the formation of new DBs and a
thickening of DBs formed previously [38]. Furthermore, it turned out from EBSD
measurements that bands formed at low number of cycles are indexed still as

Fig. 6.15 Evolution of strain-induced martensitic phase transformation obtained under tensile
loading of Fe–16Cr–6Mn–6Ni–0.05C steel at RT up to 10% of elongation and at failure
(e = 60%). a, c Phase maps. b, d Band contrast map. Red lines: Twin boundaries (R3). White
arrows indicating d-ferrite. Loading axis horizontal. a, b Reproduced from [39]. c, d Reproduced
from [40]. Permission of Elsevier
6.4 Microstructure Evolution 227

Fig. 6.16 Evolution of deformation bands in dependence on the number of cycles during fatigue
loading of Fe–16Cr–6Mn–6Ni–0.05C steel at RT with a total strain amplitude of ea;t = 3  10−3.
Results of EBSD measurements. Phase maps with grey as austenite, yellow as e-martensite and
blue of a′-martensite and d-ferrite. a After N1 = 250 cycles. b After N2 = 500 cycles. Loading axis
horizontal. Reproduced from [38]. Permission of Elsevier

austenite, but with a lower band contrast. With increasing number of cycles,
identified crystal lattice inside the DBs shifts from fcc to hex.
Figure 6.16 shows exemplarily two EBSD maps of same AOI at N1 = 250
(a) and N2 = 500 (b) cycles, respectively [38]. Clearly, at N1 , deformation bands
with hex crystal lattice as well as a′-martensite nuclei within these bands are
detected. In addition, deformation bands are observed in austenitic matrix (grey) as
dark lines (marked by black arrows). These bands still have austenitic structure, but
are characterized by a lower band contrast caused by higher defect density. At N2 ,
number of DBs, their thickness as well as amount of e-martensite and a′-martensite
have increased significantly. Deformation bands or areas within these bands
detected previously with a fcc crystal lattice transformed into e-martensite (marked
by black ellipses). In addition, areas within DBs detected previously as e-martensite
transformed into a′-martensite (marked by black rectangles) at N2 . In addition, it
turned out that subgrain boundaries occurring within one individual austenitic grain
(marked by white arrows) result in small angular deviations of deformation bands
formed along primary slip system (regions marked by white ellipses).
Influence of temperature. As already well demonstrated by stress-strain behaviour,
temperature has a significant influence on onset of strain-induced martensitic phase
transformation as well. An increase in temperature leads to significant reduction of
amount of formed e-martensite and a′-martensite. The influences of both—plastic
strain and temperature—are demonstrated in Fig. 6.17 at an elongation of 10% and
at failure at 100 °C. In comparison with results shown in Fig. 6.15 at same elon-
gations significant differences become obvious. Already at 10% of elongation, a
pronounced reduction of strain-induced martensitic phase transformation to a′-
martensite is apparent. Along with deformation bands with their hex crystal lattice,
only marginal volume fraction of a′-martensite can be recognized (white arrows in
228 6 Object of Investigations—High-Alloy …

Fig. 6.17a indicate d-ferrite). Instead, few microtwins are visible (black arrows
Fig. 6.17b). The amount of microtwins is increased significantly at failure. Locally,
only small amount of a′-martensite (white arrows in Fig. 6.17c) and e-martensite is
detected. This is in good agreement with analysis of stress-strain behaviour since a
change of the stress-strain curve from a sigmoidal shape to a classical stress-strain
curve is observed at about 100 °C. It is also in agreement with the measurements of
the ferromagnetic phase fraction, as no a′-martensite is detected at 100 °C.

Fig. 6.17 Influence of temperature on the evolution of the strain-induced martensitic phase
transformation. Results of EBSD measurements obtained after tensile loading of Fe–16Cr–6Mn–
6Ni–0.05C steel at 100 °C at 10% of elongation (a, b) and at elongation to failure (e = 33%) (c, d).
a, c Phase maps. b, d Band contrast maps with indicated twin boundaries (red lines). a,
b Reproduced from [39]. c, d Reproduced from [40]. Permission of Elsevier
6.4 Microstructure Evolution 229

Similar observations on influence of temperature on microstructure are made


during cyclic loading. At 60 °C, no martensitic phase transformation is observed
anymore for high total strain amplitudes. Instead, higher amounts of microtwins are
detected (cf. [28]), whereas at 200 °C dislocation glide is observed only.
Influence of local chemical composition. Among large grain size, a typical feature
of as-cast microstructure is the dendritic structure characterized by opposed
microsegregations of elements Cr and Ni. Alloying elements like manganese,
carbon and nitrogen have a tendency to segregate as well in a dendritic structure.
Figure 6.18 shows results of combined EBSD/EDS analysis of an AOI in a Fe–
16Cr–6Mn–6Ni–0.05C. Figure 6.18a shows dendritic microstructure using band
contrast map. The crystallographic orientation map shown in Fig. 6.18b reveals
orientation variations within individual austenitic grains caused by the subgrains
formed during solidification process. Figure 6.18c, d shows EDS element maps for
nickel (c) and chromium (d). It is clearly visible that these two elements are enri-
ched in opposed regions. Thus, bright grey regions in Fig. 6.18a are enriched with
nickel, whereas darker areas are enriched by chromium. Depending on the segre-
gated elements, the driving force for martensitic phase transformation of austenite
can be influenced locally. This has a significant influence on local activation of
different deformation mechanisms. Thus, the stability of austenite as well as
stacking-fault energy varies locally depending on local concentration of alloying
elements and chemical gradients.

Fig. 6.18 Dendritic structure of the as-cast microstructure with opposed segregation of the
elements Ni and Cr of Fe–16Cr–6Mn–6Ni–0.05C steel. Results of combined EBSD/EDS
measurements. a, e Crystallographic orientation maps. b, f Band contrast maps with indicated
large-angle boundaries. c, g EDS element maps of nickel and d chromium. e–g Enlarged region
marked by rectangle in (a) with indicated grain 1. Arrows in (g) indicate regions with enhanced
nickel enrichment in grain part 1a
230 6 Object of Investigations—High-Alloy …
6.4 Microstructure Evolution 231

JFig. 6.19 Two examples of results obtained by post-mortem EBSD measurements on specimen of
Fe–16Cr–6Mn–6Ni–0.05C steel after quasi-hydrostatic, high-pressure experiment up to 18 GPa.
a–f Larger overview on several austenitic mother grains. g–l Enlarged view at higher
magnification within one individual austenitic mother grain. a, g SEM images using BSE
contrast. b, h Phase maps. c, i Crystallographic orientation map of fcc phase. d, j Crystallographic
orientation maps of hexagonal phases. e, f, k, l Crystallographic orientation maps of bcc phase. e,
k Colour code of the inverse pole figure with respect to the normal direction. f, l Colour code of the
inverse pole figure with respect to the transverse direction. Reproduced from [15]. Permission of
Springer

As shown by Martin et al. [41], there is a direct correlation between local


chemical composition, corresponding difference between Gibbs energies of
austenite and martensite, martensite start temperature Ms , calculated stacking-fault
energy, observed stacking-fault density and prevailing deformation mechanism.
Figure 6.18e–g is enlarged area of Fig. 6.18a. Special attention has to be paid on
the grain 1 consisting of three subgrains (1a, 1b, 1c). Especially, subgrain part 1a is
of interest for further investigation due to reduced grain size compared to other
grains. In addition, here two Ni enriched areas (marked by arrows) are separated by
a region with less Ni content.
Influence of hydrostatic pressure. The microstructure of metastable steel deformed
under monotonic and cyclic biaxial planar loading conditions is comparable to
microstructures obtained after uniaxial monotonic or cyclic loading. The
strain-induced martensitic phase transformation occurs via formation of deforma-
tion bands with hex crystal lattice transforming into a′-martensite with an increase
in plastic strain.
However, the phase transformation during monotonic biaxial loading is more
intense than under uniaxial tensile conditions [29]. Similar, cyclic loading under
shear conditions yields the most pronounced martensitic phase transformation
during biaxial cyclic loading leading to improved fatigue life [14].
Quasi-hydrostatic high-pressure experiments up to 18 GPa revealed [15] that it is
possible to obtain a phase transition of metastable austenitic Fe–16Cr–6Mn–6Ni–
0.05C TRIP steel into high-pressure e-iron phase with a hcp crystal lattice, which is,
normally, thermodynamically stable in pure iron at pressures of about 10 GPa only.
Figure 6.19 shows two examples of post-mortem EBSD analysis of a specimen
after a quasi-hydrostatic, high-pressure experiment [15]. It is clearly visible that
deformation bands with pronounced surface profile consisting of hex and bcc phase
are formed, which are labelled as e1 and a01 (marked by white ellipses). The in situ
synchrotron XRD measurements revealed that these bands are formed at pressures
below 6–8 GPa. In contrast to e-martensite ðe1 Þ occurring in these deformation
bands, the high-pressure e-iron (called e2 ) is formed across whole grains. Thus,
strain- or deformation-induced e-martensite ðe1 Þ can be well separated from
pressure-induced e-iron phase ðe2 Þ. In addition, during unloading path of
high-pressure experiment part of e2 -phase transformed into bcc crystal lattice
occurring as needle-like martensite labelled as a02 . The difference between the two
martensite variants a01 and a02 becomes also apparent.
232 6 Object of Investigations—High-Alloy …

Fig. 6.20 Schematic summary of the characteristic phase transformation processes as a function
of hydrostatic pressure in combination with EBSD maps (red: austenite, yellow: hexagonal (e1 , e2 )
and blue: martensite (a01 , a02 ). Open red squares—compression path. Open black squares—
decompression bath. At 14 GPa during decompression a blow-out occurred terminating the test.
Reproduced from [15]. Permission of Springer

The microstructure evolution during quasi-hydrostatic high-pressure experi-


ments evolved from post-mortem EBSD measurements and in situ synchrotron
XRD measurements is summarized in Fig. 6.20. Thus, clearly three different pro-
cesses can be distinguished:
(i) Strain- or deformation-induced formation of deformation bands with pro-
nounced surface profile consisting of e1 and a01 at pressure below 6 GPa
caused by deviations from fully hydrostaticity.
(ii) Pressure-induced formation of e-iron phase ðe2 Þ at pressures above 6–8 GPa
(iii) Formation of thin plate-like a02 martensite in areas of pressure-induced e-iron
phase ðe2 Þ during unloading.
Influence of strain rate. Among above-discussed parameters of influence on
martensitic phase transformation, the influence of strain rate is important as well.
Thus, an increase in strain rate up to 103 s−1 leads to a significant reduction of
martensitic phase transformation due to adiabatic heating, which counteracts the
driving force for a′-martensite formation [42]. However, uniaxial compression tests
performed at RT and a strain rate of 103 s−1 revealed still about 20% of
6.4 Microstructure Evolution 233

strain-induced a′-martensite. Comparable to small strain rates, the strain-induced


phase transformation occurs via formation of deformation bands with e-martensite
and nucleation of a′-martensite within these bands. Even at higher strain rates of
104 s−1 obtained during flying-plate impact test [43], the strain-induced martensitic
phase transformation is observed.
Nature of deformation bands. The strain-induced martensitic phase transformation
observed in the high-alloy Fe–16Cr–6Mn–xNi–0.05C steels with low and medium
nickel content occurs in the sequence c-austenite (fcc) ! e-martensite (hex) ! a′-
martensite (bcc), which is described in literature (cf. Sect. 3). The e-martensite
formed via this sequence is discussed as a metastable, intermediate phase prior to
a′-martensite formation. The e-martensite formed in deformation bands is detected
by EBSD with a hex crystal lattice.
e-martensite is also well known in high-manganese TWIP steels (Mn > 12%).
Here, e-phase is a thermally induced martensite and is present already in initial
microstructure [44]. The crystal lattice of e-martensite is hex as well. The appear-
ance of thermally induced e-martensite is completely different to e-martensite
detected in deformation bands. Thermally induced e-martensite appears as a blocky
structure covering large areas of austenitic parent grains. The amount of e-mar-
tensite in these steels depends on carbon content. The amount of e-phase is reduced
by an increase in carbon [45].
As shown before, Ackermann et al. [15] demonstrated that under
quasi-hydrostatic, high-pressure experiments up to 18 GPa, the high-pressure e-iron
phase with hcp crystal lattice is formed in metastable high-alloy Fe–16Cr–6Mn–
6Ni–0.05C and is clearly different from strain-induced e-martensite within defor-
mation bands.
However, the question arises: What is the nature of strain-induced e-martensite
found in deformation bands? High-resolution ECCI analyses in SEM were performed
on deformation bands in cyclically or tensile deformed specimens [20]. It turned out
that deformation bands formed in high-alloy Fe–16Cr–6Mn–xNi–0.05C TRIP steels
are formed by stacking-faults. Figure 6.21 shows individual stacking-faults with a
small dissociation width of partial dislocations in austenitic matrix concurrently to
deformation bands on primary slip system after tensile deformation up to 10% of
elongation (Fig. 6.21a) or after cyclic loading (Fig. 6.21b). However, these small
stacking-faults are related to slip systems with lower Schmid factor l. Thus,
stacking-faults are not that much extended. However, on primary slip systems the two
partial dislocations—leading and trailing partial—form largely extended stacking-
faults due to applied stress [46]. The density of extended overlapping stacking-faults
within deformation bands cannot be detected by SEM anymore.
However, Fig. 6.21c shows the beginning of formation of a deformation band at
a tensile strain of 8%. Clearly, a band-like structure with an inclination angle of
about 40° with respect to loading axis is visible. Inside the band, SFs on three
different slip systems marked by numbers becomes apparent. Whereas the density
of SFs is higher at upper left region of the band, the density of SF in the middle and
lower right part is much less. Nevertheless, the interaction of SFs on three different
234 6 Object of Investigations—High-Alloy …

Fig. 6.21 Appearance of individual stacking-faults after plastic deformation of Fe–16Cr–6Mn–


6Ni–0.05C steel in the austenitic steel matrix concurrently to deformation bands on primary and
secondary slip systems. a After tensile deformation. b After cyclic deformation. c Onset of the
formation of an individual deformation bands with individual SF on different slip planes. In
addition, individual regular dislocations are visible (black arrows). d SF on at least three different
slip planes with intersection points, which are favoured places for the formation of martensite
nuclei. a, b Reproduced from [20]. c Reproduced from [26]. d Reproduced from [47]. Permission
of Elsevier and Taylor&Francis, respectively

f111g planes can be recognized. Similar situation is shown by Fig. 6.21d for
interacting SFs in the austenitic matrix close to a deformation band (upper right
corner). These intersection points of individual SFs on different slip planes are
favoured places for martensitic phase transformation.
TEM investigations as well as t-SEM studies performed on tensile deformed
specimens proved the appearance of individual stacking-faults in metastable aus-
tenitic matrix and the high density of largely extended stacking-faults inside
deformation bands as shown in Fig. 6.22. Stacking-faults are visible on different
slip systems interacting and overlapping and even reactions of leading and trailing
partial dislocations on different slip planes forming sessile Lomer-Cottrell locks are
observed (see Fig. 6.22d). Especially at the boundaries of deformation bands, LC
locks are observed causing thickening of deformation bands according to the model
of Cohen and Weertman [48]. Moreover, TEM investigation performed on
non-deformed TRIP steel specimens revealed along with individual stacking-faults
6.4 Microstructure Evolution 235

and LC locks a further defect related to SFs—so-called SF tetrahedra [6]. SF


tetrahedra are formed by cutting of stacking-faults lying on various f111g planes
[49]. These SF tetrahedra can occur either as tetrahedra fully or partially closed and
are existing together with individual SFs already in non-deformed, as-cast material
as preferred nucleation sites for formation of deformation bands.
Thus, it becomes evident from ECCI as well as TEM and t-SEM investigations
that the hex crystal lattice detected by EBSD measurements within deformation
bands is the consequence of high density of stacking-faults grouped together inside
these bands. Intrinsic stacking-faults formed on each second lattice plane cause a
change in the stacking-sequence of atomic layers from ABCABC sequence of fcc
materials into ABCABABC sequence of hcp materials (see Sect. 2.2.1).
Consequently, in the present work e-martensite is regarded as a highly distorted and
faulted austenite (high density of stacking-faults) and not as an individual phase

Fig. 6.22 Arrangement of stacking-faults in tensile deformed Fe–16Cr–6Mn–6Ni–0.05C steel


obtained on electron transparent foils. a Bright field image of conventional TEM showing
deformation band consisting of several overlapping stacking-faults (marked by white lines) and
individual stacking-faults with small width (marked by white arrows). b, c t-SEM images showing
individual stacking-faults on two different slip systems. d Bright field images of t-SEM showing
reaction between stacking-faults on different slip planes forming Lomer-Cottrell locks.
a Reproduced from [50]. b–d Reproduced from [39]. Permission of Elsevier
236 6 Object of Investigations—High-Alloy …

(e.g. [51]). Therefore, in the following these bands with a crystal lattice indexed by
EBSD as hexagonal caused by SFs on in average each second lattice plane are
called stacking-fault bands.
This aspect is supported by XRD measurements performed by Martin et al.
[24, 52]. It is shown that the diffraction peaks related to e-martensite occurring in a
diffraction profile of deformed TRIP steel specimens can be described by a structure
model of high density of intrinsic stacking-faults placed on in average each second
lattice plane. The best match of measured diffraction pattern and fit function based
on this structure model is obtained for a probability of intrinsic SFs of about 1.5%
for both austenite and e-martensite. Consequently, the crystal lattice of these bands
is changing from fcc to hex with increasing density of stacking-faults inside
deformation bands during plastic deformation. This is in agreement with results of
EBSD measurements after cyclic loading where deformation bands detected with a
fcc crystal lattice at lower number of cycles transformed into hex crystal lattice with
increasing number of cycles caused by accumulation of more stacking-faults as
shown in Fig. 6.23 (cf. also Fig. 6.16). The inverted ECCI micrographs in Fig. 6.23
illustrate well the formation of new SFs concurrently to thickening of already
formed deformation bands (area marked by white ellipse).

Fig. 6.23 Microstructure of Fe–16Cr–6Mn–6Ni–0.05C steel deformed cyclically at


ea;t = 5  10−3 up to two different number of cycles N1 = 250 (a) and N2 = 500 cycles (b). a,
b EBSD phase maps. c, d inverted ECCI micrographs. a, b Band contrast image with overlapped
phase identification; yellow…hex, blue… bcc (a′-phase), rest fcc (c-phase), black…zero solutions.
c, d Arrangement of stacking-faults within the same individual grain as shown in (a, b).
Reproduced from [31]. Permission of Elsevier
6.4 Microstructure Evolution 237

Fig. 6.24 Influence of temperature on the microstructure of Fe–16Cr–6Mn–6Ni–0.05C steel


deformed in tension up to 10% of elongation. a, b Results of EBSD measurements after
deformation at RT. c, d Results of EBSD measurements after deformation at 100 °C. a,
c Crystallographic orientation maps in inverse pole figure colouring according to the loading axis
of the hex stacking-fault areas. b, d Crystallographic orientation maps of austenite exhibiting twin
orientations inside deformation bands (marked by white arrows). Loading axis horizontal.
Reproduced from [47]. Permission of Elsevier

However, EBSD measurements revealed also the coexistence of regions with


hex crystal lattice and microtwins within individual deformation bands. Thus,
Fig. 6.24 shows results of EBSD measurements performed on Fe–16Cr–6Mn–6Ni–
0.05C steel deformed in tension at RT (a, b) and 100 °C (c, d) up to 10% of
elongation. At RT, the amount of twins found in proximity of hex crystal lattice is
even increasing with an increase in plastic strain [39, 47]. Figure 6.24a, c shows
crystallographic orientation maps of regions with hex crystal lattice and Fig. 6.24b,
d of fcc areas. The twin orientation relationship within the band and austenitic
matrix is visible clearly. Quite recently, similar observations were obtained on Fe–
16Cr–6Mn–9Ni–0.05C steel after deformation in compression at RT [53]. Ullrich
et al. [53] observed concurrently regions of twinned austenite and hex crystal lattice
inside the same grain as well as even within individual deformation bands.
This aspect is corroborated by detailed high-resolution transmission electron
microscopy (HRTEM) investigations. Thus, Borisova et al. [6], Martin et al. [52]
and Ullrich et al. [53] revealed complex arrangement of stacking-faults on atomic
scale. Thus, high density of intrinsic SFs on in average each second f111g plane
causes hex crystal lattice, whereas intrinsic SFs on consecutive f111g planes result
in twin configuration. Quite frequently, both SF arrangements are observed con-
currently in an intermixed state within deformation bands as shown in Fig. 6.25.
Furthermore, above-mentioned experimental observations are supported by the
theoretical considerations of Geissler et al. [54] on thermodynamical aspects of the
SFE. The thermodynamical formalism introduced by Olson and Cohen [55] in
1976, which describes the SFE by the difference of Gibbs free energy between
metastable austenitic phase and intermediate e-martensite and an additional term of
surface energy at phase boundary, is critically discussed. Geissler et al. [54]
238 6 Object of Investigations—High-Alloy …

Fig. 6.25 Results of high-resolution transmission electron microscopy investigations on Fe–


16Cr–6Mn–6Ni–0.05C steel after deformation up to 5% compression strain. a HRTEM image
together with corresponding fast Fourier transformation (FFT) patterns of characteristic areas
consisting of the e-martensite (hex) and nanotwins (tw) with fcc crystal lattice in the closest
vicinity on the atomic scale within the thin individual deformation band. Reproduced from [6].
Permission of Wiley VCH. b SAED pattern taken on a deformation band in Fe–16Cr–6Mn–9Ni–
0.05C specimen after deformation in compression up to 25%. Diffraction spots assigned to
austenite (black), twinned austenite (red) and e-martensite (hex) are indicated. Reproduced from
[53]. Permission of Elsevier

presented and discussed a modified energy relation that explained simultaneous


appearance of highly disordered and faulted austenite interrupted or accompanied
by twinned austenite observed frequently (cf. Sect. 3.5).

6.4.2 Fe–16Cr–6Mn–9Ni–0.05C Steel

As described above, the stability of austenite increases with an increase in nickel


content. As discussed already for stress-strain behaviour and cyclic deformation
behaviour, dominant deformation mechanism in Fe–16Cr–6Mn–9Ni–0.05C steel
with highest austenite stability is mechanical twinning. Figure 6.26 shows results of
EBSD measurements at RT and 100 °C obtained at elongation to rupture.
Mechanical twinning is observed on two different twin systems (see Fig. 6.26a, d),
whereas the thicker ones are related to primary twin system. The thinner twins
occur on secondary twin system, which is activated due to changes of initial ori-
entation of austenitic grain caused by grain rotations in order to keep integrity at
grain boundaries. Clearly, it is visible that thinner, secondary twins are terminated
by primary twins and do not intercept them (see Fig. 6.26b, e). The kernel average
misorientation (KAM) maps shown in Fig. 6.26c, d indicate clearly a higher local
misorientation inside mechanical twins than in surrounding austenitic matrix. Thus,
twins are not defect-free. Furthermore, it is obvious that an increase in temperature
6.4 Microstructure Evolution 239

Fig. 6.26 Mechanical twinning occurring during tensile deformation of Fe–16Cr–6Mn–9Ni–


0.05C steel up to elongation of failure. Results of EBSD measurements. a–c After deformation at
RT, e = 70%. d–e After deformation at 100 °C, e = 55%. a, d Band contrast maps with indicated
twin boundaries (red lines). b, e Orientation maps with inverse pole figure colouring according to
the loading axis. c, f Kernel average misorientation maps with maximum misorientation angle of
5° between the nearest 8 neighbours of each individual measuring point. Loading axis horizontal.
Reproduced from [40]. Permission of Elsevier

leads to decrease in mechanical twinning activity. However, it should be mentioned


here that quantification of mechanical twins using EBSD is a challenging task.
The microtwins formed during mechanical twinning are in the size of few
nanometres. Sometimes, they occur as twin bundles in deformation bands with a
thickness up to few micrometres (cf. Fig. 6.26b, e). Depending on step size,
acceleration volume during EBSD and inclination of twin boundary to specimen
surface respective electron beam an overlap of Kikuchi patterns of non-deformed
austenite and twin orientation can occur [56].
Thus, as described by Steinmetz et al. [57] the detectability of nanometre-sized
microtwins can be improved by improvement of resolution of EBSD measurements
applying small step size, reduced acceleration voltage, small aperture, low beam
current and adapted working distance. However, all these strategies cause a
decrease in intensity of Kikuchi patterns resulting in higher exposure times, longer
measuring time and loss of indexing quality. Therefore, only qualitative statements
on twinning activity based on EBSD measurements can be provided.
The onset of mechanical twinning and evolution of twin density as well as
thickening of microtwins was investigated at different strain levels by SEM
micrographs taken in SE contrast (Fig. 6.27) as well as EBSD measurements
(Fig. 6.28) during in situ tensile deformation. Already at a strain level of e = 2.5%,
twins with a thickness of about 1 µm are detected (bright straight lines; black
arrows) in individual austenitic grains. In addition, two other slip systems are
240 6 Object of Investigations—High-Alloy …

Fig. 6.27 Evolution and thickening of microtwins with increasing applied strain for Fe–16Cr–
6Mn–9Ni–0.05C steel during tensile test at RT. a e = 2.5%. b e = 3.75%. c e = 5.0%. d e = 7.5%.
e e = 8.75%. f e = 10%. Secondary electron contrast. Loading axis horizontal

detected (black dashed arrows). Furthermore, two scratches remained on the


specimen surface after vibration polishing. With an increase in plastic strain, the
initially developed twins become thicker and new twins are formed. The slip
activities on second and third slip systems become more intense. These slip steps
are related really to slip activities, since the slip steps are crossing the thicker twin
bundles.
The twin orientation of the developed bands at 2.5% of elongation becomes
evident from Fig. 6.28. Whereas the matrix grain has an orientation close to h011i
parallel to the loading axis, the twin orientation is close to h001i. The thinnest twin
orientation detected by EBSD at 2.5% of elongation is about 70 nm (left side) since
the dark line of the band contrast contains only one pixel of the twin orientation
(step size of EBSD measurement is 70 nm). The increase in plastic strain leads to
formation of additional thin bands with twin orientation very close to those ones
formed previously. In this way, the twin bundles become thicker and thicker.
However, due to the plastic straining the orientation of the austenitic matrix is
changing as can be followed from the inverse pole figure with a rotation towards
h111i. The activated twin system calculated from the crystallographic orientation of
the austenitic grain is a ð111Þ½211 (cf. Table 6.2). The two scratches mentioned
already in Fig. 6.27 are even better visible in the band contrast map with overlaid
crystallographic orientation (Fig. 6.28). The shear of these two scratches by the
penetrating twin is nicely recognizable (black arrows). The measured displacement
of the two parts of both scratches in the shear direction ½ 211 is about 500 nm
already at an elongation of 2.5%.
6.4 Microstructure Evolution 241

Fig. 6.28 Twin formation during tensile deformation of Fe–16Cr–6Mn–9Ni–0.05C steel at RT at


different strain levels. Results of in situ EBSD measurements. Overlay of band contrast map and
crystallographic orientation map in combination with inverse pole figure with respect to loading
axis resembling both twin orientation and change of the crystallographic orientation of the
austenitic grain due to tensile deformation

Table 6.2 Activated slip systems for grain ð137Þ½011 investigated during in situ tensile
deformation of Fe–16Cr–6Mn–9Ni–0.05C steel in combination with EBSD shown in Figs. 6.27
and 6.28
g-matrix
0:0801 0:3135 0:9454
0:6132 0:7321 0:2964
0:7858 0:6035 0:1350
SP btrace Primary SS Secondary SS Third SS Forth SS
SDreg SDP1 SDP2 SDreg SDP1 SDP2 SDreg SDreg
½101 ½211 ½112 ½101 ½112 ½211 ½
110 ½110
ð111Þ 81.9° 0.476 0.48 0.32 – – – 0.373 –

ð111Þ 106.7° – – – 0.426 0.31 0.43 – 0.322

6.4.3 Fe–16Cr–6Mn–3Ni–0.05C Steel

The Fe–16Cr–6Mn–3Ni–0.05C steel exhibits among all three investigated steel


variants the lowest austenite stability. Consequently, this steel has the highest
driving force for martensitic phase transformation. The Ms temperature is with
60 °C above RT. Thus, a certain amount of martensite will be present already in
microstructure, which is formed already during cooling process of as-cast material
after solution annealing. In addition, martensite can be generated in this steel variant
also during metallographic preparation. Therefore, careful characterization of initial
state before deformation is needed. Moreover, d-ferrite has to be separated from
martensite.
242 6 Object of Investigations—High-Alloy …

Fig. 6.29 Strain-induced martensitic phase transformation of Fe–16Cr–6Mn–3Ni–0.05C steel


during tensile deformation up to 10% of elongation. a, b After deformation at RT. c, d After
deformation at 100 °C. Results of EBSD measurements in terms of phase maps. a, c Initial state. b,
d 10% of elongation. Modified according to [30]

Figure 6.29 shows EBSD investigations on two specimens deformed in tension


at RT (a, b) and 100 °C (c, d), respectively. Figure 6.29a, c characterizes initial
state before deformation. Clearly, small round shaped areas with bcc crystal lattice
identified as d-ferrite (white arrows) can be distinguished from a′-martensite caused
by cooling and specimen preparation (indicated by black arrows). After tensile
deformation up to 10% of elongation, pronounced strain-induced martensitic phase
transformation via stacking-fault bands (hex) is observed [30].
Comparing with Fe–16Cr–6Mn–6Ni–0.05C steel (see Figs. 6.17a and 6.24a),
the martensitic phase transformation is more intense in Fe–16Cr–6Mn–3Ni–0.05C
steel with the lowest austenite stability at both temperatures. In addition, no
mechanical twinning is observed in this steel variant at deformation up to 100 °C
(cf. Fig. 6.30). At failure, the microstructure is even more complex. Nevertheless,
strain-induced martensitic phase transformation via deformation bands of e-mar-
tensite and different a′-martensite variants can be recognized. Dark contrast in BSE
micrographs is correlated to d-ferrite, which can be separated from a′-martensite
also in orientation maps. The elongated d-ferrite areas exhibit various but within
individual d-ferrite grains uniform crystallographic orientations. In contrast, a′-
martensite nuclei are much smaller and exhibit different crystallographic orienta-
tions [40].
References 243

Fig. 6.30 Strain-induced martensitic phase transformation of Fe–16Cr–6Mn–3Ni–0.05C steel


during tensile deformation up to elongation of failure. a, c After deformation at RT (e = 33%). d–
f After deformation at 100 °C (e = 45%). Results of EBSD measurements. a, d SEM micrographs
in BSE contrast. b, e Phase maps. Red—austenite, yellow—e-martensite, blue—a′-martensite + d-
ferrite. c, f Orientation maps of the bcc phases in inverse pole figure colouring according to the
loading axis. Reproduced from [40]. Permission of Elsevier

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Chapter 7
Case Studies on Localized Deformation
Processes in High-Alloy Fe–16Cr–6Mn–
xNi–0.05C Cast Steels

Abstract This chapter is together with Chap. 6 the principal part of this book. This
chapter provides detailed results on the application of the in situ characterization
techniques introduced in Chap. 5 in terms of three case studies: (i) the microscopic
strain localizations during plastic deformation, (ii) the temporal evolution of
deformation processes and (iii) the macroscopic strain localization during plastic
deformation. The part on microscopic strain localizations provides high-resolution
(sub-µm) results of strain field calculations obtained during both tensile deforma-
tion at different temperatures (RT, 100 and 200 °C) and cyclic deformation at room
temperature. Furthermore, the magnitude of shear for individual microstructural
constituents (austenite, e-martensite and a′-martensite) was experimentally deter-
mined and shows a good agreement with theoretical calculated values. The part on
temporal evolution of deformation processes shows that the acoustic emission is a
powerful tool to study the kinetics of deformation processes since it allows to
separate acoustic signals belonging to different sources such as dislocation move-
ment, twinning, formation of stacking faults and martensitic phase transformation.
The part on macroscopic strain localizations demonstrates well that the combination
of different in situ characterization techniques such as digital image correlation,
infrared thermography and acoustic emission applied to the Portevin–Le Chatelier
effect can gain a deeper knowledge and understanding on ongoing processes and
material behaviour.

7.1 Significance of Complementary In Situ


Characterization Techniques

In Sects. 6.1–6.5, the class of low-carbon, high-alloy Fe–16Cr–6Mn–xNi–0.05C


steels developed according to design by Weiss et al. [1] was described in detail with
respect to both the mechanical behaviour under different loading conditions such as
(i) static (e.g. [2–4]), (ii) cyclic (e.g. [5]), (iii) biaxial (e.g. [6], (iv) dynamic (e.g. [7])
and (v) hydrostatic high-pressure loading [8] and development of microstructure
using different techniques such as (i) scanning electron microscopy (e.g. [2, 9–11])

© Springer Nature Switzerland AG 2020 245


A. Weidner, Deformation Processes in TRIP/TWIP Steels,
Springer Series in Materials Science 295,
https://doi.org/10.1007/978-3-030-37149-4_7
246 7 Case Studies on Localized Deformation Processes …

(ii) X-ray diffraction (e.g. [12, 13]) and (iii) high-resolution transmission electron
microscopy (e.g. [14]). As shown by numerous results, a deep understanding and
knowledge of ongoing microstructural processes and their influence on mechanical
properties were gained. In addition, these results were complemented by investi-
gations on wrought steels [15], powder metallurgically produced steels [16] and
ultrafine-grained TRIP steels [17] within the same steel alloying concept. Thus, a
comprehensive body of knowledge of this class of low-carbon, high-alloy Fe–16Cr–
6Mn–xNi–0.05C steels was generated.
As demonstrated in detail in Sect. 6.4, the microstructure associated with TRIP
and TWIP effects in high-alloy Fe–16Cr–6Mn–xNi–0.05C cast steels is quite
complex and depends on various parameters such as temperature, strain rate, grain
size and grain orientation. Thus, different deformation processes such as (i) dislo-
cation glide, (ii) the formation of stacking faults, (iii) mechanical twinning as well
as (iv) martensitic phase transformation occur simultaneously leading to different
microstructural features and phases being observed concurrently in deformed

Fig. 7.1 Deformation-induced microstructure of high-alloy Fe–16Cr–6Mn–6Ni–0.05C cast steel


facilitating TRIP effect. Complex microstructure consisting of a deformed austenitic matrix with
individual dislocations and short SF, deformation bands formed by the high density of SFs and,
locally, microtwinning (red line) as well as a′-martensite grains with dimensions  1 µm.
Reproduced from [18]. Permission of Springer
7.1 Significance of Complementary In Situ Characterization Techniques 247

microstructure—as shown exemplarily in Fig. 7.1 (e.g. cf. [19] for tensile loading
or [11] for compressive loading).
Within deformed austenite that is characterized by regular dislocations and
individual SFs, deformation bands are formed that belong to different activated slip
systems. Depending on arrangement of SFs, these bands appeared either with a hex
crystal lattice (SF on in average each second f111g plane) or as microtwins with fcc
crystal lattice (SF on consecutive f111g planes). Intersecting deformation bands or
individual SFs caused nucleation of a′-martensite variants.
In order to understand strengthening behaviour of TRIP/TWIP steels caused by
this complex microstructure, it is necessary to gain a deeper knowledge of both:
(i) local contribution of individual microstructural constituents to global deforma-
tion and strengthening behaviour and (ii) evolution of underlying microstructural
processes such as dislocation glide, formation of stacking faults, twinning and
martensitic phase transformation during straining of material. Both aspects can be
incorporated into already existing approaches for modelling TRIP or TWIP effect
(e.g. [20]).
Therefore, the performance of in situ deformation experiments in combination
with further characterization techniques is an excellent and powerful method for
investigation of these aspects. The field of in situ experiments offers a broad
spectrum of different methods such as (i) optical microscopy, (ii) SEM analysis,
(iii) full-field measurements using DIC and IR-TG, (iv) acoustic emission mea-
surements (AE) and, finally, (v) fully-coupled, full-field measurements as shown in
Sect. 5. In addition, it was shown that all these methods possess their respective
advantages and disadvantages. However, their complementary application in
combination with other post-mortem investigations provides great potential for the
investigation of complex correlations.
The high lateral resolution of SEM-DIC combined with the high thermal reso-
lution of IR-TG and the high time resolution and integral volume information of AE
can be used for gaining comprehensive knowledge of evolution of deformation
processes occurring in high-alloy TRIP/TWIP steels. Thus, Fig. 7.2 provides an
overview of different types of investigations performed on high-alloy TRIP/TWIP
steels. Figure 7.2a shows the overall mechanical behaviour of TRIP and TWIP
steels that is together with strain hardening, the subject of the modelling approa-
ches. The mechanical behaviour investigated depends on chemical composition,
temperature, strain rate and loading path, as shown exemplarily for tensile tests in
Fig. 7.2b. This was corroborated by intense post-mortem microstructural investi-
gations using SEM (EBSD, EDS, ECCI, t-SEM) and TEM (HRTEM) (see
Fig. 7.2c–f). On the other hand, tensile tests were accompanied by AE measure-
ments revealing clearly which deformation mechanism prevails at which defor-
mation state (see Fig. 7.2j) and explaining, ultimately, the evolution of formation of
a′-martensite (see Fig. 7.2i). On a microscopic level, high-resolution SEM-DIC was
used to obtain information on local shear strain as covered by individual con-
stituents of microstructure such as austenitic matrix, DBs with SFs (stacking fault
bands), DBs with twins (twin bundles) or a′-martensite. Finally, nano-indentation
experiments performed in SEM can also be used for investigation of microme-
chanical behaviour of these individual microstructural constituents.
248 7 Case Studies on Localized Deformation Processes …

Fig. 7.2 Schematic overview of applied methods of characterization and in situ techniques in
combination with general information obtained for the comprehensive description of the
deformation behaviour of Fe–16Cr–6Mn–xNi–0.05C TRIP/TWIP steels. a Schematic
stress-strain curves of steels with TRIP and TWIP effects in comparison with steel without these
effects. b, c Stress-strain curves of Fe–16Cr–6Mn–xNi–0.05C steels obtained from tensile tests
representing the influence of chemical composition and strain rate (b) as well as of deformation
temperature on the mechanical properties (c). d Phase composition determined by EBSD
measurements. e, f Microstructure and defect arrangements obtained by the electron channelling
contrast imaging (ECCI) technique on bulk specimens (e) and using transmission electron detector
in the SEM (t-SEM) on an electron transparent foil (f). g Calculated magnitude of shear of
individual microstructural constituents based on combined DIC and EBSD measurements.
h Load–displacement curves of individual microstructural constituents obtained by in situ
nano-indentation inside SEM. i Kinetic of the martensitic phase transformation obtained from AE
measurements during tensile testing at room temperature. j Kinetics of all deformation
mechanisms occurring in Fe–16Cr–6Mn–xNi–0.05C TRIP steels. Reproduced from [18].
Permission of Springer

Therefore, this section will demonstrate the high potential of complementary


in situ investigations shown in Fig. 7.2 on three case studies of strain localizations
and the evolution of deformation processes in high-alloy Fe–16Cr–6Mn–xNi–
0.05C TRIP/TWIP steels. Thus, Sects. 7.2, 7.3 and 7.4 describe (i) strain local-
izations at a microscale investigated by SEM-DIC, (ii) temporal evolution of
deformation processes investigated by AE and (iii) strain localizations occurring on
a macroscale and investigated by fully-coupled full-field measurements in combi-
nation with AE.
7.2 Microscopic Strain Localizations During Plastic Deformation 249

7.2 Microscopic Strain Localizations During Plastic


Deformation

Depending on their nickel content, the steel variants investigated exhibited either
TRIP or TWIP effect or combined TRIP/TWIP. Both effects are correlated with
microscopic strain localizations such as formation of deformation bands with high
stacking fault density, strain-induced martensitic phase transformation as well as
formation of twin bundles under quasi-static as well as cyclic loading conditions.
The occurrence of these strain localizations and their dependence on temperature
applied were investigated using in situ deformation experiments in SEM in com-
bination with high-resolution DIC and post-mortem EBSD measurements.

7.2.1 In Situ Deformation in the Scanning Electron


Microscope

In situ deformation experiments were performed in a FE-SEM (Mira3 XMU;


Tescan; Czech Republic) equipped with a retractable four-quadrant BSE detector
and a co-planar EBSD/EDS detector system (EDAX, AMETEK, USA). The in situ
tests were carried out using a tension/compression loading device (Kammrath and
Weiss, Dortmund, Germany), which was mounted on SEM motor stage.
Flat, miniaturized specimens with dog bone-shaped geometry according to
Fig. 7.3a with a rectangular cross section of about 4  2.5 mm2 and a gauge length
of 12 mm were used for tensile and cyclic loading tests. The specimens were
manufactured out of casting plates after solution annealing. The surface preparation
was performed by a careful grinding and polishing procedure down to 1 µm. Final
preparation step involved 24 h vibration polishing (VibroMet; Bühler) using a
0.02 µm colloidal SiO2 suspension for final removal of any preparation-induced
deformation/damage layer.

Fig. 7.3 In situ tensile and cyclic loading experiments in SEM. a Specimen geometry.
b Stress-strain curve of quasi in situ tensile test at room temperature. c Stress-strain hysteresis
loops of quasi in situ cyclic loading with a total strain amplitude of ea;t = 4  10−3 up to 1450
cycles
250 7 Case Studies on Localized Deformation Processes …

In situ tensile tests were performed at room temperature (RT) as well as at


elevated temperatures (100 and 200 °C). The tests were conducted under dis-
placement control using a low motor velocity of 2 µm/s resulting in a nominal
strain rate of 2  10−4 s−1. The tests were carried out as quasi in situ tests. Thus,
tensile test was interrupted at well-defined elongation intervals (typically 50 µm) to
record high-resolution images. After interrupting tensile tests at certain elongations,
some load relaxation occurred due to low stiffness of the whole device (see
Fig. 7.3b). Thus, image recording began after allowing some time for load
stabilization.
In situ cyclic experiments were conducted under displacement control using an
extensometer on the rear of the specimen. The quasi in situ tests were carried out at
a total strain amplitude of ea;t = 4  10−3 and were interrupted at a defined number
of cycles. Individual cycles were performed at a low motor velocity (2 µm/s)
resulting in a cycle time of about 40 s. For performing higher numbers of cycles,
the maximum motor velocity of 20 µm/s was used.
The experiments at elevated temperatures were carried out using a heating
device clamped to rear of the specimen (the side opposite to the electron beam).
Between heating plate and specimen, a heat-conducting paste (non-silicon heat
transfer compound, RS Components Ltd., UK) was used as a coupling medium.
The push–pull loading device was cooled by a water pipe system (see Fig. 7.4). The
heating rate was chosen by setting PID control in such a manner that desired
temperature (100 and 200 °C) was reached within few minutes and was then kept
constant with an accuracy of ±1 K. During heating-up procedure, the specimen
was kept under constant load control (F = 0 N) in the loading device in order to
compensate for elongation of the specimen and to avoid compressive stresses due to
thermal expansion. Tests were started 30 min after reaching deformation temper-
ature in order to guarantee thermal stability.
Secondary electrons (SEs) as well as backscattered electrons (BSEs) were used
for imaging the changes occurring in the material under mechanical load. Whereas
SEs are, due to their small information depth (a few nanometres), ideally suited for

Fig. 7.4 View inside the SEM chamber (Mira3 XMU, Tescan, Brno, Czech Republic) with
tension/compression module (Kammrath and Weiss, Dortmund, Germany) mounted on the SEM
motor stage. a Total view of the loading stage inside the SEM in combination with heating and
cooling system. b Detailed view on a deformed specimen with mounted heating device on the rear
of the specimen. c Position of the tension/compression module for in situ testing in combination
with BSE detector
7.2 Microscopic Strain Localizations During Plastic Deformation 251

topographic imaging, BSEs are useful for the observation of material contrast and/
or orientation contrast, since the intensity of BSE contrast strongly depends on both
atomic number (material contrast) and angle between PE and lattice planes (ori-
entation contrast).
The AOI was chosen randomly, but located close to the centre of specimen.
A few Vickers hardness indents were set to the left and to the right side of the AOI
for both the calculation of macroscopic strain and better recognition of the AOI for
subsequent microstructural investigations after in situ tests. After in situ deforma-
tion tests, detailed characterization of the microstructure was performed using
EBSD measurements both in terms of the martensitic phase transformation and in
terms of characteristic orientation relationships. To this end, the pronounced surface
profiles developed during tests were removed carefully by vibration polishing only
for at least 24 h (or multiples thereof). EBSD measurements were carried out again
at an acceleration voltage of 20 kV, a beam current of 2 nA, a working distance of
15 mm and a step size of 0.07 µm or 0.1 µm using the OIM© data acquisition
software.

7.2.2 High-Resolution DIC (Sub-µDIC) for Evaluation


of Local Strain Fields

The SEM images recorded sequentially during quasi in situ tensile and cyclic tests
were used for calculation of local strain fields by application of digital image
correlation technique (cf. Sect. 5.4.1). The main goal of DIC applied on mechanical
in situ tests for high-alloy Fe–16Cr–6Mn–xNi–0.05C cast steels was the
high-resolution detection of resolved local strain fields. The microstructure of
investigated steels was quite complex, as shown exemplarily in Fig. 7.1, and
consisted of (i) deformation bands with a high density of stacking faults,
(ii) martensitic islands within the deformation bands, (iii) microtwins and (iv) de-
formed austenite with regular dislocations and stacking faults. As shown in
Fig. 7.1, the thickness of deformation bands was in the order of a few micrometres
or less—at least for early deformation states. Consequently, a′-martensite islands
formed were in the same order of magnitude or even below 1 µm. Thus, contrast
pattern required on surface of specimen for successful DIC calculation on these
microstructural features should have been at least in the range close to/or below
1 µm. The further demand was a randomly distributed greyscale contrast without
any sharp edges on black or white colour side.
Different contrast methods like BSE contrast of the polished surface, SiO2
particles retained after vibration polishing, Pt nanoparticles deposited on the
specimen surfaces or carbon contamination spots after long-term exposure of the
electron beam during EBSD measurements were tried for the DIC measurements.
However, in all cases the results of the DIC calculations were less than satisfactory.
The images in BSE contrast were not suitable for DIC measurements since the
252 7 Case Studies on Localized Deformation Processes …

ongoing microstructural processes led to significant changes in the crystallographic


orientation. The intensity of BSE is quite sensitive to small changes in the crys-
tallographic orientation. Thus, the formation of deformation bands leads to pro-
nounced changes in greyscale distribution, which was a drawback for good
correlation results.
The greatest problems were caused by insulating SiO2 particles, which resulted
in drift phenomena during image recording. The drift problems were solved out by
the application of Pt nanoparticles deposited by through thin film ablation (TTFA).
However, the problem here was inhomogeneous distribution of particles on spec-
imen surface (see Fig. 7.5a, b). Areas without any or with only few particles were
separated by areas with agglomerated nanoparticles. The result of DIC was quite
satisfactory (cf. Fig. 7.5c). However, another problem occurred at higher strain
levels. Due to the deposition of Pt nanoparticles, a very thin layer covered the
specimen surface. This layer cracked at higher strain levels (>3% of elongation) due
to pronounced surface roughening of coarse-grained as-cast microstructure during
tensile deformation.
Thus, it became necessary to return to the tried and trusted technique of contrast
etching. The specimen surfaces were etched using V2A etching agent (100 ml
distilled water, 100 ml hydrochloric acid, 10 ml nitric acid and 0.2 ml pickling
inhibitor according to Voglers) for 1–2 min at 40 °C in order to obtain randomly
distributed and high-contrast etching patterns recommended for digital image cor-
relation technique. The contrast etching yielded different etch pit pictures depending
on material and grain orientation. However, etch pits were randomly distributed and
their size was definitely in the order of less than 500 nm. The SE contrast micro-
graphs shown in Fig. 7.6 correspond to initial states before different quasi in situ
tests: (a) tensile tests at RT of Fe–16Cr–6Mn–3Ni–0.05C steel; etching after
vibration polishing, (b) tensile test at RT of Fe–16Cr–6Mn–6Ni–0.05C steel;
etching after mechanical polishing, and (c) tensile test at RT of Fe–16Cr–6Mn–
9Ni–0.05C steel; etching after vibration polishing.

Fig. 7.5 Surface contrast obtained by deposition of Pt nanoparticles on the vibration-polished


specimen surface of a Fe–16Cr–6Mn–6Ni–0.05C steel. a Initial state before tensile loading.
b Same AOI at a maximum elongation of e = 2.3%. c Result of digital image correlation in terms
of Von Mises equivalent strain at e = 2.3%
7.2 Microscopic Strain Localizations During Plastic Deformation 253

Fig. 7.6 Examples of etched specimen surfaces for high-resolution digital image correlation.
a Fe–16Cr–6Mn–3Ni–0.05C steel. b Fe–16Cr–6Mn–6Ni–0.05C steel. c Fe–16Cr–6Mn–9Ni–
0.05C steel. Etch pits are different depending on the specific grain orientation. a, c Etched after
vibration polishing. b Etched without vibration polishing. Scratches are visible

The quasi in situ tests were performed in SEM at an acceleration voltage of


20 kV, a beam current of about 1.5 nA (resulting in a beam diameter of <20 nm)
and a working distance of about 15 mm (restricted due to the clamp holders of the
specimen and the conical shape of end lens of electron column; cf. Fig. 7.4).
SE images were captured with a pixel resolution of 2048  1538 pixels2, a
dwell time of 1 µs/pixel and 20 times line iteration. Thus, an image capture time of
67 s produced almost distortion-free images. Depending on applied magnification,
a pixel resolution of <30 nm was resolved.
The digital image correlation was performed using commercial available soft-
ware packages—VEDDAC 5.1 (Chemnitzer Werkzeugmechanik GmbH, Germany)
and Aramis (GOM Optical Measuring Techniques, Germany). The DIC calcula-
tions were performed using a step size of 10 pixels, a subset size ðn  nÞ of
30  30 pixels2 and a search field size ðN  N Þ of 80  80 pixels2. The VEDDAC
software facilitated the control of the results of cross-correlation by the
cross-correlation coefficient CZNCC (for definition, see Sect. 5.4.1.2). CZNCC was
calculated for all possible locations of facet n  n in search field ðN  N Þ according
to (5.51). CZNCC could be displayed as a two-dimensional field of cross-correlation
coefficients CZNCCi0 j0 for all displacements i0 and j0 of the measuring points i and j:
The average maximum correlation coefficient CZNCCmax of analysed AOI was
determined for all of quasi in situ tests performed and DIC calculations using etched
specimen surfaces. In all cases, CZNCCmax was at about 0.8–0.98, which was an
excellent result for cross-correlation performed on SEM micrographs. Figure 7.7
shows an example for quasi in situ tensile testing of Fe–16Cr–6Mn–6Ni–0.05C
steel performed at RT. The highest correlation coefficients were found in regions,
where small scratches are still visible, since the etching was performed without
previous vibration polishing. Nevertheless, in areas of deformation bands the cor-
relation coefficient is with values of about >0.8 still satisfactory (see Fig. 7.7b).
The results of DIC were visualized in terms of colour-coded maps representing
either displacement fields or strain fields. The strain field tensor was obtained
directly from displacement tensor U according to (7.1) [21] (see also Sect. 5.4.1.3):
254 7 Case Studies on Localized Deformation Processes …

Fig. 7.7 Two-dimensional cross-correlation field CZNCCmax for the quasi in situ tensile test
performed on Fe–16Cr–6Mn–6Ni–0.05C steel at room temperature up to a maximum elongation
of e = 15%. a SEM image in SE contrast showing the etched surface in the initial state.
b Cross-correlation coefficient of the DIC

   
U 11 U 12 1 þ exx exy
U¼ ¼ ð7:1Þ
U 21 U 22 eyx 1 þ eyy

The strain fields were represented for different components of the strain tensor
such as normal strain in x-direction exx , normal strain in y-direction eyy or shear
strain exy using false colour rendering maps. Furthermore, Von Mises equivalent
strain evM , major and minor strain, direction of major and minor strain or shear
angle was displayed. The major and minor strains were obtained by transformation
of symmetrical displacement tensor on main diagonal form. The two eigenvalues k1
and k2 (stretch ratios) obtained could be transformed into strain values depending
on choice of strain measure. The major strain e1 was based on larger eigenvalue and
minor strain e2 on smaller eigenvalue (cf. Sect. 5.4.1.3).

7.2.3 Strain Localization During Tensile Deformation

The evolution of local strain fields was investigated on high-alloy Fe–16Cr–6Mn–


xNi–0.05C TRIP/TWIP cast steels under tensile deformation using a combination
of quasi in situ experiments in the SEM and digital image correlation on sequences
of SEM micrographs captured in SE contrast. The following explanations are
subdivided according to chemical composition, starting with (i) Fe–16Cr–6Mn–
6Ni–0.05C steel enabling both TRIP and TWIP effects depending on the defor-
mation temperature, followed by (ii) Fe–16Cr–6Mn–9Ni–0.05C steel exhibiting
TWIP effect and (iii) finished by Fe–16Cr–6Mn–3Ni–0.05C steel resulting in TRIP
effect. The statements according to each steel variant start with results obtained at
RT followed by results at elevated temperatures (100 °C and 200 °C, respectively).
(i) Fe–16Cr–6Mn–6Ni–0.05C steel. Room temperature. Deformation bands
developed even at small strains immediately after passing yield stress (about 0.2–
0.3% of elongation) of about 250 MPa. It is assumed that favoured places for
nucleation of deformation bands are SF tetrahedra or individual SFs, which are
7.2 Microscopic Strain Localizations During Plastic Deformation 255

already present in as-cast microstructure. Both the density and the thickness of these
deformation bands increased rapidly. As shown in Sect. 6.4, these bands contain a
high density of largely extended stacking faults placed on f111g planes of the
austenite. These deformation bands correlate well with strain localizations detected
by DIC calculations. Figure 7.8 shows the results obtained from DIC in combi-
nation with etched specimen surface in SE contrast as a sequence of six consecutive
strain intervals for interior of one individual grain out of as-cast microstructure. The
macroscopic applied strain level is provided in SEM micrographs. The developed
strain fields are provided in terms of Von Mises equivalent strain. It should be noted
that DBs do not cross the entire grain. Furthermore, they did not develop at the
grain boundaries. Indeed, the formation of these DBs started in grain interior.
The formation of deformation bands at a macroscopic strain level of 1% became
apparent from both the SEM micrograph and the strain field. Whereas the austenitic
matrix remained almost unstrained, the strain was well localized inside bands (up to
maximum local Von Mises equivalent strain evM ¼ 8%). Moreover, the strain was
distributed homogenously inside bands, whereas small differences between various
bands were observed. With an increase in macroscopic strain level, the number of
bands increased, bands thickened and localized strain values inside the bands
increased as well. At around 4% macroscopic strain, locally increased strain values
are detected within one individual DB accompanied by microstructural features

Fig. 7.8 Sequence of six consecutive strain intervals of an in situ deformation experiment in
tension at RT for Fe–16Cr–6Mn–6Ni–0.05C steel. A comparison of the SEM micrographs (SE
contrast) and the calculated strain fields evM is shown. Macroscopic strain level is provided in the
SEM micrographs. Loading axis horizontal. Grain orientation with respect to the loading axis is
indicated in the SST in (f)
256 7 Case Studies on Localized Deformation Processes …

emerging from specimen surface (cf. area marked by the white arrow). At higher
macroscopic strain levels, the number of areas with higher localized strain values
increased inside DBs.
Figure 7.9 shows a comparison of the results of DIC with results obtained from
EBSD measurements on same AOI after finishing tensile test at 15% of elongation
and re-polishing of specimen surface. The comparison of results from DIC
(Fig. 7.9a) with EBSD phase map (Fig. 7.9b) shows that uniform strain within
deformation bands correlated with hex crystal lattice, whereas higher strain values
correlated with areas where formation of a′-martensite occurred. It is worth men-
tioning that even small deformation bands were detected by DIC with a thickness of
about 200 nm (marked by white arrows). Thus, the applied technique of contrast
etching led to remarkably high resolution in sub-micrometre range. Therefore, the
method developed is called as sub-µDIC.
Figure 7.9c shows crystallographic orientation map of martensitic phase. In the
lower right part, in particular, a large number of individual grains of martensite are
recognized with different crystallographic orientations. A comparison of calculated
shear strain and crystallographic orientation map of martensitic phase (cf. Fig. 7.9a,
c, respectively) led to the assumption that higher shear strain levels within defor-
mation bands were correlated with individual a′-martensite grains of a specific
orientation. This will be discussed in more detail in Sect. 7.2.4, where the mag-
nitude of shear was calculated for a′-martensite grains of different orientations.
Furthermore, EBSD measurements clearly revealed that microtwins occurred con-
currently with stacking fault bands in the microstructure at 15% of elongation (red
lines in Fig. 7.9c). From the point of view of Von Mises equivalent strain
(Fig. 7.9a), no clear difference was recognized between areas with high stacking
fault density and microtwins. This will be also discussed later in Sect. 7.2.4.
It was mentioned in Sect. 7.3 that locations favoured for the nucleation of a′-
martensite are the intersection points of deformation bands or even the intersection
of individual stacking faults on different slip planes. In the present case, however,
macroscopically one set of deformation bands could be recognized only as shown

Fig. 7.9 Local strain fields and EBSD measurements of Fe–16Cr–6Mn–6Ni–0.05C steel
deformed in tension at RT up to a total elongation of 15%. a Local strain calculated at 15% of
elongation provided in Von Mises equivalent strain. b Phase map. c Crystallographic orientation
map in inverse pole figure colouring with respect to the normal direction (ND). Red lines—twin
boundary austenite. Loading axis horizontal. Reproduced from [22]. Permission of Elsevier
7.2 Microscopic Strain Localizations During Plastic Deformation 257

in Fig. 7.9, though a′-martensite nuclei have formed as well. A specific crystallo-
graphic orientation of austenitic grain is present here. It turned out from calculations
of Schmid factors and arrangements of different slip systems from g-matrices
obtained by EBSD measurements that the slip plane ð111Þ of primary slip system
(l = 0.482) and ð 111Þ of the secondary slip system (l = 0.37) had similar trace
angles a at the specimen surface of 110° and 105°, respectively. Thus, on a
microscopic scale both activated slip systems formed the visible deformation band
with an inclination angle of 110° related to primary slip system. For more detail, see
Sect. 7.2.4.
For better understanding of evolution of local strain fields in combination with
microstructurally based glide processes, a detailed examination was carried out of
individual components of the strain tensor and other calculated parameters such as
major and minor strain as well as strain directions were performed. At first, the
normal strain exx was examined in combination with the direction of minor strain
(black arrows) as shown in Fig. 7.10 for several strain levels below 10% of
macroscopic elongation. It is clearly apparent that at e = 0.22%, which corre-
sponded well to the Rp0:2 yield stress, the formation of first two deformation bands
occurred (marked by white arrows). The early beginning of formation of these
bands is indicated by the formation of a preferred direction of minor strain—the
black arrows are starting to align parallel to each other in small thin bands.

Fig. 7.10 Evolution of the normal strain exx up to e = 5.30% during tensile deformation of Fe–
16Cr–6Mn–6Ni–0.05C steel at RT. The black small arrows indicate the direction of the minor
strain. Loading axis horizontal
258 7 Case Studies on Localized Deformation Processes …

Even before enhanced strain values could be detected, the parallel arrangement of
vectors representing direction of minor strain became apparent. With further increase
in strain, more and more, band-like areas with preferred directions of minor strain
became visible, accompanied by further increase in localized strain. Whereas the
angle of microscopic bands with respect to loading axis is detected to be 110°, the
direction of minor strain had an angle of 107° to the loading axis. The importance of
these two angles for further interpretation of strain localizations will be discussed
later in Sect. 7.2.4. It should be noted that the localized strain within deformation
bands increased several times with respect to externally strain applied. Thus, at
e = 1.3% localized strain exx of DB1 already reached values of 10–12%. At e = 15%,
the maximum localized strain within DBs was still twice that of applied strain.
Figure 7.11 facilitates a closer look at the evolution of minor strain e2 with
direction of major strain e1 indicated. It becomes apparent that minor strain e2
remained almost homogeneously constant at zero until a macroscopic strain level of
about >2.3% was reached. It is noteworthy to mention that minor strain, thus, is not
sensitive to DBs as the equivalent Von Mises strain (cf. Fig. 7.11) is. A few small
discontinuities observed at 2.32% appeared as horizontal lines crossing the entire
image and were related to miscalculations due to scanning character of captured
SEM images. At around 3.6% of elongation, first inhomogeneities of minor strain
are observed, which correlated well with the onset of higher values of Von Mises
equivalent strain.
Positive and negative minor strain values are observed inside same bands with
higher Von Mises strain values. With ongoing deformation, the number of areas
with positive or negative minor strain increased. Normally, regions of higher minor
strain levels were accompanied by two areas with negative minor strain values.
Moreover, absolute values of minor strains are independent of the ongoing defor-
mation of the specimen. However, the areas of given minor strain increase.

Fig. 7.11 Evolution of the minor strain e2 up to an applied strain of e ¼ 12:2% during tensile
deformation of Fe–16Cr–6Mn–6Ni–0.05C steel at RT. The small black arrows indicate the direction
of the major strain e1 . Black arrows indicate areas with negative minor strain. Loading axis horizontal
7.2 Microscopic Strain Localizations During Plastic Deformation 259

A comparison with the shear strain component of strain tensor shown in


Fig. 7.12 revealed that these butterfly-like contrasts of positive and negative minor
strain were definitely not related to miscalculations. Indeed, these differences were
true and were most likely related to crystallographic orientation of a′-martensite
variants that occurred at these areas.
Thus, areas exhibiting negative minor strain (cf. Fig. 7.11) showed highest
values of shear strain and are indicated by white arrows in Fig. 7.12. In contrast,
areas with positive minor strain in Fig. 7.11 did not exhibit significant shear strain
in Fig. 7.12. The different shear strain values and values of minor strain correlated
well with the crystallographic orientation of a′-martensite variants, which became
evident from Fig. 7.13.
Thus, areas with negative minor strain and the highest shear strain values cor-
responded directly with the green-coloured a′-martensite variant. A deeper inter-
pretation of this correlation in terms of the calculated magnitude of shear for
different martensite variants will be provided in Sect. 7.2.4.
Influence of grain orientation, grain size and local chemical composition. The
crystallographic orientation, grain size and local chemical composition have a sig-
nificant influence on strain-induced martensitic phase transformation. In similar way,
they also influence strain localization. Whereas only deformation bands with a
macroscopic inclination angle of 110° to loading axis were observed in Figs. 7.10,
7.11, 7.12 and 7.13, deformation bands on two different activated slip systems were
observed in other grain orientations. Figure 7.14 shows an example for an austenitic
grain with an orientation close to h112i with respect to the loading axis. This grain
corresponds to grain 1a shown previously in Sect. 6.4 in Fig. 6.18. Figure 7.14
shows different strain values exx , eyy , exy and evM at an applied strain of e = 18%. In

Fig. 7.12 Evolution of the shear strain exy up to an applied strain of e ¼ 12:2% during tensile
deformation of Fe–16Cr–6Mn–6Ni–0.05C steel at RT. White arrows indicate areas with increased
shear strain, the same areas that exhibit negative minor strain (cf. Fig. 7.11). Loading axis
horizontal
260 7 Case Studies on Localized Deformation Processes …

Fig. 7.13 Local strain fields at an applied strain of e ¼ 12:2% tensile deformation of Fe–16Cr–
6Mn–6Ni–0.05C steel at RT in combination with crystallographic orientation. a Normal strain exx .
b Minor strain e2 . c Shear strain exy . d Crystallographic orientation map in inverse pole figure
colouring according to loading axis. Loading axis horizontal. Reproduced from [22]. Permission of
Elsevier

Fig. 7.14 Local strain fields obtained during tensile deformation of Fe–16Cr–6Mn–6Ni–0.05C
steel at RT. a Normal strain in the x-direction exx . b Normal strain in the y-direction eyy . c Shear
strain exy . d Von Mises equivalent strain evM . Applied strain e ¼ 18%. Loading axis horizontal.
Grain corresponds to grain 1a shown in Sect. 6.4 by Fig. 6.18

addition, results of EBSD measurements of same AOI are shown in Fig. 7.15. The
activation of slip on two different slip systems became apparent from both calculated
local strain distributions exx (Fig. 7.14a) and evM (Fig. 7.14d) and band contrast map
7.2 Microscopic Strain Localizations During Plastic Deformation 261

Fig. 7.15 Results of EBSD measurement on AOI shown in Fig. 6.13 for Fe–16Cr–6Mn–6Ni–
0.05C steel tensile deformed at RT. Applied strain e = 18%. a Band contrast map. b,
e Crystallographic orientation of austenite and a′-martensite, respectively. Inverse pole figure
colouring with respect to the loading axis. c, f Kernel average misorientation of austenite and a′-
martensite, respectively. Maximum misorientation angle is 5°. d Phase map. Loading axis hori-
zontal. Grain corresponds to grain 1a shown in Sect. 6.4 by Fig. 6.18

(Fig. 7.15a). Thus, numerous deformation bands belonging to primary slip system
(inclination angle of 118° to the LA) and few DBs on secondary slip system (in-
clination angle of 25° to the LA) were developed. However, only a small part of
primary DBs exhibited hex crystal lattice (see Fig. 7.15d).
In addition, a′-martensite only occurred in a few areas limited to regions within
DBs close to grain boundaries (marked by arrows). Both exx and evM exhibited
locally high strain values mainly within DBs of primary slip system or at inter-
section points with the secondary slip system.
According to the crystallographic grain orientation, the primary slip system led
to a positive shear strain, whereas secondary slip system resulted in a negative shear
strain. Moreover, the austenitic phase in grain interior was free of e-martensite and
a′-martensite. This correlated well with an increased nickel concentration in this
area due to microsegregation leading to higher austenite stability. In addition, this
area was characterized by high orientation spread, which was caused by a high local
misorientation—as shown in Fig. 7.15c.
However, the deformation bands observed on primary and secondary system
were thinner and more densely arranged than in the large austenitic grain shown
previously in Fig. 7.8. In addition, strain was more homogenously distributed
across entire grain. In contrast to grain investigated in Fig. 7.8 (grain diameter
about 200 µm), the grain shown in Figs. 7.14 and 7.15 was much smaller. The
thickness of the grain parallel to the y-axis is about 45 µm, which is smaller by a
factor of 4. Thus, the reduced grain diameter led to a reduced mean free path for
dislocation motion and, therefore, to reduced length of pile-ups at grain boundaries.
262 7 Case Studies on Localized Deformation Processes …

Thus, parallel slip planes were activated more frequently, which led to higher
volume fraction of deformation bands and more homogenous slip distribution in
grain interior.
Figure 7.16 shows a comparison of strain evolution within two austenitic grains
with different grain sizes of 200 µm (Fig. 7.16a) and 45 µm (Fig. 7.16b).
Exemplarily, the evolution is shown in Fig. 7.16c, d along the measuring line indi-
cated in Fig. 7.16a, b over deformation process. It should be mentioned that AOI for
DIC in the smaller grain is two times larger than for larger grain. Nevertheless,
significant difference became already apparent at low applied strain level of 1%. For
the large grain, only a few deformation bands with increased strain level were present
at this low macroscopic strain level. The calculated local strain of these bands
increased continuously. In addition, the thickening of deformation bands became
apparent. Whereas at 5% elongation the DBs No. 1, 2, 3 and 4 are individual DBs, at
9% of elongation the bands 1 and 3 were grown together since No. 5 developed new
in between. The thickness of band 4 increased significantly, and the band was grown
together with late developed band No. 6. Thickening of DBs occurs via the formation
of further stacking faults in the vicinity of previously formed bands. In contrast, for
the small grain (Fig. 7.16d) numerous DBs already developed at small macroscopic
strains in the grain interior. Close to grain boundary (marked by black arrow), the
density of bands is reduced. With ongoing deformation, more and more DBs
developed and grew together. Finally, the strain distribution within smaller grain was
much more homogenous at a higher strain level than in larger grain. However,
absolute values of the localized strain are significantly higher in the smaller grain.
Influence of temperature. As already mentioned in Sects. 6.2 and 6.4, deformation
temperature has a significant influence on ongoing deformation mechanisms and,
consequently, on developed microstructure. The Fe–16Cr–6Mn–6Ni–0.05C steel
with medium austenite stability, in particular, facilitates a change from TRIP effect
driven by martensitic phase transformation to TWIP effect caused by
deformation-induced twinning at an increase in deformation temperature up to
100 °C. Along with mechanical and microstructural investigations, the influence of
temperature on strain localizations was studied via quasi in situ tensile deformation
at 100 °C in SEM in combination with DIC. Figure 7.17 shows two examples of
SEM images using SE contrast of etched specimen surface at applied strain of 6%
and 15%, respectively. Clearly, slip bands were observable at 6% of elongation.
However, slip lines do not cross entire grain. Moreover, these bands start to develop
at grain boundaries and grow towards interior of grain. Whereas only a few slip
lines, which were visible in lower left corner, were inclined by 40° to loading axis,
numerous slip lines in upper right corner were inclined by 43° to loading axis. The
angles 40°/43° correspond to activated slip system ð111Þ½ 211 (l = 0.45; compare
Sect. 7.2.5; Table 7.5). With ongoing deformation, the inclination angle of these
bands with respect to loading axis has changed. In this way, the DBs get a curved
shape that is characterized by an angle of 42° in central part of the grain, whereas
angles of DBs in lower left and upper right corner of the grain were decreasing
(40° ! 37°) or increasing (43° ! 51°), respectively.
7.2 Microscopic Strain Localizations During Plastic Deformation 263

Fig. 7.16 Comparison of the evolution of strain localization within deformation bands in coarse
austenitic grain (a) and smaller austenitic grain (b) for four different applied strain values
(provided in images) during tensile deformation of Fe–16Cr–6Mn–6Ni–0.05C steel at RT.
c, d Evolution of exx over deformation process followed along the indicated measuring line in
(a) and (b), respectively. Grain shown in (b) and (d) corresponds to grain 1a shown in Sect. 6.4 by
Fig. 6.18

Fig. 7.17 SEM images in secondary electron contrast taken during quasi in situ tensile tests at
100 °C on Fe–16Cr–6Mn–6Ni–0.05C steel at an elongation of 6% (a) and 15% (b), respectively.
Inclination angles of slip lines with loading axis are indicated. Loading axis horizontal
264

Fig. 7.18 Local strain fields in terms of Von Mises equivalent strains evM calculated from quasi in situ tensile test of Fe–16Cr–6Mn–6Ni–0.05C steel at
100 °C. a e = 3%, b e = 6%, c e = 9% and d e = 15%
7 Case Studies on Localized Deformation Processes …
7.2 Microscopic Strain Localizations During Plastic Deformation 265

The results of calculated local strain fields are summarized in Fig. 7.18 showing
the Von Mises equivalent strain at different global strain levels.
Comparable to slip bands, strain localizations developed at small global strains
at e = 0.4% (see lower left corner of the area of interest). It should be noticed that
the bands with strain localizations do not develop in sudden bursts over the entire
AOI. Instead, the length of these bands, which were characterized by strain
localizations, their number and their thickness increased continuously with ongoing
deformation in accordance with global strain increments. However, highest values
of localized strains were detected at lower left corner and decreased in direction to
upper right corner. However, the overall strain distribution was more homogenous
than at RT, where the strain was more concentrated on DBs.
Using results of EBSD measurements on this area of interest, which are sum-
marized in Fig. 7.19, it became evident that regions with higher strain localization
corresponded to areas of twin bundles formed during the in situ tensile test at
100 °C. The band contrast map clearly revealed twin bundles with the typical R3
grain boundary misorientation of 60° h111i: However, deformation-induced twin
bundles were accompanied by areas of stacking fault bands (hex), whereas no
a′-martensite formation was observed. Thus, within DBs areas with SFs on in
average each second lattice plane coexist with areas of SFs on each lattice plane. In
addition, areas of twin bundles were characterized by a high local misorientation
(see Fig. 7.19d). The simultaneous appearance of twin bundles and stacking fault
bands (hex) is in agreement with observations made by HRTEM shown in Sect. 6.4
[14] and investigations of Ullrich et al. [11]. Moreover, it became obvious from

Fig. 7.19 Results of EBSD measurements on AOI shown in Fig. 7.18 obtained after tensile test at
100 °C up to 15% of elongation. a Band contrast map with indicated twin boundaries (red).
b Phase map with austenite (red) and e-martensite (yellow). c Crystallographic orientation map in
inverse pole figure colouring with respect to the loading axis. d Kernel average misorientation map
(maximum misorientation angle 5°). Loading axis horizontal
266 7 Case Studies on Localized Deformation Processes …

both Figs. 7.17 and 7.19c that twin bundles develop either on lower left side or on
upper right side and grow than further into interior of austenitic grains. Thus, the
bended appearance of twin bundles was a consequence of highly localized strain
within these bundles.
Finally, the increase in temperature up to 100 °C led to a change from martensitic
phase transformation to deformation-induced twinning. In addition, dislocation glide
was also preferred, since overall strain distribution of entire grain was more
homogenous. High local strain values were only observed in thicker twin bundles.
(ii) Fe–16Cr–6Mn–9Ni–0.05C steel. Room temperature. The dominant
microstructural processes during mechanical loading of Fe–16Cr–6Mn–9Ni–0.05C
steel with high austenite stability at RT are mechanical twinning accompanied by
dislocation glide. Detailed results of calculation of local strain fields using DIC are
shown in Fig. 7.20. Here, Von Mises equivalent strain, minor strain and shear angle
are provided for different levels of applied strain. It is obvious that slip bands on two
different slip systems occurred directly at beginning of deformation process (e = 1%).
The bands with an inclination angle of 122° to loading axis occurred at first in the
microstructure and belong to primary slip system ð111Þ½ 101 (l = 0.45 (bold white
line in Fig. 7.20a). The second type of bands appeared slightly later and was inclined
at 37° to loading axis (dashed white line in Fig. 7.20a). These bands were related to
secondary slip system ð111Þ½011 (l = 0.36. The number of bands related to sec-
ondary slip system was significantly higher compared to primary SS. Whereas
inclination angle of primary SS remained nearly constant over deformation process
(cf. bold black line Fig. 7.20e), inclination angle of secondary SS decreased during
deformation process to 22° (cf. dotted white line in Fig. 7.20e). At the intersection
point of bands belonging to both systems, bands of primary SS were shifted slightly by
the secondary SS resulting in slightly increased strain values indicated by black lines
and arrows, respectively. In contrast, the minor strain exhibited low minor strain
(negative values) in regions with high equivalent Von Mises strain. No remarkable
shear angle could be detected at smallest global strain. With increasing applied strain,
the number of bands on secondary SS increased further. In addition, only a few bands
(numbers 1, 2 and 3) exhibited higher Von Mises strain, more negative minor strain
and negative shear angle. With ongoing deformation, new bands with higher strain
values formed, such as bands No. 4 and No. 5 shown in Fig. 7.21c. Similar to pre-
viously described results on Fe–16Cr–6Mn–6Ni–0.05C steel deformed at 100 °C,
new band structure developed from opposite sides. Thus, band No. 4 nucleated at the
lower left corner, whereas band No. 5 started to develop on the upper right corner.
Both band structures were grown towards centre of the grain during ongoing defor-
mation leading to bended structure of twin bundles. Moreover, it became obvious that
these band structures did not develop suddenly (with velocity of sound as expected for
mechanical twinning). Indeed, these bands were grown continuously with increasing
strain increments. The strain within regions between bands became more and more
homogenously distributed. Finally, at an applied strain of 15% all labelled bands
(No. 1–9) showed highest local values of Von Mises strain, lowest minor strain values
and most negative shear angles. Similar to Von Mises strain, normal strain in
7.2 Microscopic Strain Localizations During Plastic Deformation 267

Fig. 7.20 Results of digital image correlation obtained on SEM micrographs taken in secondary
electron contrast on Fe–16Cr–6Mn–9Ni–0.05C steel during in situ tensile test at RT. a e = 1%.
b e = 3%. c e = 5%. d e = 8%. e e = 15%. Left: Von Mises equivalent strain evM . Middle: Minor
strain e2 . Right: Shear angle cxy . Loading axis horizontal

x-direction and major strain exhibited same behaviour. The normal strain in y-
direction is comparable to the minor strain, and shear strain is comparable to shear
angle. Comparing results, it became obvious that band structures No. 1–9 corre-
sponded to twin bundles indicated in Fig. 7.20d–f. In contrast to Fe–16Cr–6Mn–6Ni–
0.05C steel deformed at 100 °C, however, the twin bundles formed in Fe–16Cr–
6Mn–9Ni–0.05C steel at RT were not accompanied by areas of hex crystal lattice.
Finally, the deformation was triggered by dislocation glide on regular slip systems
passing yield strength. At higher applied strain levels, slip bands transformed into twin
bundles exhibiting higher localized strain. The areas between bundles deformed
further by regular dislocation glide leading to a quite homogenous strain distribution,
which is roughly in the order of applied strain.
Table 7.1 summarizes minimum, maximum and average values of the normal
strain in the x-direction exx , the Von Mises equivalent strain evM and the shear strain
exy . Thus, average strain values for whole AOI were comparable during the seven
268 7 Case Studies on Localized Deformation Processes …

Table 7.1 Minimum, maximum and average values of strain exx , Von Mises equivalent strain evM
and shear strain exy obtained for Fe–16Cr–6Mn–9Ni–0.05C steel during in situ tensile test at RT
Strain Applied exx evM exy
increment strain (%) Min. Max. Mean Min. Max. Mean Min. Max. Mean
2 1 –1.0 8.1 0.9 0.4 9.7 1.4 –3.1 1.2 –0.3
3 2 –0.5 12.1 1.9 0.6 14.7 2.4 –3.6 0.9 –0.5
4 3 –0.4 13.4 2.9 0.4 15.7 3.4 –4.3 2.0 –0.6
5 4 –0.1 17.9 3.9 0.5 19.5 4.5 –4.5 1.9 –0.8
6 5 –0.1 21.9 4.9 0.5 29.6 5.5 –5.4 1.6 –0.9
7 6 0.0 25.4 5.8 0.6 27.6 6.4 –4.9 2.2 –1.0
20 8 4.2 45.7 15.5 5.0 57.7 17.2 –19.2 3.9 –2.7
30 10 5.2 64.0 22.1 8.8 98.2 24.9 –33.0 4.8 –4.0
40 12 8.1 73.1 28.6 10.7 96.3 32.6 –38.7 8.6 –5.2
50 15 9.9 85.7 35.6 12.2 124.6 41.0 –45.6 14.2 –6.4

first strain increments (approximately 6% of elongation) to applied strain, and


minimum strain values of exx and evM were close to zero. Starting with eighth strain
increment, the local strain increase became significantly higher. Thus, average
strain level of AOI was above applied strain. However, minimum strain values
corresponded to strain in regions between twin bundles. The shear strain behaves in
a similar manner. Whereas average shear strain changed only marginally during
first seven strain increments, the average shear strain was significantly enhanced at
last strain increment. Regarding the two parts a and b of shear angle cxy [cf. (5.71)]
observed from macroscopical deformations of the AOI, the value b ¼ @u @y remains
x

@uy
zero over whole deformation test, whereas the value a ¼ @x is significantly
increased over entire deformation test.

Fig. 7.21 Results of the determination of local strain fields and EBSD measurements of Fe–
16Cr–6Mn–9Ni–0.05C steel tensile strained at RT up to total elongation of 15%. a Von Mises
equivalent strain evM . b Band contrast map with indicated twin boundaries (red lines). c Kernel
average misorientation KAM. d–f Crystallographic orientation in IPF colouring for normal
direction (d), loading axis (e) and transverse direction (f)
7.2 Microscopic Strain Localizations During Plastic Deformation 269

Results of DIC and EBSD measurements of AOI are summarized in Fig. 7.21.
Figure 7.21a shows the strain field in terms of Von Mises equivalent strain. Thus,
deformation bands with high strain values were identified in a matrix, which was more
or less homogenously strained; see Fig. 7.20 for whole evolution. Results of strain
localizations were corroborated by EBSD measurements—as shown in Fig. 7.21b–f.
The band contrast map in Fig. 7.21b clearly indicated that the nine deformation
bands labelled in Fig. 7.21a were twin bundles, which were characterized by R3
boundaries (red lines). Furthermore, the irregular shape of twin boundaries should
be noticed. Thus, most twin bundles were characterized by a thicker part, which is
running out in a thinner part marked by black arrows (cf. bands 2, 4, 5 or 8 in
Fig. 7.21d) In addition, twin orientation became also evident from crystallographic
orientation maps (Fig. 7.21d–f). Twins on secondary system were also activated
(marked by arrows). The KAM map shown in Fig. 7.21c indicates an overall high
local misorientation, in particular, in regions between twin bundles implicating a
high dislocation glide activity in this steel variant.
Influence of temperature. Figure 7.22 summarizes results of DIC calculations for
Fe–16Cr–6Mn–9Ni–0.05C steel deformed in tension at 200 °C. As seen, only
single slip was observed. Furthermore, numerous bands already occurred at small
applied strain levels. In addition, strain localizations were not that pronounced

Fig. 7.22 Results of the determination of local strain fields and EBSD measurements of Fe–
16Cr–6Mn–9Ni–0.05C steel deformed in tension at 200 °C up to total elongation of 15%. a,
b Von Mises equivalent strain at e = 2% (a) and e = 15% (b). c Band contrast map of EBSD
measurement at e = 15%. Loading axis horizontal. d Calculated magnitude of shear at e = 15%
270 7 Case Studies on Localized Deformation Processes …

inside these bands as it was at RT. At e = 15%, the strain was more or less
homogenously distributed with slightly increased strain values inside the bands.
Thus, these bands could be correlated with normal slip bands caused by regular
dislocation glide. Figure 7.22c shows the band contrast map of AOI. Traces
belonging to slip bands identified through the DIC with localized strain values are
hardly distinguishable. However, different grey levels visible correspond to lattice
distortion due to plastic deformation. Figure 7.22d shows the magnitude of shear
calculated within slip bands in slip direction. Only small strain localization within
bands can be recognized.
(iii) Fe–16Cr–6Mn–3Ni–0.05C steel. Room temperature. The Fe–16Cr–6Mn–3Ni–
0.05C steel has the lowest austenite stability and exhibits, therefore, the most pronounced
a′-martensite formation. The results of the local strain field calculations performed on
in situ tensile tests at RT are summarized in Fig. 7.23. Here, the evolution of strain
localizations is apparent already at a global strain of 3% inside deformation bands devel-
oping along two different activated slip systems—as shown in Fig. 7.23a. The deformation
bands along the primary slip system showed equivalent Von Mises strain values of about
evM = 15%. The number of the localized deformation bands increased significantly
with further increase in tensile load. Some of the formed deformation bands showed
small narrow areas of strain localizations of up to evM = 35% inside the bands at a
global strain of e = 15% (see Fig. 7.23b). At a global strain of 15%, a high density of
deformation bands along the primary and secondary slip systems is observed and
deformation is almost completely localized in deformation bands. The austenitic
matrix between the bands showed no significantly increased equivalent Von Mises
strain values. The results of the microstructure investigations of the AOI after
re-polishing the etched surface are provided in Fig. 7.23d–f in terms of ECC imaging
and EBSD measurements. The microstructure analyses showed a good agreement
with the calculated strain distribution at 15% global strain. The ECCI micrograph
showed a high density of deformation bands along two slip systems (indicated in
Fig. 7.23d). The phase distribution map of the EBSD measurement in Fig. 7.23e
revealed a high amount of hex (yellow) and bcc crystal lattice inside deformation
bands. Depending on their thickness, some of deformation bands were still identified
with fcc crystal lattice. This is in agreement with statements of Sect. 6.4, where it was
described that austenitic matrix transforms into hex crystal lattice depending on
density and arrangement of stacking faults. The deformation bands with hex crystal
lattice were preferred nucleation places for a′-martensite formation. However, a′-
martensite grains occurred not only inside these deformation bands. At some areas,
martensitic grains overcome boundaries of deformation bands (marked by white
arrows). Whereas for martensitic grains inside bands KS-OR is fulfilled, in the latter
areas another OR is observed—so-called Pitsch OR (cf. [23]).
In addition, a large d-ferrite grain was identified in microstructure of AOI (uni-
form orientation close to <001> in Fig. 7.23d–f). Using ECCI micrograph
(Fig. 7.23d) and crystallographic orientation map (Fig. 7.23f), this grain was clearly
identified as d-ferrite. However, the d-ferrite grain was not observed in secondary
electron contrast images during in situ tensile testing. The d-ferrite grain appeared at
7.2 Microscopic Strain Localizations During Plastic Deformation 271

Fig. 7.23 Results of the determination of local strain fields and EBSD measurements of Fe–
16Cr–6Mn–3Ni–0.05C steel tensile strained at RT up to total elongation of 15% in combination
with results of EBSD measurements. a, b Evolution of local strain fields at two different applied
strain levels during tensile deformation in terms of Von Mises equivalent strain evM . c Calculated
magnitude of shear after 12% global strain. d ECCI micrograph of the AOI after re-polishing.
e Band contrast map with highlighted phase distribution (austenitic phase (fcc)—grey; deformation
bands (hex crystal lattice)—yellow; a′-martensite and d-ferrite (bcc)—blue). f Crystallographic
orientation map of the bcc phase in the inverse pole figure colouring code according to the loading
direction. Loading axis horizontal

surface as a consequence of re-polishing of etched surface after finishing in situ test.


The d-ferrite grain below surface had a less significant influence on evolution of
local strains in AOI. In comparison with austenitic matrix, local strain distribution
around the d-ferrite showed less pronounced local strain values at higher global
strain levels. The calculated magnitude of shear is provided in Fig. 7.23c. The
highest shear values up to 0.3 were determined in areas with an intensive a′-mar-
tensite formation (marked by ellipse). In the present case, however, the resolution of
local strain field measurements is not high enough to reflect individual formation of
a′-martensite grains. Both thickness of deformation bands and size of a′-martensite
grains were much smaller compared to Fe–16Cr–6Mn–6Ni–0.05C steel.
Influence of temperature. The increase in temperature to 100 °C had only a small
influence of deformation behaviour of Fe–16Cr–6Mn–3Ni–0.05C steel with lowest
austenite stability. Thus, formation of stacking fault bands (hex) and of a′-martensite
still occurred at 100 °C, however, with a lower volume fraction (cf. Sect. 6.4). The
local strain fields obtained during in situ tensile tests at 100 °C in terms of equivalent
Von Mises strain are provided in Fig. 7.24a, b.
At a global strain of 3%, formation of several deformation bands was observed.
The evM values within the deformation bands were between 15 and 20%. The
number, thickness and evM values increased with ongoing deformation process. In
contrast to room temperature deformation, strain was not only localized inside
deformation bands at 100 °C. A significant increase in strain values was clearly
272 7 Case Studies on Localized Deformation Processes …

Fig. 7.24 Results of the determination of local strain fields and EBSD measurements of Fe–16Cr–
6Mn–3Ni–0.05C steel tensile strained at 100 °C up to total elongation of 15%. a, b Evolution of
local strain fields at two different applied strain levels during tensile deformation in terms of Von
Mises equivalent strain evM . c Band contrast map with highlighted phase distribution (austenitic
phase (fcc)—grey; deformation bands (hex)—yellow; a′-martensite (bcc)—blue) at a global strain
of 15%. d Calculated magnitude of shear after 15% global strain. Loading axis horizontal

recognizable in matrix between deformation bands at an applied strain of e = 12%.


It is concluded that the austenitic matrix exhibited a higher plastic deformation
compared to RT experiments, which was caused by dislocation glide. The influence
of the temperature on the microstructure evolution showed a significant reduction of
the amount of the strain-induced a′-martensite. Only tiny areas of a′-martensite
were identified by the EBSD analysis (Fig. 7.24c). However, the number and the
thickness of the deformation bands do not match in the calculated strain field and
the EBSD phase analysis. Few deformation bands detected in the EBSD mea-
surements could be correlated with strain localizations as marked in Fig. 7.24b, c
by black arrows. The increased strain values between the deformation bands were
caused by dislocation glide. The contribution of dislocation glide to the overall
plastic deformation was increased at 100 °C compared to RT deformation. The
calculated magnitude of shear is provided in Fig. 7.24d. The magnitude of shear
within deformation bands reaches values between 0.2 and 0.3. No significant dif-
ference was detected in the magnitude of shear between the dislocation glide bands
with a high density of stacking faults and a′-martensite. A direct correlation of local
areas with high magnitude of shear and areas of the formation of a′-martensite is
impossible.
7.2 Microscopic Strain Localizations During Plastic Deformation 273

7.2.4 Orientation-Dependent Magnitude of Shear


of Individual Martensitic Grains

The comparison of the shear strain calculated by DIC shown in Fig. 7.13c with the
crystallographic orientation map (Fig. 7.13d) revealed that the crystallographic
orientation of a′-martensite variants had a significant influence on the occurring
shear strain. Knowledge of the crystallographic orientation matrix (g-matrix), which
reflects the crystallographic orientations of individual crystals with respect to the
specimen coordinate system, allows the calculation of activated slip systems
including the Schmid factor l, the vector of the slip plane normal and the slip
direction as well as their trace angles atrace and btrace with respect to the specimen
coordinate system (see Sect. 6.2.2). Table 7.2 summarizes the results for the acti-
vated slip systems (SSs) of the austenitic grain shown in Fig. 7.13 including both
SSs according to regular dislocations as well as for leading and trailing partial
dislocations. The leading partial dislocation corresponds to the higher Schmid
factor and the trailing partial dislocation to the lower l value. Thus, it turned out
that the trace angles of the primary and secondary slip planes were quite similar.
The SEM micrographs only reveal deformation bands according to the primary SS,
which is inclined 110° to the loading axis. The trace angle of the secondary SS
(105°) is only locally visible inside DBs.
Traces according to third SS were completely invisible, whereas slip lines cor-
responding to fourth SS were locally visible between deformation bands of primary
system. The cutting edge of primary ð111Þ and secondary ð 111Þ slip plane corre-
sponded to a ½011 direction. This is well in agreement with Schumann [24] (cf.
with Fig. 3.16). The trace angle of the ½011 direction is 107° and corresponded well
with direction of minor strain as shown in Fig. 7.10.
Figure 7.25 shows trace angle of activated slip planes and a schematic repre-
sentation of part of Thompson tetrahedron related to primary ð111Þ and secondary
ð111Þ slip planes. On a superficial view, deformation bands became apparent,
which were arranged only parallel to the slip trace of primary slip plane (see

Table 7.2 Activated slip systems of the investigated austenitic grain in a Fe–16Cr–6Mn–6Ni–
0.05C TRIP steel deformed in tension at RT (cf. Figs. 7.9 and 7.13)
SP atrace (°) Primary SS Secondary SS Third SS Forth SS
SDreg SDP1 SDP2 SDreg SDP1 SDP2 SDreg SDreg
 
½101 ½211 ½112
  ½101 ½1
12 ½211 1
½ 01  
½110
ð111Þ 110 0.482 0.45 0.36 – – – – –
ð
111Þ 105 – – – 0.37 0.37 0.31 – –
ð11
1Þ 25 – – – – – – 0.34 –
 Þ
ð111 6.5 – – – – – – – 0.31
SS—slip system, SP—slip plane, SDreg—slip direction of regular dislocations, SDP1—slip
direction of leading partial dislocations, SDP2—slip direction of trailing partial dislocations,
atrace —trace angle of the slip plane on the specimen surface
274 7 Case Studies on Localized Deformation Processes …

Fig. 7.25 Illustration of the activated slip systems of the austenitic grain under investigation using
digital image correlation. a EBSD band contrast map showing deformation bands parallel to
primary slip plane ð111Þ: b ECC image of the marked area in (a) at higher magnification with
indication of all four f111g slip planes activated at an applied strain of 15%. c Part of the
Thompson tetrahedron related to slip planes ð111Þ and ð111Þ: The cutting edge of ð111Þ and ð 111Þ
slip planes is the ½0
11 direction. Trace angle of this direction on the specimen surface is inclined
of 107° to the loading axis. Loading axis horizontal

Fig. 7.25a). The more detailed view in Fig. 7.25b, however, revealed that all four
f111g slip planes were activated at an applied strain of 15%, which seems rea-
sonable, since Schmid factors l of second, third and fourth slip systems were quite
similar (l > 0.3). The leading and trailing partial dislocations according to primary
and secondary SS were also indicated. According to Schumann [24], different
reactions are possible for leading and trailing partial dislocations on two inter-
secting slip planes.
They became apparent from Fig. 7.25c and can be summarized as follows:
(i) P1 ð111Þ and P1 ð111Þ 1 
6 ½211 and 1 
6 ½112
(ii) P2 ð111Þ and P2 ð111Þ 1 
6 ½112 and 1
6 ½211
(iii) P1 ð111Þ and P2 ð111Þ 1 
6 ½211 and 1
6 ½211
(iv) P2 ð111Þ and P1 ð111Þ 1 
6 ½112 and 1 
6 ½112
1  1 
(v) P1 ð111Þ and P2 ð111Þ 6 ½211 and 6 ½112
(vi) P1 ð111Þ and P2 ð111Þ 1 
6 ½112 and 1
6 ½211:

where only (i)–(iv) described the double shear reactions, which were required for
the a′-martensite formation. The reactions (v) and (vi) were classical dissociation
processes of regular dislocations. Finally, this would result in four different
martensite variants, which could be formed by these double shear reactions. Overall
24 martensitic variants could be formed taking into account all four active slip
systems and the interactions of partial dislocations.
As already described by Schumann [24], however, not all possible shear
directions led to favourable distortion of the austenitic lattice for nucleation of a′-
martensite. This is in good agreement with observed martensitic variants in the
example shown in Fig. 7.10 focusing on the lower right corner of the EBSD
map. Four different a′-martensite variants were clearly observable from the crys-
tallographic orientation map and the stereographic standard triangle (SST) shown in
Fig. 7.26—which are further called a0i (green colour), a0ii (orange colour), a0iii
(purple colour) and a0iv (magenta colour). However, a0iv only occurred to a very
7.2 Microscopic Strain Localizations During Plastic Deformation

Fig. 7.26 Different martensite variants occurring in deformation bands in Fe–16Cr–6Mn–6Ni–0.05C after tensile deformation at RT (cf. Fig. 7.10).
a Crystallographic orientation map of the austenitic matrix, deformation bands with stacking faults and a′-martensite grains inside deformation bands.
b Stereographic standard triangle reflecting the orientation of the austenite (c) and the three major a′-martensite variants (a0i , a0ii and a0iii ) with respect to the
normal direction
275
276 7 Case Studies on Localized Deformation Processes …

limited amount, was, therefore, not shown in SST and was also not included in
further interpretations. The a0ii variant exhibited a twin relationship to the a0i variant,
while a0iii and a0iv variants are also twin-related. The activation of slip systems of
different a′-martensite variants was also analysed using the g-matrices obtained
from EBSD measurements. The results are summarized in Table 7.3 for one indi-
vidual grain out of each martensite variant.
The alignment of the slip systems both of austenite and of martensite variants
with respect to specimen coordinate system is illustrated by stereographic projec-
tion—as shown in Fig. 7.27 containing slip plane normal directions (triangles) and
slip directions of regular (filled circles) and partial (open circles) dislocations. The
primary and secondary slip systems were provided in red and blue colours,
respectively.
It became apparent that only a0i variant fulfilled KS-OR for primary slip system,
i.e. ð111Þfcc k ð101Þbcc and ½101fcc k ½111bcc . However, a0ii variant fulfilled KS-OR
only for secondary slip system in the form of ð111Þfcc k ð101Þbcc and
½101fcc k ½111bcc . The ½101fcc is also indicated in Fig. 7.25b. It is visible that the
shape of martensite variants a0i and a0ii is given by this direction.
The magnitude of shear s of deformation bands consisting of high density of
stacking faults and of a′-martensite nuclei was calculated according to Schumann
[24] in the plane of observation (x-y) and in the direction ½0 11 of cutting edge of

Table 7.3 Activated slip systems of the martensitic variants formed in a Fe–16Cr–6Mn–6Ni–
0.05C TRIP steel deformed in tension at RT (cf. Figs. 7.9 and 7.13)
Martensite variants Primary SS Secondary SS
µ SP atrace;SP SD atrace;SD µ SP atrace;SP SD atrace;SD
a0i (green) 0.48 ð101Þ 110 ½111 159.5 0.46 ð101Þ 156.4  
½111 31.3
a0ii (orange) 0.49  Þ
ð101 111.5 ½111 –27.6 0.48 ð101Þ 107.7  
½111 157.3
a0iii (purple) 0.41 ð101Þ 56.8 ½111 –128.7 0.34 ð011Þ 113.4 ½111 112.6
SS—slip system, SP—slip plane, SD—slip direction of regular dislocations, atrace —trace angle of the slip plane on the
specimen surface

Fig. 7.27 Stereographic projection of the slip plane normal (triangle) and slip directions (circles)
of activated slip systems of austenite and a′-martensite variants a0i , a0ii and a0iii . Filled circles—
regular dislocations. Open circles—partial dislocations. Red—primary slip system. Blue secondary
slip system. x; y; z—specimen coordinate system
7.2 Microscopic Strain Localizations During Plastic Deformation 277

Fig. 7.28 Influence of the crystallographic orientation of a′-martensite on the calculated


magnitude of shear at 15% applied global strain. a Shear angle cxy determined by DIC.
b Crystallographic orientation map. c Calculated magnitude of shear s½011 . Loading axis horizontal

primary ð111Þ and secondary ð111Þ slip plane. The results are summarized in
Fig. 7.28 showing shear angle cxy , crystallographic orientation map and magnitude
of shear s½011 calculated in direction ½011: The calculated shear angle cxy is defined
according to (5.18) in Sect. 5.3.1.3 and could be separated into a and b values,
which can be different.
Although the shear angle shown in Fig. 7.28a was significantly different within the
microstructure ranging from +12° (maximum inside DBs) up to –4°(minimum inside
DBs), the values a and b were quite similar. Thus, the overall distortion of the AOI was
negligibly small. Moreover, areas with highest shear angle cxy (Fig. 7.28a) corre-
sponded to regions with highest magnitude of shear s½011 (Fig. 7.28c) and were related
to a0i martensite variant. According to sequence of evolution of x-component of shear
angle a, the a0i martensite grains developed first during the plastic deformation. This is
in good agreement with finding that only for this variant the KS-OR is fulfilled related
primary slip system. The negative shear angles were caused by other two martensite
variants a0ii and a0iii . The calculated magnitude of shear s½011 is between 0.2 and 0.3 for
the areas of deformation bands with stacking faults only, which is in good agreement
with theoretical calculation of Schumann [24].
Schumann [24] showed that shear related to a c–e martensite transformation or
individual stacking faults is given by sh112i = 0.354 (cf. Sect. 3.4.2). The magnitude
of shear s½011 is up to twice higher for the a0i -martensite variant. For the a0ii and a0iii
variants, the magnitude of shear s½011 remained zero in observed surface plane of AOI.

7.2.5 Magnitude of Shear of Twin Bundles

Similar to calculation of magnitude of shear for individual a′-martensite grains, the


magnitude of shear could be also determined for twin bundles formed in austenite
during tensile deformation.
At first, Fe–16Cr–6Mn–9Ni–0.05C steel with highest austenite stability will be
discussed, since here formation of twin bundles occurred during deformation at RT.
Results of EBSD measurements and local strain fields obtained from DIC
278

Table 7.4 Activated slip systems of the investigated austenitic grain in a Fe–16Cr–6Mn–9Ni–0.05C TWIP steel deformed in tension at RT (cf. Fig. 7.21)
SP atrace Primary SS Secondary SS Third SS Fourth SS
SDreg SDP1 SDP2 SDreg SDP1 SDP2 SDreg SDP1 SDP2 SDreg SDP1 SDP2

½101 ½
211 1
½ 12  
½011 2
½1 1 1
½ 1
2 ½101 ½211 ½112 
½110 12
½ 1 ½
211
ð111Þ 125.6 0.45 0.44 0.34 – – – – – – 0.31 0.10 0.44
ð111Þ 24.7 – – – 0.36 0.34 0.23 – – – – – –
ð111
 Þ 99.4 – – – – – – 0.32 0.24 0.32 – – –
SS—slip system, SP—slip plane, SDreg—slip direction of regular dislocations, SDP1—slip direction of leading partial dislocations, SDP2—slip direction of
trailing partial dislocations
7 Case Studies on Localized Deformation Processes …
7.2 Microscopic Strain Localizations During Plastic Deformation 279

Fig. 7.29 Magnitude of shear for twins formed in Fe–16Cr–6Mn–9Ni–0.05C TWIP steel
deformed in tension at RT (cf. Fig. 7.21). a Traces of the three possible slip planes (black lines)
and the projections of the slip directions of the corresponding partial dislocations (red lines) on the
specimen surface. Primary SS—bold lines, secondary SS—dashed lines, third SS—dash-dot lines.
b Crystallographic orientation map of the AOI in IPF colouring with respect to the loading axis.
The twin system is indicated, and 6 twin bundles are labelled. c Magnitude of shear calculated in
the twin shear direction ½121

calculations are summarized already in Figs. 7.20 and 7.21. Using the g-matrix of
austenitic mother grain, a detailed analysis of activated slip/twin systems was
performed. The results are summarized in Table 7.4 and Fig. 7.29. Figure 7.29a
shows a schematic drawing of traces of the three different slip planes together with
the projection of slip directions of corresponding partial dislocations. Thus, the
primary slip system of regular dislocations and of partial dislocations exhibited
highest Schmid factors (cf. Fig. 7.20a, bold white line). However, thick twin
bundles (numbers 1–6) were formed along the secondary slip plane ð11 1Þ: The
projection of the slip direction of the corresponding leading partial dislocations
½ 1
21 lays parallel to the trace of the slip plane (cf. Fig. 7.29b). Thus, the calculated
magnitude of shear in the direction ½121 was about 0.75 for the thicker twin
bundles (cf. bands No. 1, 3, 4 in Fig. 7.29c). This is in good agreement with
theoretical calculations [25], where the magnitude of shear for twins was deter-
mined to be of 0.7 (see Sect. 3.4.2).
However, smaller twin bundles (cf. bands 2, 5, 6 in Fig. 7.29b) exhibited sig-
nificantly smaller values for magnitude of shear (0.3–0.5). Moreover, bands in
between No. 4 and No. 5 showed even less shear values (around 0.25). One reason
for this could be that these regions were characterized by dislocation glide. Another
reason could be that twins formed in these regions were in the size of nanotwins,
which were non-detectable for EBSD. Similar to EBSD, these regions would be
below resolution of DIC measurements. On the other hand, it is more likely that
these regions belong also to dislocation glide of partial dislocations. Here, the
magnitude of shear in the order of 0.25 would fit very well. This assumption is even
supported by fact that twin bundles occurring in investigated TRIP/TWIP steels
were formed by partial dislocations and can be, therefore, regarded as partial
dislocation-mediated twins.
The same analysis of slip systems was performed for Fe–16Cr–6Mn–6Ni–0.05C
steel, which exhibited a transition from MPT to formation of twin bundles at higher
280 7 Case Studies on Localized Deformation Processes …

Table 7.5 Activated slip systems of the investigated austenitic grain in a Fe–16Cr–6Mn–6Ni–
0.05C TRIP steel deformed in tension at 100 °C (cf. Fig. 7.19)
SP atrace Primary SS Secondary SS Third SS
SDreg SDP1 SDP2 SDreg SDP1 SDP2 SDreg SDP1 SDP2
 
½101 ½211 ½112
   
½110  1
½12  
½211 1
½01  ½ 1
21 ½
11
2
ð111Þ 37.9 0.39 0.45 0.23 0.39 0.22 0.45 – – –
ð11
1Þ 13.7 – – – – – – 0.205 0.21 0.14
SS—slip system, SP—slip plane, SDreg—slip direction of regular dislocations, SDP1—slip
direction of leading partial dislocations, SDP2—slip direction of trailing partial dislocations

temperatures. Results of EBSD measurements and local strain fields obtained from
DIC calculations are summarized already in Figs. 7.18 and 7.19. Using g-matrix of
austenitic mother grain, activated slip systems were calculated, which are sum-
marized in Table 7.5 and Fig. 7.30. As seen already from Fig. 7.19, the austenitic
grain was oriented for co-directional slip on the primary slip plane ð111Þ: The two
possible slip directions ½101 and ½110 had identical Schmid factors (l = 0.39). The
leading partial dislocations with slip direction ½211 are more favourably oriented
(l = 0.45) and are part of both slip systems. The two corresponding trailing partial
dislocations exhibited a significantly less Schmid factor and are, therefore, most
likely not involved in formation of twin bundles. Thus, magnitude of shear shown
in Fig. 7.30 was calculated in ½211 direction. Thus, calculated magnitude of shear
was between 0.20 and 0.30 for twin bundles Nr. 1–4 in Fig. 7.30b. This is less than
the theoretically calculated value (0.7). In addition, it is even less compared to
magnitude of shear calculated for Fe–16Cr–6Mn–9Ni–0.05C steel exhibiting
twinning mechanism already at RT. However, regions between twin bundles also
exhibited in field of magnitude of shear a band-like structure with even lower shear
magnitudes (around 0.1). Similar to Fe–16Cr–6Mn–9Ni–0.05C steel, one reason

Fig. 7.30 Magnitude of shear for twins formed in Fe–16Cr–6Mn–9Ni–0.05C TWIP steel
deformed in tension at RT (cf. Fig. 7.19). a Traces of the three possible slip planes (black lines)
and the projection of the slip directions of the corresponding partial dislocations (red lines) on the
specimen surface. Primary SS—bold lines, secondary SS—dashed lines, third SS—dash-dot lines.
b Crystallographic orientation of the AOI in IPF colouring with respect to the normal direction.
The activated twinning system is indicated. c Magnitude of shear calculated in the twinning shear
direction ½
211
7.2 Microscopic Strain Localizations During Plastic Deformation 281

for lower magnitudes of shear could be that the thickness of these twin bundles is
below resolution of the DIC measurements. On the other hand, it is more likely that
these regions belong also to dislocation glide of partial dislocations. Here, the
magnitude of shear in the order of 0.25 would fit very well. This would be in
agreement with phase map of AOI shown in Fig. 7.21b, where it became obvious
that part of these bands are stacking fault bands (hex). In addition, this is a further
example for the finding that twinned regions and regions with hex crystal lattice
occurred both within same individual deformation band.

7.2.6 Strain Localization During Cyclic Deformation

Microscopic strain localizations occur also in terms of deformation bands during


cyclic deformation of TRIP/TWIP steels. However, these deformation bands have
to be distinguished from persistent slip bands (PSBs) as known for other fcc
metallic materials and alloys. The deformation bands occurring in low-carbon
high-alloy TRIP steels were formed by Shockley partial dislocations resulting in
stacking faults (cf. Sect. 6.4). The stacking fault bands, in particular intersection
points of these bands, were favoured locations for MPT. However, as demonstrated
in Sect. 6.3, onset of martensitic phase transformation depends significantly on

Fig. 7.31 Mechanical stress-strain hysteresis loops for in situ cyclic loading of a Fe–16Cr–6Mn–
6Ni–0.05C TRIP steel at RT and a total strain amplitude of ea;t ¼ 4  103 for selected number of
cycles
282 7 Case Studies on Localized Deformation Processes …

applied total strain amplitude and, consequently, on applied number of cycles. As


shown by Biermann et al. [16], MPT starts after a certain incubation period, which
is determined by threshold of cumulated plastic strain. Thus, the incubation period
is shortened with increase in applied total strain amplitude.
The strain localization during cyclic deformation was also studied by DIC in
combination with quasi in situ tests in SEM. A total strain amplitude of ea;t = 4  10−3
was chosen according to experimental results of Biermann et al. [16] for the in situ test
in order to keep time for in situ tests in a reasonable frame. In addition, SEM images
were not captured for all cycles, but rather at selected numbers of cycles N (1, 5, 15, 30,
50, 75, 100, 150, 200, 250, 300, 350, 400, 475, 550, 625, 700, 775, 850, 925, 1000,
1050, 1100, 1150, 1200, 1250, 1300, 1350, 1400 and 1450 cycles).
The SE contrast images were taken at F = 0 N after unloading from maximum
tensile load. Figure 7.31 shows mechanical hysteresis loops for selected cycles. It
became apparent that with increasing number of cycles a pronounced strain hard-
ening occurred. Thus, maximum tensile and compressive stress amplitudes
increased and plastic strain amplitude decreased. The strain hardening was already
observed at about 30 cycles, which is in agreement with threshold of cumulative

Fig. 7.32 Etched specimen surface of Fe–16Cr–6Mn–6Ni–0.05C TRIP steel during cyclic
loading at ea;t = 4  10−3 at RT at different cycles. SEM images taken in SE contrast at F = 0 N
after unloading from maximum tensile load (cf. Fig. 7.29). a Initial state. b N = 100 cycles.
c N = 400 cycles. d N = 800 cycles. Loading axis horizontal
7.2 Microscopic Strain Localizations During Plastic Deformation

Fig. 7.33 Evolution of the displacement fields and the calculated strain fields of the in situ cyclic loading experiment shown in Fig. 7.29 for different cycles
(N = 100, N = 400, N = 850, N = 1450). From left to the right: SEM image of the specimen surface. Equivalent Von Mises strain evM . Normal strain exx .
Normal strain eyy . Shear strain exy . Formation of deformation bands (white dashed lines) along the primary SS and changes on the specimen surface caused by
283

MPT (red rectangles) are indicated in the SEM images


284 7 Case Studies on Localized Deformation Processes …

plastic strain of about 20 cycles for ea;t = 4  10−3 determined according to


Biermann et al. [16]. At N = 400, pronounced strain hardening was detected.
Comparable to tensile tests, specimen surface was etched resulting in a good
contrast pattern for DIC. Figure 7.32 shows a sequence of SEM micrographs taken
in SE contrast. First deformation band (black line) and a′-martensite grain (black
arrow) became visible at about N = 100 and N = 400 cycles, respectively.
Afterwards, more and more a′-martensite grains appeared on etched surface parallel
to the first one. Due to volume expansion, a′-martensite grains stacked out of
specimen surface causing a pronounced surface profile.
Figure 7.33 shows results of DIC calculation at different cycles. Here, not all
cycles are included. Only these cycles are summarized, where major changes
occurred in local strain field: (a) N = 100, (b) N = 400, (c) N = 850 and
(d) N = 1450. Equivalent Von Mises strain evM , normal strain in x-direction exx ,
normal strain in y-direction eyy and shear strain exy are shown together with SEM
images. However, both crystallographic orientation and phase distribution infor-
mation were necessary for detailed understanding of strain fields.
Figure 7.34 shows results of EBSD measurements of AOI shown in Fig. 7.32.
Thus, along with phase map of AOI in Fig. 7.34a and band contrast map
(Fig. 7.34b), crystallographic orientation of a′-martensite (Fig. 7.34c) and of hex
crystal lattice (Fig. 7.34d) is shown. In addition, region of a′-martensite grains is
shown using band contrast map at higher magnification (Fig. 7.34e). First of all, it

Fig. 7.34 Results of the EBSD measurements of the AOI of the DIC calculations (see Fig. 7.33)
on a Fe–16Cr–6Mn–6Ni–0.05C steel specimen after cyclic loading at RT with a total strain
amplitude of ea;t = 4  10−3 up to 1450 numbers of cycles. a Phase map with indicated
orientation of the austenitic mother grain (loading axis). Red—austenite, yellow—hex crystal
lattice, blue—a′-martensite. b Band contrast map. c, d Crystallographic orientation map of the a′-
martensite and hex crystal lattice, respectively. Colour code with respect to the loading direction,
which lies horizontal. e Region of a′-martensite grains at higher magnification where it becomes
obvious that the macro deformation band is composed of several very thin individual bands (see
white arrows) with a thickness <1 µm (500–750 nm)
Table 7.6 Activated slip systems in the investigated grain of a Fe–16Cr–6Mn–6Ni–0.05C TRIP steel cyclically deformed at RT
SP atrace Tension
Primary SS Secondary SS Third SS Fourth SS
SDreg SDP1 SDP2 SDreg SDP1 SDP2 SDreg SDP1 SDP2 SDreg SDP1 SDP2
½
101 ½
211 1
½ 12 ½101 ½1
12 ½211 ½
110 ½121 ½211 ½110 ½211 1
½ 2
1
ð111Þ 83.5 0.43 0.48 0.26 – – – 0.40 – 0.48 – – –
ð111
 Þ 92.5 – – – 0.42 0.26 0.46 – – – 0.39 0.46 –
Compression
SDreg SDP1 SDP2 SDreg SDP1 SDP2 SDreg SDP1 SDP2 SDreg SDP1 SDP2

½101 1
½21 ½11
2 10
½ 1 11
½ 2 2
½ 1
1 ½1
10 ½121 ½211 ½110 2
½11 ½121
ð111Þ 83.5 0.41 – – – – – 0.39 0.21 – – – –
ð111Þ 92.5 – – – 0.43 – – – – – 0.37 – 0.18
7.2 Microscopic Strain Localizations During Plastic Deformation

SS—slip system, SP—slip plane, SDreg—slip direction of regular dislocations, SDP1—slip direction of leading partial dislocations, SDP2—slip direction of
trailing partial dislocations. Distinction into tensile half-cycle and compressive half-cycle (cf. Fig. 7.31)
285
286 7 Case Studies on Localized Deformation Processes …

became obvious that two different types of deformation bands formed with different
inclination angles to loading axis.
It is clearly visible that the macro deformation band consisted of numerous very
thin individual bands (see white arrows in Fig. 7.34e). The size of these thin bands
is about 500–750 nm. Consequently, a′-martensite grains formed within these
individual bands have similar dimensions (<1 µm). The g-matrix obtained for
austenitic matrix yielded that crystallographic orientation of investigated austenitic
grain is ð100Þ½011 as shown in SST included in Fig. 7.34a. Results of calculation
of activated slip systems for austenitic grain are summarized in Table 7.6. Here, a
differentiation between tension and compression half-cycle loading has been done.
Thus, it turned out that at about 100 cycles, deformation bands formed along two
activated slip systems within austenitic grain with ð100Þ½0 1
1 orientation (cf.
Fig. 7.33a). Both slip systems for regular dislocations ð111Þ½101 and ð
 111Þ½101
had comparable Schmid factors l1 = 0.43 and l2 = 0.42, respectively (cf.
Table 7.6). As seen from location within SST, the grain orientation facilitated for
co-planar and co-directional slip. Therefore, both primary ð111Þ and secondary
ð111Þ slip planes contained each a second Burgers vector with a high Schmid factor
resulting in ð111Þ½110 with l3 = 0.40 and ð111Þ½110 with l4 = 0.39. Thus,
multiple slip on two co-planar, co-directional slip systems was observed.
Figure 7.35a shows stereographic projection of both two slip plane normal
directions (bars; red—primary; blue—secondary SS) and the slip directions (circles;
red—primary, blue—secondary SS) with respect to specimen coordinate system.
Moreover, stereographic projection is combined with traces of slip planes (black
lines) and Burgers vectors (blue lines).

Fig. 7.35 Crystallographic orientation of a′-martensite variants formed during cyclic loading.
a Stereographic projection of the slip plane normal (bars) and slip directions (circles) of the
primary (red) and secondary (blue) slip system in combination with the trace angles of the slip
planes (black lines) and slip directions (blue lines) on the specimen surface. Red lines correspond
to the projections of the slip directions of the Shockley partial dislocations. Dotted blue line
corresponds to the cutting edge with a direction of ½011 of the two slip planes (cf. Fig. 7.25c). b–
d Variants of a′-martensite formed within deformation bands using different IPF colour code maps:
loading axis (b), normal direction (c) and transverse direction (d). Loading axis horizontal
7.2 Microscopic Strain Localizations During Plastic Deformation 287

In addition, the phase map shown in Fig. 7.34a reveals the formation of
deformation bands with hex crystal lattice and a′-martensite grains inside these
bands. Majority of these bands were aligned at 83.5° with respect to loading axis,
which is related to primary slip system ð111Þ½101: However, small deformation
bands with mostly fcc crystal lattice became apparent from Fig. 7.34d, where band
contrast map is shown together with inverse pole figure colouring of hex crystal
lattice according to the loading axis. These bands were inclined at 92.5° with
respect to loading axis belonging to secondary slip system ð 111Þ½101 and include
only quite small a′-martensite areas. Since hex crystal lattice inside deformation
bands is caused by arrangement of stacking faults resulting from dissociation of
regular dislocations into Shockley partial dislocations of type: a6 h112i.
Schmid factors calculated for partial dislocations for all four slip systems are
included in Table 7.6. Regarding partial dislocations, it became obvious that there
are differences between activation of slip systems during tension and compression
half-cycle loading. Thus, for third and fourth SS, trailing partial dislocations were
not activated during tensile half-cycle loading, since slip of these partial dislocations
would lead to a contraction of specimen under tensile load. Vice versa, these trailing
partials were activated during compression, while leading partials (tension) were not
activated, since they would cause a dilation of specimen under compressive load. In
contrast, the regular dislocations on all four slip systems are activated under both
tensile and compressive loads. The projections of slip direction of partial disloca-
tions on specimen surface are shown in Fig. 7.35 (red lines). The distinction between
compression and tension is indicated by letters C and T, respectively.
The number of deformation bands and localized strains within these bands
increased with ongoing cyclic deformation. However, the amount of equivalent
Von Mises strain was significantly less compared to tensile testing. At around 400
cycles, a larger area of higher strain values appeared in images of the Von Mises
strain. Areas with increased or decreased strain values in close vicinity occurred
concurrently in fields of normal strain in exx , eyy and shear strain exy .
In comparison with Fig. 7.34a, c showing phase map and crystallographic ori-
entation of a′-martensite grains, respectively, it turned out that these increased local
strain values correlated well with regions of a′-martensite formed inside macro band
with hex crystal lattice. According to IPF colour codes for all three axes of spec-
imen coordinate system (Fig. 7.35b—loading axis; Fig. 7.35c—normal direction;
Fig. 7.35d—transverse direction), it seemed that only six different types of a′-
martensite types (T) out of 24 possible ones were formed such as: (i) purple (T1),
(ii) magenta (T2), (iii) blue (T3), (iv) orange (T4), (v) rose (T5) and (vi) lilac (T6)
(cf. Fig. 7.35b). This is in agreement with data reported in the literature (e.g. [26]).
In addition, it became apparent that these a′-martensite variants exhibited dif-
ferent shapes and arrangements with respect to both deformation bands and loading
axis. Thus, it is assumed that it is possible to distinct a′-martensite variants, which
were formed according to activation of different shear systems. Moreover, it is
assumed that a distinction should be possible between variants, which formed
during tensile loading part, and those which formed during compressive loading
part of a full cycle loading. Thus, four of these six a′-martensite variants visible by
the IPF colour code maps had their maximum dimension almost parallel to the
288 7 Case Studies on Localized Deformation Processes …

loading axis (T1–T4), whereas two of them are elongated parallel to the y-axis (T5–
T6) (cf. Fig. 7.35b–d).
However, the correlation between the individual a′-martensite variants (T1–T6)
and the local strain values is not straightforward. Therefore, Figs. 7.36 and 7.37
show the local strain fields with overlays of hex crystal lattice and a′-martensite
variants for N = 400 and N = 1450, respectively. The visibility of a′-martensite
formation at N = 400 is in good correlation with knowledge that a certain incu-
bation period for a′-martensite formation is necessary, which is related to cumulated
plastic strain according to Biermann et al. [16]. Thus, according to [16] macro-
scopic threshold of cumulated plastic strain for MPT under cyclic loading is about
20 cycles for a total strain amplitude of 0.4% (ea;t = 4  10−3).
As seen from strain hardening represented by the stress-strain hysteresis loops
shown in Fig. 7.29, MPT within the whole specimen starts already around 30
cycles. In investigated austenitic grain, however, the cyclic MPT started between
350 and 400 cycles. This delay is related to crystallographic orientation of inves-
tigated austenitic grain ð100Þ½011: Nevertheless, between N = 350 and N = 400,
four different a′-martensite variants are formed (T1–T4). The variants T1–T4 cause
different strain values as demonstrated by Fig. 7.36. The clearest picture is obtained
from normal strain eyy . Here, it is easily seen that areas with different strain levels
could be distinguished and were correlated with individual martensite variants.
Thus, variant T2 exhibited strain values eyy between 6 and 12%. In contrast, T1
showed negative values for eyy . The variants T3 and T4 had no contribution to the
normal strain in the y-direction. It became obvious that the local strain caused by the
individual martensite variants was compensated by each other. This became even
more obvious for the higher number of cycles (N = 1450)—as shown in Fig. 7.37.
In particular, normal strain eyy showed alternating regions with positive and neg-
ative eyy values, which could be correlated with two variants T1/T2. Variant T5
caused significant shear strain exy . However, normal strain exx was mostly related to
glide of partial dislocations along four activated slip systems.
More clarity about the martensite variants formed during cyclic loading—in-
volving both compressive and tensile loadings of material—could be achieved by a
detailed analysis of the crystallographic data. According to Kitahara et al. [27], 24
martensite variants (V1–V24), which can be formed out of an austenitic grain of
any orientation maintaining the KS-OR, were calculated using provided orientation
transformation matrices in [27]. Table 7.7 summarizes the g-matrices for all 24
martensite variants for the investigated grain including both the KS-OR and the
misorientation relationship of each variant with respect to V1. Figure 7.38a shows
calculated 24 theoretically possible a′-martensite variants for investigated austenitic
grain using SST ½001  ½011  ½111 for loading axis (x-direction). The data point
belonging to crystallographic orientation of austenitic mother grain ð100Þ½0 11 is
marked by a red cross.
Figure 7.38b shows IPF map with identified variants T1–T6, and in Fig. 7.38c a
comparison of theoretically possible 24 variants V1–V24 with determined crys-
tallographic orientation of formed a′-martensite grain using IPF colour code is
7.2 Microscopic Strain Localizations During Plastic Deformation

Fig. 7.36 Combination of results of DIC calculations with results of EBSD measurements for N = 400. From left to right: normal strain exx , normal strain eyy ,
shear strain exy , equivalent Von Mises strain evM . Middle row: Deformation bands with hex crystal lattice. Bottom row: Crystallographic orientation of hex
crystal lattice together with orientation of a′-martensite grains
289
290

Fig. 7.37 Combination of results of DIC calculations with results of EBSD measurements for N = 1450. From left to right: normal strain exx , normal strain
eyy , shear strain exy , equivalent Von Mises strain evM . Middle row: Deformation bands with hex crystal lattice. Bottom row: Crystallographic orientation of hex
crystal lattice together with orientation of a′-martensite grains
7 Case Studies on Localized Deformation Processes …
Table 7.7 Calculated g-matrices for 24 martensite variants V1–V24 using the g-matrix of the austenitic mother grain and the transformation matrixes
provided by Kitahara et al. [27]
Variant nr. g-matrix Kurdjumov–Sachs OR Misorientation to V1
g11 g12 g13 g21 g22 g23 g31 g32 g33 Plane Direction Angle (°) Axis
V1 0.523 –0.352 0.777 –0.374 0.724 0.580 –0.766 –0.593 0.247 ð111Þc k ð011Þa0 ½101
  k ½111
c a0
– –
 
V2 0.087 0.996 –0.036 –0.984 0.081 –0.160 –0.156 0.050 0.986 ð111Þc k ð011Þa0 ½101c k ½111a0 60 111
 
V3 –0.502 –0.631 –0.593 –0.348 –0.480 0.806 –0.792 0.610 0.021 ð111Þc k ð011Þa0 ½011
  k ½111 0
c a
60 011
V4 0.463 –0.517 0.721 –0.310 0.667 0.678 –0.830 –0.537 0.149 ð111Þc k ð011Þa0 ½011c k ½111a0 10 ½011
V5 –0.021 0.983 –0.184 –0.989 –0.049 –0.146 –0.152 0.179 0.972 ð111Þc k ð011Þa0 ½110
  k ½111 0
c a
60 ½011
 
V6 –0.551 –0.479 –0.684 –0.417 –0.553 0.722 –0.723 0.682 0.105 ð111Þc k ð011Þa0 ½110c k ½111a0 49.4 011
 
V7 –0.999 –0.026 –0.056 0.030 –0.998 –0.058 –0.054 –0.060 0.997 ð111Þc k ð011Þa0 ½101 k ½111 0
c a 49.4 111
 
V8 0.388 –0.617 –0.685 0.640 –0.355 0.682 –0.664 –0.702 0.257 ð111
 Þ k ð011Þ 0
c a ½101c k ½111a0 10.3 111
V9 0.448 0.588 0.674 –0.645 –0.310 0.699 0.620 –0.747 0.240 ð111Þc k ð011Þa0 ½110 k ½111 0
c a 50.4 0.615 –0.184 0.767
V10 –0.993 0.096 0.082 –0.100 –0.994 –0.056 0.076 –0.064 0.995 ð111
 Þ k ð011Þ 0
c a ½110c k ½111a0 50.4 0.739 0.463 –0.491
V11 0.550 –0.562 –0.618 0.579 –0.278 0.768 –0.602 –0.779 0.172 ð111Þc k ð011Þa0 ½011 k ½111 0
c a 14.7 –0.946 –0.359 –0.066
V12 0.604 0.522 0.603 –0.576 –0.237 0.783 0.551 –0.820 0.157 ð111
 Þ k ð011Þ 0
c a ½011c k ½111a0 57.2 0.357 –0.603 –0.714
V13 –0.441 0.664 0.605 –0.335 0.504 –0.797 –0.833 –0.553 0.000 ð111
 Þ k ð011Þ 0
c a ½011
  k ½111 0
c a 14.7 –0.359 0.946 0.066
V14 0.479 0.484 –0.733 –0.373 –0.644 –0.669 –0.795 0.593 –0.128 ð111
 Þ k ð011Þ 0
c a ½011c k ½111a0 50.4 0.490 –0.464 0.739
V15 –0.085 –0.980 0.185 –0.979 0.117 0.172 –0.190 –0.167 –0.967 ð111
 Þ k ð011Þ 0
c a ½101 k ½111 0
c a 57.2 0.739 0.246 –0.628
7.2 Microscopic Strain Localizations During Plastic Deformation

V16 –0.498 0.516 0.698 –0.396 0.581 –0.712 –0.772 –0.630 –0.085 ð111
 Þ k ð011Þ 0
c a ½101c k ½111a0 20.5 –0.663 0.863 0.365
V17 0.526 0.316 –0.791 –0.439 –0.696 –0.570 –0.729 0.645 –0.227 ð111
 Þ k ð011Þ 0
c a ½110 k ½111 0
c a 51.7 0.659 –0.363 0.659
V18 0.019 –1.000 0.035 –0.983 –0.012 0.186 –0.186 –0.038 –0.982 ð111
 Þ k ð011Þ 0
c a ½110c k ½111a0 47 0.720 0.302 –0.626
V19 –0.423 –0.425 0.801 0.667 0.453 0.593 –0.614 0.784 0.092 ð111Þc k ð011Þa0 ½110
  k ½111 0
c a 50.4 0.186 –0.767 –0.615
V20 0.995 –0.079 0.067 0.095 0.957 –0.276 –0.043 0.280 0.959 ð111Þ k ð011Þ 0
c a ½110c k ½111a0 57.2 –0.357 –0.714 0.603
V21 –0.573 0.415 –0.707 –0.553 0.441 0.707 0.605 0.796 –0.023 ð111Þc k ð011Þa0 ½011 k ½111 0
c a 20.5 –0.962 0 0.298
(continued)
291
Table 7.7 (continued)
292

Variant nr. g-matrix Kurdjumov–Sachs OR Misorientation to V1


g11 g12 g13 g21 g22 g23 g31 g32 g33 Plane Direction Angle (°) Axis
V22 –0.582 –0.375 0.723 0.601 0.401 0.692 –0.548 0.836 –0.008 ð111Þc k ð011Þa0 ½011c k ½111a0 47 0.303 –0.626 –0.720
V23 0.996 0.010 –0.094 –0.035 0.962 –0.274 0.087 0.276 0.957 ð111Þ k ð011Þ 0
c a ½101 k ½111 0
c a 57.2 0.246 0.628 0.739
V24 –0.414 0.454 –0.790 –0.618 0.498 0.609 0.669 0.739 0.075 ð111Þc k ð011Þa0 ½101c k ½111a0 20.9 –0.918 0.412 0
In addition, Kurdjumov–Sachs orientation relationships and misorientation are given
7 Case Studies on Localized Deformation Processes …
7.2 Microscopic Strain Localizations During Plastic Deformation 293

Fig. 7.38 Stereographic standard triangle containing the crystallographic orientations of the
theoretical possible 24 a′-martensite variants (a) and the experimentally observed orientations
(c) shown in the IPF colouring mode (loading axis) displayed in (b). Red cross indicates the
orientation of the austenitic mother grain

Fig. 7.39 Crystallographic orientations of all grains labelled in Fig. 7.35 and listed in Table 7.7
using the SST both with respect to the loading axis and with respect to the surface normal direction
in comparison with the calculated theoretical 24 martensite variants. In addition, IPF colour map of
loading axis is displayed
294 7 Case Studies on Localized Deformation Processes …

provided. Thus, it turned out that all martensite grains visible in Fig. 7.38b correlate
with at least 6 different variants of a′-martensite, which are denoted as V1–V6 in
Table 7.7. However, it is also visible that each colour type T1–T6 can be related to
different martensite variants V1–V6. For more clarity, therefore, the SSTs are
shown in Fig. 7.39 in more detail according to each type T1–T6. Here, the SST for
each variant T1–T6 is shown with respect to loading axis (left side) and to normal
direction (right side). For the sake of simplicity, the experimentally determined data
points are shown in IPF colouring code of loading axis (cf. Fig. 7.38b). Indeed, it
became obvious that each type T consisted at least of three up to six variants V1–
V6. Consequently, the IPF colouring was not unique for one individual crystallo-
graphic orientation. This is in agreement with Nolze and Hielscher [28], where it is
shown that the actual used IPF colour coding concept does not allow in all cases a
clear distinction of different orientations based on the IPF colour map only. It is
stated that “… for higher symmetries a simultaneous IPF mapping of two or three
standard reference directions is insufficient for an unequivocal orientation assign-
ment…” [28]. The proposed new colour keys are available in MTEX—a free
available MatLab toolbox. The fact that each IPF colouring type T consists of
several variants of a′-martensite is consistent with the pole figure representation for
the a′-martensite shown in Fig. 7.39.
In a next step, it was proved for each individual martensitic grain included in IPF
pole figure map (approximately 100 grains) to which variant it belongs.
Figure 7.40a shows labelling of individual grains, and a list of grains belonging to
different types of martensite is provided in Table 7.8. Thus, it is obvious that the
majority of grains belongs to T1 (purple) and T3 (blue) followed by T2 (magenta)
and T4 (orange).

Fig. 7.40 Pole figure representation for both the austenitic mother grain and the cyclic
strain-induced a′-martensite formed within deformation bands. The colouring corresponds to the
IPF colour code with respect to the loading axis x
7.2 Microscopic Strain Localizations During Plastic Deformation 295

The smallest number of grains is related to T5 (rose) and T6 (lilac). In addition, it


became obvious that well-defined orientation relationships in terms of twin
boundaries existed between different variants of martensite. Thus, boundaries
between T1/T2 and T3/T4, respectively, were R3 boundaries (60° h111i) (see white
lines in Fig. 7.41b). Second-order twin boundaries (R11; 49° h110i) were observed
between T1/T3 and T4/T5, respectively (see green lines in Fig. 7.41b).
Activated slip systems, their Schmid factors, trace of slip planes and projection of
slip directions on specimen surface were calculated for each individual grain labelled
in Fig. 7.41a and listed in Table 7.8, and are summarized in Table 7.9. The grains
were sorted according to Schmid factors in descending order. In addition, grains
were labelled according to theoretically calculated variants (compare Table 7.6).
First of all, it turned out that each IPF colour type of martensite T1–T6 contained at

Table 7.8 Assignment of grain labelling to different types of martensite according to IPF colour
code
Type of martensite Grain number
T1 (purple) 4, 8, 10, 16, 21, 23, 24, 28, 29, 30, 39, 40, 42, 61, 64, 67, 87, 89
T2 (magenta) 5, 6, 18, 19, 20, 22, 25, 31, 35, 36, 44, 49, 52, 53, 55, 88
T3 (blue) 14, 15, 27, 33, 34, 43, 45, 47, 50, 51, 54, 62, 63, 72, 74, 77, 78, 86
T4 (orange) 18, 38, 48, 59, 60, 66, 68, 75, 76, 79, 81, 82, 85
T5 (rose) 7, 9, 41, 46, 56, 70, 80, 91
T6 (lilac) 2, 11, 65, 71

Fig. 7.41 a′-martensite formed during cyclic loading of Fe–16Cr–6Mn–6Ni–0.05C steel at RT


within deformation band. a Labelling of martensite grains. b Twin boundaries between different
martensite types: R3 (white lines) and R11 (green lines)
Table 7.9 Activated slip systems of martensitic variants (primary and secondary)
296

IPF colour type T Grain nr. Variant Schmid factor Primary SS Schmid factor Secondary SS KS-OR
SP SD SP SD
µ 
ð101Þ ½11
1 µ ð101Þ ½111
T1: purple 89 V1 0.463 83.0 32.0 – – – ð1
11Þc k ð011Þa0
40 V6 0.463 83.5 –39.7 – – – –
24 V2 0.460 –49.7 –47.0 0.460 39.6 35.1 ð111Þc k ð011Þa0
30 V2 0.460 –49.7 –47.0 0.460 39.6 35.1 ð111Þc k ð011Þa0
21 V2 0.459 –49.9 –47.2 0.459 39.4 35.0 ð111Þc k ð011Þa0
64 V5 0.459 47.4 36.8 0.459 –43.3 –44.6 ð111Þc k ð011Þa0
16 V1 0.449 83.6 39.2 – – – –
4 V1 0.436 82.7 44.8 – – – –
10 V1 0.435 83.6 44.3 – – – –
8 V1 0.435 83.5 44.5 – – – –
28 V1 0.432 83.4 44.9 – – – –
29 V1 0.431 83.5 45.2 – – – –
39 V1 0.431 83.5 45.2 – – – –
87 V1 0.430 83.7 45.4 – – – –
23 V1 0.429 83.9 45.5 – – – –
42 V6 0.412 84.6 –39.7 – – – ð1
11Þc k ð011Þa0
61 V6 0.400 83.5 –41.1 – – – ð1
11Þ k ð011Þ 0
c a
67 V6 0.395 82.0 –41.0 – – – ð1
11Þc k ð011Þa0
(continued)
7 Case Studies on Localized Deformation Processes …
Table 7.9 (continued)
IPF colour type T Grain nr. Variant Schmid factor Primary SS Schmid factor Secondary SS KS-OR
SP SD SP SD
µ 
ð101Þ ½11
1 µ ð101Þ ½111
Number of variants 4 4
T2: magenta 19 V2 0.461 –49.6 –46.9 0.460 39.6 35.2 ð111Þc k ð011Þa0
25 V2 0.460 –45.8 –46.0 0.459 44.2 35.4 ð111Þc k ð011Þa0
35 V2 0.458 –50.5 –47.9 0.458 38.8 34.2 ð111Þc k ð011Þa0
53 V2 0.458 –51.1 –47.8 0.458 38.2 34.5 ð111Þc k ð011Þa0
44 V1 0.458 –44.6 –45.6 – – – –
18 V2 0.455 –50.1 –47.5 0.458 45.9 36.0 ð111Þc k ð011Þa0
5 V2 0.453 82.9 45.0 0.455 39.4 35.6 ð111Þc k ð011Þa0
6 V2 0.452 –50.2 –47.8 0.451 39.2 35.3 ð111Þc k ð011Þa0
22 V1 0.432 83.1 45.4 – – – –
36 V1 0.430 83.7 45.4 – – – –
20 V1 0.429 83.6 45.6 – – – –
55 V4 0.424 81.2 –30.8 – – – ð1
11Þc k ð011Þa0
7.2 Microscopic Strain Localizations During Plastic Deformation

31 V6 0.403 83.1 –41.2 – – – ð1


11Þ k ð011Þ 0
c a
88 V6 0.402 83.8 –41.4 – – – ð1
11Þc k ð011Þa0
49 V6 0.402 83.2 –40.6 – – – ð111
 Þ k ð011Þ 0
c a
52 V6 0.398 82.5 –40.9 – – – ð1
11Þc k ð011Þa0
(continued)
297
Table 7.9 (continued)
298

IPF colour type T Grain nr. Variant Schmid factor Primary SS Schmid factor Secondary SS KS-OR
SP SD SP SD
µ 
ð101Þ ½11
1 µ ð101Þ ½111
Number of variants 4 3
T3: blue 74 V5 0.466 47.0 37.0 0.465 –43.3 –44.9 ð111Þc k ð011Þa0
78 V1 0.464 83.0 32.4 – – – ð111
 Þ k ð011Þ 0
c a
77 V5 0.462 47.0 37.0 0.461 –43.3 –44.9 ð111Þc k ð011Þa0
54 V4 0.462 83.4 –34.4 – – – –
43 V2 0.459 –50.4 –47.8 0.459 38.8 34.2 ð111Þc k ð011Þa0
50 V2 0.459 –51.5 –48.3 0.459 37.7 33.6 ð111Þc k ð011Þa0
47 V2 0.459 –49.7 –46.7 0.459 39.6 35.7 ð111Þc k ð011Þa0
86 V2 0.458 –49.8 –47.4 0.457 39.6 34.9 ð111Þc k ð011Þa0
34 V2 0.458 –50.4 –46.9 0.456 38.2 35.6 ð111Þc k ð011Þa0
51 V2 0.448 –50.2 –48.1 0.448 39.4 –35.5 ð111Þc k ð011Þa0
63 V3 0.436 83.8 –27.5 – – – –
62 V1 0.433 83.7 44.5 – – – –
27 V1 0.433 83.3 45.0 – – – –
72 V4 0.411 81.7 –36.2 – – – ð1
11Þc k ð011Þa0
14 V6 0.409 84.3 –40.5 – – – ð111
 Þ k ð011Þ 0
c a
33 V6 0.404 83.5 –41.1 – – – ð1
11Þc k ð011Þa0
15 V6 0.402 83.3 –41.1 – – – ð111
 Þ k ð011Þ 0
c a
45 V6 0.398 83.7 –41.9 – – – ð1
11Þc k ð011Þa0
(continued)
7 Case Studies on Localized Deformation Processes …
Table 7.9 (continued)
IPF colour type T Grain nr. Variant Schmid factor Primary SS Schmid factor Secondary SS KS-OR
SP SD SP SD
µ 
ð101Þ ½11
1 µ ð101Þ ½111
Number of variants 6 5
T4: orange 82 V2 0.462 –50.4 –47.9 0.461 38.8 33.7 ð111Þc k ð011Þa0
68 V1 0.462 82.8 34.6 – – – –
81 V2 0.461 –49.3 –46.9 – – – –
66 V5 0.455 46.9 36.4 0.455 –43.9 –45.1 ð111Þc k ð011Þa0
18 V2 0.455 –44.6 –45.6 0.454 45.9 36.0 ð111Þc k ð011Þa0
79 V5 0.454 46.5 35.9 0.453 –44.3 –45.6 ð111Þc k ð011Þa0
85 V1 0.433 82.5 45.6 – – – –
38 V1 0.433 82.6 45.4 – – – –
59 V1 0.432 82.7 45.6 – – – –
48 V6 0.403 84.7 –41.5 – – – –
76 V6 0.401 82.7 –40.7 – – – ð1
11Þc k ð011Þa0
60 V6 0.399 82.6 –40.6 – – – ð1
11Þ k ð011Þ 0
c a
7.2 Microscopic Strain Localizations During Plastic Deformation

75 V6 0.399 83.7 –42.0 – – – ð1


11Þc k ð011Þa0
(continued)
299
Table 7.9 (continued)
300

IPF colour type T Grain nr. Variant Schmid factor Primary SS Schmid factor Secondary SS KS-OR
SP SD SP SD
µ 
ð101Þ ½11
1 µ ð101Þ ½111
Number of variants 4 3
T5: rose 56 V1 0.465 82.7 33.1 – – – ð1
11Þc k ð011Þa0
7 V1 0.463 83.5 44.0 – – – –
46 V5 0.461 47.7 37.2 0.461 –42.8 –43.7 ð111Þc k ð011Þa0
9 V1 0.460 83.3 44.0 – – – –
80 V5 0.459 46.8 36.6 0.459 –43.7 –44.6 ð111Þc k ð011Þa0
41 V1 0.435 83.2 44.5 – – – –
70 V6 0.402 82.5 –39.7 – – – ð1
11Þc k ð011Þa0
91 V6 0.396 83.2 –42.2 – – – ð111
 Þ k ð011Þ 0
c a
Number of variants 3 3
T6: lilac 71 V5 0.458 47.2 36.9 0.458 –43.4 –44.4 ð111Þc k ð011Þa0
11 V3 0.444 84.1 –26.7 – – – ð111
 Þ k ð011Þ 0
c a
2 V3 0.441 83.1 –26.7 – – – ð1
11Þc k ð011Þa0
65 V1 0.429 82.8 46.6 – – – V
Number of variants 3 2
Total number of variants 24 20
Schmid factors l, trace angles of slip planes (SP) and angles of the projection of the slip direction (SD) on the specimen surface
7 Case Studies on Localized Deformation Processes …
7.2 Microscopic Strain Localizations During Plastic Deformation 301

Table 7.10 Summary of observed variants and their orientation or misorientation relationships,
respectively
Variants KS-OR KS-OR No. of Specific
primary SP secondary SP KS-OR misorientation
ð111Þc k ð011Þa0 ð111Þ k ð011Þ
c a0
T1—purple 4 V2, V5 V1, V6 – –
T2—magenta 4 V2 V4, V6 V1 Twin (R3)
T3—blue 6 V2, V5 V1, V4, V6 V3 Twin (R11)
T4—orange 4 V2, V5 V6 V1 Twin (R3)
T5—rose 3 V5 V1, V6 – –
T6—lilac 3 V5 V3 V1 Twin (R3)
Total 24 9 11 4 4 twin systems

least 3 to 6 different a′-martensite variants of type V1–V6. Therefore, 24 different a′-


martensite variants were formed within deformation bands in the austenitic grain
with the ð100Þ½011 orientation during cyclic loading. However, 20 variants fulfilled
the KS-OR regarding either primary slip plane or secondary slip plane of austenitic
mother grain. The remaining four variants fulfilled twin orientation relationships as
summarized in Table 7.10. Moreover, two martensite variants exhibited orienta-
tions, which facilitated double slip (identical µ values for primary and secondary slip
systems) on nearly symmetric arranged slip systems: V2 and V5. In this case, an
effective slip direction could be expected. Furthermore, habit planes, direction of
shape change (long direction), invariant shear system of the austenite and corre-
sponding shear system of related a′-martensite variants were obtained from detailed
slip system analysis according to [26] and are summarized in Table 7.11.

Table 7.11 Habit planes, invariant shear systems in austenite and corresponding shear systems in
a′-martensite according to variants V1–V6 and IPF colour types T1–T6
T V Habit Invariant Shear Invariant Shear Invariant Shear
plane shear system in shear system in shear system in
system in c a′ system in c a′ system in c a′
T1 V2 ð1
21Þ – – ð111Þ½211 ð101Þ½011 – –
V5 ð1
21Þ – – – – ð111Þ½121 ð101Þ½110
T2 V2 ð1
21Þ – – ð111Þ½211 ð101Þ½130 – –
T3 V2 ð1
12Þ ð111Þ½211 ð101Þ½101 – – – –
V5 ð1
21Þ – – – – ð111Þ½121 ð101Þ½110
T4 V2 ð1
12Þ ð111Þ½211 ð101Þ½101 – – – –
V5 ð1
21Þ – – – –  
ð111Þ½121  Þ½110
ð101
T5 V5 ð
211Þ – – – –  
ð111Þ½121  Þ½110
ð101  
T6 V5 ð
211Þ – – – –  
ð111Þ½121  Þ½101
ð101
302 7 Case Studies on Localized Deformation Processes …

Fig. 7.42 Habit planes and long directions of a′-martensite variants in combination with invariant
shear directions of austenite and corresponding shear directions of martensite. a Band contrast map
of area with a′-martensite grains. b Traces of habit planes (black) and projections of long directions
(blue) and invariant shear directions of austenite (red). c Correlation of invariant shear systems
austenite/shear systems martensite with respect to the martensite variants V1–V6. d Visualization
of the arrangements of slip systems for individual variants V1–V6 belonging to IPF colour types
T1–T6. Traces of slip planes are given by bold black lines and projection of slip directions by
dashed black lines. Note for V2 and V5 double slip is indicated

Thus, Fig. 7.42 shows band contrast map (Fig. 7.42a) of area with a′-martensite
grains together with arrangements of both habit planes and long directions of a′-
martensite as well as invariant shear directions of austenitic mother grain (Fig. 7.42b).
It turned out that three different habit planes were detected such as ð1 21Þ; ð112Þ and
ð211Þ (black lines) with their corresponding long directions ½101; ½1
  10 and ½011
(blue lines), respectively, which is in agreement with [26]. The possible invariant shear
directions related to primary and secondary slip planes of the austenite were also
indicated: ½211; ½211; ½112 and ½121 (red lines). It turned out in Tables 7.9 and 7.10
that grains belonging to one IPF colour type T exhibited different crystallographic
orientations related to variants V1–V6. Furthermore, the two variants V2 and V5
fulfilled KS-OR for primary slip plane according to ð111Þc k ð011Þa0 : In addition, the
variant V2 is present at least in T1 to T4, whereas V5 is present in all types T except T2.
The variant V5 is related to shear direction ½121; which is only activated during
compressive loading. Therefore, grains belonging to T5 and T6 were formed definitely
during the compressive half-cycle loading, since no other invariant shear systems were
available, whereas all grains having V2 orientation were formed during tension
half-cycle deformation. The shear systems shown in Fig. 7.42 for the variants V1, V3,
V4 and V6 fulfilled the KS-OR for the secondary slip system. Since secondary slip
7.2 Microscopic Strain Localizations During Plastic Deformation 303

system is not involved in MPT with same extent as primary ones, it is assumed that
these shear systems are not activated. Instead, these variants act as
stress-accommodating systems due to dislocation glide or twinning. As shown in
Fig. 7.41, some of them are twin-related: e.g. V1 and V3. In addition to shear systems,
a visualization of traces of slip planes and projection of slip directions on surface for
each variant according to different IPF colour types is shown in Fig. 7.42d.
It became obvious that nearly for all IPF colour types an ideal compensation of
the shear strain is expected due to the operating shear/slip systems. Thus, in T1
(purple), T3 (blue) and T4 (orange) the V2 and V5 exhibited double slip on sym-
metrically oriented slip planes with opposite traces and slip directions. These two
variants fulfilled the KS-OR belonging to the primary slip plane of the austenite
ð111Þ: The variants V1, V3, V4 and V6 had a common slip plane but different slip
directions and were related to the KS-OR of the secondary austenitic slip plane
ð111Þ: In addition, the variants marked by red rectangle belong to twinning systems.
However, since each individual grain belongs to another crystallographic variant of
a′-martensite, specific grain arrangements have to be regarded separately in order to
interpret the calculated complex local strain fields. Therefore, four examples of indi-
vidual grain arrangements are shown in Fig. 7.43a–d. Here, grains in IPF colouring and
labelling according to Fig. 7.41 and Table 7.8, respectively, are shown together with
(i) visualization of slip plane traces and projection of slip direction for each individual
grain with indicated variant, (ii) invariant shear systems of the austenite and (iii) three
strain components of the strain tensor such as exx , eyy and exy . However, how complex
the situation of interpretation of strain fields is will be demonstrated by first example—
as shown in Fig. 7.43a. Here, two grain arrangements are depicted consisting of both
grains belonging to T1 (purple) and T2 (magenta). However, as shown before grains of
same IPF colour type could have different orientations leading to different activations
of invariant shear systems, twinning or dislocation glide.
The crystallographic orientation of the six grains 20, 21, 22, 25, 29 and 35 with
respect to the loading axis is apparent from the SST. For grains 21, 25 and 35, the
invariant shear system of variant V2 is activated, which fulfil the KS-OR of the
primary slip plane. The other grains—20, 22 and 29—are oriented for the activation
of variant V1, which fulfil the KS-OR for the secondary slip plane. The invariant
shear system for this variant is similar to the shear system of variant 2; however, the
primary slip plane ð111Þc is here parallel to a ð101Þa0 plane and the invariant shear
direction ½211c parallel to the ½011a0 direction. It becomes obvious that the shear
systems of V2 and V1 are twin-related, which resulted in opposite shear contri-
butions leading, finally, to a self-accommodation of strain. Thus, the opposite shear
contribution in terms of eyy becomes obvious for the grain arrangement 25/29/35.
Whereas for the grains 25 and 35 positive values for eyy were determined, the eyy
values for grain 29 were negative. The situation for the grain combination 20/21/22
was not that clear as for the previous one. However, also for grain 21 a positive eyy
value is detected. However, grains 20 and 22 exhibit eyy strain value around zero
(20) or even positive (22), but less than for 21. Nevertheless, this could be inter-
preted in terms of the interaction between grain 22 (V1, T2) and grain 25 (V2, T1).
304 7 Case Studies on Localized Deformation Processes …

Fig. 7.43 Interpretation of local strain fields obtained from DIC for different individual
arrangements/combinations of a′-martensite grains (a–d). IPF colour code with grain labelling
is shown together with the specific alignment of invariant shear systems for each grain. The
specific grain orientations and a′-martensite variants are indicated in the SST. Furthermore, the
strain tensor components exx , eyy , exy are shown with indicated specific alignments of slip systems
and invariant shear systems. The colour code of the strain maps is simplified as follows: green—
zero values, red—maximum positive values, blue—maximum negative values
7.2 Microscopic Strain Localizations During Plastic Deformation 305

Figure 7.43b shows another combination of a′-martensite grains. As seen from


the SST, grains 4 and 6 were related to V1 and grain 10 to V2. In addition, both
grains were twin-oriented (R3) to grain 10. Grain 14, however, was related to V6,
which is also a twin orientation (R11) to grain 10. Similar to the first example, grain
6 belonging to V2 resulted in positive eyy values, whereas the grains 4 and 10
exhibited negative eyy values. Vice versa, the shear strain exy is positive for grains 4
and 10, whereas grain 6 causes a negative shear strain. In contrast, the grain 14 (V6)
occurred during compression due to the activation of the shear direction ½1 21:
However, it is also visible that the self-accommodating counterpart to grain 14
(V6), which would be of V2, is missing. Therefore, the shear strain caused by the
formation of grain 14 (V6) with a pronounced negative shear strain is not com-
pensated by the twin variant of this grain. Consequently, higher positive shear strain
values were found in the surrounding of this grain. In addition, in the normal strain
field exx is visible that positive exx values of grain 14 were accompanied by negative
exx values symmetrically on each side, which could be most likely, in addition, the
results of volume expansion caused by a′-martensite.
A third example is shown in Fig. 7.43c. Here, we have a combination of grains
5, 8, 15, 18. The exact crystallographic orientation is again represented by the SST.
It becomes obvious that different twin relationships were present in this configu-
ration. Thus, grains 5 and 8 belonging to V2 and V1, respectively, are twin-related
(R3) and had a habit plane of ð121Þ: The grains 15 and 18 related to V6 and V2,
respectively, also exhibit a twin orientation relationship (R3), but were character-
ized by a habit plane ð112Þ: Finally, also grains 8 (V1) and 15 (V6) were twins,
however, of type R11. Thus, the activation of V2 for both grains 5 and 18 should
result in positive strain values eyy . It is true for grain 5. However, grain 8 is maybe
too small to be detected by the DIC. Nevertheless, in contrast to grain 5, both grains
8 and 15 exhibited negative strain values eyy .
The first three examples discussed above were just taken at the border areas of
the a′-martensite region. Thus, in these cases, the individual a′-martensite variants
were influenced more or less only by the activation of self-accommodating twin
systems. The example shown in Fig. 7.43d, however, is taken from middle part of
martensitic region. Here, the strain fields caused by martensite variants will be most
likely also influenced by variants formed in adjacent tiny deformation bands. Here,
two different grain configurations will be discussed. The first one is related to grains
51, 54 and 60. Each of the grains 51 and 54 is twin-related to grain 60, but they are
also twin-related to each other, since all three grains belong to different variants
(51 ! V2, 54 ! V4 and 60 ! V6). Both variants V2 (grain 51) and V4 (grain
54) caused positive strain values eyy , whereas V6 resulted in negative eyy values.
The interpretation of the shear strain exy was not that clear, since here definitely
interactions with the other martensitic grains have to be taken into account. More
suitable for the interpretation of the shear strain exy is the second grain configuration
shown in Fig. 7.43d. These two grains—66 and 80—belong to T4 and T5. As
stated already above, the grains of T5 were formed during the compression
half-cycle loading. Both grains belong to variant V5. However, it becomes obvious
306 7 Case Studies on Localized Deformation Processes …

that there is a difference in the long direction between grain 60 (discussed before),
which is also of V5, and grain 66. The long direction of grain 66 is closer to d0 11e
than d110e for grain 60 (cf. Fig. 7.42b). Thus, it could be assumed that grain 66 was
also formed during a compressive half-cycle loading. Since DIC calculation was
performed only for selected intervals and not distinguished between tension and
compression half-cycle loading, this argumentation, however, remains quite spec-
ulative. Nevertheless, grain 66 is related to pronounced positive normal strain
values eyy , whereas grain 80 exhibits positive shear strain values exy .
Even more intuitive seems the interpretation of normal strain fields exx . At all
investigated cyclic loading intervals, a similar picture was present as demonstrated
in Fig. 7.44 for entire AOI at different numbers of cycles (N = 400, 850, 1100 and
1450). Positive and negative strain values exx were aligned with slip traces of both
primary ð111Þ and secondary ð111Þ slip planes. The positive and negative strain
values could be interpreted in terms of different activated partial dislocations and
projection of their slip directions distinguished into tensile and compressive load-
ing. Thus, during tensile half-cycle loading, on the ð111Þ plane two slip directions
of partial dislocations were activated—½211 and d 1
12e.
Both shear directions led to positive strain values exx . On the other hand, during
the compressive half-cycle loading the slip directions d 12
1e and d121e were acti-

vated on the primary ð111Þ and secondary ð111Þ slip plane, respectively, resulting
both in negative strain values exx . However, these strain values caused by activation
of partial dislocations are less compared to values in regions where a′-martensite
grains are formed. In addition, negative exx strain values alongside with the max-
imum positive strains exx are most likely caused by volume expansion due to
formed a′-martensite grains.

Fig. 7.44 Normal strain fields exx at different numbers of cycles (N = 400, 850, 1100 and 1450) in
combination with the arrangement of slip traces and the projections of slip directions of partial
dislocations. Differences between tension and compression are indicated by T and C, respectively
7.2 Microscopic Strain Localizations During Plastic Deformation 307

7.2.7 Discussion

Sections 7.2.1 to 7.2.6 have demonstrated well that strain localizations occurring
under tensile or cyclic loading at RT or even at elevated temperatures (up to 200 °C)
can be investigated using the DIC technique in combination with in situ experiments
in a high-resolution SEM. In the following, some specific aspects regarding both the
spatial resolution and the accuracy of the SEM-DIC technique used in the present
work will be discussed.
General aspects of resolution and accuracy of SEM-DIC. According to Schreier
et al. [29], the resolution and the accuracy of strain results obtained by DIC depend
generally on different parameters. These parameters are:
(i) The field of view (FOV): L  L (m2)
(ii) The recorded image resolution: R  R (pixels2)
(iii) The magnification factor: MT (pixels/m)
(iv) The subset size: n  n (pixels2)
(v) The image displacement accuracy: bl (pixels)
(vi) The image speckle dimension: gl (pixels)
(vii) The object speckle dimension: g0 (m)
(viii) The object dimension: l0 (m).
Using these parameters, the object displacement accuracy b0 , the minimum
object speckle size g0 and the minimum spatial resolution ðl0 Þmin achievable with
DIC can be calculated according to the following equations [29]:

L
b0 ¼ b ð7:2Þ
R l
L
g0 ¼ g ð7:3Þ
R I
n
ðl0 Þmin ¼ ð7:4Þ
MT

In case of the SEM-DIC, in particular, the occurrence of image shifts and image
distortions related to the scanning nature of the imaging process have to be
accounted for. Schreier et al. [29] showed that for individual SEM types (Zeiss
Gemini, FEI Nova Nano, Hitachi 4800S) different magnitudes of shifts in both
horizontal and vertical directions in the image plane are measured. Thus, the
maximum horizontal and vertical shift varied from 1 nm (ZEISS) up to 7 nm (FEI,
Hitachi).
In the present work, the SEM-DIC was performed with a FE-SEM Mira3 XMU
(Tescan), with a FOV of 51  38 µm2 and an image resolution R = 2048  1538
pixels2, which resulted in 25 nm/pixel (L/R) in horizontal (x) and vertical direction
(y) (Fig. 7.45).
308 7 Case Studies on Localized Deformation Processes …

Fig. 7.45 Resolution of SEM-DIC obtained in the present work. a Etch pit surface contrast
pattern used for SEM-DIC with a FOV 51  38 µm2, the subset size of 30  30 pixels2 and 10
pixels distance of measuring points exemplarily shown for a reference image. b Same FOV after
15% tensile deformation at 200 °C of a Fe–16Cr–6Mn–9Ni–0.05C TWIP steel. Obviously,
identical features in (a) and (b) are marked by white arrows

In addition, drift distortions and stress relaxations have to be accounted for


during SEM-DIC in combination with in situ mechanical testing. Stress relaxations
occurred on each interruption at selected applied strain levels for capturing SEM
image, which results in the typical stress drops as shown in Fig. 7.3b. Therefore, a
relaxation time of at least 90 s was accounted for after interrupting the tensile test
before capturing the SEM image. In addition, the capturing time with 67 s per
image was kept as low as possible for good signal-to-noise ratio. As shown by
Kammers and Daly [30], the drift distortions are negligible for capturing times less
than 120 s. Furthermore, it is shown that the drift velocity was depending on the
image resolution. Thus, the drift velocity in the x- and y-direction was about 0.1
pixel/min at high image resolution of about 25 nm/pixel as used in the present
investigations. The strain error caused by this drift distortion could be as large as
0.01 as shown by Kammers and Daly [30]. Figure 7.46 shows the strain error from
distortion for exx , eyy and exy . Thus, as it turned out from these strain error fields, the
7.2 Microscopic Strain Localizations During Plastic Deformation 309

Fig. 7.46 Strain error fields from drift distortion achieved at maximum load of a tensile test on
aluminium alloy used for SEM-DIC. a exx . b eyy . c exy . Reproduced from [30]. Permission of
Springer

drift distortion can result in either an overestimation (right bottom corner of exx or
middle part of exy ) or underestimation (left side of exx , right and left part of eyy ,
upper and lower part of exy ) of the strain values.
The maximum pixel drift occurring in the present experiments is expected not to
be higher than 0.1 pixel per image with a capturing time of 67 s after a relaxation
time of 90 s. Therefore, the strain error from distortion drift should be less than
0.01. This is consistent with the experimental outcome of the strain field calcula-
tions. Thus, the strain fields exx, eyy and exy determined in all experiments disclosed
that systematically over- or underestimated strain regions are obviously not present
within the FOV (compare, e.g., Figs. 7.10, 7.14, 7.21, 7.36 and 7.37). Therefore, no
effort was applied on a distortion correction in the present experiments.
Sub-µDIC. The application of the etching technique as a classical method for the
creation of a high-quality contrast pattern on the specimen surface resulted in
high-resolution local strain fields in terms of both the lateral resolution and the
resolution of the localized strains. Thus, regarding the lateral resolution it can be
concluded that this technique is suitable to detect strain localizations on a micro-
scopic level down to few hundreds of nanometres. Therefore, the terminus µDIC
introduced by Tasan et al. [31] with a lateral resolution in dual-phase steels of few
micrometres can be extended to sub-µDIC, where even microstructural features
below 1 µm were detected by DIC (cf. Fig. 7.9a, b). The smallest detected
deformation band by both techniques the DIC and the EBSD is in the order of less
than 500 nm. A second indicator for the excellent lateral resolution of the DIC is
the fact that the local strain values for individual martensitic grains formed within
deformation bands can be determined even for martensitic grains with dimensions
less than 1 µm. The resolution in terms of the strain values is also reasonably good.
The absolute resolution of strain values is about 0.001. This is perfectly demon-
strated for the magnitude of shear determined for different individual constituents of
the microstructure such as (i) deformation bands with stacking faults, (ii) individual
a′-martensite grains as well as (iii) twin bundles. Thus, the magnitude of shear
calculated for stacking fault bands and twin bundles is in good agreement with
310 7 Case Studies on Localized Deformation Processes …

theoretically determined values (s = 0.35 and 0.7, respectively). Furthermore, the


orientation dependence of the magnitude of shear was demonstrated. In addition, it
was demonstrated by the application of this technique for cyclic experiments that
the formation of martensite grains during tensile and compressive half-cycle
loading could be separated. Again, the localized strains caused by different
martensitic variants could be separated in combination with a detailed analysis of
slip systems and the analysis of the variant selection. Finally, these investigations
are the proof of the self-accommodation of strains caused by different variants due
to twinning. However, it turned out that the interpretation of the local strain fields
requires the combination with a detailed crystallographic analysis and under-
standing. Therefore, the combination of the SEM-DIC with in situ EBSD mea-
surements would lead to an improvement in understanding and knowledge of
variant selection. In particular, a stepwise following of the formation of a′-mar-
tensite variants during a complete loading cycle seems to be of high interest. Thus,
it is clear from the actual DIC results in combination with the crystallographic
analysis that the formation of one specific a′-martensite variant is directly accom-
panied by a second variant in order to self-accommodate the resulting shear strain
mainly by twinning. But, up to now, it is not clear when this self-accommodating
variant is formed: (i) at the maximum tension load or during the unloading up to
zero load. Therefore, it would be of high interest to follow one complete individual
load cycle within a specific grain with a suitable grain orientation for MPT with
both SEM-DIC and in situ EBSD. But, the etched surface as a necessary require-
ment for high-resolution DIC is in contradiction to the requirements for EBSD
measurements, which need a flat and smooth specimen surface without any (or at
least with low) roughness profile. Thus, here some other techniques creating suit-
able surface patterns for high resolution according to recommendations by the
literature (e.g. [29, 30]) have to be studied for future investigations.
Influence of testing conditions. The presented sub-µDIC technique together with
in situ mechanical testing in the SEM revealed that a large variety of testing
conditions could be applied without a loss of resolution or accuracy. Thus,
microscopic strain localizations caused by both tensile and cyclic loadings were
investigated at the same high lateral resolution and with the same accuracy
according to the strain values. In addition, tensile tests performed at elevated
temperatures up to 200 °C revealed that the increase in temperature did not result in
significantly higher drift distortions or a loss of the spatial resolution. As shown in
Figs. 7.22 and 7.44, the slip bands occurring during tensile deformation at 200 °C
in a Fe–16Cr–6Mn–9Ni–0.05C TWIP steel have a width of about 250 nm and are
perfectly detected by the sub-µDIC.
Influence of grain size. The grain size of the investigated material has, however, a
significant influence on the detectability of strain localizations on microscopic level
in terms of deformation bands or martensitic grains. Thus, the experiments described
7.2 Microscopic Strain Localizations During Plastic Deformation 311

in Sect. 7.2 were performed on as-cast Fe–16Cr–6Mn–xNi–0.05C TRIP/TWIP steel


exhibiting a large grain size in a range of 50–2000 µm. In these cases, the strain
localizations started either in the interior of a grain on pre-existing lattice defects
such as SFs, SF tetrahedrons and subgrain boundaries or at large angle grain
boundaries (LAGBs). In addition, these deformation bands do not cross the entire
austenitic grains. Therefore, these bands could be interpreted as single-ended bands
or single-ended pile-ups (at grain boundary). According to (2.20), the average shear
strain is determined by the ratio of the product of number of dislocations and the
corresponding Burgers vector and two times the length of the deformation band.
Thus, in case of Fig. 7.10, the length of the deformation band at e = 15% is about
140 µm with respect to an overall grain size of 500 µm. Assuming the shear strain of
partial dislocations h112i is about 0.01, the number of dislocations involved in this
shear is about 1.9  104. Further assuming that these partials are operating on in
average each second f111g lattice plane, this would result in a thickness of a
deformation band of about 8 µm. The double shear strain of 0.02 carried by the
partial dislocations would involve 3.8  104 dislocations resulting in a deformation
band with 16-µm thickness. Thus, the shear strains exy between 0.01 and 0.02 are in
good agreement with the present investigations performed under tensile load up to
macroscopic strain of e = 15% for a Fe–16Cr–6Mn–6Ni–0.05C TRIP steel.
Assuming the same shear strain of exy = 0.01 in twins, where partial dislocations
operate on each f111g lattice plane, the thickness of the twin bundles should be
around 4 µm. This is again in good agreement with the experimental findings for the
Fe–16Cr–6Mn–9Ni–0.05C TWIP steel.
Reducing the grain size and, consequently, the length of the deformation bands
or the pile-ups will result in deformation bands with significantly reduced thick-
nesses assuming the same amount of shear strain exy = 0.01. Thus, for a
single-ended deformation band with a length of 30 µm, the involved partial dis-
locations would be in the order of 4  103 resulting in a width of the deformation
band of about 1.7 µm. This fits well with the investigations of a smaller austenitic
grain in Fe–16Cr–6Mn–6Ni–0.05C steel as shown in Fig. 7.14. Thus, here the
thickness of deformation bands is in the order of 1–2 µm. Moreover, it becomes
obvious that the shear strain is higher than 0.01 and is nearly homogenously dis-
tributed in the area with a high density of deformation bands. The smaller grain size
causes already at lower macroscopic strain values double-ended pile-ups, which
results, finally, either in the activation of parallel slip planes or in a slip transition
into neighbouring grains. Table 7.12 and Fig. 7.47 summarize these results for the
Fe–16Cr–6Mn–6Ni–0.05C TRIP and Fe–16Cr–6Mn–9Ni–0.05C TWIP steels
under different loading conditions and with different lengths of slip planes,
respective deformation bands. Thus, it becomes obvious that with decreasing length
of the deformation bands the corresponding thickness of the deformation bands is
also decreasing at similar assumed shear strains exy , and the strain is more
homogenously distributed within the grain (except for deformation bands along
another slip system).
312 7 Case Studies on Localized Deformation Processes …

Table 7.12 Calculation of the involved number of dislocations in the formation of stacking fault
bands and twin bundles according to (2.20) and the resulting thickness of the corresponding bands.
The necessary parameters are: lattice constant a = 0.3593 nm; Burgers vector ~ bh112i = 0.1467 nm;
lattice spacing d f111g = 0.2047 nm
exy Tensile loading Cyclic loading
(c) Stacking fault bands (6% Twin bundles (9% Ni) Stacking fault bands (6%
Ni) Ni)
L (µm) ndis dDB L (µm) ndis dDB L (µm) ndis dDB
(104) (µm) (104) (µm) (104) (µm)
0.01 140 1.9 7.8 70 0.9 1.8
0.02 140 3.8 15.6 70 1.9 3.8
0.01 30 0.4 1.6 30 0.4 0.82
0.05 30 2 8.2 30 2 4.1
0.001 50 0.68 0.28
0.002 50 1.4 0.54
0.004 50 2.7 1.1

Fig. 7.47 Comparison of the shear strain fields for Fe–16Cr–6Mn–6Ni–0.05C steel (a, c, d) and
Fe–16Cr–6Mn–9Ni–0.05C steel (b) with different lengths of deformation bands after tensile
loading (a–c) and cyclic loading (d). a Single-ended stacking fault bands; L = 140 µm.
b Single-ended twin bundles; L = 70 µm. c Double-ended stacking fault bands; L = 30 µm.
d Single-ended stacking fault bands; L = 50 µm
7.3 Time Sequence of Deformation Processes 313

7.3 Time Sequence of Deformation Processes

A powerful tool for investigations on the evolution of deformation processes is the


acoustic emission (AE) measurement technique since it is a non-destructive,
real-time and volume-integrating method (cf. Sect. 5.3). As demonstrated before,
the occurring microstructural processes during mechanical testing of high-alloy Fe–
16Cr–6Mn–xNi–0.05C TRIP/TWIP cast steels are quite complex. Thus, processes
such as (i) dislocation glide, (ii) formation of stacking fault bands or twin bundles
providing strain localizations and (iii) martensitic phase transformation are running
simultaneously. Using the AE data analysis, it becomes possible to separate the
different processes and to determine which process is predominant at different
deformation levels. The overall goal is the determination of temporal evolution of
the deformation mechanisms.

7.3.1 Acoustic Emission Measurements and Analysis

Tensile deformation tests on high-alloy Fe–16Cr–6Mn–xNi–0.05C cast steels were


performed in combination with in situ AE measurements in order to investigate the
time sequence of the ongoing deformation processes. The individual deformation
mechanisms have to be identified from the registered AE signals. In addition, their
evolution over the entire deformation process has to be evaluated. Hence, the
threshold-less, continuous AE signal acquisition method using a single AE sensor
was applied (cf. Sect. 5.3.4).
Flat tensile specimens with a rectangular cross section of 8  4 mm2 and a gauge
length of 35 mm were machined from cast plates after solution annealing. The gauge
length was tailored two times in order to reduce the amount of plastic deformation in
the area where the AE sensor was mounted. Tensile deformation of the specimens
was conducted under cross head displacement control with a nominal initial strain
rate of 3  10−3 s−1 and 1  10−2 s−1, respectively, on electromechanical testing
frames (Hegewald & Peschke, Germany, and Zwick 1476, Germany). The tests were
done in a temperature range of RT  T  100 °C. Temperatures > RT were
realized at Zwick 1476 equipped with a climate chamber. The temperature was
controlled using thermocouple fixed at the gauge length of the specimen.
Figure 7.48 shows the used specimen geometry as well as the experimental setup for
RT experiments (Hegewald & Peschke) and at elevated temperatures (Zwick 1476).
The experimental setup for the AE signal registration was based on an 18-bit
PCI-2 data acquisition board (Mistras, USA). The AE sensor was fixed at the
shoulder part of the test specimens using rubber band. Machine oil was used as a
coupling media between sensor and specimen surface. Two different types of dif-
ferential broadband sensors were used—(i) sensor 1045D (Fuji Ceramics, Japan)
with an applicable temperature range up to 80 °C and (ii) senor WD FS63 (Mistras,
USA) with a temperature range up to 140 °C.
314 7 Case Studies on Localized Deformation Processes …

Fig. 7.48 Experimental setup for in situ AE measurements during tensile deformation at RT and
elevated temperatures. a Geometry of flat tensile specimens and AE sensor location. b Specimen
mounted for RT experiments on the electromechanical testing device of Hegewald & Peschke.
c Specimen mounted for tensile deformation at elevated temperature on the electromechanical
testing device of Zwick in combination with climate chamber

The AE signals from the sensor output were amplified by 60 dB using a


low-noise PAC 2/4/6 preamplifier (Mistras, USA) and passed through a 30–
1200 kHz band-pass filter (FA01, Microsensors AE). The AE data were recorded
with a high sampling rate of 2 million samples per second (MSPS).
The processing of the recorded AE data was performed according to descriptions
of spectral analysis provided in Sect. 5.3.5. The AE noise signal was recorded at
least for 2–3 s before starting the tensile deformation. The continuously streamed
data were sectioned into consecutive individual realizations of 4096 readings. The
number of the individual realizations depends on the overall length of the recorded
AE data stream and should be always in the order of 2n. For each of these 4096
readings, the FFT was performed and corrected by the FFT of the laboratory noise
level [see (5.40) and (5.41)] resulting in PSDFs for each of the individual reali-
zation consisting of 4096 readings [see (5.22) and (5.41)]. The average AE energy
E and the median frequency fm of each PSDF were computed by definitions pro-
vided in Table 5.4. As a result of the spectral analysis, different types of PSDFs
were obtained. In order to compare them, normalized averaged PSDFs according to
(5.23) were determined. Based on the different normalized PSDFs, a clustering
procedure using the quite recently developed adaptive sequential k-means
(ASK) algorithm [32] (cf. Sect. 5.3.4) was performed as demonstrated by an
example in Fig. 5.25 in Sect. 5.3.5. The results of the cluster analysis were used in
order to follow the temporal evolution of individual clusters respective deformation
processes. The interpretation of the results of the AE cluster analysis was corro-
borated by post-mortem SEM investigations with backscattered electron
(BSE) imaging and electron backscattered diffraction (EBSD). In order to avoid any
preparation influence on the material state, the gauge parts of the specimens were
7.3 Time Sequence of Deformation Processes 315

vibration-polished for 24 h with 0.02 µm colloidal silica. The SEM investigations


were performed using the field-emission scanning electron microscope (Mira 3
XMU, Tescan, Czech Republic) equipped with the OIM™ technology from
EDAX/TSL.
The time duration of the deformation tests depends on the material, the defor-
mation temperature and mostly the nominal strain rate and was, therefore, in a range
between 110 and 240 s. Because of the relatively high data acquisition rate, the
amount of data received in a single continuously recorded AE stream is in the range
of 0.5–1 G byte resulting in time-consuming calculations involving millions of
Fourier transforms and data manipulation during clustering. Therefore, the
above-described ASK procedure was applied only to the first 60 s of the test.
Actually, this region was of greatest interest since all major structural transforma-
tions occur during this time.

7.3.2 Acoustic Emission During the Deformation Process

The acoustic emission signals were recorded threshold-less and continuously during
the entire deformation process. Figure 7.49a shows exemplarily the complete AE
data stream obtained during tensile test at RT and 10−2 s−1 on the Fe–16Cr–6Mn–
3Ni–0.05C steel synchronized with the stress–time curve. The marked red windows
in Fig. 7.49a are shown as a detail of Dt = 1 s in Fig. 7.49b. It becomes apparent
that over the entire deformation process a high intensity of acoustic emission sig-
nals occurs. As seen from Fig. 7.49a, the acoustic emission activities start directly
at the beginning of the tensile tests. Here, a high number of transient burst signals
appeared, which are overlapping each other simulating a continuous signal flow
with high amplitude. However, the detail in Fig. 7.49b revealed the high density of
burst signals with different amplitudes.

Fig. 7.49 Threshold-less and continuously recorded AE data stream. a AE data stream (green)
synchronized with the stress–time curve (black) for Fe–16Cr–6Mn–3Ni–0.05C steel tested in
tension at room temperature and at a strain rate of 1  10−2 s−1. b Detail of the marked area in the
AE time-series in (a) showing a very intensive flux of AE bursts of different amplitudes.
Reproduced from [33]. Permission of Elsevier
316 7 Case Studies on Localized Deformation Processes …

The complete AE data streams synchronized with the stress–time curves


obtained for the three different Fe–16Cr–6Mn–xNi–0.05C TRIP/TWIP cast steel
variants obtained at RT and the nominal strain rate of 10−2 s−1 are provided in
Fig. 7.50. In all cases, the level of AE activity significantly increases after the

Fig. 7.50 AE data streams (green) synchronized with the stress–time curves (black) obtained
during tensile testing at room temperature and at a strain rate of 1  10−2 s−1 of the three
investigated high-alloy TRIP/TWIP steels: a Fe–16Cr–6Mn–9Ni–0.05C, b Fe–16Cr–6Mn–6Ni–
0.05C and c Fe–16Cr–6Mn–3Ni–0.05C. Reproduced from [33]. Permission of Elsevier
7.3 Time Sequence of Deformation Processes 317

beginning of mechanical loading and is well above the electronic laboratory noise
level over the entire deformation process. Overall, the AE data streams consist of
high density of burst signals; thus, the appearance of continuous-type AE signals
cannot be revealed simply by superficial observation. However, differences in the
detected AE activities for the tested steel variants become obvious already by naked
eye. The Fe–16Cr–6Mn–3Ni–0.05C steel, which has the lowest austenite stability
and, therefore, the most pronounced TRIP effect, exhibits the highest AE signal
activity in terms of both the number of burst-type signals and the amplitude U of
recorded signals. Different scales of the ordinate axis in terms of AE signals and the
stress values for the three different steel variants should be noted. However, from
the overall complete AE data streams a distinction between different deformation
mechanisms is impossible. Thus, mechanical twinning, stacking faults, martensitic
phase transformation and crack initiation are powerful sources of AE leading to
burst-type signals. Instead, dislocation glide will result in continuous flow of AE
signals, but it is hidden probably by the numerous burst-type signals. Only
burst-type signals occurring after necking and passing the UTS can be related most
probably to crack initiation and final failure of the materials. In Fe–16Cr–6Mn–
3Ni–0.05C steel, some of the bursts at higher strain values can be related to the
stress drops in the stress-strain curve (see Sect. 7.4).
According to the AE data analysis described in Sect. 5.3.5, the complete AE data
stream is sectioned into individual windows of 4096 data points. The subsequently
performed FFT resulted in the PSDF, which is characterized by the two main
parameters—the AE energy E and the median frequency fm. Before discussing
various specific shapes of the PSDF, temporal evolution of these two parameters in
combination with the stress-strain curves of the three investigated steel variants as
shown in Fig. 7.51 will be in the focus. Similar to Fig. 7.50, differences in the AE
behaviour of the steel variants become obvious. Thus, the Fe–16Cr–6Mn–9Ni–
0.05C steel exhibits unusual oscillatory behaviour of AE parameters during
straining (see Fig. 7.51a), which is still noticeable for Fe–16Cr–6Mn–6Ni–0.05C
steel but less pronounced (Fig. 7.51b). However, the parameter E is in antiphase
with the parameter fm. If the AE energy decreases, the median frequency increases
and vice versa. In addition, high energy AE bursts are observed over the entire
deformation process.
In contrast, the Fe–16Cr–6Mn–3Ni–0.05C steel shows a quite different beha-
viour in comparison with the other two steel variants (see Fig. 7.51c). Thus, the
median frequency jumps up at around the yield stress and decreases then contin-
uously during the entire deformation process. However, it should be noted that for
this steel variant the evaluated median frequencies are in general on a higher level
than for the other two steel variants. The energy of the AE signals reached maxi-
mum values around the yield point and drops significantly to lower levels.
However, high energy bursts are recognized at higher strain levels correlated with
the occurring serrated plastic flow.
Thus, the different deformation behaviours of the three TRIP/TWIP steel vari-
ants become already apparent from the two general parameters of the power spectral
density function (PSDF). Whereas the AE histories of Fe–16Cr–6Mn–6Ni–0.05C
318 7 Case Studies on Localized Deformation Processes …

Fig. 7.51 Time sequence of the parameters AE energy E and median frequency fm derived from
the power spectral density function obtained by fast Fourier transformation of the AE data in
combination with the stress-strain curves; a 9 wt% nickel, b 6 wt% nickel and c 3 wt% nickel.
Room temperature and strain rate 1  10−2 s−1. Reproduced from [33]. Permission of Elsevier
7.3 Time Sequence of Deformation Processes 319

steel and Fe–6Cr–6Mn–9Ni–0.05C steel are comparable with the AE behaviour


observed commonly on pure fcc metals and single-phase materials [34–36], the AE
behaviour of the steel with the lowest austenite stability is different. In materials
such as copper [35], aluminium [36] or a-brass [34], dislocation glide is a dominant
mechanism of plastic deformation. Here, the time sequence of AE is characterized
by a decrease in the energy and an increase in the median frequency over the whole
deformation process, which can be understood in terms of reduced mean free path
for the dislocation motion and increased average dislocation velocity with increased
strain hardening. Moreover, it was shown that the stacking-fault energy has a
significant influence on the AE energy. Thus, Vinogradov et al. [34] and Hatano
[37] showed that the AE energy is decreasing significantly with the stacking-fault
energy, which can be understood in terms of the dislocation mobility. The dislo-
cation mobility is higher in materials with higher stacking-fault energy where
dislocation motion via cross-slip is much easier. The stacking-fault energies of the
investigated steel variants decrease with reduction of nickel content. Thus, it can be
concluded that dislocation motion has to be taken into account as possible defor-
mation mechanism in steels with higher SFE (Fe–16Cr–6Mn–9Ni–0.05C steel and
Fe–16Cr–6Mn–6Ni–0.05C steel), but it does not play the dominant role in Fe–
16Cr–6Mn–3Ni–0.05C steel.
In order to obtain more details on different deformation mechanisms and their
interaction, a classification of the AE data in terms of the shape of the average
normalized PSDF derived from the FFT of the AE data streams was performed
according to the ASK algorithm described in Sect. 5.3.5.
Thus, three specific types of PSDF were obtained at least for each steel variant as
shown in Fig. 7.52. Here, the normalized averaged PSDFs are plotted vs. the entire
frequency range 20 kHz  f  1000 kHz. Both the different shapes of the specific
types of PSDFs in terms of frequency and energy and the differences between
individual steel variants become apparent.
Steel variants Fe–16Cr–6Mn–9Ni–0.05C and Fe–16Cr–6Mn–6Ni–0.05C exhibit
at least one common type of PSDF, which is called type 1 and given by red PSDF
curve (see Fig. 7.52a, b). This type of PSDF is characterized by strong peak at low
frequencies at about 70–80 kHz. The shape of the PSDF is comparable to the PSDF
calculated from electronic laboratory noise level detected before starting tensile
deformation given in black. This curve also has a pronounced peak at low fre-
quencies but a lower intensity. Thus, PSDF of type 1 describes AE signals with low
energy and low frequency. The laboratory noise can be described as a continuous
AE signal. Therefore, AE signals belonging to type 1 PSDF also should be con-
tinuous AE signals and can, thus, be correlated with the dislocation glide behaviour.
Type 1 PSDFs are observed in both Fe–16Cr–6Mn–9Ni–0.05C steel and Fe–16Cr–
6Mn–6Ni–0.05C steel, but are not detected for steel with lowest austenite stability.
PSDF of type 2 (blue curve Fig. 7.52a) identified in Fe–16Cr–6Mn–9Ni–0.05C
steel looks completely different to type 1. There is also a remarkable amount of AE
signals with low frequencies at about 70–200 kHz. However, in addition a high
amount of signals with higher frequencies at about 700–1000 kHz was observed.
320 7 Case Studies on Localized Deformation Processes …

Fig. 7.52 Different types of average normalized power spectral density functions of AE signals
derived from fast Fourier transformation of AE data streams collected during tensile testing of Fe–
16Cr–6Mn–9Ni–0.05C steel (a), Fe–16Cr–6Mn–6Ni–0.05C steel (b) and Fe–16Cr–6Mn–3Ni–
0.05C steel (c) at room temperature and at a strain rate of 1  10−2 s−1. Reproduced from [33].
Permission of Elsevier
7.3 Time Sequence of Deformation Processes 321

Thus, this type of PSDF belongs to AE signals, which can be described by higher
energies and higher frequencies compared to type 1.
Type 3 PSDF (green; Fig. 7.52a) of Fe–16Cr–6Mn–9Ni–0.05C steel just lies in
between type 1 and type 2. Even more pronounced in terms of high-energy and
high-frequency signals are the PSDFs of type 1 (blue) detected in Fe–16Cr–6Mn–
3Ni–0.05C steel (Fig. 7.52c) and type 3 (blue) in Fe–16Cr–6Mn–6Ni–0.05C steel
(Fig. 7.52b). Type 2 PSDFs (magenta) observed in Fe–16Cr–6Mn–6Ni–0.05C and
Fe–16Cr–6Mn–3Ni–0.05C steels exhibit quite similar behaviour.
Evidently, the mean PSDF shapes are different even for naked eye. However, for
naked eye it also seems that some mean PSDFs are similar (e.g. type 2 and type 3
for Fe–16Cr–6Mn–6Ni–0.05C steel, type 3 for Fe–16Cr–6Mn–6Ni–0.05C steel and
type 1 for Fe–16Cr–6Mn–3Ni–0.05C steel), while the others are absolutely specific
for each material. Thus, each specific type of PSDF can be correlated with a specific
deformation mechanism. This seems to be quite straightforward for the type 1
PSDF in Fe–16Cr–6Mn–9Ni–0.05C and Fe–16Cr–6Mn–6Ni–0.05C steels, which
is linked to the dislocation glide. However, the interpretation of the other types of
PSDFs needs further clarification. Thus, the different types of PSDFs could be used
in order to identify differences in the occurring deformation mechanisms and their
kinetics. Therefore, the different PSDFs are used for a cluster analysis. According to
the algorithm described in Sect. 5.3.5, signals with similar features (energy and

Fig. 7.53 Results of the AE cluster analysis in terms of energy E and median frequency fm
coordinates based on the different types of PSDFs identified by FFT for Fe–16Cr–6Mn–9Ni–
0.05C steel (a, b), Fe–16Cr–6Mn–6Ni–0.05C steel (c) and Fe–16Cr–6Mn–3Ni–0.05C steel (d),
respectively. b Enlarged detail of (a). Reproduced from [33]. Permission of Elsevier
322 7 Case Studies on Localized Deformation Processes …

median frequency) are grouped together. The aim of the clustering procedure is to
minimize dissimilarities between individual cluster members and to maximize
dissimilarities between signals belonging to different clusters—here based on the
Kullback–Leibler divergence criterion (see Sect. 5.3.4). The results of the per-
formed cluster analysis are shown in Fig. 7.53 using scatter plots of the two
parameters E and fm.
The indicated clusters are identical in terms of colour and labels of the types of
PSDFs provided in Fig. 7.52. Clearly, three specific clusters can be distinguished
for each steel variant. Nevertheless, overlap of individual clusters occurs as well.
Again, significant differences between the individual clusters and the steel variants
become apparent.
Steel with highest and medium austenite stability. Cluster 1 behaves in similar way
for Fe–16Cr–6Mn–9Ni–0.05C and Fe–16Cr–6Mn–6Ni–0.05C steels and is char-
acterized by low energy and low median frequency. In addition, cluster 2 (9 wt%
Ni) and cluster 3 (6 wt% Ni) exhibit comparable features and are completely
different to cluster 1 as mentioned already for the PSDFs shown in Fig. 7.52.
Signals belonging to these types of PSDFs do not form a dense cluster like cluster
1. However, these signals are characterized by significantly higher values of AE
energy and median frequency. The characteristics of cluster 3 (9 wt% Ni) and
cluster 2 (6 wt% Ni) are quite similar to cluster 1 and show a significant overlap
with this cluster. However, they are shifted to higher median frequencies, which are
even more pronounced for cluster 2 of Fe–16Cr–6Mn–9Ni–0.05C steel than for
cluster 3 of Fe–16Cr–6Mn–6Ni–0.05C steel.
Steel with lowest austenite stability. The characteristics of clusters identified on this
steel variant are completely different to the other two steel variants. Cluster 1 shows
similar characteristics as cluster 3 of Fe–16Cr–6Mn–6Ni–0.05C steel, but is more
pronounced in terms of number of elements contributing to this cluster.
Finally, the results of the cluster analysis give rise to both the qualitative and
quantitative distinctions between different AE sources and their varying contribu-
tion on different states of the entire deformation process.
Therefore, in a next step the time sequence of individual clusters was evaluated.
Both the number of clusters and the cumulated energy were regarded with respect to
their evolution during the entire deformation process. Figure 7.54 shows the evo-
lution of specific AE clusters over a larger timescale. Clearly, each specific cluster
evolves its own specific time sequence over the entire deformation process. The
grey line in Fig. 7.54a indicates the noise level. A number of events belonging to
this cluster are just jumping up at the beginning of the mechanical test and remain
then constant over the whole deformation process. Moreover, it becomes once more
evident that the AE activity of each specific cluster is well above the noise level.
Thus, in combination with the recorded stress-strain curves the evolution of the
specific clusters allows to determine the onset of individual deformation mecha-
nisms and its dominance during the deformation process. However, the explicit
7.3 Time Sequence of Deformation Processes 323

Fig. 7.54 Schematic representation of temporal evolution of cumulated number of elements


(a) and cumulated energy (b) for each cluster identified by cluster analysis shown in Figs. 7.52 and
7.53, which can be correlated with different sources of AE associated with different deformation
mechanisms

correlation of each AE cluster with individual deformation mechanism should be


corroborated by detailed characterization of the microstructure developed during
the mechanical tests.

7.3.3 Influence of Chemical Composition

In the following, it will be shown how the specific clusters identified for each steel
variant can be correlated with individual deformation mechanisms. Hence, the
results are categorized according to the austenite stability and stacking-fault energy.
High austenite stability. The Fe–16Cr–6Mn–9Ni–0.05C steel reveals the highest
austenite stability (Ms = –60 °C) as well as the highest SFE (cSF  23 mJ/m2).
Therefore, the deformation behaviour of this steel is dominated by
deformation-induced twinning resulting in the TWIP effect as described compre-
hensively already in Sects. 6.3 (mechanical behaviour) and 6.4 (microstructure).
Martensitic phase transformation is not observed in a considerable amount. Thus,
possible sources of acoustic emission during plastic deformation of this steel should
be (i) the dislocation glide and (ii) deformation-induced twinning. This is in good
agreement with the detected clusters of AE signals and their evolution during the
deformation process. Figure 7.55 shows the time sequence of the individual AE
clusters derived from the cluster analysis in combination with the stress-strain curve
obtained during tensile test at RT and a strain rate of 10−2 s−1. Immediately with the
beginning of the deformation process, cluster 1 (red) starts to develop. As already
discussed in Figs. 7.52 and 7.53, this cluster can be correlated with dislocation
glide. Both the number of elements and the cumulated energy of this cluster are
increasing continuously until the end of the deformation process. However, the
slope of the increase is changing over the deformation process. After passing the
324 7 Case Studies on Localized Deformation Processes …

Fig. 7.55 Time sequence of AE clusters evaluated for Fe–16Cr–6Mn–9Ni–0.05C steel and
correlated with different deformation mechanisms—dislocation glide and mechanical twinning—
shown in combination with the stress-strain curve obtained during tensile test a room temperature.
a Cumulated AE energy. b Number of elements per cluster. Reproduced from [33]. Permission of
Elsevier

yield point, cluster 2 (blue) appears. However, it is much less intense both in
number of cluster elements and in accumulation of AE energy. Nevertheless, the
number of elements increases up to an applied strain level of about 30%. At
e > 30%, the number of cluster elements remains more or less constant. The
accumulated AE energy by these cluster elements is significantly low. At e  30%,
cluster 3 (green) evolves in the time sequence of the AE signals. The number of
elements and the cumulated energy of this cluster increase until the end of defor-
mation process, but again changing the slope at around e = 40%. The stationary
part of cluster 2 and the beginning of cluster 3 correlate well with a decreased slope
in cluster 1. Vice versa, the decreased slope in cluster 3 at e  40% results in an
increased slope of cluster 1.
Corroborating these results by microstructural characterizations, it turned out
that both clusters 2 and 3 are correlated with mechanical twinning. Figure 7.56
shows typical microstructure of this steel variant obtained after tensile deformation
at RT to strain at failure (e = 42%). The SEM micrograph using BSE contrast (see
Fig. 7.56a) reveals clearly a banded structure of two different kinds. There is on one
the hand a quite thick band structure, slightly bended and in some cases elongated
nearly parallel to the loading direction. On the other hand, there are a higher number
of straight and thin bands terminated by the thicker band structure. As it turned out
from EBSD measurements, both band structures are related to deformation twins as
demonstrated by the red lines in Fig. 7.56b indicating twin boundaries with the
typical misorientation axis/angle pair of 60° h111i and by the crystallographic
orientation map in Fig. 7.56c. The thicker bands are twins of primary generation.
These twins start to develop in well-oriented grains early in the deformation process
and can be, therefore, correlated with cluster 2. Caused by the large grain size and
the demand of deformation compatibility at the grain boundaries, significant
changes of the crystallographic orientations occur by grain rotations. Thus, at
higher strain values twinning is activated also on secondary twin systems, which are
7.3 Time Sequence of Deformation Processes 325

unfavourably oriented at lower strain levels. These twins are twins of second
generation and can be correlated with the thinner bands terminated by the twins of
first generation. The twins of second generation are related to cluster 3 becoming
dominant at around 40% of elongation. However, in situ experiment in combination
with DIC revealed that secondary twins can occur as well earlier in the deformation
process depending on the specific grain orientation (cf. Fig. 7.20). The number of
twins of second generation is increased in comparison with twins of first generation.
Moreover, the accumulated AE energy of this cluster is significantly higher. This
can be understood in terms of reduced mean free path due to the twins of first
generation and an increased velocity. The lower energy of the twins of first gen-
eration can be understood as well. Due to the large grain size of the as-cast
microstructure, they do not develop with the sound of velocity across the entire
grain as expected commonly. Since deformation-induced twins are formed by
regular arrangement of stacking-faults on consecutive f111g planes, they grow
continuously with increasing strain as well demonstrated by the DIC results pre-
sented in Sect. 7.2.3. In addition, it turned out from the kernel average

Fig. 7.56 Microstructure of Fe–16Cr–6Mn–9Ni–0.05C steel after tensile test to strain to failure at
e = 42% at room temperature. a SEM micrograph in BSE contrast. b–d Results of EBSD mapping
of an area of interest marked in (a). b Band contrast map with indicated R3 twin boundaries (red).
c Orientation map in inverse pole figure colouring with respect to the surface normal direction.
f Kernel average misorientation. Loading axis horizontal. Reproduced from [33]. Permission of
Elsevier
326 7 Case Studies on Localized Deformation Processes …

misorientation map shown in Fig. 7.56d (maximum misorientation angle 5°) that
mainly twins of first generation are related to high misorientation, indicating that
deformation occurs as well in the twinned areas—probably by dislocation glide.
Medium austenite stability. Lowering the nickel content leads to a reduction of the
austenite stability and the stacking-fault energy. Thus, Fe–16Cr–6Mn–6Ni–0.05C
steel has among the three investigated steel variants a medium austenite stability
(Ms = –40 °C) and medium stacking f-ult energy (cSF  17 mJ/m2). According to
these parameters, this steel variant exhibits a martensitic phase transformation as
described in detail in Sect. 6.3. As shown in Sect. 6.4, this phase transformation
occurs via an intermediate state of stacking-fault bands with arrangement of
stacking-faults on in average each second f111g lattice plane, which are related to
pronounced strain localization as shown in Sect. 7.2. Therefore, possible sources of
acoustic emission can be (i) dislocation glide, (ii) the formation of stacking-fault
bands or stacking-fault-mediated twin bundles and (iii) martensitic phase trans-
formation. Figure 7.57 shows the time sequence of the three evaluated AE clusters
over the entire deformation process. Similar to the most stable steel variant, cluster
1 evolves immediately with beginning of deformation process and is correlated with
dislocation glide. Both the cumulated energy and the number of elements related to
this cluster are growing nearly over the entire deformation process. A saturation is
observed at about 40% of elongation. Around the yield point, cluster 3 starts to be
predominant. The time sequence of the cumulated AE energy is characterized by
certain jumps, which are related to individual events with higher energy level. The
number of elements tends to saturate at around 20% of elongation. Cluster 2
becomes significant at about 12% of elongation. According to this time sequence,
cluster 3 and cluster 2 can be well correlated with the formation of stacking-fault
bands and the formation of a′-martensite, respectively. Thus, cluster 3 is related to
the formation of deformation bands caused by motion of partial dislocations
forming either stacking-fault bands or twin bundles. The saturation of the number of

Fig. 7.57 Time sequence of AE clusters evaluated for Fe–16Cr–6Mn–6Ni–0.05C steel and
correlated with different deformation mechanisms—dislocation glide, formation of deformation
bands by motion of partial dislocations and formation of a′-martensite—shown in combination
with the stress-strain curve obtained during tensile test a room temperature. a Cumulated AE
energy. b Number of elements per cluster. Reproduced from [33]. Permission of Elsevier
7.3 Time Sequence of Deformation Processes 327

elements contributing to this cluster is consistent with the findings by EBSD and
XRD measurements, which revealed that the amount of the hex phase/e-martensite
evolves over a maximum at about 20% of elongation (cf. [38]).
The onset of cluster 2 at about 12% of elongation is in good agreement with the
inflection point occurring in the stress-strain curve seen in Fig. 7.57 (cf. also
Sect. 6.3; Fig. 6.6). Cluster 2 is increasing continuously with further ongoing
deformation. The saturation of the cluster 1 related to dislocation glide is accom-
panied by an increase in the slope of cluster 2 related to a′-martensite formation and
a saturation of cluster 3 as well. This is in agreement with experimental findings that
at higher strain values a′-martensite can be formed as well on places of strain
concentrations as grain boundary triple points as well as in front of crack tips
occurring at the point of macroscopic strain localizations due to necking. The
findings of AE cluster analysis are corroborated by microstructural investigations as
well. However, SEM investigations were performed already after 10% of elonga-
tion since the majority of interesting mechanisms are active at this point.
Investigations on the steel variant after failure would reveal a high volume fraction
of martensitic microstructure (cf. [2]) and only small amount of hex crystal lattice.
Thus, Fig. 7.58 shows the microstructure developed during tensile test at RT and a

Fig. 7.58 Microstructure of Fe–16Cr–6Mn–6Ni–0.05C steel after tensile test interrupted at 10%
elongation. a SEM micrograph in BSE contrast. b Inverted ECC image of the region indicated in
(a) showing individual stacking-faults (SF) arranged in between deformation bands as well as
lentil-like a′-martensite nuclei inside the deformation bands with high SF density. c, d Results of
EBSD measurements of a typical area of interest. c Phase map: fcc austenite—red, bands with
stacking-faults indicated as hex phase (e-martensite)—yellow, bcc a′-martensite—blue.
d Orientation map in inverse pole figure colours with respect to the surface normal direction for
the martensitic a′-phase. e Overlay of crystallographic orientation map of austenite and phase map
of martensite (blue) and stacking-fault band (yellow) corresponding to the marked area (white
rectangle) in (d). Loading axis horizontal. Reproduced from [33]. Permission of Elsevier
328 7 Case Studies on Localized Deformation Processes …

slower strain rate than during the AE tests. The deformation bands with the hex
crystal lattice caused by the SFs on each second f111g plane are visible clearly in
the microstructure, and a′-martensite grains appear inside deformation bands.
Individual stacking-faults as well as regular dislocations are observed as shown in
Fig. 7.58b. In addition, small deformation twins occurring simultaneously to hex
crystal lattice are visible in Fig. 7.58e.
Lowest austenite stability. The steel with the lowest austenite stability as well as the
lowest SFE is the variant with the lowest content of nickel—Fe–16Cr–6Mn–3Ni–
0.05C. The Ms temperature of this steel variant is well above RT (Ms = 60 °C).
Thus, this steel contains a′-martensite already in the as-cast microstructure due to
the cooling process. Moreover, in addition to the strain-induced formation of a′-
martensite this steel exhibits as well a stress-assisted martensitic phase transfor-
mation. The SFE is about 8 mJ/m2 leading to high tendency of dissociation of
regular dislocations and, consequently, to largely extended stacking-faults.
Therefore, the deformation behaviour of this steel is dominated by stress-assisted
and strain-induced martensitic phase transformations resulting in an even more
pronounced TRIP effect than observed for Fe–16Cr–6Mn–6Ni–0.05C steel. The
deformation behaviour and the occurring microstructure are described compre-
hensively already in Sects. 6.3 and 6.4, respectively. Deformation-induced twin-
ning is, therefore, not expected for this unstable steel variant. In addition, among all
three investigated steels Fe–16Cr–6Mn–3Ni–0.05C steel is the only one exhibiting
pronounced inhomogeneous plastic deformation (serrations) at higher strain values.
Thus, possible sources of acoustic emission during plastic deformation of this steel
should be (i) the formation of stacking-fault bands, (ii) martensitic phase trans-
formation and (iii) serrated plastic flow in terms of propagation of PLC bands.
Figure 7.58 shows the results of the AE cluster analysis (Fig. 7.59).
It is clearly visible that the three identified AE clusters exhibit different time
sequences. Thus, cluster 1 evolves immediately with beginning of the plastic

Fig. 7.59 Time sequence of AE clusters evaluated for Fe–16Cr–6Mn–3Ni–0.05C steel and
correlated with different deformation mechanisms—formation of deformation bands by motion of
partial dislocations, formation of a′-martensite and occurrence of PLC bands—shown in combination
with the stress-strain curve obtained during tensile test a room temperature. a Cumulated AE energy.
b Number of elements per cluster. Reproduced from [33]. Permission of Elsevier
7.3 Time Sequence of Deformation Processes 329

deformation. The cumulated AE energy increases rigorously until the yield point is
reached accompanied by significant increase in the number of elements as well.
Even after passing the yield stress, the cumulative energy and the number of
elements are increasing continuously, but less pronounced. Immediately after
passing the yield stress, cluster 2 becomes dominant well before the inflection point
in the sigmoidal stress-strain curve is reached. The cumulated AE energy is less
pronounced than for cluster 1. However, the number of elements of this cluster is
increasing continuously over the entire deformation process. At about 22% of
elongation, cluster 3 develops. The onset of this cluster correlates well with the
occurrence of serrated plastic flow in the stress-strain curve (see Sect. 7.4).
According to their time sequence and their characteristics, cluster 1 is related to the
formation of deformation bands by movement of partial dislocations, cluster 2 to

Fig. 7.60 Microstructure of Fe–16Cr–6Mn–3Ni–0.05C steel after tensile test interrupted at 10%
of elongation. a SEM micrograph in BSE contrast. b Inverted ECC image showing individual
stacking-faults arranged in between deformation bands. c, d Results of EBSD measurements of a
typical area of interest. c Phase map—austenitic phase in red, bands with stacking-faults indexed
as hex phase (e-martensite) in yellow, martensitic a′-phase in blue. d Orientation map in inverse
pole figure colouring with respect to the surface normal direction for the martensitic a′-phase.
Loading axis horizontal. Reproduced from [33]. Permission of Elsevier
330 7 Case Studies on Localized Deformation Processes …

the formation of a′-martensite and cluster 3 to the occurrence of serrated plastic


flow. Results of supporting microstructural investigations are shown in Fig. 7.60. In
comparison with the microstructure of Fe–16Cr–6Mn–6Ni–0.05C steel shown in
Fig. 7.60, more deformation bands (a) and higher amount of a′-martensite (c) be-
come obvious. Individual stacking-faults occur between deformation bands
belonging to primary slip systems shown in Fig. 7.60b. The high AE energy of
cluster 1 is caused by the pronounced fragmentation of the austenitic microstructure
due to deformation bands leading to a reduction of the mean free path similar to the
primary twins in Fe–16Cr–6Mn–9Ni–0.05C steel. The effect of serrated plastic flow
will be discussed in more detail later in Sect. 7.4.

7.3.4 Evolution of Martensitic Phase Transformation


at Room Temperature

Cluster 2 evaluated for Fe–16Cr–6Mn–6Ni–0.05C steel and Fe–16Cr–6Mn–3Ni–


0.05C steel, respectively, is related in accordance with microstructural investigation
to the formation of a′-martensite. In order to validate the obtained time sequence of
this cluster, the AE results were corroborated by measurements of the volume
fraction of a′-martensite using ferritescope. The average ferromagnetic phase

Fig. 7.61 Volume fraction of the strain-induced a′ martensite in Fe–16Cr–6Mn–6Ni–0.05C steel


and Fe–16Cr–6Mn–3Ni–0.05C steel obtained during tensile tests at RT and at a strain rate of
1  10−3 s−1 in combination with the cumulative AE energy calculated independently of the
group of signals belonging to AE cluster 2 identified and separated from other sources by the AE
cluster analysis. Reproduced from [33]. Permission of Elsevier
7.3 Time Sequence of Deformation Processes 331

fraction was measured for both steel variants during interrupted tensile test on 10
individual measuring points distributed along the gauge length on the two opposite
specimen surfaces. The ferromagnetic measurements were repeated for two dif-
ferent specimens for each steel variant. The volume fraction of a′-martensite was
then calculated using the equation according to Talonen [39]. Figure 7.61 shows
the results of the measurements of the ferromagnetic phase fraction in combination
with the time sequence of the cumulative energy of cluster 2 evaluated for both
steels.
The average volume fraction values of a′-martensite obtained via ferromagnetic
measurements are provided as individual measuring points at certain strain inter-
vals. The indicated scatter resembles the standard deviation over 40 measuring
points. The kinetics of a′-martensite formation related to AE cluster is given by
magenta lines. It should be noted that the AE results and the results of ferromagnetic
measurements were obtained on different specimens explaining different final strain
levels until failure of specimens. Furthermore, the as-cast microstructure with
segregations and the large grain size can influence the amount of martensitic phase
transformation. Nevertheless, a reasonable good agreement between both kinetics
obtained by different techniques is apparent. Thus, not only the different onsets of
the martensitic phase transformation are reflected well by both techniques, also the
different amounts of a′-martensite are represented qualitatively in the right way. It
should be noted that the results of AE analysis are given in terms of cumulated AE
energy in arbitrary unites (a.u.).

7.3.5 Influence of Deformation Temperature

Sections 7.3.2 and 7.3.3 illustrated well that AE analysis is a suitable tool for
determination of the time sequence of the deformation processes occurring in TRIP/
TWIP steels. Thus, different clusters were identified due to the AE cluster analysis,
which are related to different sources of AE respective individual deformation
processes. Along with the chemical composition, the deformation temperature has a
significant influence on both the thermodynamic driving force and the
stacking-fault energy and, consequently, on the ongoing deformation mechanisms.
Thus, it was already shown that the deformation behaviour (see Sect. 6.3) and the
developed microstructure (see Sect. 6.4) change significantly with an increase in
temperature. In the following, it will be shown that these changes are reflected by
AE measurements and different time sequences of deformation processes due to
higher deformation temperatures.
Similar to the studies on the influence of the chemical composition, investiga-
tions on the influence of temperature were conducted in tension at different tem-
peratures (RT, 40, 60, 80 and 100 °C) and at a strain rate of 3  10−3 s−1.
However, due to the elevated temperatures other AE sensor (WD) with an appli-
cable temperature range up to 177 °C was applied during these tests. As mentioned
already before this sensor had different frequency spectra with two resonant peaks
332 7 Case Studies on Localized Deformation Processes …

at about 200 and 700 kHz, which made the cluster analysis more difficult.
Nevertheless, different AE clusters were separated as will be shown in the fol-
lowing. Figure 7.62 shows the obtained stress-strain curves (black curves) in
combination with the calculated parameters of the AE energy E (green curves) and
median frequency fm (blue curves) for all three steel variants and the two temper-
atures—RT and 100 °C. First of all, the different deformation behaviours
depending on the different chemical compositions as well as the influence of the
elevated deformation temperature become obvious. Thus, at RT the steel with the
highest austenite stability shows the highest elongation to failure but the lowest
tensile strength. In contrast, the steel with the lowest austenite stability shows a
pronounced secondary hardening resulting in the highest tensile strength and the
shortest elongation to failure. The stress-strain curve is sigmoidal, which is

Fig. 7.62 Temporal evolution of AE energy E and median frequency fm derived from power
spectral density functions obtained by fast Fourier transformation of AE data streams collected
during tensile tests of TRIP/TWIP cast steels at room temperature (a, c, e) and 100 °C (b, d, f) at
nominal strain rate of 3  10−3 s−1. a, b Fe–16Cr–6Mn–9Ni–0.05C steel. c, d Fe–16Cr–6Mn–
6Ni–0.05C steel. e, f Fe–16Cr–6Mn–3Ni–0.05C steel. Reproduced from [40]. Permission of
Elsevier
7.3 Time Sequence of Deformation Processes 333

indicative of a martensitic phase transformation. The temperature increase up to


100 °C has a strong effect on the stress-strain behaviour, which is most pronounced
for Fe–16Cr–6Mn–6Ni–0.05C steel and Fe–16Cr–6Mn–3Ni–0.05C steel,
respectively.
Considering the AE results, the AE data sets obtained at elevated temperatures
appear similar to data at RT as a random time-series consisting of high-amplitude
bursts overlapping with a low-amplitude continuous signal, which is well above the
electronic laboratory noise. Overall, the temporal evolution of AE energy and
median frequency obtained at RT are quite similar to those described in Sect. 7.3.2.
However, the anticyclical oscillating behaviour of these two parameters observed in
Fe–16Cr–6Mn–9Ni–0.05C steel and less pronounced in Fe–16Cr–6Mn–6Ni–0.05C
steel is not approved, which is caused by the different frequency responses of the
other AE sensor. Nevertheless, the Fe–16Cr–6Mn–3Ni–0.05C steel revealed the
same behaviour—pronounced maximum of median frequency at the onset of
deformation followed by graduate reduction over the entire deformation process. At
100 °C, the two parameters behave in an opposite way. Thus, at 100 °C the median
frequency shifts to higher frequency domain before dropping when macroscopic
strain localization sets in on the late deformation stage. In addition, the AE energy
is approximately a factor five higher at RT than at 100 °C. Both findings indicate
changes in the deformation mechanism caused by the elevated temperature.
For Fe–16Cr–6Mn–6Ni–0.05C steel and Fe–16Cr–6Mn–9Ni–0.05C steel,
respectively, the influence of temperature is not that pronounced as for Fe–16Cr–
6Mn–3Ni–0.05C steel. Nevertheless, the median frequency is shifted to slightly
higher frequency domain, whereas the overall behaviour remained nearly unchan-
ged. However, changes in the predominant deformation mechanisms at elevated
temperatures should occur as well for these two steel variants, since the overall
deformation behaviour changed significantly.
Therefore, detailed cluster analysis is performed in order to evaluate the influ-
ence of temperature on the time sequence of different deformation processes.
However, the cluster analysis is performed for the first 60 s of the entire defor-
mation process only, since this is the part where the most interesting microstructural
processes have been activated. Figure 7.63 shows the results of the AE cluster
analysis for the three steel variants at RT (a, c, e) and 100 °C (b, d, f), respectively.
For each steel variant, different clusters are revealed and related to specific defor-
mation mechanisms.
Room Temperature. The behaviour of Fe–16Cr–6Mn–9Ni–0.05C steel is described
by two clusters—(i) dislocation glide and (ii) formation of twin bundles. From the
AE data sets obtained on Fe–16Cr–6Mn–6Ni–0.05C steel, four different clusters are
extracted—(i) dislocation glide, (ii) formation of deformation bands by motion of
partial dislocations leading to stacking-fault bands or (iii) twin bundles, and
(iv) formation of a′-martensite. However, the cluster related to twins is quite small.
This is in agreement with detailed microstructural investigations based on EBSD
(cf. Figs. 6.24 and 7.58e) and HRTEM (see [14]), which showed that stacking-fault
bands (hex) coexist with twin bundles. The cluster analysis performed on AE data
334 7 Case Studies on Localized Deformation Processes …

Fig. 7.63 Scatter plots showing bivariate distributions of AE descriptive variables—average


energy E and median frequency fm—for austenitic stainless steels with different Ni contents tested
at room temperature and 100 °C. Parameters related to individual realizations assigned to different
AE clusters (i.e. to different deformation mechanisms). Reproduced from [40]. Permission of
Elsevier

of Fe–16Cr–6Mn–3Ni–0.05C steel revealed only two clusters—(i) motion of partial


dislocations and (ii) formation of a′-martensite. Although the latter two clusters
occur as well in Fe–16Cr–6Mn–6Ni–0.05C steel, they are much more pronounced
in terms of AE energy and number of events in Fe–16Cr–6Mn–3Ni–0.05C steel.
Elevated temperature—100 °C. The scatter plots obtained at 100 °C are signifi-
cantly different in comparison with RT for all three investigated steel variants.
Thus, a new cluster occurred in Fe–16Cr–6Mn–3Ni–0.05C steel, which is con-
centrated on the lower frequency domain. Concurrently, the energy of clusters 1 and
2 decreased significantly. For Fe–16Cr–6Mn–6Ni–0.05C steel, cluster 2 related at
RT to the partial dislocations is replaced completely by formation of twin bundles at
7.3 Time Sequence of Deformation Processes 335

100 °C. The two clusters related to dislocation glide and twinning for the steel with
the highest austenite stability are also identified at 100 °C, but with changed
intensities.
In the following, the temporal evolution of the cumulated AE energy and the
number of cluster elements will be discussed in correlation with the stress-strain
curves for the three different steel variants starting with the steel with the highest
austenite stability.
Pronounced TWIP effect. The comparison of the temporal evolution of the eval-
uated clusters obtained at RT and 100 °C shown in Fig. 7.64 demonstrates clearly
the influence of the temperature on the deformation mechanisms.
The changes in the deformation behaviour due to the increased temperature
become obvious from both the cumulated AE energy and the number of cluster
elements. At 100 °C, twinning is still an active deformation mechanism, but less
pronounced compared to RT.
Thus, the cumulated AE energy and the number of cluster elements are reduced
significantly. In contrast, the parameters characterizing cluster 1—dislocation glide
—are increased significantly in comparison with RT. Thus, TWIP effect is still
occurring at 100 °C resulting in still remarkably high elongation of about 50%.
Deformation twins are also observed by EBSD measurements on specimens
deformed at 100 °C as shown in Fig. 6.26. Thus, the EBSD maps show mechanical
twins of first and second generation at both temperatures. However, twins of pri-
mary generation are thinner at higher temperature.

Fig. 7.64 Results of the AE cluster analysis for Fe–16Cr–6Mn–9Ni–0.05C steel tested in tension
at RT (a, c) and 100 °C (b, d). Time sequence of the cumulative AE energy (a, b) and of the
number of AE cluster elements (c, d). Reproduced from [40]. Permission of Elsevier
336 7 Case Studies on Localized Deformation Processes …

However, it should be mentioned again that EBSD is not the appropriate tech-
nique for the evaluation of the volume fraction of deformation-induced twins. As it
is well demonstrated by Fig. 6.28, only twin bundles with a thickness of few
micrometres are detected by EBSD, whereas microtwins with a size of few
nanometres will be disregarded by the electron beam due to the resolution of the
EBSD measurements. Nevertheless, since the kinetic of the a′-martensite evolution
over the deformation process is described well by the time sequence of the
cumulated AE energy, this parameter can be used as well in order to describe the
kinetic of deformation-induced twinning.
Transition from TRIP to TWIP effect. A significant change of the dominant
deformation mechanism occurs for Fe–16Cr–6Mn–6Ni–0.05C steel. Whereas this
steel exhibits at RT a remarkable TRIP effect, it shows at temperatures above 60 °C
a pronounced TWIP effect (cf. Fig. 6.4).
This outcome of investigations on the deformation behaviour as well as on the
microstructure is confirmed by the results of the AE cluster analysis as it is well
demonstrated by Fig. 7.65.
In the present case, at RT at least four different deformation mechanisms are
extracted from the AE data, where the cluster related to twinning is quite small in
number of elements at RT. However, the time sequence of all clusters changed
significantly at 100 °C. Thus, the cluster related to partial dislocations disappeared

Fig. 7.65 Results of the AE cluster analysis for Fe–16Cr–6Mn–6Ni–0.05C steel tested in tension
at RT (a, c) and 100 °C (b, d). a, b Temporal evolution of the cumulative AE energy. c,
d Temporal evolution of the number of AE cluster elements. Reproduced from [40]. Permission of
Elsevier
7.3 Time Sequence of Deformation Processes 337

completely at higher temperature. Instead, the number of elements contributing to


the cluster of twins is increasing significantly. The activity of dislocation glide
behaves in a similar way. In addition, the martensitic phase transformation occurs at
100 °C as well, but the onset is shifted to significantly higher strain values.
Figure 7.66 summarizes the microstructural results corroborating these findings.
Figure 7.66a–c show the results of EBSD measurements obtained at RT with the
typical formation of stacking-fault bands (hex) and a′-martensite grains. In addition,
a certain amount of twin boundaries in the close vicinity to hex-indexed areas are
indicated by red lines. At 100 °C, twin bundles of primary generation as well as
thinner twins according to secondary twin system are observed. Small amount of
hex crystal lattice is detected as well next to twin boundaries. Even twins of a third
generation have been developed (marked by white arrows in Fig. 7.66f).
Only locally, very small amount of a′-martensite was detected in this AOI
(marked by white arrows in Fig. 7.66d). However, the shown example resembles
only one AOI of 70  70 µm of one individual grain orientation. Since AE
detected a cluster related to martensitic phase transformation, there should be other
grain orientations with higher amount of a′-martensite.

Fig. 7.66 Summary of microstructure observations and EBSD measurements on Fe–16Cr–6Mn–


6Ni–0.05C steel after tensile test at RT (a–c) and 100 °C (d–f). a, d Phase map with austenitic
phase (fcc) in red, e-martensite (hex) in yellow and a′-martensite (bcc) in blue colour (b, e).
Crystallographic orientation map in the inverse pole figure colouring code according to the surface
normal direction; (e, f) band contrast images with indicated twin boundaries (red). Stress axis is
horizontal. Reproduced from [40]. Permission of Elsevier
338 7 Case Studies on Localized Deformation Processes …

Fig. 7.67 Results of the AE cluster analysis for Fe–16Cr–6Mn–3Ni–0.05C steel tested in tension
at RT (a, c) and 100 °C (b, d). a, b Temporal evolution of the cumulative AE energy. c,
d Temporal evolution of the number of AE cluster elements. Reproduced from [40]. Permission of
Elsevier

Pronounced TRIP effect. The Fe–16Cr–6Mn–3Ni–0.05C steel exhibits even at


100 °C a pronounced TRIP effect. Therefore, clusters related to partial dislocations
as well as formation of a′-martensite are separated from the AE data at both RT and
100 °C as shown in Fig. 7.67. However, the cumulated energy (note the different
scales at RT and 100 °C) of cluster 1 and cluster 2 is reduced significantly at
100 °C. On the other hand, a third cluster related to dislocation glide emerges at
100 °C. The results of the cluster analysis are in good agreement with the devel-
oped microstructure shown in Figs. 6.29 and 6.30.

7.3.6 Discussion

The potential of the in situ AE measurements during mechanical loading is both the
high time resolution in the range of microseconds and the integrating information on
the bulk material behaviour giving reasonable grain statistics. In contrast, all other
methods applied for the characterization of the developed microstructure on inter-
rupted tests such as OM, SEM, EBSD, XRD phase analysis, ferritescope, magnetic
balance or MSAT in order to obtain information on the time sequence of deformation
processes, have a worse time resolution and deliver mainly 2D information at the
specimen surface (OM, SEM, EBSD) or at least a small volume information (XRD).
7.3 Time Sequence of Deformation Processes 339

In order to obtain microstructural information depending on the applied stress or


strain, interrupted tensile tests are performed based on multiple specimens. Thus,
chemical variations as well as other features of the initial casting microstructure
could affect the results. Similarly, the preparation of specimens for specific inves-
tigations such as EBSD could influence the results as well (e.g. Fe–16Cr–6Mn–3Ni–
0.05C steel, which shows martensite formation already during grinding due to the
high Ms temperature). Thus, the AE is the only method delivering real-time inte-
grated volume information on the ongoing deformation processes.
At least, the good agreement of the AE results with the ferromagnetic mea-
surements reflecting the kinetics of the a′-martensite formation at RT is an indicator
for the accuracy of the spectral analysis and subsequent cluster analysis. Both the
evolution of the ferromagnetic volume fraction and the evolution of the AE cluster
related to the a′-martensite formation are in good agreement with the Olson–Cohen
model describing the evolution of the volume fraction of a′-martensite during the
entire deformation process according to (3.5). The empirical parameters a and b
were chosen according to [38] with a = 1 and b = 4.85. The exponent n was chosen
as n = 3.5 for steel with 6 wt% Ni and n = 2 for steel with 3 wt% Ni. In both cases,
the Olson–Cohen model exhibits typical S shape curve and fits well both the data
obtained from ferritescope measurements and the evolution of the AE energy
related to the cluster for martensitic phase transformation as shown in Fig. 7.68.
It should be noted that AE results and ferritescope measurements were not
obtained for one and the same specimens. Therefore, slight variations between AE
and ferromagnetic phase fraction are related to as-cast microstructure. Nevertheless,
especially for steel with 3 wt% Ni, the evolution of the cumulated AE energy of the
cluster related to martensitic phase transformation fits well the model description

Fig. 7.68 Comparison of cumulated AE energy and volume fraction of a′-martensite determined
from ferritescope measurements with model description of Olson and Cohen for steel with 6 and 3
wt% nickel. Modified according to [33]. Permission of Elsevier
340 7 Case Studies on Localized Deformation Processes …

over large range of deformation process. However, the AE emission does not
provide real numbers of martensitic phase fraction. Therefore, the corroboration by
other parameters which can be determined experimentally is necessary.
Nevertheless, this gives rise to assumption that also the evolution of fraction of
twins formed during the deformation process can be qualitatively correlated with
the time sequence of the cluster related to the twin formation at least in Fe–16Cr–
6Mn–9Ni–0.05C steel. Moreover, at least the threshold value for the onset of
twinning could be derived from the AE measurements. Since both the EBSD and
TEM have their limitations regarding the experimental determination of the fraction
of twins, the AE technique seems to have the highest potential to serve with
determination of the fraction of twins out of time sequence of the cumulated energy
related to the cluster for twin formation. As shown in previous sections, twins
observed in the investigated steels can be described as partial dislocation-mediated
twins. The occurrence of partial dislocations can be also well described by X-ray
line profile analysis. Thus, the so-called stacking-fault probability P can be deter-
mined from the line broadening of X-ray profiles. Therefore, it is expected that a
correlation of the temporal evolution of the AE energy related to the cluster for
twins and the stacking-fault probability will shed some light on the evolution of the
fraction of twins during plastic deformation of steels with twinning-induced plas-
ticity. Since both the fraction of twins and the threshold value for the onset of
twinning are crucial parameters for the modelling of the TWIP effect (see
Sects. 4.2.3 and 8.3), it is expected that AE measurements can contribute in a
substantial way to the determination of these parameters.

7.4 Macroscopic Strain Localization During Plastic


Deformation

The high-alloy Fe–16Cr–6Mn–xNi–0.05C cast steels exhibit a pronounced


martensitic phase transformation depending on their chemical design and the
deformation temperature that yields the TRIP effect with excellent strengthening
behaviour and high ductility. The good ductility of the TRIP steels is the conse-
quence of the shift of the macroscopic strain localizations leading to necking and,
finally, to failure of the material to higher strain values. However, the TRIP steel
with the lowest austenite stability (3 wt% nickel) exhibits, in addition, another
macroscopic strain localization that occurs before necking during tensile defor-
mation. Serrated plastic flow is observed—well known as the Portevin–Le Chatelier
effect (cf. Fig. 2.27 in Sect. 2.6.2.2 and Fig. 6.6a in Sect. 6.3.1).
The occurrence of the PLC effect in high-alloy Fe–16Cr–6Mn–3Ni–0.05C TRIP
steel during tensile deformation was investigated in dependence on the deformation
temperature as well as on the strain rate. The mechanical tests were complemented
by fully-coupled full-field measurements in terms of recording (i) local strain fields
using optical images for digital image correlation, (ii) local thermal fields using
infrared thermography and (iii) time sequence of deformation and damage pro-
cesses using acoustic emission.
7.4 Macroscopic Strain Localization During Plastic Deformation 341

7.4.1 Fully-Coupled Full-Field Measurements

The investigations on the PLC effect occurring in Fe–16Cr–6Mn–3Ni–0.05C steel


were performed under tensile deformation on an electromechanical testing system
(Zwick, Germany) in a wide range of temperature 20 °C  T  140 °C. The tensile
deformation was conducted under cross head displacement control in a range of
nominal initial strain rates of 10−4 s−1  e_  10−1 s−1. The fully-coupled full-field
measurements were carried out using the two-camera setup (cf. Sect. 5.4) consisting
of a digital camera for DIC and a thermo-camera for thermographic measurements
viewing on opposite part of the gauge length of tensile specimens as shown in
Fig. 7.69. The tests were complemented by an acoustic emission sensor adapted on the
shoulder part of tensile specimens (for specimen geometry, see Fig. 7.48) [41].
A digital camera (Canon EOS 420D; labelled as 3 in Fig. 7.70) with a 70 mm
lens was used for recording of optical micrographs during tensile deformation with
a frame rate of 22 fps and a resolution of 848  560 pixels2. The specimen surfaces
were prepared for DIC calculations similar to in situ tests in the SEM using V2A
etching solvent (cf. Sect. 7.2.2). The DIC calculations were performed using
Aramis software package (GOM).
An infrared LWIR (7–14 µm) thermography system VarioCamhr (InfraTec,
Dresden; labelled as 1 in Fig. 7.69) with a thermal resolution of <0.03 K and a
frame rate of 60 Hz was used for investigation of the temperature evolution during
the tests. The camera was used with two different objective lenses—
macro-objective and microscopic objective, resulting in different fields of view
(FOV) and pixel sizes. Whereas the macro-objective allows the inspection of the
whole gauge length of the tensile specimen (about 30 mm), the microscopic

Fig. 7.69 Two-camera setup for fully-coupled full-field measurements in combination with AE
measurements during tensile tests on Fe–16Cr–6Mn–3Ni–0.05C TRIP steel in a wide range of
temperatures and strain rates. 1—Thermo-camera. 2—AE sensor. 3—Digital camera. 4—Gripping
system. 5—Specimen. a Setup in the electromechanical testing device (Zwick). b Higher
magnification with clamped specimen and AE sensor fixed by a rubber band (blue) to the specimen
surface. According to [41]
342 7 Case Studies on Localized Deformation Processes …

Fig. 7.70 Flow curves of the metastable Fe–16Cr–6Mn–3Ni–0.05C TRIP steel tested in tension
at room temperature and different nominal strain rates (a). Vertical bars indicate the onset of
instability flow. b Details of the flow curves indicated by rectangles in (a) at higher resolution.
Reproduced from to [41]. Permission of Springer

objective lens (shown in Fig. 7.69) results in a smaller FOV (16 mm  12 mm)
and a higher lateral resolution (25 µm). The specimen surfaces used for thermo-
graphic measurements were grounded mechanically and, finally, covered by black
thermolacquer enabling a high emissivity of 0.96. The infrared thermograms
obtained were analysed by the software package Irbis3plus (InfraTec, Dresden).
The acoustic emission was recorded using the AE setup described in Sect. 7.3.1
with the sensor WD (labelled as 2 in Fig. 7.69) allowing for higher temperature
application.

7.4.2 The Occurrence of Portevin–Le Chatelier (PLC) Effect

Influence of initial strain rate at RT. The flow curves obtained at RT and four
different nominal initial strain rates are shown in Fig. 7.70a. For better visibility, the
true stress-true strain curves are shifted by 0.05 on the strain axis. In addition, the
peak temperature (Tmax [°C]) and the volume fraction of strain-induced a′-mar-
tensite (a0tot [%]) developed during the tensile tests are indicated. Moreover, small
vertical bars mark the onset of the serrated plastic flow. The marked rectangles are
shown in Fig. 7.70b at higher resolution 0.25  e  0.295 and 900  r 
1200 MPa. PLC bands of type B are observed only at the lowest nominal strain
rate, whereas type A bands occurred at higher nominal strain rates.
At RT, the serrated plastic flow is observed at all strain rates except the highest
strain rate of 10−1 s−1. Furthermore, a shift of the onset of the serrated plastic flow
to higher strain values is observed with an increase in strain rate. In addition, the
7.4 Macroscopic Strain Localization During Plastic Deformation 343

appearance of serrations in the flow curves changed as well. Whereas at the lowest
strain rate numerous irregular inhomogeneities in the stress-strain curve occurred,
the serrations become more regular with the increase in the strain rate. All tensile
tests are accompanied by an increase in temperature, which becomes more pro-
nounced with the increase in the strain rate. Thus, whereas the temperature increase
is about 4 K only at the lowest strain rate, an increase in temperature of about 70 K
is observed for the highest strain rate. Nevertheless, all flow curves reveal a sig-
moidal shape with a pronounced inflection point indicating martensitic phase
transformation, which leads to pronounced strain hardening. However, the increase
in the strain rate shifts the inflection point to higher strain values and the strain
hardening is decreasing. The occurrence of martensitic phase transformation is
corroborated by ferromagnetic measurements using ferritescope. The calculated
volume fraction of strain-induced a′-martensite lies between 50 and 60% for tensile
tests at RT. However, a reduction of the volume fraction of strain-induced a′-
martensite with the increase in the strain rate is detected as well.
Influence of temperature. Since the temperature has a significant effect on the
ongoing deformation mechanisms and, in particular, on the martensitic phase
transformation, its influence on the occurrence of the serrated plastic flow was
investigated in a temperature range RT  T  140 °C. Exemplarily, Fig. 7.71
summarizes the results of tensile tests at 60 °C (a) and 80 °C (b), respectively.
Significant changes in the deformation behaviour between 60° and 80° become
obvious. Whereas the flow curves at 60 °C still exhibit a sigmoidal curve shape and
at least 20% of strain-induced a′-martensite is detected post-mortem, the sigmoidal
shape of the flow curves disappears completely at 80 °C and no a′-martensite is
detected via ferritescope measurements. The serrated plastic flow is observed at
60 °C for the two lower strain rates of 10−4 s−1 and 10−3 s−1, only. Again,
increasing strain rate shifts the onset of serrated plastic flow to higher strain values.
The measured temperature increase for tests at 60 °C is less pronounced than at RT
tests. The appearance of the serrations at higher temperatures is identified as type B.
The tensile tests at RT revealed a significant increase in the temperature
depending on the applied nominal strain rate (_e  10−3 s−1) as shown in
Fig. 7.70a. In order to eliminate the temperature influence due to strain rate,
so-called quasi-isothermal tests were tried to carry out. For this purpose, an addi-
tional cooling system using compressed air (spot cooler) was applied. The cooling
system was well effective at the strain rate of 10−3 s−1 (DT = 6 K). At the strain rate
of 10−2 s−1, the temperature increase was reduced to DT = 40 K, whereas the
cooling system was ineffective for highest strain rate of 10−1 s−1 as shown in
Fig. 7.72. The quasi-isothermal tensile tests at room temperature revealed that no
PLC effect occurred at all tested nominal strain rates. However, the flow curves
exhibited a pronounced strengthening related to the TRIP effect. A comparison with
the tensile tests without additional cooling showed no significant difference in the
volume fraction of the formed deformation-induced a′-martensite.
Influence of ultrafine grain size. In general, it is stated that the effect of serrated
plastic flow is increased for smaller grain size. However, in the present work the
344 7 Case Studies on Localized Deformation Processes …

Fig. 7.71 Flow curves of metastable Fe–16Cr–6Mn–3Ni–0.05C TRIP steel at higher tempera-
tures and the four nominal strain rates: 10−4 s−1, 10−3 s−1, 10−2 s−1 and 10−1 s−1. a 60 °C and
b 80 °C. A vertical bar indicates the onset of serrated plastic flow. c Detail of the flow curve
marked by the rectangles in (a) at higher resolution. Reproduced from [41]. Permission of Springer

Fig. 7.72 Quasi-isothermal


stress-strain curves of
metastable Fe–16Cr–6Mn–
3Ni–0.05C TRIP steel tested
at room temperature and
strain rates of 10−3 s−1 and
10−2 s−1, respectively, with
additional compressed
air-cooling device.
Reproduced from [41].
Permission of Springer

influence of grain size on the occurrence of serrated plastic flow for Fe–16Cr–6Mn–
3Ni–0.05C steel could not be investigated due to lack of material with smaller grain
sizes than the as-cast state. However, an ultrafine-grained (ufg) metastable austenitic
microstructure was obtained by reversion annealing [17]. In contrast to the as-cast
material with an average grain size of at least 500 µm, the ufg microstructure
7.4 Macroscopic Strain Localization During Plastic Deformation 345

consisted of grains with a mean diameter <1 µm. This ufg microstructure was
generated by thermomechanical treatment consisting of cold rolling and subsequent
reversion annealing treatment (see [17]). The tensile deformation behaviour changed
completely. No serrated plastic flow occurred during tensile testing of the ufg aus-
tenitic steel at RT and different strain rates. Instead of serrated plastic flow, a pro-
nounced yield point followed by a Lüders strain plateau was observed. Moreover, a
pseudoelastic behaviour was registered below the yield point indicating a
stress-assisted martensitic phase transformation. Such a Lüders strain effect is
reported mostly for materials with nanocrystalline or ufg microstructure (e.g. [42]).
The results of the tensile tests performed at different temperatures and strain rates
on the Fe–16Cr–6Mn–3Ni–0.05C steel yielding the most pronounced TRIP effect
can be summarized as follows:
• Along with the pronounced martensitic phase transformation, serrated plastic
flow occurs during tensile deformation at RT in a wide range of nominal strain
rates, except at the highest strain rate of 10−1 s−1.
• At elevated temperatures, serrated plastic flow occurred only for slow strain
rates, whereas at T  80 °C neither serrated plastic flow nor martensitic phase
transformation is observed.
• The increase in the strain rate as well as of the deformation temperature shifts
the onset of serrated plastic flow to higher strain values.
• At RT, an increase in the strain rate changes the appearance of the serrations
from type B to type A, whereas type B serration is observed at elevated
temperatures.
• At RT, a significant increase in the temperature of the specimen is observed with
increasing strain rate. The performance of quasi-isothermal tests using additional
cooling system during RT deformation showed that similar amount of a′-mar-
tensite is formed in comparison with RT tests without additional cooling.
However, no PLC effect is observed.
• No PLC effect occurred during tensile testing at RT and different strain rates for
an ultrafine-grained variant of Fe–16Cr–6Mn–3Ni–0.05C steel exhibiting a
mean grain size of <1 µm.
The experimental outcome of the tensile tests at different temperatures and strain
rates was corroborated by investigations on the strain rate sensitivity. The occur-
rence of serrated plastic flow is correlated strictly with a negative strain rate sen-
sitivity (SRS) [43–46], whereas pure metals exhibit always a positive SRS.
The SRS S is defined as the dependence of the flow stress r on the strain rate e_ at a
given strain e [47–49] according to (2.24) (see Sect. 2.6.2.2).
Figure 7.73 summarizes the results of the evaluated SRS at RT and elevated
temperatures (60, 80 and 140 °C). At RT, negative SRS values are observed at true
strain of e  0.2, whereas with an increase in temperature the threshold strain
value for negative SRS is shifted to larger strains. Thus, at 80 °C negative SRS is
reached at high strain levels (e  0.35), only. However, at 140 °C the SRS is
positive in the whole deformation range. Finally, the investigations on the strain
346 7 Case Studies on Localized Deformation Processes …

Fig. 7.73 Strain rate sensitivity of the metastable Fe–16Cr–6Mn–3Ni–0.05C TRIP steel in
dependence on the applied strain at different temperatures. a Room temperature. b 60 °C. c 80 and
140 °C. Reproduced from [41]. Permission of Springer

rate sensitivity agree very well with the observation of serrated plastic flow
depending on strain rate and temperature.
The explanation for the occurrence of the serrated plastic flow in this steel
variant as well as the interpretation of the mechanism behind is given later in
Sect. 7.4.5.

7.4.3 Temperature and Strain Fields

The occurrence of the serrated plastic flow during tensile deformation of the steel
variant with the lowest austenite stability (3 wt% nickel) was studied intensively by
concurrent in situ measurements of localized temperature fields using IR-TG and of
localized strain fields using DIC on optical digital micrographs.
Localized temperature fields. The temperature evolution occurring during the
tensile tests at RT and different nominal strain rates was intensively investigated
using thermographic measurements. The temperature increase during tensile
deformation is caused by different ongoing microstructural processes such as:
(i) plasticity, (ii) martensitic phase transformation and (iii) macroscopic strain
localizations, which can either occur as serrated plastic flow or necking.
Figure 7.74 shows exemplarily the results of infrared thermographic measure-
ments during tensile test at RT and a nominal strain rate of 10−3 s−1. For this
measurement, the macroscopic objective lens is used in order to follow the whole
gauge length during the test. The flow curve is shown in Fig. 7.74a together with
three thermographic images for small strain values (e < 0.15) and temperature
profiles evaluated at three different points along the gauge length, which are indi-
cated in the thermogram taken at e = 0.036. For better visibility, the T-t curves of
the three points along the gauge length are shifted along the T-axis. The thermo-
grams and the T-t curves revealed clearly a continuous temperature increase for
strain values e < 0.15. This temperature increase is correlated directly with both the
plastic deformation (formation of deformation bands) and the martensitic phase
transformation. As shown before (see Sects. 7.2.3 and 7.3.4), both the strain
localization and the martensitic phase transformation start immediately after passing
7.4 Macroscopic Strain Localization During Plastic Deformation 347

Fig. 7.74 Infrared thermographic measurements during tensile tests of Fe–16Cr–6Mn–3Ni–0.05C


steel at room temperature and a nominal strain rate of 10−3 s−1. a True stress-true strain curve in
combination with temperature evolution curves (T-t) measured at three different points along the
gauge length (green, grey, red) and a sequence of infrared thermograms of the whole gauge length
for low strain levels (e < 0.15). b Sequence of infrared thermograms of the whole gauge length for
higher strain level (e > 0.289) showing the development and propagation of two individual
macroscopic bands of localized plastic strain. Reproduced from [50]. Permission of Elsevier

the yield point. However, due to the limited lateral resolution of the thermo-camera
individual deformation bands and a′-martensite formation cannot be resolved.
However, at higher strain levels (e > 0.15) a change in the temperature evolution
is observed. The T-t curves reveal clearly an oscillating temperature evolution,
where a small time shift is registered between the three individual measuring points.
The oscillations of the temperature are correlated with the serrations observed in the
flow curve. Moreover, the oscillations are related to bands propagating along the
gauge length known as PLC bands. These PLC bands evolve on the left side of the
gauge length (green curve) and move along the gauge length (grey and red curves)
until next band is evolving. The maximum temperature at the three different points
along the gauge length is followed and shows directly that one band is followed by
another one. In addition, Fig. 7.74b shows a sequence of thermographic images at
higher strain level (e > 0.28). The sequence of thermograms at different subsequent
strain levels (indicated in the thermograms) illustrates well the development and
propagation of two individual bands along the gauge length. It becomes evident that
the macroscopic localization of strain in bands is related to a remarkable increase in
temperature.
Localized strain fields. The evolution of local strain fields related to PLC bands was
evaluated by digital image correlation of optical micrographs taken with a digital
camera during the tensile test at RT. The strain fields were recorded on the opposite
side used for IR-TG measurements. The initiation and propagation of bands along
the gauge length are accompanied by an increase in both temperature and strain as
348 7 Case Studies on Localized Deformation Processes …

Fig. 7.75 Results of the full-field measurements on two opposite sides of the gauge length of the
specimen of Fe–16Cr–6Mn–3Ni–0.05C steel tested in tension at RT and 10−3 s−1. a Part of the
flow curve and the temperature–time curve. b Thermograms taken at points indicated in (a).
c Corresponding local strain fields calculated for the opposite side of the gauge length. According
to [51]

shown in Fig. 7.75. Figure 7.75 shows not the entire deformation process. Instead,
only a short sequence of two subsequently generated bands is presented. The local
strain fields are provided in terms of Von Mises equivalent strain. The obtained
temperature fields (Fig. 7.75b) and calculated strain fields (Fig. 7.76c) correspond
to the numbers given in the temperature–time curve in Fig. 7.75a. It turned out from
the fully-coupled measurements that the PLC bands are characterized by both strain
and temperature localization.
The localized Von Mises strain within an individual band is about 3%. In the
present case, the PLC bands initiated always at the lower part of the gauge length
and propagated in bottom-up direction on both sides of the specimen as seen from
the thermograms and DIC images in Fig. 7.75b, c.
Influence of strain rate. The applied nominal strain rate has a significant influence
both on the onset of the serrated plastic flow in the stress-strain curve and on the
appearance of the serrations as described before. As shown in Figs. 7.74 and 7.75,
the serrations are related to localized bands propagating along the gauge length. The
thermographic measurements were used to study the influence of the strain rate both
on the formation and propagation of these bands and on the temperature increase
caused by these bands. Figure 7.76 shows two sequences of thermographic images
taken at a certain strain interval during tensile tests at RT and strain rates of 10−4 s−1
(Fig. 7.76a) and 10−2 s−1 (Fig. 7.76b), respectively.
In addition, corresponding flow curves are shown and the related strain levels are
provided directly in the thermograms. The initiation of a new band and the direction
of the band propagation are marked by black arrows. Three significant differences
in PLC bands developed at these two different strain rates become evident: (i) the
frequency of the band initiation, (ii) the band propagation rate and (iii) the increase
in temperature within individual bands. Thus, the increase in temperature due to
initiation and propagation of individual bands at the lowest strain rate (10−4 s−1) is
not significant (2 K only). Consequently, the gauge length of the specimen cools
down nearly completely until a new band is initiated. In contrast, the PLC bands
developed at the highest strain rate (10−2 s−1) cause a long-lasting high-temperature
7.4 Macroscopic Strain Localization During Plastic Deformation 349

Fig. 7.76 Results of in situ thermographic measurements during tensile tests of Fe–16Cr–6Mn–
3Ni–0.05C steel at room temperature and with two different strain rates: a and c = 10−4 s−1 and
b and d = 10−2 s−1. Each thermographic image corresponds to a certain true strain, which is noted
in the images. Black arrows mark the direction of the movement of individual PLC bands. Each
sequence is related to the initiation and motion of two individual bands. Reproduced from [41].
Permission of Springer

profile. In addition, the time for the initiation of a new band is much shorter.
Figure 7.77 demonstrates the influence of the strain rate both on the band initiation
and propagation behaviour and on the corresponding temperature profile. The T-
t curves are evaluated at three specific points determined across the gauge length,
where point 1 is in the upper part of the gauge length and point 3 at the lower part. It
should be noted that not the whole temperature–time profile is shown, just the parts
with the oscillations are selected. Attention should be also paid on the different
timescales for the four investigated strain rates. Whereas the bands occur in a time
interval of 3500 s at the lowest strain rate, the time interval is much shorter (<20 s)
at the highest strain rate. Thus, as lower the strain rate is as more frequently PLC
bands occur. In contrast, both the temperature increase and the band velocity are
smaller than at high strain rates. Moreover, different band propagation directions
become apparent. At lowest strain rate, bands nucleate at different places and
running either top-down or bottom-up. At higher strain rates, bands nucleate at
350 7 Case Studies on Localized Deformation Processes …

Fig. 7.77 Temperature–time curves evaluated on three distinct points across the gauge length of
specimens of Fe–16Cr–6Mn–3Ni–0.05C steel during tensile tests at RT and four different strain
rates. a 10−4 s−1. b 10−3 s−1. c 3  10−3 s−1. d 10−2 s−1. According to [51]

either at the upper or lower part of the gauge length and propagate then in one
direction, only.
The correlation of the serrations of the stress-strain curve with the temperature
profile is shown in Fig. 7.78 for the lowest and the highest strain rate. In addition,
six thermographic images of the gauge length taken by the microscopic objective
lens with a higher lateral resolution are indicated.

Fig. 7.78 Correlation of stress-strain curves and time-resolved temperature evolution obtained
during tensile tests of Fe–16Cr–6Mn–3Ni–0.05C steel at room temperature in combination with
six infrared thermograms indicated in the temperature profile. a Lower strain rate 10−4 s−1.
b Higher strain rate 10−2 s−1. Reproduced from [41]. Permission of Springer
7.4 Macroscopic Strain Localization During Plastic Deformation 351

For the lower strain rate, no clear correlation of the serrations and the temper-
ature increase is apparent due to the high number of bands nucleating at different
places of the gauge length. In contrast, each stress drop in the stress-strain curve is
accompanied by a significant increase in the temperature at the highest strain rate.
Moreover, the temperature rise due to individual bands increases with an increase in
the strain rate. Thus, temperature increase within one individual band is 0.5 K only
at the lower strain rate, whereas it is about 4 K at the higher strain rate.
The observations of IR-TG were corroborated by the calculation of local strain
fields at these two different strain rates as shown in Fig. 7.79. The strain localization
appeared to be more pronounced at the higher strain rate. Thus, the increase in local
strain by passing one PLC bands is about 3% (see Fig. 7.79b) at the higher strain
rate 10−2 s−1, whereas it is less than 0.8% at the lower strain rate 10−4 s−1 (cf.
Fig. 7.79a).
The strain increase caused by individual bands was calculated by comparing the
strain level before a band initiates with the maximum strain that is measured when
the band has passed the gauge length. The irregular shape of the DIC images is
related to the pronounced surface roughness occurring in general during the tensile
test of coarse-grained materials and is even enlarged by passing of several PLC
bands.
Using both thermographic and strain field maps, the velocity of propagating PLC
bands was determined according to Fig. 7.80.

Fig. 7.79 Local strain fields obtained by the digital image correlation technique during tensile
tests of Fe–16Cr–6Mn–3Ni–0.05C steel at room temperature and two different strain rates,
10−4 s−1 (a) and 10−2 s−1 (b). The sequences show the movement of individual PLC band.
Reproduced from [41]. Permission of Springer
352 7 Case Studies on Localized Deformation Processes …

Fig. 7.80 Evaluation of band velocity using thermographic measurements with microscopic
objective lens at RT and a strain rate of 3  10−3 s−1. According to [51]

The velocity was calculated using (7.5):

L
vB ¼ ð7:5Þ
tout  tin

where L is the length of AOI parallel to the loading axis detected by the
thermo-camera using microscopic objective lens or the digital camera on the
opposite side, and tin and tout are the times when an individual band is entering or
leaving the AOI as shown exemplarily in Fig. 7.80 for a strain rate of 3  10−3 s−1.
Thus, the velocity of bands passing the gauge length increases with the increase in
the strain rate. Whereas the bands propagate with 0.2 mm/s at a strain rate of 10−4
s−1, the band velocity is about 7 mm/s at strain rate of 10−2 s−1.
Influence of deformation temperature. Accompanying thermographic measure-
ments were performed in the temperature range up to 60 °C for all strain rates. The
increase in deformation temperature yields (i) a decrease in the number of initiated
bands, (ii) a decrease in the average temperature increase caused by the initiation of
a new band and (iii) a decrease in the band velocity. Thermographic measurements
carried out during the quasi-isothermal tensile tests at a moderate strain rate of 10−3
s−1 revealed a small continuous increase in temperature. Thus, in agreement with
the stress-strain curves no serrations and no PLC bands propagating along the
gauge length are detected.
Finally, typical band parameters characterizing the PLC bands occurring in a
certain range of temperature and strain rate such as DTB per band, the number of
bands NB , the velocity vB of bands or the localized strain inside bands DeB were
determined and are summarized in Table 7.13. At a given temperature, the increase
in the strain rate results in (i) an increase in the temperature rise within an individual
band, (ii) a higher localized strain and (iii) a faster band propagation across the
gauge length. However, the number of bands is decreasing and the band type is
changing from type B at slow strain rate to type A at high strain rate.
7.4 Macroscopic Strain Localization During Plastic Deformation 353

Table 7.13 Band parameters determined using thermographic measurements during tensile tests
at RT and different strain rates. T0 —initial temperature, e_ 0 —initial strain rate, NB —number of
bands, DTB —temperature increase inside PLC band, DeB —local strain increase inside PLC band,
vB —average band velocity
T 0 (°C) e_ 0 (s−1) Band type NB DT B [K] DeB (%) vB (mm/s)
20 10−2 A 9 4 ± 0.5 3 ± 0.7 6.9 ± 1.3
20 10−3 A 9 2.5 ± 0.2 1.5 ± 0.3 1.8 ± 0.3
20 10−4 B 19 0.5 ± 0.1 0.8 ± 0.2 0.2 ± 0.01
40 10−2 A 6 2 ± 0.4 1.5 ± 0.4 7.2 ± 1.5
40 10−3 B 17 1 ± 0.1 1.0 ± 0.1 2.2 ± 0.1
40 10−4 B 17 0.8 ± 0.2 0.8 ± 0.3 0.3 ± 0.02
60 10−3 B 10 0.8 ± 0.1 0.9 ± 0.2 0.5 ± 0.2
60 10−4 B 17 0.6 ± 0.2 0.6 ± 0.2 0.1 ± 0.01

The influence of the deformation temperature on the band velocity is negligible


at least for RT and T = 40 °C. However, at T = 60° significant reduction of the
band velocity is observed.
These results are in good agreement with investigations performed by
Saeed-Akbari on TWIP steels [52], where band velocities were also determined
from thermographic measurements. The reported band velocities were about 1.5, 3
and 28 mm/s for tensile tests performed at RT and strain rates of 10−4 s−1, 10−3 s−1
and 10−2 s−1, respectively.

7.4.4 Portevin–Le Chatelier Effect and Acoustic Emission

The evolution of the ongoing deformation processes leading to serrated plastic flow
was evaluated using the analysis of acoustic emission signals as described in
Sect. 7.3.1.
Figure 7.81 shows the typical stress-strain curve at RT and a strain rate of
10−2 s−1 exhibiting serrated plastic flow at higher strain levels in combination with
the parameters AE energy E and median frequency fm. The evolution of these two
parameters was discussed already in Sect. 7.3.3. Here, the focus should be on the
time interval t > 20 s shown in Fig. 7.81b, where the high energy burst-type AE
signals are correlated clearly with the serrated plastic flow in the stress-strain curve.
Both the time sequence of the two main deformation mechanisms such as the
formation of deformation bands consisting of stacking-faults and MPT and the
influence of temperature on it are described comprehensively already in Sect. 7.3.3
(cf. Figs. 7.63e, f and 7.67). It turned out from these diagrams that the motion of
partial dislocations and the formation of a′-martensite are dominant at RT (see
Fig. 7.67) and 100 °C as well. The scatter plots of the identified clusters in terms of
AE energy and median frequency are plotted together with the time sequence of
these clusters over the entire deformation process in Fig. 7.82.
354 7 Case Studies on Localized Deformation Processes …

Fig. 7.81 Results of the analysis of acoustic emission signals obtained during tensile test at room
temperature and a nominal strain rate of 10−2 s−1 for Fe–16Cr–6Mn–3Ni–0.05C steel. Stress-strain
curve in combination with development of the average energy E of the AE signals (green) and the
mean frequency fm (blue) determined from the power spectral density function. a Complete data
set. b Data for t > 20 s

Similar to results shown in Fig. 7.67, cluster 1 related to partial dislocations


evolves directly at the beginning of the deformation process followed promptly by
cluster 2 related to the formation of a′-martensite during RT deformation. However,
a third cluster starts to develop at around 10% of elongation. The cluster is then
growing continuously in terms of cumulated energy as well as number of cluster
elements. As it becomes apparent from the scatter plot (Fig. 7.82a), signals of this
cluster are characterized by high-energy level and are located in the lower fre-
quency domain. In accordance with the stress-strain curve showing serrations at
strain levels above 20% of elongation (cf. Fig. 7.70), this cluster is correlated with
the occurrence of PLC bands propagating along the gauge length.
Since AE is a highly time-resolved and volume-integrating technique, the cluster
3 starts already earlier than serrated flow is detectable from the stress-strain curve.
As the deformation temperature increases, the intensity of all clusters decreases. In
addition, the onset of cluster 3 is shifted to higher strain levels. This is also in good
agreement with flow curves shown in Fig. 7.70a, where the temperature increase
shifts the onset of serrated plastic flow to higher strain levels. Thus, the onset of
serrated plastic flow determined from the time sequence of cluster 3 is around 25%
of elongation during tensile deformation at 40 °C. At even higher temperatures
(60 °C), cluster 3 disappears completely and no serrated plastic flow is observable
in the stress-strain curve anymore.

7.4.5 Correlation of PLC Effect with Martensitic Volume


Fraction

All results obtained from the above-mentioned investigations on (i) the stress-strain
response, (ii) the ferromagnetic phase fraction, (iii) the thermography and (iv) the
acoustic emission measurements are summarized in Table 7.14 and allow a detailed
7.4 Macroscopic Strain Localization During Plastic Deformation
355

Fig. 7.82 Results of the AE cluster analysis of Fe–16Cr–6Mn–3Ni–0.05C steel during tensile tests at a strain rate of 1  10−2 s−1 and different temperatures.
a RT. b 40 °C. c 60 °C. Left: Scatter plots of AE energy E and median frequency fm . Middle: Time sequence of identified clusters in terms of cumulated AE
energy in combination with stress-strain curve. Right: Time sequence of identified clusters in terms of number of cluster elements
356 7 Case Studies on Localized Deformation Processes …

Table 7.14 Parameters describing the occurrence of the PLC effect in Fe–16Cr–6Mn–3Ni–0.05C
steel. e_ 0 —initial strain rate, T0 —initial temperature, Tmax —maximum temperature of the specimen
without additional cooling, et;max —maximum true strain to failure, a0max —maximum content of a′-
martensite, eTG t;c —critical true strain identified by IR-TG, et;c —critical true strain identified from
SSC

stress-strain curves, et;c —critical true strain identified by acoustic emission


AE

e_ 0 (s−1) 10−2 10−3 10−4


T 0 (°C) 20 40 20 40 60 20 40 60
T max (°C) 89 79 61 43 63 24 40 59
et;max (−) 0.36 0.39 0.36 0.50 0.38 0.37 0.42 0.41
a0max (vol. %) 49 30 58 50 19 58 47 31
eSSC
t;c (−)
0.22 0.24 0.15 0.22 0.25 0.09 0.13 0.15
eTG
t;c (−)
0.23 0.26 0.16 0.23 0.21 0.09 0.15 0.14
eAE
t;c (−) 0.15 0.21 – – – – – –

discussion on the correlation of the occurrence of the PLC effect with temperature,
strain and martensitic volume fraction. Finally, it is possible to calculate the acti-
vation energy of the interstitial diffusion of carbon or nitrogen atoms causing the
PLC effect in the Fe–16Cr–6Mn–3Ni–0.05C TRIP steel. The results provided in
Table 7.14 are limited to the range of temperatures and strain rates, where the PCL
effect occurred, i.e. T  60 °C and strain rates e_  10−2 s−1.
The upper part of Table 7.14 contains all parameters related to the deformation
behaviour and MPT depending on deformation temperature and strain rate. Here, it
is distinguished between the start temperature of the deformation test T0 and the
maximum temperature Tmax reached during the tensile test. In the lower part, the
critical strain values for the onset of PLC are provided, which were obtained by the
different methods—(i) stress-strain curve analysis, (ii) thermography and
(iii) acoustic emission.
It is obvious that the serrated flow is observed for this type of steel only in a
limited range of the testing parameters, which is shown in Fig. 7.83a. At the highest
strain rate (10−1 s−1), no PLC effect occurred at all, whereas the PLC effect is
pronounced at temperatures up to T0 = 60 °C at lower strain rates (10−3 and 10−4
s−1). However, the temperature of the specimen increased due to plastic work and
the formation and propagation of PLC bands, as it has been demonstrated by
infrared thermographic measurements ðTmax Þ: Thus, the influence of the strain rate
on Tmax is more pronounced at high strain rates and T0 = RT. Since the temperature
increase in the specimen is also depending on the strain rate, the occurrence of PLC
effect caused at various strain rates can also be related to Tmax reached during the
tensile tests as shown in Fig. 7.83b. In addition, Fig. 7.83b contains two data points
(marked by arrows), which are obtained by so-called quasi-isothermal tests per-
formed with additional cooling in order to prevent the specimen heating during
plastic deformation.
7.4 Macroscopic Strain Localization During Plastic Deformation 357

Fig. 7.83 Occurrence of the PLC effect in the Fe–16Cr–6Mn–3Ni–0.05C TRIP steel depending
on the strain rate, the temperature at the beginning of the deformation test (a) and the maximum
temperature reached during the tensile test (b). Black circles indicate the absence of the PLC effect,
while red diamonds indicate its occurrence. Reproduced from [41]. Permission of Springer

Consequently, the field of the occurrence of the PLC effect has changed. Thus, at
the lowest strain rate the PLC effect occurs in a temperature range Tmax between 24
and 59 °C. In contrast, the temperature range becomes even narrower at the higher
strain rates—compare 79 °C  Tmax  89 °C at 10−2 s−1. However, it should be
noticed that the real temperatures at which the PLC effect occurs lie in between the
start and finish temperature of the tensile tests.
In addition, it is recognizable that both the initial deformation temperature T0
and the applied strain rate have a significant influence on the martensitic phase
fraction formed during the tensile tests. Thus, both an increase in T0 and an increase
in the strain rate result in a decrease in the martensitic volume fraction. Whereas
about 60% martensite is formed at RT, only 30% occurred at 60 °C for tests
performed with the lowest strain rate. At the strain rate of 10−2 s−1, still 50%
martensite is formed during RT deformation, while only 19% developed during
tests at 60 °C and no PLC effect occurred anymore. Thus, the reduction of a′-
martensite volume fraction is understandable in terms of temperature increase. With
increasing temperature, the amount of martensitic phase transformation is
decreased. Since the increase in strain rate is accompanied by an increase in tem-
perature, this effect also counteracts MPT.
Furthermore, it becomes obvious that the temperature T0 and the strain rate also
have a significant influence on the critical strain for the onset of PLC effect. Since
the beginning of dynamic strain ageing is of course not equivalent with the start of
plastic flow, a critical strain level has to be reached. Thus, the critical true strain
values are determined either from (i) the start of serrated flow in the stress-strain
curve, (ii) the first appearance of PLC bands in the thermographic images and
(iii) the start of the evolution of the AE cluster related to PLC bands. As seen from
Table 7.14, there is a good agreement between the different techniques used for the
determination of this critical strain. The critical true strain estimated from the
acoustic emission measurements is lower than the values obtained from the other
358 7 Case Studies on Localized Deformation Processes …

methods. This is caused by the high sensitivity of the acoustic emission


measurements.
However, the critical true strain for the onset of PLC effect depends both on the
temperature and on the strain rate. Thus, both an increase in T0 at a given strain rate
and an increase in strain rate at a given T0 result in a shift of the beginning of
serrated flow to higher strain levels.
Moreover, the critical strain level is related to the volume fraction of
strain-induced a′-martensite. As mentioned above (cf. Sect. 6.4), it is well known
that MPT starts locally early in the deformation process. However, a macroscopi-
cally relevant volume fraction of deformation-induced a′-martensite develops at
about the inflection point in the stress-strain curve. Therefore, at T0 = RT and the
lowest strain rate (10−4 s−1) the inflection point and the onset of PLC effect fit very
well (cf. Fig. 7.70). If the d-ferrite (10%) and/or the athermal martensite (15%)
pre-existing in the initial microstructure of the material would be responsible for the
PLC effect, then a start of serrated flow would be expected at lower strains.
Therefore, the fact that the serrated flow occurs at temperatures T0  60 °C and at
strain rates e_  10−2 s−1 after the inflection point indicates that the PLC effect is
related to the formation of deformation-induced a′-martensite in the studied
metastable Fe–16Cr–6Mn–3Ni–0.05C TRIP steel.
The increase in the strain rate at a given deformation temperature T0 results in an
increase in the difference between the inflection point and the onset of serrated flow
in the stress-strain curve. However, the maximum volume fraction of a′-martensite
is reduced only slightly. Therefore, the shift of the onset of PLC effect to higher
strains is mainly caused by the increased temperature due to deformation. Since the
martensitic phase transformation significantly depends on the grain orientation, the
measured volume fraction of a′-martensite varies from specimen to specimen.
Therefore, a minimum value for the volume fraction of a′-martensite can only be
roughly estimated. Since even at a volume fraction of a′-martensite of 19%
(T0 = 60 °C, e_ = 10−3 s−1) the PLC effect occurred, it is assumed that a PLC effect
occurs above a minimum value of a′-martensite a0min = 10%.
Since the commonly accepted reason for the DSA is the interaction of interstitial
atoms with the dislocations, the activation energy for the diffusion of interstitial
atoms like carbon and nitrogen in the bcc structure of the formed a′-martensite was
calculated from the experimental data regarding the occurrence of the PLC effect.
The correlation between the critical strain for the onset of serrated flow, the tem-
perature and the strain rate of the deformation experiments is expressed according
to [53–55] by the following empiric equation:
DG
e_ ¼ K  em
c
þb
 eð kT Þ ð7:6Þ

Here, m and b are constants describing the dependence of the critical strain on
the dislocation density and on the vacancy concentration, respectively. DG is the
activation energy of the interstitial diffusion and k the Boltzmann constant. K is a
material constant.
7.4 Macroscopic Strain Localization During Plastic Deformation 359

The values for DG and b were calculated in dependence on the critical true
strain, the strain rate e_ and the deformation temperature T by (7.7) and (7.8),
respectively (according to [53–55]):

@ln_e
b¼ ð7:7Þ
@ec T

DG @lnec
¼ ð7:8Þ
b @1=kT e_

Whereas (7.7) allows for the experimental determination of the b parameter


describing the dependence of the critical strain on the vacancy concentration, (7.8)
allows for experimental determination of the activation energy DG of the interstitial
diffusion. Figure 7.84 shows the results of the calculations according to (7.7)
(Fig. 7.84a) and (7.8) (Fig. 7.84b), respectively. For the
 critical strain, both the
values obtained from the stress-strain curve SSC eSSC
t;c and from the thermogra-
−4 −1
phy (eTG
t;c ) (cf. Table 7.14) are used. The lowest strain rate (10 s ) was chosen for
the calculations, since the temperature increase during the tensile tests was negli-
gible (see Table 7.14).
According to Fig. 7.84, the activation energy for the present steel variant is
determined to be 62 kJ/mol. This activation energy is definitely less than the
activation energies reported by Oettel et al. [56] for the carbon (DG = 134 kJ/mol)
or nitrogen (DG = 118 kJ/mol) diffusion in the fcc austenitic steels. Roberts et al.
[57] reported on DG = 81 kJ/mol for the carbon diffusion in the ferritic phase and
DG = 78 kJ/mol for the nitrogen diffusion in martensitic phase. However,

Fig. 7.84 Calculation of the activation energy for the diffusion of interstitial atoms. a Double
logarithmic plot of the critical strain versus strain rate at constant temperature (20 °C) for the
calculation of b according to (7.7). b Arrhenius plot of the critical strain versus the deformation
temperature at constant strain rate (10−4 s−1) for the calculation of DG according to (7.8).
Experimental values are obtained from stress-strain curve (SSC) and thermography (TG), cf.
Table 7.14. Reproduced from [41]. Permission of Springer
360 7 Case Studies on Localized Deformation Processes …

according to Oettel et al. [56] the diffusion velocity of nitrogen atoms is appreciable
higher in the martensite than the diffusion velocity of carbon atoms.
Therefore, it is very likely that the PLC effect in the present studied Fe–16Cr–
6Mn–3Ni–0.05C TRIP steel is caused by the diffusion of interstitials (C, N) in the
bcc a′-martensite interacting with the mobile dislocations, although the calculated
activation energy DG = 62 kJ/mol is smaller than values reported in the literature.
However, a distinction between carbon and nitrogen as responsibility for the ser-
rated plastic flow is impossible, since the investigated TRIP contained carbon and
nitrogen at equal quantities.
In comparison with the other steel variants with higher nickel content (6 and 9 wt
%), the steel with 3 wt% nickel is the only one exhibiting serrated plastic flow in a
limited range of deformation temperatures and strain rates. The Fe–16Cr–6Mn–
9Ni–0.05C steel exhibits only mechanical twinning in a purely austenitic
microstructure. Therefore, in the investigated temperature range no PLC effect is
expected. On the other hand, the Fe–16Cr–6Mn–6Ni–0.05C steel also exhibits
MPT resulting in the TRIP effect in the temperature range T  100 °C (cf.
Sect. 7.3.4), and the martensitic phase transformation is significantly less pro-
nounced due to the higher austenite stability compared to Fe–16Cr–6Mn–3Ni–
0.05C steel. In addition, the overall amount of bcc phase present in Fe–16Cr–6Mn–
3Ni–0.05C steel is significantly higher due to 10% delta ferrite and 15% sponta-
neous martensite in the initial microstructure, which leads together with the for-
mation of 10% a′-martensite at least to a volume fraction of bcc phase >30%.

7.4.6 Discussion

The above-mentioned results regarding the development of macroscopic strain


localizations in combination with local temperature increase were obtained by
fully-coupled full-field measurements during tensile deformation at RT and dif-
ferent strain rates. The used experimental setup for the fully-coupled measurements
was the two-face measurement approach using a digital camera and a
thermo-camera on opposite surfaces of a flat specimen as described by Chrysochoos
[58] first (compare Sect. 5.3.3). This two-face approach has the big advantage that
both specimen surfaces can be prepared in optimum conditions for the two different
measurement techniques. Thus, one of the surfaces is covered by black lacquer to
provide a high emissivity for the thermographic measurements and the second
surface is prepared with a reasonable contrast pattern allowing good resolution for
the digital image correlation. However, one of the main disadvantages of the
two-face approach is that temperature and local strain fields are not registered from
the same area of interest. Especially for polycrystalline materials, this could yield
different results on opposite specimen surfaces. The best materials for the appli-
cation of the two-face approach would be, therefore, single crystals or at least oligo
crystals.
7.4 Macroscopic Strain Localization During Plastic Deformation 361

As shown by the above-described results, the two-face approach worked well in


most of the performed tests on Fe–16Cr–6Mn–3Ni–0.05C steel. Thus, in most
cases, the results of the thermographic measurements correlated well with the DIC
results in terms of the initiation sites of PLC bands and their propagation direction.
Such an example is shown in Fig. 7.85a for a tensile test at RT and a strain rate of
10−3 s−1. In this case, the band initiation was detected on both specimen surfaces at
the lower part of the gauge length and bands propagated in bottom-up direction. In
contrast, Fig. 7.85b shows the opposite for tensile test at RT and a strain rate of
10−2 s−1. Here, the thermo-camera detected bands initiating at the upper part of the
gauge length and propagating top-down. However, the DIC detected PLC bands
initiating at the lower part with a propagation in the opposite direction (bottom-up).
This is clearly an indicator that variations in the microstructure on both specimen
surfaces are responsible for this behaviour.
Therefore, in order to follow the PLC band initiation and propagation in the
same area of interest, the better choice for experimental setup would be the one-face
approaches in terms of either a two-camera setup or a single-camera setup using
thermo-camera only—the so-called IRIC. However, both of these two one-face
approaches have their respective limitations.
The one-face approach using two cameras in combination with a dichroic mirror
has two limitations. The first is the preparation of the specimen surface in a way,
which is suitable for both—the infrared measurements and the DIC. The second
limitation is to find a dichroic mirror with the appropriate cut-off wavelength. The
idea of the dichroic mirror is to transmit the infrared radiation sent out from the
specimen surface and to reflect the visible light into the digital camera placed at 90°

Fig. 7.85 Fully-coupled full-field measurements of temperature and strain fields during tensile
tests at RT and two different strain rates. a Strain rate 10−3 s−1. b Strain rate 10−2 s−1. In addition,
part of the stress–time and the temperature–time curves is shown. The sequence of initiation and
propagation of an individual band is indicated by numbers in the temperature–time curve. Both the
thermograms and the local strain fields show the complete gauge length of the tensile specimen.
Local strain is given in terms of Von Mises strain. According to [51]
362 7 Case Studies on Localized Deformation Processes …

with respect to the thermo-camera. Thus, the experiments described in the literature
were performed solely with thermo-cameras working in the SWIR (0.8–2 µm),
where suitable dichroic mirrors could be applied. Commercially available dichroic
mirrors are either short-pass dichroic mirrors or long-pass dichroic mirrors with
different cut-off wavelengths. For the purpose of transmitting infrared radiation and
reflecting visible light, the long-pass dichroic mirrors are suitable, since depending
on the cut-off wavelength the wavelength band of transmitted radiation can be
chosen. Thus, available are, e.g., long-pass filters with a cut-off wavelength of
900 nm. Figure 7.86 shows the fields of transmittance and reflectance of this
mirror. Thus, the band of transmittance is above 900 nm up to 1.3 µm and the band
for reflectance is between 400 and 850 nm perfectly fitting with the wavelength of
visible light. However, the band of transmittance for wavelengths between 900 and
1300 nm fits only to SWIR cameras. Therefore, the one-face approach based on the
dichroic mirror of [59] is not possible with the present thermo-camera equipment.
The one-face approach with the co-planar arrangement of the two cameras is
limited by the angle of view and the depth of view of both cameras. Thus, in order
to avoid miscalculations the digital camera should be placed exactly perpendicular
to the surface and exactly parallel to the gauge length of the specimen. The
thermo-camera can then be placed above or below the digital camera. Depending on
the physical dimensions of both cameras, this results in difference of the view angle
of both cameras in the range of several degrees, which is, however, not crucial for
metallic specimens. Here, a view angle of 50°–90° with respect to the specimen
surface provides still accurate temperature measurements. However, some distor-
tions in the thermograms and some difficulties in the coupling between thermo-
grams and local strain fields could arise.
The most demanding method is the one-face one-camera setup resulting in IRIC.
Along with the high recommendations according to the specimen surface prepara-
tion, the requirements according to the exact temperature control of the surrounding
and the exact temperature determination at the specimen are the most crucial points.

Fig. 7.86 Wavelength windows for transmission and reflection of a dichroic mirror with
long-pass filter and a cut-off wavelength of 900 nm. Band of transmission: 900–1300 nm. Band of
reflection: 400–850 nm. According to [60]
7.4 Macroscopic Strain Localization During Plastic Deformation 363

However, in contrast to the drawbacks of the two-face two-camera setup again


the acoustic emission measurement technique confirmed its high potential in terms
of a real-time and volume-integrating method. Thus, as demonstrated by Table 7.14
the acoustic emission measurements detect PLC bands significantly earlier than
they become apparent from the stress-strain curves or they are visible in thermo-
grams or local strain fields.
Thus, the future of in situ measurements lies in their combination. The high
potential of the application of complementary in situ measurement methods is the
combination of the high resolution on different scales—lateral, thermal and
temporal.

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Chapter 8
Prospects of Complementary
In Situ Techniques

Abstract This chapter summarizes benefits of the application of complementary


in situ characterization techniques. First of all, the advantages and disadvantages of
each in situ characterization technique are summarized and discussed. Furthermore,
the contribution of the results out of these complementary techniques to the
modelling of materials behaviour is discussed. Furthermore, four examples are
presented where the author sees a benefit from the application of these techniques:
(i) modelling of the strain-hardening behaviour of TRIP/TWIP steels, (ii) damage
behaviour of TRIP matrix composites, (iii) deformation and damage behaviour of
laminated TRIP/TWIP steels and (iv) the application to shape memory alloys.

8.1 General Remarks

The case studies presented in Sect. 7 demonstrated in situ testing and characteri-
zation of TRIP/TWIP steels under different loading conditions and on different
length scales. Thus, SEM-DIC in combination with EBSD provides information on
local strain fields on a micrometre or even sub-micrometre scale for individual
microstructural constituents, whereas thermography is related to macroscopic
deformation behaviour and provides information on local temperature fields caused
by macroscopically inhomogeneous deformation. Acoustic emission measurements,
however, are bridging micrometre and macrometre scale due to their volume
integrating character and give information on both the onset and the dominance of
individual deformation mechanisms on microsecond scale. In particular, results
obtained from these three different in situ techniques—strain fields, thermal fields
and temporal evolution of deformation mechanisms—together with further infor-
mation on microscopic scale (grain orientation, defect arrangement, phase com-
position and nanohardness) and macroscopic scale (deformation behaviour under
different loading conditions) gain a high potential for studying microstructural
phenomena in relation to macroscopic deformation behaviour as demonstrated by
Fig. 7.2. However, each of the techniques used in the present work has its own
advantages and limitations. Therefore, before describing the potential of the

© Springer Nature Switzerland AG 2020 365


A. Weidner, Deformation Processes in TRIP/TWIP Steels,
Springer Series in Materials Science 295,
https://doi.org/10.1007/978-3-030-37149-4_8
366 8 Prospects of Complementary In Situ Techniques

application of complementary in situ techniques a short summary of advantages and


limitations of the individual techniques will be provided.
In situ SEM testing. The high resolution of today’s FE-SEMs allows the
detailed investigation of microstructural features down to the nanometre scale.
Therefore, a deeper insight into microstructure property relationships can be gained
by the performance of in situ deformation tests in SEM. Since specimens with
dimensions on a mesoscale (several millimetres up to centimetres) were used, the
in situ testing in SEM offers a great benefit regarding the interpretation of
microstructural changes with respect to the macroscopic deformation behaviour.
This is the great advantage in comparison to in situ TEM deformation experiments
on electron transparent foils or so-called small-scale testing on specimens with
dimensions on the micrometre scale (pillar tests, microbending tests and nanoin-
dentation), which are far from a direct correlation to macroscopic material beha-
viour due to the “…as smaller as stronger paradigm…”. Beside the size of the
specimens used, in situ SEM testing allows manifold loading paths such as tensile,
compressive, cyclic or bending deformations experiments as well as deformation
under shear or multiaxial loading. In addition to the mechanical loading, thermal
treatments can be superimposed either by high or low temperatures.
However, the in situ testing in SEM provides also some challenges and restrictions.
First restriction is given by the scanning character of the capturing process of SEM
images. In order to obtain high-resolution images with low-noise level, slow scanning
rates or larger dwell times per pixel have to be applied. Therefore, real-time imaging
with high-quality images is only possible in case of SEM equipped with fast scanner
devices (e.g. 300 image per min, or even higher). In most cases, therefore, quasi in situ
tests were performed using well-defined deformation intervals (elongation, number of
cycles, etc.). Moreover, in situ SEM testing provides only two-dimensional surface
observations. Second restriction is the reduction of field of view to micrometre scale
with increasing magnification for higher resolution, which is almost problematic for
large-grained materials and is of minor importance for ultrafine-grained or
nanocrystalline materials. The third restriction occurs for materials, which can be
investigated. Here, no problems arise for any metallic materials since they are con-
ductive. More problematic is the in situ testing of non-conductive materials or com-
posite materials containing high volume fraction of non-conductive reinforcements.
As a corrective, thin layer (few nanometre thick only) of conductive coating using
carbon or precious metals (Pt, Au) can be used. However, the conductive layer can
cause a loss of intensity and, therefore, information depending on the used electron
signals (SE, BSE, EBSD and EDS). In situ SEM tests on ceramic materials have to be
performed with high caution due to the almost brittle damage behaviour of this class of
materials. Fourth restriction is related to the applied loading stages regarding
dimensions and weight of these devices or related to the size of the vacuum chamber or
their positioning to the primary electron beam (e.g. nanoindentation devices or AFM
devices for application in SEM). Moreover, depending on the used SEM analysing
technique, e.g. EBSD, special adapters or modifications on the loading devices are
necessary to fit the optimum imaging or analysing conditions (e.g. specimen tilt of 70°
with respect to the electron beam).
8.1 General Remarks 367

Digital image correlation. Digital image correlation can be applied to all kind of
digital images captured by different devices such as optical microscopes, digital
cameras, CT, SEM, TEM, AFM, FIB and infrared cameras. All of these different
DIC applications have their own advantages and limitations. Since in the present
work only optical DIC and SEM-DIC were used, pros and contras will be discussed
only with respect to these two approaches. The overall benefit of both DIC
approaches is the possibility to calculate local strain fields or even stress fields on
different length scales, which are, however, related to the macroscopical behaviour.
The essential prerequisite for DIC—either optical or SEM-DIC—is a good
contrast pattering at the specimen surface. This is almost unproblematic for optical
DIC on the majority of materials. Either these materials exhibit an own intrinsic
patterning contrast, or a kind of speckle pattern can be applied, or surface structure
due to manufacturing process present on the specimen surfaces can be used.
However, the pixel size of the pattern contrast dictates the resolution of DIC cal-
culations. This becomes a first challenge for SEM-DIC. Here, however, the con-
trasting method used for optical DIC cannot be applied. Due to the micrometre scale
of the FOV, smaller length scales of the contrast pattern have to be achieved. This
can be done by different techniques summarized in Sect. 5.4.1.1. In addition, a
compromise between desired resolution of the DIC calculations and additional
information on microstructural changes (e.g. orientation changes by EBSD) has to
be found. A second challenge for SEM-DIC is rised by the formation of pronounced
surface profile during out-of-plane deformation occurring during in situ deforma-
tion depending on material, microstructure and loading condition. Therefore, before
testing the proper imaging mode (SE contrast, InLense-SE contrast and BSE con-
trast) has to be chosen. In addition, the formation of pronounced surface profile
limits the application range of SEM-DIC to a certain range of applied global strain.
A third challenge is inherent to the electron beam and the scanning nature of image
capture process, which can cause artificial displacements into SEM images.
Kammers et al. [1], however, provided improvements on SEM-DIC in order to
capture nearly distortion-free images (see Sect. 7.5.)
Acoustic emission measurements. The method of acoustic emission measure-
ments is one of the few methods enabling real-time and volume integrating
investigations of microstructural process occurring in bulk materials. The record of
AE data is quite simple presupposed the proper choice of AE transducer regarding
the frequency domain, which is planned to analyse as well as the temperature range
of the mechanical tests. Most broadband AE transducers have a limited temperature
application range between −40° < T < 140 °C caused by the piezo-ceramic used.
For higher or lower temperatures, special AE transducers (mostly resonant sensors)
can be used. In addition, waveguides can be applied, which yield, however, often a
loss of AE signals due to damping behaviour of the waveguide and the coupling
between waveguide and AE transducer. Second important point for high-quality AE
measurements is the location of the AE transducer on the specimen surface. It
should be guaranteed that no pronounced surface roughening or other changes at
the location of the AE senor occur during tests, since they would result in a loss of
good connectivity between sensor and specimen, which is an essential prerequisite
368 8 Prospects of Complementary In Situ Techniques

for good detection of surface displacements in the order of 10−14 m. The biggest
challenge of the AE method is the data evaluation depending on the processes or
information interested in. Thus, in case of identification of location of different AE
sources, the application of more than one AE sensor is necessary and the source
location can be then solved by triangulation of the AE signals recorded by several
AE transducers placed at different locations on the specimen under test. In addition,
it has to be distinguished into continuous AE processes such as occurring during
plastic deformation and/or damage of various kinds of materials during quasi-static
monotonic or cyclic loading and single AE events such as occurring during
dynamic loading (impact tests, etc.). Here, different approaches for data treatment
are available and each of them has its one advantages and complications. The AE
measurements can be also combined with in situ SEM testing due to the application
of small-sized AE transducers (see Sect. 8.3.2).
Infrared thermography. The method of infrared thermography is also an
image-based, contactless measuring technique, which is quite close to a real-time
method depending on the frame rate of the thermo-camera used. Thermography can
be applied for all kinds of materials. Only prerequisite is the high emissivity of the
measuring object, which is ensured more or less for non-metallic materials. In case
of metallic materials, the emissivity can be improved by application of black colour
on the specimen surfaces. Furthermore, it has to be paid attention on the temper-
ature of background and avoiding additional temperature influences from the sur-
rounding. The lateral resolution of thermography depends on the detector size and
objective of the used thermo-camera and lies usually in arrange between 100 and
25 µm. Quite new developments of high-resolution thermo-cameras allow for
resolutions down to 2 µm (e.g. Infratec, Vario Cam High definition). Accounting
for heat conduction, the evolution of heat sources and dissipated energy can be
followed. More complexity is achieved for fully-coupled full-field measurements
due to counteracting prerequisites for the preparation of specimen surfaces.
However, fully-coupled measurements enable the investigation of thermomechan-
ical coupling during plastic deformation. In contrast to AE measurements, infrared
thermography cannot be applied as in situ SEM technique.

8.2 Complementary In Situ Techniques


and Microstructural-Based Modelling

Taking into account the advantages and limitation of each of the used in situ
techniques, the combination of complementary in situ experiments performed on
different length (and time) scales offers a great potential to serve with parameters for
multiscale modelling.
One outstanding approach for multiscale modelling is in the field of Integrated
Computational Materials Engineering (ICME), which is in development since
several years. Nowadays, important issues of materials research are prediction,
8.2 Complementary In Situ Techniques and Microstructural-Based Modelling 369

control and variation of properties of newly developed advanced materials for


further improvement of applicability of these materials under various kinds of
conditions. Hereby, both a comprehensive knowledge of materials behaviour down
to the atomic scale as well as well-developed theoretical approaches (computer
simulations, models and statistics) are essentially necessary.
According to Olson, the main goal of ICME is to capture the “…four-element
paradigm of modern materials science and engineering…” [2]: (i) processing,
(ii) structures (iii) properties and (iv) performance of materials by using multiscale
modelling as illustrated by Fig. 8.1a. In general, ICME is, therefore, an approach to
design products based on associated materials processing methods linked with
material models at multiple length scales—from structural scale over macro, meso
and microscale down to the atomic and electronic level [2]. The variety of models
includes finite element modelling (FEM), crystal plasticity (CP) modelling, phase

Fig. 8.1 Integrated computational materials engineering. a Four-element paradigm of modern


Materials Science and Engineering, b top-down approach for structure–property relationship in the
field of plasticity of metallic materials. Modified according to [2, 3], respectively. Permission of
Science and Elsevier, respectively
370 8 Prospects of Complementary In Situ Techniques

field (PF) modelling, discrete dislocation dynamics (DDD) modelling, molecular


dynamic (MD) modelling and density functional theory (DFT) modelling.
In the field of the plasticity of metallic materials, one approach of “top-down”
multiscale modelling related, in particular, to the structure–property relationships
can be described according to McDowell and Dunne [3] starting from models for
macroscale plasticity down to atomistic and/or discrete dislocation dynamic sim-
ulations as illustrated by Fig. 8.1b. As demonstrated by Fig. 8.1b, scale bridging
modelling is based on microstructural data gained by various kinds of experiments
ranging from mechanical testing at a laboratory scale over testing on small-scale
specimens and/or SEM investigations down to TEM studies. Since the invention of
the field of ICME at the beginning of the year 2000 many examples for multiscale
modelling has been developed. In the following, some of them, in particular, in the
field of plasticity of metallic materials, will be reviewed.
McDowell and Dunne [3] had chosen the nucleation of a fatigue crack in a
polycrystalline metallic material as an example for multiscale modelling corrobo-
rated by numerous experimental investigations on different length scales. The
described approach is, however, valid for any other phenomenon in metals plas-
ticity. Therefore, in the following four examples of multiscale modelling approa-
ches related to the aim of ICME will be discussed, in order to demonstrate the broad
variety of multiscale modelling approaches.
Quite recently, Tasan et al. [4] offered a novel integrative experimental-
numerical approach in the field of metals plasticity for analysing stress and strain
partitioning in a complex multiphase steel (DP steel). They showed that the com-
bination of in situ deformation in SEM with EBSD, DIC and FIB contributed in a
substantial manner to the creation of physically based models in Düsseldorf
Advanced Materials Simulation Kit (DAMASK) [5] describing the stress and strain
partitioning during plastic deformation. On the other side, local strain and stress
distributions were revealed from two-dimensional full-field CP simulations. These
simulations were corroborated by additional inverse simulations of nanoindentation
measurements of the initial microstructure.
Song et al. [6] used various simulation models such as ab initio calculations and
phase field modelling in combination with advanced characterization techniques
such as atom probe tomography (APT) and TEM for an improved understanding of
the formation of bainite in 100Cr6. It was shown that both carbon partitioning and
carbon trapping within bainite ferrite has to be taken into account for bainite
transformation simulations.
Prahl et al. [7] and Song et al. [8] demonstrated a guided design of new
iron-based materials enabling for TRIP or TWIP effect using quantum mechanics.
Applying CALPHAD software and ab initio calculations, composition-dependent
SFE maps were calculated, which facilitated the prediction of deformation mech-
anisms. Moreover, a new Fe–Mn–Al–C steel alloy was designed containing kappa
carbide precipitates enabling for pronounced strengthening at concurrent excellent
ductility.
The topic of strain localization in heterogeneous cast iron during fatigue and its
implementation in a three-dimensional multiscale simulation at a structural scale
8.2 Complementary In Situ Techniques and Microstructural-Based Modelling 371

was demonstrated by Salomonsson and Olofsson [9]. Here, the microstructural


features of cast iron with different graphite morphologies were analysed using µCT,
which served for three-dimensional modelling. The aim of these studies was to
obtain a deeper understanding of the effect of graphite morphology under similar
cyclic loading conditions. It was shown that strain localizations are more pro-
nounced in case of spherical graphite compared to vermicular or lamellar graphite.
In the context of the discussed examples, it turned out that the complementary
in situ techniques applied at microscopic and macroscopic length scales demon-
strated by the present work are also useful for the implementation in the framework
of multiscale modelling of plasticity and damage behaviour of various kinds of
materials. Therefore, in the following sections, the high potential of complementary
in situ techniques for studying different metal plasticity phenomena in terms of
strain localizations and time sequence of deformation mechanisms will be explained
on four different examples: (i) modelling of strain-hardening behaviour of TRIP/
TWIP steels, (ii) damage behaviour of TRIP matrix composites, (iii) deformation
and damage behaviour of laminated TRIP/TWIP steels and (iv) mechanical beha-
viour of shape memory alloys. Example (i) deals still with the modelling of the
strain-hardening behaviour of the previously described class of high-alloy CrMnNi
TRIP/TWIP steels and how the presented in situ techniques can serve to this
modelling. Example (ii) shows the potential for studying the damage behaviour of
metal matrix composites, in particular, to TRIP matrix composites. In example (iii),
the applicability for studies on the improved damage behaviour of metallic com-
posite laminates is described. Finally, example (iv) illustrates that these techniques
have also a high potential for investigations on other materials with similar effects
of strain localizations caused by martensitic phase transformation such as shape
memory alloys.

8.3 Example 1: Modelling of Strain-Hardening Behaviour


of CrMnNi TRIP/TWIP Steels

The strain-hardening behaviour of TRIP/TWIP steels is in the focus of modelling


activities since several decades. Different approaches ranging from phenomeno-
logical up to micromechanical modelling are available in literature. The main goal
of development of a microstructural parameter-driven model is its applicability for
low-carbon, high-alloy CrMnNi TRIP/TWIP steels in a wide range of austenite
stability and stacking-fault energy. Therefore, a model should be developed
describing the influence of various parameters such as chemical composition,
deformation temperature and strain rate as well as grain size and grain orientation
on the behaviour of these steels under tensile loading conditions. Figure 8.2 shows
schematically, how different in situ techniques together with further characterization
techniques can contribute to achieve the final goal of this modelling.
372 8 Prospects of Complementary In Situ Techniques

Fig. 8.2 Contributions of complementary in situ characterization techniques to the microstruc-


tural parameter-based modelling of the strain-hardening behaviour of TRIP/TWIP steels [10]

Since the steel with the highest austenite stability exhibits only two dominant
deformation mechanisms—dislocation glide and formation of stacking-fault-
mediated twins—the model should be developed first for this steel variant. After
successful implementation of the developed model for description of the strain-
hardening behaviour of TWIP steels, the model can be adapted also for describing
the influence of chemical composition, temperature or strain rate on the material
behaviour as demonstrated by Fig. 8.2.
Most promising model candidate for adaption to present studied high-alloy
CrMnNi TWIP steels is the constitutive model description by Kim, Lee and Estrin
presented already in Sect. 4.2.3. The modelling is based on a rule of mixture
describing both the global stress as well as the evolution of dislocation density
related to grains without deformation twins (twin-free) and grains containing
deformation twins (twinned). Moreover, in twinned grains, the volume fraction of
twins and the twin spacing—both depending on the applied strain level as well as
on the initial grain orientation—have to be taken into account. These microstruc-
tural parameters can be provided by results from EBSD measurements (grain size,
grain orientation, fraction of grains with and without twins and twin spacing), from
8.3 Example 1: Modelling of Strain Hardening Behaviour … 373

ECCI investigation (arrangements of dislocations and stacking faults) at small


strains, from XRD measurements (line broadening and peak shift) as well as from
TEM investigations (interaction of individual defects). Furthermore, SEM-DIC can
provide information on strain localization depending on applied strain and indi-
vidual grain orientation. On macroscopic scale, tensile tests at different strain rates
can be corroborated by DIC measurements using video extensometer providing
macroscopic strain localizations (e.g. during necking) as well as AE measurements
providing threshold values (stress or strain) for the onset of twinning as well as the
temporal evolution of twin related cluster of AE signals. In best case, the formation
of twins on primary and secondary systems can be extracted.
However, the most crucial point here is the experimental determination of vol-
ume fraction of twins. It is quite sophisticated due to the fact that tiny micro or even
nanotwins are sometimes below the resolution threshold of EBSD measurements.
Therefore, one possibility to gain information on twinned volume fraction in
dependence on applied strain can be obtained via XRD line profile measurements.
One parameter obtained from line profile analysis beside the microstrain is the
so-called stacking fault probability. Since twin bundles formed during plastic
deformation of steel Fe–16Cr–6Mn–9Ni–0.05C can be regarded as stacking-fault-
mediated twins, the stacking fault probability P can be used in order to describe the
evolution of twinned volume fraction at small strain levels applied. An increase in
stacking fault density depending on applied strain level yields besides a broadening
of the diffraction peaks a shift of peak positions of XRD line profiles. Furthermore,
the arrangement and the density of SFs have an influence on the peak symmetry as
well as peak intensity (cf. [11]). Here, the acoustic emission measurements can used
to corroborate the results from the XRD line profile analysis. AE provides the
temporal evolution of cumulated AE energy of cluster related to partial dislocations
(or stacking fault bands or twin bundles). However, the AE does not provide any
absolute values of the volume fraction of twin bundles. Nevertheless, in case of a
good correlation of evolution of stacking fault probability and temporal evolution of
AE energy of twin related cluster at low strain levels, the information from AE
measurements can be used to model the evolution of stacking fault probability at
higher strain levels. Moreover, AE can definitely provide the threshold parameter
for the onset of twinning related to the investigated grain size.
In order to obtain microstructural parameters necessary for the modelling of
strain-hardening behaviour of TWIP steels, small-scale deformation experiments
will be performed on steel Fe–16Cr–6Mn–9Ni–0.05C manufactured by field
assisted sintering (FAST) with mean grain size of about 15 µm [10]. Tensile tests
will be performed up to different strain levels accompanied by strain measurements
via video extensometer (VEDDAC) and AE measurements. Microstructure before
and after testing has to be analysed by both EBSD measurements (grain size, grain
orientation, texture and spacing of twin bundles) and XRD line profile analysis
(microstrain and stacking fault probability). In addition, ECCI can be applied at low
strain levels.
374 8 Prospects of Complementary In Situ Techniques

8.3.1 Orientation Dependence of Deformation Mechanisms


Detected by AE

Acoustic emission measurements applied on CrMnNi TRIP/TWIP steels with


as-cast microstructure revealed clear time sequence of the onset and evolution of
individual deformation mechanisms characteristic for certain austenite stability and
stacking-fault energy. Furthermore, the change in time sequence with variation of
temperature was followed as well. Biggest advantages of AE measurements are
their high-time resolution as well as their volume integrating character. Whereas
SEM-DIC provides only 2D surface information in a very limited AOI, AE is
sensitive to all processes in bulk specimens. Therefore, AE is also very sensitive for
the onset of individual deformation mechanisms. It was shown for example in
Sect. 7.3 that AE used for the determination of the critical strain for the onset of
PLC effect during macroscopic tensile tests revealed always the lowest critical
strain compared to other methods applied such as thermography or from serrations
in the stress-strain curve. This means AE detects the earliest beginning of an
individual deformation mechanism in well-oriented grains. Moreover, it was
demonstrated that the transition in deformation mechanisms from MPT towards
stacking-fault-mediated twinning due to an increase in temperature was affirmed by
AE measurements regarding the threshold for the onset of MPT or twinning.
However, in all cases, the results of the AE data analysis in terms of clustering
algorithm according to specific AE parameters such as AE energy or median fre-
quency were corroborated post mortem by intensive microstructural investigations
using mostly EBSD or ECCI.
In order to convince researchers of the Materials Science and Engineering
community that acoustic emission measurements are capable to separate individual
AE sources related to different microstructural processes, investigations on the
influence of grain orientation on the AE activity during small-scale testing can be
performed. Furthermore, in order to bridge the gap between real-time in situ AE
measurements and post-mortem microstructural investigations, two possible
approaches can be followed.
The first approach is the combined application of AE and quasi in situ SEM
deformation. The quasi in situ testing can be combined either with EBSD mea-
surements providing orientation changes or phase transformations or with capturing
of high-resolution SEM images for DIC providing information on strain localiza-
tions. Providing information on time sequence of deformation mechanisms an AE
sensor has to be adopted to the in situ loading stage. The application of AE sensor
during in situ SEM deformations is related to a higher background noise due to
vacuum pump, etc. Nevertheless, in case of coarse-grained microstructure, the
overall AE activity is significantly larger than background noise. Due to the fact that
quasi in situ tests were performed in well-defined deformation intervals allowing for
EBSD scans or image capture, a good synchronization between load signal and AE
data stream is necessary, which is achieved by coupling the load signal and the AE
signal via the parametric channel on the AE data requisition board. This approach
8.3 Example 1: Modelling of Strain Hardening Behaviour … 375

would be most suitable for the investigation on single crystals with different ori-
entations or oligocrystalline materials with only few grains of different orientations
within the AOI (see Sect. 8.3.2).
The second approach is the investigation of AE depending on grain orientation
during very local plastic deformation such as obtained during scratch testing or
hardness measurements (indentation). This approach has the advantage that the
involved volume is limited to the occurring plastic zone, which is definitely below
the grain diameter. Thus, the direct correlation between AE signals and
microstructure is given. However, due to the small involved specimen volume the
overall AE activity is quite low and it can be a challenging task to separate them
from the electrical background noise.
However, such investigations were performed already by Danjuk et al. [12] for
coarse-grained, well-annealed polycrystalline copper. It was shown that the acti-
vation of dislocation slip could be detected by AE emission in dependence on the
individual grain orientation. However, a special “denoising” technique had to be
developed for subtracting the continuous signal related to dislocation glide from the
background noise.
Similar investigations are already in progress for CrMnNi TRIP/TWIP steels
with coarse-grained microstructure [13]. Thus, scratch tests were performed on
pre-characterized specimens with well-known grain orientations. First promising
results were obtained already for steel with 6 wt% Ni. Here, different AE activities
related to individual deformation mechanisms were identified depending on grain
orientation as shown by Fig. 8.3. Thus, whereas grains 1–4 exhibit a high AE
activity by pronounced transient signals with high amplitudes, the AE activity
occurring in grain 5 was quite low. The cluster analysis revealed that signals
occurring in grains 1–4 were caused by the formation of stacking fault bands and
a′-martensite, the lower activity in grain 5 is related to movement of regular
dislocations.
In analogy to scratch tests, the application of AE during indentation (hardness
measurements) is also conceivable. Such investigations were performed already for
various kinds of ceramic materials. Faisal et al. [14] gave a comprehensive over-
view on AE application during indentation experiments. However, since the stress
state below the indenter during both scratch test as well as microhardness mea-
surements are quite complex, these investigations have to be corroborated by
numerical simulations.

8.3.2 Strain Localizations Across the Length Scale


of Microstructure

In order to understand the influence of grain size on strain localization as well as


time sequence of deformation processes, investigations of these phenomena on
different length scales of the microstructure have to be performed. Section 7.2
376 8 Prospects of Complementary In Situ Techniques

Fig. 8.3 Correlation of AE with the grain orientation of a Fe–16Cr–6Mn–6Ni–0.05C steel during
scratch test using Vickers indenter at 1 N applied load. a Complete AE data stream with indicated
start and finish of the scratch, b scratch together with microstructure shown in terms of IPF
colouring according to the scratch direction, c correlation with the temporal evolution of AE
clusters identified from AE stream. Grain orientations are given in IPF colour code with respect to
the scratch direction [13]
8.3 Example 1: Modelling of Strain Hardening Behaviour … 377

demonstrated well that strain localizations occurring during tensile deformation in


high-alloy CrMnNi steels enabling TRIP and/or TWIP effect can be characterized at
a submicron resolution using DIC. Furthermore, the change of deformation
mechanisms as a function of temperature was analysed well by application both of
AE measurement technique as well as DIC. In addition, all in situ measurements
were corroborated by detailed microstructure investigations before and/or after
in situ testing using different methods such as EBSD, ECCI, TEM or t-SEM. All
methods were well established for coarse-grained as-cast microstructure.
As a next step, the combined application of the high-resolution SEM-DIC and
the volume integrative AE method to all dimensions across the length scale of
microstructure as illustrated by Fig. 8.4 is promising in order to serve for scale
bridging modelling. Thus, testing material is produced by different processing
routes based on the chemical concept of the high-alloy CrMnNi TRIP/TWIP steels:
Single crystalline material for steels Fe–16Cr–6Mn–6Ni–0.05C and Fe–16Cr–
6Mn–9Ni–0.05C was manufactured by Bridgman method (Doncasters, Bochum,
Germany). The crystal rods had dimensions of 100–150 mm in length and 12 mm
in diameter. However, the obtained crystal rods were not perfectly single crys-
talline. For the steel with 6% nickel this is caused by the ferritic solidification.
Therefore, a certain amount of d-ferrite is present in the microstructure. In addition,
the microstructure of both steel variants is characterized by a pronounced subgrain
structure.

Fig. 8.4 Experimental approach for investigations of the influence of grain size and orientation on
temporal evolution of deformation mechanisms, strain localizations and local hardening
378 8 Prospects of Complementary In Situ Techniques

Therefore, a small-scale specimen geometry [15], but still in the range of mil-
limetres, was developed allowing for the preparation of different crystallographic
orientations or specimens with oligocrystals for performing in situ SEM investi-
gations in combination with DIC, EBSD and AE.
Fine-grained material with a mean grain size of 15–25 µm can be manufactured
based on a powder metallurgical route followed by field assisted sintering (FAST)
technology or by hot pressing (HP). The ultrafine-grained microstructure is
obtained by thermomechanical treatment in terms of cold rolling followed by
subsequent reversion annealing [16]. Here, the grain size of <1 µm can be reached.
The reduction of grain size bears some difficulties for both techniques—DIC and
AE. Since the reduction of grain size results in a reduction of the mean free path of
dislocations DIC and AE will reach their limitations for ultrafine-grained
microstructures.
A first promising example of DIC applied on in situ tensile testing of HP steel
Fe–16Cr–6Mn–6Ni–0.05C up to e = 15% is shown in Fig. 8.5 [17]. It is clearly
visible both from local strain fields according to Von Mises equivalent strain
(Fig. 8.5a) and EBSD measurements (Fig. 8.5b) that strain localizations occur also
in the fine-grained microstructure related to deformation bands with hex crystal
lattice. However, the developed deformation bands are much smaller than in
coarse-grained as-cast microstructure. Therefore, formed a′-martensite grains are
even smaller and not resolvable at the used resolution as for thicker bands in as-cast
microstructure. However, strain evolution as well as evolution of MPT differs
significantly for grains with different orientations (Fig. 8.5c).

Fig. 8.5 Strain localizations and MPT in a fine-grained microstructure of a hot-pressed Fe–16Cr–
6Mn–6Ni–0.05C steel after tensile deformation up to 15% of global applied strain. a Local strain
field in terms of Von Mises equivalent strain with indicated grain boundaries, b phase map from
EBSD measurements showing stacking fault deformation bands and a’-martensite grains,
c crystallographic orientation map using inverse pole figure colour code with respect to the loading
axis (horizontal) [17]
8.4 Example 2: Damage Behaviour of TRIP Matrix Composites 379

8.4 Example 2: Damage Behaviour of TRIP Matrix


Composites

The CrMnNi TRIP steels with medium and low austenite stability serve as matrix
material for a new class of metal matrix composites—the TRIP matrix composites.
These composites are based on TRIP effect of the austenitic steel matrix and an
additional phase transformation of the ceramic reinforcement leading to more
damage tolerant composite material. The ceramic reinforcement is of MgO partially
stabilized ZrO2 (Mg-PSZ), which undergoes a stress-assisted martensitic phase
transformation from tetragonal to monocline crystal lattice both during compressive
[18] as well as cyclic loading [19] accompanied by a volume dilation. These TRIP
matrix composites can be manufactured by powder metallurgical route followed by
classical sintering procedure [20] or FAST [21].
The deformation and damage behaviour of these TRIP matrix composite
materials can be investigated as well using in situ tests in SEM in combination with
DIC and/or AE. However, the application of both techniques bears some challenges
regarding different aspects. First of all, the most critical problem up to now is the
interface between steel matrix and ceramic reinforcement, which has some limi-
tations, in particular, under tensile and/or cyclic loading conditions. However,
beside this fact, the composite nature of metallic matrix and ceramic reinforcement
produces some difficulties for the application of DIC and AE. In particular, in case
of DIC, the contrast pattering at the surface is challenging. The etching technique
applied for the steel matrix is not useful at all, since the interface between steel and
ceramic particles will be attacked by the etching solvent leading most probably to a
degradation of the interface behaviour. Here, good solution for pattering at the
surface, eventually by SiO2 or graphite particles has to be found.
However, the first DIC results on steel Fe–16Cr–6Mn–6Ni–0.05C with 10 vol.%
of ZrO2 particles are quite promising for detection of strain localisations at interface
steel/ceramic leading to delamination as shown by Fig. 8.6 [22]. Both the SEM
images as well as the results of DIC in terms of Von Mises equivalent strain reveal
clearly that first damage at the steel/ceramic interface occurs already at 1% of
elongation (marked by black arrows) followed by martensitic phase transformation
in steel grains (marked by white arrows) corroborated by post-mortem EBSD
measurements. At an elongation of about 3.5% certain extend of steel/ceramic
interface boundaries has been damaged and individual short cracks are grown
together leading to final failure of the specimen (outside AOI).
The application of AE measurements to TRIP steel composites is complicated by
the fact that in addition to the deformation mechanisms occurring in the steel matrix
the deformation mechanisms occurring in the ceramic reinforcement as well as the
damage behaviour of the composite material act as sources for acoustic emission
and has to be separated from each other. In total at least seven different sources for
acoustic emission beside the background noise level have to be distinguished and
interpreted: (i) dislocation glide, (ii) formation of stacking fault bands, (iii) forma-
tion of stacking-fault-mediated twin bundles, (iv) formation of a’-martensite,
380 8 Prospects of Complementary In Situ Techniques

Fig. 8.6 Results of SEM-DIC obtained on TRIP matrix composite after tensile deformation at RT
up to 4% global applied strain. Fe–16Cr–6Mn–6Ni–0.05C with 10% Mg-PSZ [22]. Loading axis
horizontal

(iv) MPT of zirconia, (v) particle fracture, (vi) delamination and (vii) crack initi-
ation and growth. The deformation mechanisms in TRIP steel are already
well-understood as shown by results described in Sect. 7.3. For the sake of sim-
plicity and to learn more about the stress-assisted martensitic phase transformation
of zirconia, compressive tests were performed on ceramic material. From literature
data, it is well-know that this phase transformation occurs at compressive stress
levels well above 1 GPa. For this purpose, the in situ loading stage of Kammrath
and Weiss was modified for compression tests. Here, the gripping system for
microtensile specimens was replaced by two plungers made of high-strength steel
with glued in tungsten-carbide hard metal plates. The modified loading stage was
then used ex situ in combination with a video extensometer based on DIC in
combination with a compucentric optic supported by ring illumination [23]. First,
interrupted compression test on small ZrO2 cube with a cross-section of 2  4 mm2
were performed up to 2 GPa with partial unloading at 1.2, 1.4, 1.6 and 1.8 GPa. AE
sensor was fixed by a mechanical clamp on one plunger of the setup. Recorded AE
data streams revealed clearly increasing AE activity with increasing stress level.
First promising AE data analysis [24] showed a clear tendency of the evolution of at
least two clusters beside the background noise, which can be most probably
attributed to crack initiation and martensitic phase transformation. However, these
findings still have to be corroborated by XRD phase analysis as well as SEM
8.4 Example 2: Damage Behaviour of TRIP Matrix Composites 381

investigations including EBSD measurements. However, after gaining knowledge


about the AE sources related to crack initiation and martensitic phase transforma-
tion in the pure ceramic materials, the next step can be done to investigate and to
understand the damage behaviour of the TRIP matrix composites [24].
The TRIP matrix composites based on TRIP steels as metallic matrix and zir-
conia particles as reinforcement is only one example of composite materials, which
can be analysed and investigated by the described complementary in situ tech-
niques. Thus, the transfer of these approaches to other types of composite materials
such as light-weight metal composites (e.g. aluminium MMC etc.) is conceivable.

8.5 Example 3: Deformation and Damage Behaviour


of Laminated TRIP/TWIP Composites

Composite materials in terms of laminates produced by accumulative roll bonding


(ARB) offer a high potential for improvement of mechanical behaviour, in partic-
ular, under cyclic loading conditions, as well as of damage tolerance due to change
in damage mechanisms. The concept of metal laminate composites dates back to the
ancient Greece. Thus, the shield of Achilles was already made as a laminate
composite consisting of five alternating layers of Bronze, Tin and Gold. Also, the
examples of Damascene steel or Japanese art of forging by the blacksmith can be
correlated to the material class of metal laminate composites. Main advantages of
metal laminate composites can be summarized as follows: (i) improvement of
strength and ductility for laminates with layer thickness below 1 mm, (ii) im-
provement of fracture toughness of metallic materials both with ductile and brittle
deformation behaviour, (iii) improvement of energy absorption during dynamic
loading and (iv) enhancement of fatigue life due to reduction of crack growth rate.
The new class of metal laminates ranges from Cu–Al laminates (e.g. [25]) over Ti–
Al laminates (e.g. [26]) or laminates of different types of aluminium alloys (e.g.
[27]) up to few examples for steel laminates (e.g. [28–31]).
The studied CrMnNi TRIP/TWIP steels seem to be also good candidates for
metal laminate composites. The different strengthening behaviour of both steel
variants in combination with different adjusted grain sizes could lead to tailored
mechanical properties both under static monotonic as well as cyclic loading. Quite
recently, the accumulated roll bonding process has been already successfully
adopted to produce two-layered TRIP/TRIP, TWIP/TWIP and TRIP/TWIP lami-
nate composites [32].
The methods of DIC and AE offer a great potential for the investigation of both
the strain localization phenomena as well as the damage behaviour in TRIP/TWIP
laminated composite materials. AE can be used in order to evaluate the delami-
nation and crack initiation at the interface between individual steel layers alongside
with the already well-known deformation mechanisms. In addition, in situ tensile or
382 8 Prospects of Complementary In Situ Techniques

cyclic loading as well as bending tests in SEM in combination with DIC and EBSD
can be used to analyse possible strain localizations at the interface leading to
debonding or crack brunching.

8.6 Example 4: Shape Memory Materials

Shape memory materials (SMMs) are class of materials, “… which have the ability to
‘memorise’ or retain their previous form when subjected to certain stimulus such as
thermomechanical or magnetic variations.” Jani et al. [33]—known as the shape
memory effect (SME) discovered by Buehler et al. in 1962 on a titanium-nickel alloy.
SME occurs in broad variety of materials including (i) metals, (ii) polymers and
(iii) ceramics. The group of metals enabling SME consists of shape memory alloys
based on (i) NiTi alloys, (ii) copper alloys (CuZn, CuZnAl, CuAlNi), (iii) iron-based
alloys (FePt, FeMnSi, FeNiC), (iv) Ag-based, (v) Au-based or (vi) Co-based.
Furthermore, this group includes magnetic and ferromagnetic shape memory alloys
(e.g. NiMnGa, CoNiGa) as well as high-temperature SMA (e.g. TiMo, TiNb, TiTa).
The application of SMA alloys is manifold due to their unique behaviour and out-
standing properties including (i) automotive, (ii) aerospace, (iii) biomedical,
(iv) robotics and (v) electric (MEMS) applications. A comprehensive review on
research, applications and opportunities of shape memory alloys was given quite
recently by Jani et al. [33].
The shape memory effect is comparable to martensitic phase transformation (see
Sect. 3.1). Thus, austenite is the high-temperature phase and martensite the
low-temperature phase. The shape memory effect can be described by following
steps: (i) transformation from martensite to austenite during heating of SMA (cf.
Fig. 3.3: As , Af ) and (ii) backward transformation from austenite to martensite
during cooling according to Ms and Mf temperature (cf. Fig. 3.3). The transfor-
mation from martensite to austenite is accompanied by a volume contraction and
vice versa from austenite to martensite by a volume dilation leading the recovery of
the original shape of the SMA. The shape memory effect can be subdivided into
three categories: (i) one-way SME, (ii) two-way SME and (iii) pseudoelasticity or
superelasticity [33].
The ongoing microstructural process during SME is comparable to that one
known from the martensitic phase transformation in steels. Therefore, SMA alloys
are also good candidates for the combination of the complementary in situ tech-
niques such as digital image correlation, thermography and acoustic emission. The
reversible martensitic phase transformation under different loading conditions is
accompanied both by pronounced strain localizations as well as temperature fields.
This was already demonstrated in the past on different SMA systems by either
IR-TG or in combination with DIC. Favier et al. [34] presented an example of
fully-coupled full-field measurements on thin tube of NiTi SMA allowing for the
analysis of coupling effects occurring during stress-assisted MPT. Delpuyeo et al.
[35] performed thermographic measurements on a Cu–Al–Be SMA exhibiting a
8.6 Example 4: Shape Memory Materials 383

pseudoelastic response at RT. The infrared thermograms were used to determine


maps of heat sources occurring due to MPT as well as maps of amplitudes of
temperature oscillations. By this approach, it was possible to address two ther-
mocouplings occurring in these SMAs: (i) thermoelastic coupling in the austenite
and (ii) the coupling caused by the MPT resulting from the cyclic movement of the
austenite-martensite interface. Pieczyska et al. [36] demonstrated on NiTi SMA
during tensile cyclic loading the formation of exothermic and endothermic
martensitic bands occurring during forward and backward transformation,
respectively.
On the other hand, acoustic emission measurements could provide additional
information on the temporal evolution of the MPT during cyclic loading in
dependence on the number of cycles applied. Furthermore, other microstructural
mechanisms such as dislocation motion could be detected and analysed. Thus, AE
measurements performed by Bonnon et al. [37] on Cu–Zn–Al SMA single crystals
revealed a direct correlation between the acoustic emission activities and the for-
mation and propagation of thin needle domains growing parallel to the transfor-
mation front of the stress-assisted MPT. It was assumed that the acoustic emission
is caused by the interaction of dislocations with the single martensite variant.
Promising candidates for application of the complementary in situ techniques
DIC, TG and AE are NiTi, Cu-based, Co-based or Fe-based SMAs. Thus,
fully-coupled full-field DIC and thermography investigations can be used in order
to understand thermomechanical coupling both in austenite (thermoelastic) as well
as caused by the MPT. The simultaneously recorded AE data stream will discover
the onset of MPT, dislocation interaction as well as load history-dependent effects.

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Chapter 9
Concluding Remarks

The present work is concerned with the application of complementary in situ


characterization techniques for the improvement of the knowledge of microscopic
and macroscopic strain localizations as well as on the time sequence of specific
deformation processes on a class of modern low-carbon, high-alloy CrMnNi cast
steels enabling TRIP and/or TWIP effect. The overview of different types of in situ
techniques, which are suitable for the investigations of these phenomena, provided
an insight into the state of the art of the application of these techniques for the
characterization of materials.
Out of the large variety of in situ experiments, two imaging-based methods—
in situ testing in the scanning electron microscope corroborated by digital image
correlation and infrared thermography—as well as the time- and frequency-
domain-based method of acoustic emission measurements were chosen for the
characterization of microstructure–property relationships.
Thorough microstructural investigations using different methods of scanning
electron microscopy and their combination with in situ investigation techniques led
to a comprehensive description of deformation processes and their time sequence in
low-carbon, high-alloy Fe–16Cr–6Mn–xNi–0.05C cast TRIP/TWIP steels as a
function of the chemical composition and the deformation temperature.
For the first time, the applied SEM-DIC technique allowed a sub-micrometre
resolution in the range of 500 nm. The sub-micrometre resolution enabled the cal-
culation of the magnitude of shear for stacking fault bands, twin bundles and a′-
martensite grains. In addition, for the first time the magnitude of shear of a′-martensite
grains was determined experimentally. Furthermore, the activation of different vari-
ants of a′-martensite during tensile and compressive half-cycle loading was shown
and corroborated by thorough variant and slip system analysis. Moreover, the
self-accommodation by the activation of twin-oriented a′-martensite variants was
experimentally proofed using the subµSEM-DIC in cyclic loading experiments.
Similarly, for the first time, the application of the AE measurements during
tensile loading allowed the separation of the individual deformation mechanisms
such as (i) dislocation glide, (ii) partial-dislocation mediated stacking fault bands
© Springer Nature Switzerland AG 2020 385
A. Weidner, Deformation Processes in TRIP/TWIP Steels,
Springer Series in Materials Science 295,
https://doi.org/10.1007/978-3-030-37149-4_9
386 9 Concluding Remarks

and/or twinning and (iii) the martensitic phase transformation. The application of
the cluster algorithm allowed to follow the time sequence of these different
mechanisms. Moreover, it is shown that the temporal evolution of the cluster related
to the martensitic phase transformation revealed an excellent agreement with the
evolution of the martensitic volume fraction according to both experimental fer-
romagnetic measurements as well as to Olson–Cohen model.
The application of fully-coupled full-field measurements—infrared thermogra-
phy and digital image correlation based on optical microscopy—corroborated by
acoustic emission measurements allowed the investigation of propagating macro-
scopic strain localizations in terms of Portevin–Le Chatelier (PLC) effect. It was
shown that the macroscopic strain localizations were well characterized and anal-
ysed by both full-field measurement techniques. A good correlation of temperature
fields and local strain fields was obtained, which allowed the determination of
characteristic parameters for the evolution and propagation of the PLC bands.
Therefore, the combination of these techniques provided information on the origin
of the PLC effect in this type of austenitic stainless steels.
Along with the above-described aspects, the following further conclusions are
drawn:
(1) Dislocation glide, the formation of stacking-fault-mediated bands (hex) and/or
twin bundles and martensitic phase transformation are identified as the dominant
deformation mechanisms in high-alloy Fe–16Cr–6Mn–xNi–0.05C steels with
different austenite stabilities.
(2) Depending on the nominal chemical composition, these mechanisms lead to
either TRIP effect in steels with low austenite stability or TWIP effect in steels
with high austenite stability. Steels with intermediate austenite stability exhibit
combined TRIP/TWIP effects as a function of the deformation temperature.
(3) The TRIP effect is related to the martensitic phase transformation of meta-
stable fcc austenite into bcc a′-martensite. The phase transformation proceeds
via an intermediate state characterized by the formation of stacking-fault-
mediated bands. These stacking-fault-mediated bands with a hex crystal lattice
are found during plastic deformation of austenitic steel with low and medium
austenite stability. The nature of the hex crystal lattice within these bands is
due to the high density of stacking faults, which are arranged on in average
every second lattice plane. Preferred places for the nucleation of a′-martensite
are either points of intersection of stacking fault bands or even intersections of
individual stacking faults formed on different slip planes.
(4) The TWIP effect is caused by deformation-induced twinning. Both the faulted
austenite as well as the microtwins are formed by stacking faults and occur
simultaneously within the microstructure with different intensities depending
on local chemical composition, applied strain level as well as applied defor-
mation temperature.
(5) The density of deformation bands (DBs) as well as their thickness increase
significantly with increasing strain and saturate at high strain levels. At
intermediate strain levels, the formation of a′-martensite grains occurs within
9 Concluding Remarks 387

DBs. Thus, the volume fraction of the hex crystal lattice (stacking fault bands)
evolves to a maximum at medium strain levels followed by decay, whereas the
volume fraction of a′-martensite increases continuously.
(6) The strain is localized inside these deformation bands. Whereas the stacking
fault bands and the twin bundles exhibit a uniform strain distribution, a′-
martensite grains yield locally increased strain values. With a value of 0.3, the
calculated magnitude of shear within the stacking fault bands is comparable to
the theoretically calculated value of 0.35 for partial dislocations a6 112. The
magnitude of shear calculated from the digital image correlation (DIC) results
for twin bundles is close to the expected theoretical value of 0.7. However, the
high magnitude of shear is evaluated only for the thicker twin bundles, which
is correlated to the limited resolution for twins smaller than 1 µm. The
magnitude of shear of a′-martensite grains in the studied x–y plane depends
strongly on their crystallographic orientation. With a range of 0.6 to 0.7, the
maximum calculated magnitude of shear of a′-martensite is, therefore, com-
parable to value for mechanical twinning.
(7) The applied method of digital image correlation in combination with in situ
deformation in the SEM—so-called SEM-DIC—provides an excellent resolu-
tion. Thus, strain localizations within deformation bands with a thickness of less
than 500 nm were identified, and even small individual martensitic variants
(  1 µm) were distinguished regarding their individual shear strain values.
(8) Both the deformation bands consisting of stacking faults and/or twins and the
a′-martensite grains yield a fragmentation of the austenitic grain structure.
Thus, the stacking fault bands or twin bundles, which belong to the primary
activated slip or twinning systems, reduce the mean free path of dislocations
for the formation of DBs on secondary systems. A further reduction of the
mean free path of dislocations within the DBs is caused by the formation of a′-
martensite grains. These martensitic grains act as obstacles to the motion of
partial dislocations. Thus, they contribute significantly to a pronounced strain
hardening. The contribution of fragmentation due to deformation bands is,
however, less pronounced.
(9) The application of SEM-DIC to cyclic deformation experiments in combina-
tion with detailed slip trace and variant selection analyses allowed a distinction
of a′-martensite transformation occurring either during the tension half-cycle
or the compression half-cycle loading. A self-accommodation of individual
martensite variants formed during the cyclic loading was observed. Resulting
strain fields were interpreted for specific grain configurations.
(10) The time sequence of ongoing deformation processes was analysed using
acoustic emission measurements. An increase in twinning activity was
observed with increasing temperature and increase in the austenite stability.
Concurrently, a decrease in the volume fraction of a′-martensite was detected
along with a shift of the onset of a′-martensite formation to higher strain
levels. Regular dislocation motion was present over the entire deformation
process.
388 9 Concluding Remarks

(11) The high potential of the acoustic emission measurements as a real-time and
volume integrating method for the characterization of the time sequence of
individual deformation processes was demonstrated both regarding the evo-
lution of the volume fraction of a′-martensite or twinned volume fraction as
well as describing the onset of serrated plastic flow.
(12) Fully-coupled full-field measurements in combination with acoustic emission
measurements were applied for the investigation of macroscopic strain
localization in terms of serrated plastic flow. The coupling between local strain
and local temperature fields resulted in the determination of specific param-
eters of developed PLC bands. Thus, the origin of the PLC effect in the
metastable Fe–16Cr–6Mn–3Ni–0.05C steel with the lowest austenite stability
was determined via the calculation of the activation energy of the diffusion of
interstitials in the bcc phases of this steel variant.
The great potential of the applied in situ characterization techniques is their
complementarity, as it turned out, in particular, from the three case studies
described in Sect. 7. Only the combination of these different techniques—such as
the in situ deformation within the SEM combined with the digital image correlation
—enabled the deeper understanding of the strain fields caused by the formation of
stacking-fault-mediated bands, twin bundles or martensitic phase transformation.
Similarly, these complementary in situ techniques have a great potential to con-
tribute to the modelling of the deformation behaviour of TRIP/TWIP steels, in
particular, or for any other kind of materials with complex deformation processes.
In particular, here the acoustic emission measurements offer a great potential, since
this is the only real-time in situ characterization technique delivering bulk infor-
mation with a time resolution in the range of microseconds. The application of
complementary in situ techniques with high lateral resolution (e.g. subµDIC) in the
SEM and high temporal resolution in combination with integral volume information
(AE) provides an excellent tool for the investigation of material behaviour on a
multiscale level from the sub-micrometre scale up to the macroscopic scale.
In future, these complementary in situ characterization techniques can be applied
for investigations on other materials with complex deformation mechanisms
including (martensitic) phase transformation and/or twinning. In particular, the
application to materials such as magnesium or titanium is of high interest, since
these materials exhibit pronounced twinning during plastic deformation. In par-
ticular, different twinning systems are activated under tensile or compressive
loading. Although acoustic emission is already used in order to characterize the
twinning and detwinning, the combination of acoustic emission measurements with
the subµDIC would provide a deeper understanding of the strain fields occurring
during these processes. Therefore, the implementation of the AE measurement
technique inside the SEM will provide further improvements in material charac-
terization under load with concurrently high lateral and temporal resolution.
Appendix

© Springer Nature Switzerland AG 2020 389


A. Weidner, Deformation Processes in TRIP/TWIP Steels,
Springer Series in Materials Science 295,
https://doi.org/10.1007/978-3-030-37149-4
Acoustic emission measurements: State of the art (Table A.1).
390

Table A.1 Overview of AE investigations on metallic materials since 2000 classified according to the field of application
No. Year Author References Material Research Method Topic + outcome
field
1 2002 Chmelik [1] Al-1.5 wt% Mg Plasticity Two-threshold-level AE data acquisition – Lüders band phenomenon and C-type PLC
et al. alloy (continuous signals and burst signals), bands
4 Msamples/s tension tests, RT, laser – Continuous AE signals during Lüders band
extensometer propagation with few burst signals showing
enhanced rise time
2 2002 Bohemen [2] Medium carbon Plasticity Broadband sensor (100–1000 kHz), RMS of – Two peaks in the RMS at 500–600 °C and
et al. steel (C45) continuous signals during continuous cooling 200–300 °C, which are correlated with the
formation of bainite and martensite,
respectively
3 2003 Bohemen [3] Low-alloyed Plasticity Broadband sensor (100–1000 kHz), RMS of – AE power correlates with the volume
et al. steels (C60, C70, continuous signals during continuous cooling fraction of martensite and the
C80) transformation rate
4 2003 Reed et al. [4] Al-Mg alloy Plasticity Threshold-based AE data acquisition, tensile – Type B PLC bands during the entire
(AA5083) test, RT deformation path and at all strain rates
– Low energy AE correlated with isolated
serration peaks
– High energy AE related to anomalies of the
serrations
5 2003 Vinogradov [5] Cu, Cu–Ge alloy Plasticity Continuous AE data acquisition, broadband – Sensitivity of AE to solid solution
et al. GS: 80 µm, sensor (50–1000 kHz), 4 Msamples/s, tensile hardening and SFE
200 µm tests, RT – Twinning and dislocation slip exhibit
distinct features in AE power spectra,
spectral parameters and waveforms
(continued)
Appendix
Table A.1 (continued)
No. Year Author References Material Research Method Topic + outcome
field
Appendix

6 2004 Bohlen et al. [6,7] Mg alloy (AZ31) Plasticity Two-threshold-level-based AE data – Correlation of AE count rates with the
Rolled and heat acquisition, piezo-sensor (100–600 kHz), stress-strain curves revealing maximum of
treated 4 Msamples/s, tensile tests, RT the AE activity close to the macroscopic
yield point followed by a decrease in the
AE activity
7 2006 Bohlen et al. [8] Mg alloy (ZM21, Plasticity Two-threshold-level-based AE data – Deformation asymmetry between tension
ZK30, ZEK100) acquisition, tension and compression tests, and compression for all three alloys
RT – Compression: mainly burst type AE signals
(twinning)
– Tension: simultaneously continuous and
burst signals (dislocation glide + twinning)
8 2006 Mathis et al. [9] Mg alloy (AM60) Plasticity Two-threshold-level-based AE data – Three stages of deformation: primary
acquisition, LB10A sensor (100–500 kHz), twinning, twinning on other systems,
tensile tests, 20–300 °C, OM, TEM dislocation walls
– Maximum of AE activity at 200 °C
– Above 200 °C dislocation glide dominates
9 2007 Bohlen et al. [10] Mg alloy (AZ31, Plasticity Two-threshold-level-based AE data – Tension/compression asymmetry
AZ61, AZ80) acquisition, tension and compression tests, – Decreased by aluminium as alloying
RT element
– Decrease also the AE activity
10 2007 Chmelik [11] Al-3.5 wt% Mg Plasticity Two-threshold-level AE data acquisition – AE peak in the region of Lüders strain
et al. alloy (continuous signals and burst signals), related to strong dislocation multiplication
4 Msamples/s tension tests, RT, laser – Well-separated AE burst signals correlated
extensometer with type A PLC bands
11 2007 Dobron [12] Mg, Mg alloy Plasticity Two-threshold-level-based AE data – Violation of Kaiser effect in pure Mg and
et al. (AZ31, AZ61, acquisition, 4 Msamples/s, interrupted tensile AZ31 indicating activity of microstructural
AZ80) tests with stress relaxation, RT processes during unloading and stress
relaxation
– Stabilization of microstructure by increase
in solute atoms (AZ61 obey Kaiser effect)
391

(continued)
Table A.1 (continued)
392

No. Year Author References Material Research Method Topic + outcome


field
12 2007 Garcia et al. [13] Mg alloy (AZ31) Plasticity Two-threshold-level-based AE data – Increase in AE count rates up to 200 °C due
acquisition, tension and compression tests, to interaction of twin formation, dislocation
RT up to 350 °C, OM glide and recovery
– Above 200 °C decrease in AE count rate
due to dynamic recrystallization
accompanied by softening
13 2007 Janecek [14] Mg alloy (AZ31, Plasticity Two-threshold-level based AE data – Influence of hot-rolling (300 °C) and
et al. hot rolled) acquisition, 4 Msamples/s, tensile tests, RT pre-heating prior to hot-rolling
up to 200 °C, TEM – AE result of interaction of twinning and
PLC effect
14 2007 Li and [15] Mg (99.95%) Plasticity Continuous AE data acquisition, M304A – Tension/compression asymmetry
Enoki GS: 30–50 µm sensor, tension and compression tests, RT, – Correlation of AE count rate and twinning
OM strain rate
– Exponential relationship between
cumulative AE counts and twinning strain
during compression
15 2007 Maire et al. [16] Al alloy Plasticity Continuous AE data acquisition, two – Detrimental effect of relaxation occurring
(AA2124-T4 resonant sensors (micro-80), 4 Msamples/s during interrupted (slow) XCT
with tensile tests, slow and fast XCT – Energy of AE signals directly proportional
zirconia/silica to the cumulative surface of newly formed
reinforcement) cracks in the plane perpendicular to the LA
16 2008 Louche et al. [17] Al-3.3 wt% Mg Plasticity Continuous AE data acquisition, – At high strain rates, type A PLC bands,
alloy piezo-sensor (Kistler K-shear), tensile test, however multiple AE events suggest type B
RT, different strain rates, DIC bands
– At low strain rates, type C bands, stress
drops linked clearly to AE burst events
(continued)
Appendix
Table A.1 (continued)
No. Year Author References Material Research Method Topic + outcome
field
Appendix

17 2010 Akbari and [18] Low-carbon steel Plasticity Threshold-based AE data acquisition – Main source of AE: dislocation activities at
Ahmadi (AISI 1010) (40 dB), resonant sensor (125 kHz), all strains
1 Msamples/s, tensile tests, RT – Frequency range of dislocation activities
270–300 kHz
18 2010 Khamedi [19] Dual-phase steels Plasticity Threshold-based AE data acquisition – Application of wavelet transformation
et al. (with different (27 dB), broadband sensor (100–1000 kHz), – Three dominant frequency ranges correlated
volume fraction tensile tests, RT with main failure mechanisms:
of martensite) ferrite/martensite interface decohesion,
deformation of ferrite and fracture of
martensite
19 2010 Muransky [20] Mg alloy (ZM20) Plasticity Continuous AE data acquisition, two – AE results reflect the instabilities of the
et al. GS: 17, 114 µm broadband sensors (100–1000 kHz), microstructure at strains <2%, gradual
20 Msamples/s, tension and compression stabilization at strains above 2%
tests, RT, neutron diffraction
20 2011 Dobron [21] Mg alloy (AZ31) Plasticity Two-threshold-level-based AE data – AE signals related to twinning
et al. acquisition, broadband sensor (100– – Reduction of AE counts correlated with
600 kHz), 4 Msamples/s, compression tests, work hardening
RT, EBSD – Absence of AE at higher strain values
related to stop of twin nucleation
21 2011 Lugo et al. [22] Al alloy Plasticity Two sensors (100–200 kHz) – High AE activity at small strains, lower AE
(AA7075) activity at higher strains
22 2011 Mathis et al. [23] Mg (0.04 and Plasticity Two-threshold-level-based AE data – Strong asymmetry AE signals for tension
0.35% Zr) acquisition, broadband, HT sensor (S9215; and compression tests
GS: 150, 600 µm 50–650 kHz), tension and compression tests, – Compression: high AE activity at beginning
20–300 °C of deformation
– Tension: high AE activity over entire test
(continued)
393
Table A.1 (continued)
394

No. Year Author References Material Research Method Topic + outcome


field
23 2012 Vinogradov [24] a-brass Plasticity Continuous AE data acquisition, broadband – Intermittent plastic flow associated with
et al. GS: 30 µm sensor (1045D; 50–1200 kHz), continuous AE signals
2 Msamples/s, tensile tests, RT – Macroscopic AE burst correlated with
plastic instabilities in the stress-strain curve
– Shift of PSDF to lower frequencies
24 2012 Yasutomi [25] Mg alloy (AZ31) Plasticity Continuous AE data acquisition, four – Detwinning in three stages: initiation of
et al. broadband sensors (M304A; 100–1000 kHz), twin shrinkage, stable twin shrinking, twin
10 Msamples/s, tension tests after disappearance
compressive pre-deformation, RT, EBSD – Twin shrinkage and twin disappearance
strong AE sources
25 2013 Danjuk et al. [26] Cu (99.9%) Plasticity Continuous AE data acquisition, broadband – Development of appropriate data filtering
sensor (100–1000 kHz), 5 Msamples/s, and de-noising procedure
scratch test – Detection of low amplitude events caused
by dislocation glide
26 2013 Vinogradov [27] Mg alloy (ZK60) Plasticity Continuous AE data acquisition, broadband – Twinning and dislocation glide operating
et al. sensor (50–1200 kHz), 2 Msamples/s throughout the entire deformation process
– Different contribution to AE signals
depending on grain size
– Large grain size: deformation starts with
dislocation glide then twinning dominates
– Small grain size: dislocation glide
dominates
27 2014 Barat et al. [28] Austenitic Plasticity Threshold-based AE data acquisition, – Increase in AE count rates with decreasing
stainless steel resonant sensor (150 kHz), tensile tests, RT temperature caused by increased
(AISI 304LN) up to −50 °C martensitic phase transformation
28 2014 Bohemen [29] Eutectoid steel Plasticity Broadband sensor (WD; 100–1000 kHz), – AE (per unit time) energy proportional to
et al. (Fe-0.8 wt% C) waveguide, RMS of continuous signals plastic deformation rate of austenite
during continuous cooling surrounding formed martensite lath
(continued)
Appendix
Table A.1 (continued)
No. Year Author References Material Research Method Topic + outcome
field
Appendix

29 2014 Capek et al. [30] Mg (1 wt% Zr) Plasticity Threshold-based AE data acquisition (28 – Microplasticity caused by basal slip and
GS: 110 µm dB), broadband sensor (50–650 kHz), twinning well below macroscopic yield
interrupted tension and compression tests in point
combination with neutron diffraction, EBSD – Tension: twinning over the entire
deformation process
– Compression: twinning >2% of elongation
30 2014 Vinogradov [31] Ni single crystal, Plasticity Continuous AE data acquisition, broadband – Experimental determination of fractal
et al. Cu polycrystal sensor, tensile tests, white light interferometry dimension
– Inspection of surface morphology by white
light interferometry
– Correlation between AE median frequency
and strain hardening
31 2015 Haneef et al. [32] Austenitic Plasticity Threshold-based AE data acquisition (37 – Increase in RMS of AE signals with
stainless steel dB), one resonant sensor (150 kHz) and one increasing strain rate due to increase in
(AISI 316L) broadband sensor (100–1000 kHz), source activation
5 Msamples/stensile test, RT, IR-TG – Shift of AE signals to higher-frequency
domain caused by reduction of mean free
path of dislocations
32 2015 Mathis et al. [33] Mg (1-wt%Zr) Plasticity Continuous AE data acquisition, broadband – High time resolution information about
GS: 110 µm sensor, 2 Msamples/s, interrupted tension and kinetics of active deformation processes
compression tests in combination with – Distinction between dislocation glide and
neutron diffraction twinning, but also between different
twinning systems and basal and non-basal
dislocation glide events
33 2015 Murasawa [34] Ti (99.5%) Plasticity Threshold-based AE data acquisition, four – Distinction of deformation history in three
AE sensors, tensile test, RT, EBSD, DIC regions: (i) around yield point with peak of
AE count rate, (ii) after yield point with
decrease in AE count rate and (iii) early
stage of plastic flow with increasing AE
count rate
395

(continued)
Table A.1 (continued)
396

No. Year Author References Material Research Method Topic + outcome


field
34 2016 Drozdenko [35] Mg single Plasticity Continuous AE data acquisition, broadband – <11.2>: dominant basal slip related to low
et al. crystals, different sensor (100–600 kHz), 2 Msamples/s, amplitude AE signals
orientations uniaxial and channel-die compression tests, – <11.0>: more pronounced AE response
RT caused by higher twinning activity
35 2016 Vinogradov [36] Mg (99.98%) Plasticity Continuous AE data acquisition, broadband – Dependence of deformation mechanisms on
et al. GS: few mm sensor (50–1200 kHz; PICO), 2 Msamples/s, cyclic loading path (tension or
tension and compression tests, high-speed compression)
camera – Kinetics of twin accumulation
36 2016 Yin et al. [37] NiTi Plasticity Threshold-based AE data acquisition (20 – According to cumulated AE energy
GS: 10, 42, dB), AE sensor (Nano-30), tensile fatigue distinction of three stages of fatigue failure:
80 nm test, SEM, Keyence microscope (i) slow crack propagation, (ii) fast crack
propagation and (iii) final failure
37 2016 You et al. [38] Low-alloyed Plasticity Threshold-based AE data acquisition (35 – Monitoring the changes in as-received and
steel (2.25Cr– dB), broadband sensor, tensile test, SEM, hydrogen-charged specimens
1Mo) TEM
38 2017 Mathis et al. [39] Mg alloy Plasticity Continuous AE data acquisition, broadband – Long-period stacking ordered structures
(Mg-Zn-Y) sensor (100–600 kHz), 2 Msamples/s, (LPSO)
compression tests with in situ synchrotron – Three different deformation mechanisms:
measurements, RT (i) dislocation slip, (ii) twinning and
(iii) kinking
39 2001 Wu et al. [40] TiAl alloy Fatigue Threshold-based AE data acquisition – Cracks caused by pre-stressing act as failure
(Ti44Al8Nb1B) (45 dB), fatigue tests (R = 0.1), 2 AE initiation sites during fatigue
Fully lamellar resonant sensors, OM, SEM, TEM – Fatigue limit at 0.65 of 0.2% proof stress
40 2001 Vinogradov [41] Cu Fatigue Continuous AE data acquisition, broadband – High sensitivity of AE to dislocation
et al. Single crystals sensor ADC (50 kHz–2 MHz), dynamics during cyclic loading
5 Msamples/s, fatigue tests (Bauschinger effect, formation of PSBs,
crack initiation)
(continued)
Appendix
Table A.1 (continued)
No. Year Author References Material Research Method Topic + outcome
field
Appendix

41 2002 Vinogradov [42] Cu (ufg, ECAP) Fatigue Continuous AE data acquisition, broadband – No AE signals correlated with classical
et al. sensor ADC (50 kHz–2 MHz), dislocation motion
5 Msamples/s, fatigue tests – Shear banding
42 2002 Vinogradov [43] Cu-Cr-Zr alloy Fatigue Continuous AE data acquisition, broadband – High AE activity before final failure caused
et al. (ufg, ECAP) sensor ADC (50 kHz–2 MHz), by shear banding and microcracking
5 Msamples/s, fatigue tests
43 2003 Roberts and [44, 45] Steel, welded Fatigue Threshold-based AE data acquisition – Relationship between acoustic emission
Talebzadeh steel (80 dB), four resonant sensors (280 kHz), CT count rates and crack propagation rates
specimens, fatigue tests, RT – Application of source location software
– Possibility of prediction of fatigue life time
44 2004 Oh et al. [46] Austenitic Fatigue Threshold-based AE data acquisition (45 – Relationship between AE count rate and
stainless steel dB), resonant sensor (150 kHz), tensile tests stress intensity factor range
(AISI 304) and fatigue crack growth tests – Overload: AE count rate reflects the crack
growth rate
45 2006 Biancolini [47] Low-alloyed Fatigue Two resonant sensors (25 and 250 kHz), – Fractal dimension of AE signals applied as
et al. steel rotating-bending-fatigue test a damage parameter
(39NiCrMo3) – Prediction of cracks
46 2009 Chang et al. [48] Al alloy Fatigue Threshold-based AE data acquisition – Application of AE technique to measure
(LY12CZ) (30 dB), two broadband sensors, crack closure level for physical short cracks
5 Msamples/s, pre-fatigued SENB specimens
47 2011 Han et al. [49] Micro-alloyed Fatigue Two broadband sensors (10–2000 kHz), – Three distinct stages of AE: crack initiation,
steel SENB specimens activities within plastic zone ahead of crack
tip, ligament shearing between microvoids
and microcracks
48 2014 Mohammad [50] Steel Fatigue Threshold-based AE data acquisition – Capability of AE technique for predicting
et al. (39 dB) fatigue lifes
(continued)
397
Table A.1 (continued)
No. Year Author References Material Research Method Topic + outcome
field
49 2017 Chai et al. [51] Austenitic Fatigue Threshold-based AE data acquisition – K-means clustering algorithm
stainless steel (50 dB), two narrow band sensors (50– – Three clusters: (i) plastic deformation in the
(AISI 316L) 200 kHz), fatigue test, CT specimens cyclic plastic zone, (ii) ductile crack growth
and (iii) shear crack growth
50 2001 Botten et al. [52] TiAl alloy Fracture Threshold-based AE data acquisition (45 – AE signals caused by interlamellar cracking
(Ti44Al8Nb1B) mechanics dB), tensile tests, 2 AE resonant sensors, OM, at stresses below 0.2 yield stress
Fully lamellar SEM, TEM
51 2006 Carpinteri [53] Theoretical work Fracture – Lifetime assessment and prediction
et al. mechanics
52 2011 Aggelis [54] Al alloy Fracture Threshold-based AE data acquisition – Correlation of AE with damage
et al. (AA7075) mechanics (40 dB), two broadband sensors (Pico; 50– accumulation and fracture mode
800 kHz), 5 Msamples/s, CT specimens – Transition from mode I to mode II fracture
mode
53 2012 Kordatos [55] Al alloy Fracture Threshold-based AE data acquisition (40 – Correlation of AE with damage
et al. (AA7075, A359) mechanics dB), two broadband sensors (Pico; 50–800 accumulation and fracture mode
kHz), 5 Msamples/s, CT specimens, Lock-in – Before final fracture significant change of
thermography characteristic AE parameters
54 2016 Hao et al. [56] Ti-plate with type Fracture Threshold-based AE data acquisition – AE energy and IR-TG reflect deformation
I crack mechanics (40 dB), 2 Msamples/s, tensile test, RT, and fracture process of type I crack
IR-TG – Intensity of AE signals inverse proportional
to deformation rate
55 2017 Kietov et al. [57] Cast iron Fracture Continuous AE data acquisition, two – Ductile fracture behaviour (debonding of
(EN-GJS-400-15) mechanics broadband sensors (Pico and WD), impact graphite, plastic deformation, void
tests, RT formation and coalescence
– Not detectable by AE
(continued)
Table A.1 (continued)
No. Year Author References Material Research Method Topic + outcome
field
Appendix

56 2001 Fregonese [58] Austenitic Corrosion Continuous AE data acquisition, resonant – Increasing AE activity with evolving
et al. stainless steel sensor R15D, 100–500 kHz corrosion pits
(AISI 316L) – AE enables monitoring of change of
corrosion mode from pitting corrosion to
uniform corrosion
57 2003 Darowicki [59] Austenitic Corrosion Piezo-sensor Nano30 (100–1200 kHz), – AE connected with the evolution of
et al. stainless steel 10 Msamples/s, hydrogen bubbles
(AISI 304L)
58 2007 Shaikh et al. [60] Austenitic Corrosion Threshold-based AE data acquisition, – Transgranular crack initiation and
stainless steel broadband sensor, waveguide, pre-fatigued propagation
(AISI 316LN) CT specimens, stress corrosion crack growth – AE signals due to plastic deformation ahead
experiments of the crack tip
59 2010 Kovac et al. [61] Austenitic Corrosion Threshold-based AE data acquisition (30 – Correlation between electrochemical noise
stainless steel dB), two braodband sensor (100–1000 kHz), and AE related to two different
(AISI 304) 0.5 Msamples/s, tensile tests, RT, corrosion mechanisms: intergranular stress corrosion
cell, electrochemical noise, DIC cracking and small individual ductile
fracture
60 2011 Du et al. [62] Austenitic Corrosion Threshold-based AE data acquisition (29 – Similar results for electrochemical noise
stainless steel dB), two resonant sensors (Micro-80DS; 300 and AE
(AISI 304) kHz), tensile tests, RT, corrosion cell, – Application of K-means clustering
electrochemical noise, long-distance algorithm
microscope – Different AE sources: pitting, cracking,
bubble break-up
399
Digital image correlation in Materials Science and Engineering: State of the art (Table A.2).
400

Table A.2 Chronological overview of investigation of strain localizations using the digital image correlation in combination with optical microscopy and
scanning electron microscopy as well as FEM simulations starting from year 2000
No. Year Author References Material Research field Method Topic + outcome
1 2001 Bugat et al. [63] Duplex steel Plasticity In situ DIC with SEM, uniaxial tensile test, – Increasing strain heterogeneities with
RT, gold grid, grid distance 38 µm, subset size increasing deformation
2 2001 Raabe et al. [64] Aluminium Plasticity 3D in situ DIC with OM, photogrammetry, – Strain localization along diagonals
plane-strain compression tests, combined with with maxima at corners and less
EBSD, combined with finite element pronounced maxima in the centre both
calculation, grid technology found by experiments and FE
calculations
3 2002 Sachtleber [65] Aluminium Plasticity 3D in situ DIC with OM, photogrammetry, – Quantitative experimental grain- and
et al. plane-strain compression tests, combined with subgrain scale strain analysis using
EBSD, combined with finite element photogrammetry in conjunction with
calculation, speckle pattern microtexture determination
4 2003 Schroeter [66] OHFC Copper Plasticity In situ DIC with OM, compression and torsion – Localized shear and rotation of
et al. GS: 70 µm tests at RT, grid manufactured by mesoscopic size
photolithography, grid size: 10–3 µm – Heterogeneity after compression larger
than after torsion
5 2003 Biery et al. [67] c-TiAl (different Plasticity In situ DIC with SEM, uniaxial tensile test, – Strong influence of the microstructure
production evaporated gold through fine nickel grids on the distribution of strains
routes) – Strains more uniform distributed in fine
grained material states (PM) than in
coarser states
6 2003 Tatschl et al. [68, 69] OFHC copper Plasticity In situ DIC with SEM, uniaxial tensile tests, – Local deformation analysis in a wide
GS: 100 µm RT, etched surface range of magnifications
7 2004 Zhang et al. [70] Al-0.5%Mg Plasticity In situ DIC with OM using CCD camera, – Local in-plane plastic strain and rigid
GS uniaxial tensile tests, RT, combined with body rotations of grains
EBSD, speckle pattern
(continued)
Appendix
Table A.2 (continued)
No. Year Author References Material Research field Method Topic + outcome
Appendix

8 2005 Fonseca et al. [71] Antler bone Plasticity In situ DIC with OM, uniaxial tensile test, RT, – Strain resolution of about 0.05%
Ferritic steel etched microstructure (Nital), subset size: 32
GS: 100 µm pixels
9 2006 Lagattu et al. [72] Ti–6Al–4V Plasticity In situ DIC with SEM, uniaxial tensile tests, – Spatial resolution of 1 µm
RT, deposition of fine powders (100 nm),
subset size: 1 µm
10 2007 Kang et al. [73] Dual-phase steel Plasticity In situ DIC with SEM, uniaxial tensile tests, – Strain partitioning between ferritic and
(intercritical RT, etched microstructure (Nital), subset size: martensitic phases
annealed; 15 pixels – Influence of heat treatment on
tempered) heterogeneity of strain distribution
11 2008 Li et al. [74] Aluminium Plasticity In situ DIC with SEM, heating experiments up – Micro- and nanoscale thermal strain
to 125 °C, gold nanodots (100–150 nm), measurements
subset size: 47 pixels
12 2008 Jin et al. [75] Electrodeposited Plasticity In situ DIC with SEM, uniaxial tensile tests, – SEM-DIC suitable application for
Ni-base RT, natural surface, subset size: 25 pixels full-field measurements on microscale
Aluminium alloy (Ni-base) and magnetron sputtered gold mesh for plastic deformation and fracture
(AA6061-T651) with mesh pits of 25 µm and mesh bar width
GS: 100 µm of 5 µm
13 2008 Zdunek et al. [76] Aluminium alloy Plasticity In situ DIC with OM, uniaxial tensile tests, – Strain localization within PLC bands
(AA5182) sprayed graphite particles – Different kinetics of strain localization
Grain size
14 2009 Tschopp et al. [77] Ni-base Plasticity In situ SEM with SEM, uniaxial tensile tests, – Increase in average maximum shear
superalloy (René RT, Pt nanoparticles (TTFA), combined with strain with increasing Schmid factor
88DT) EBSD, subset size: 7 µm – Increase in shear strain in the vicinity
GS: 50 µm of grain boundaries and triple junctions
15 2009 Chrysochoos [78] Mild steel Plasticity In situ DIC with OM and IR-TG, uniaxial – Combination of DIC and TG
et al. tensile tests, RT, airbrushed speckle pattern – Influence of dissipated energy and
thermomechanical couplings on
stress-strain response
(continued)
401
Table A.2 (continued)
402

No. Year Author References Material Research field Method Topic + outcome
16 2009 Zavattieri [79] TWIP steel Plasticity In situ DIC with OM, uniaxial tensile tests – Spatio-temporal characteristics of PLC
et al. bands
17 2010 Canadinc [80] IF steel Plasticity In situ DIC with OM, uniaxial tensile tests –
et al. GS: UFG
18 2010 Caroll et al. [81] Non-specified Plasticity Ex situ DIC with OM, uniaxial tensile tests – Influence of strain rate and temperature
and fatigue crack growth tests, RT on compressive deformation behaviour
of ufg and coarse grained IF steel
19 2010 Ghadbeigi [82] Dual-phase steel Plasticity Ex situ DIC with SEM, uniaxial tensile tests, – Localization of deformation in bands
et al. RT, etched two-phase microstructure (Nital), inclined by 45° to the loading direction
subset size
20 2010 Savic et al. [83] Martensitic steel Plasticity In situ DIC with OM (high-speed camera), – True strain calculation during necking
uniaxial tensile tests, speckle pattern, subset using DIC
size: 60 pixels
21 2010 Tasan et al. [84] Dual-phase steel Plasticity In situ DIC with SEM, uniaxial tensile tests, – Influence of banded microstructure on
RT, natural microstructure mechanical properties
– Influence of morphology and
mechanical properties of the phase
composing the banded structure
22 2011 Nicoletto [85] Cast iron Plasticity In situ DIC with OM, uniaxial tensile test, RT, – Microstructure-related strain
et al. (GJS 400) air brush speckle pattern inhomogeneities
23 2011 Badulescu [86] Aluminium Plasticity In situ DIC with OM, uniaxial tensile tests, – Estimation of strain and heat source
et al. GS: cm RT, combined with IR-TG, grid size 0.2 mm distribution
24 2012 Abuzaid et al. [87] Hastelloy X Plasticity Ex situ DIC with OM, uniaxial tensile tests, – Investigations of slip transmission and
GS: 50 µm RT, combined with EBSD, speckle pattern, strain accumulation at GB
subset size: 14 µm – Inverse relation between residual
Burgers vector and magnitude of strain
at GB
25 2012 Walley et al. [88] Plasticity
(continued)
Appendix
Table A.2 (continued)
No. Year Author References Material Research field Method Topic + outcome
Appendix

Ni-base In situ DIC with SEM, uniaxial tensile tests, – Intra- and intergranular deformation
superalloy RT up to 700 °C, combined with EBSD, mechanisms at elevated temperatures
(René 104) speckle pattern manufactured by e-beam
GS: 32 µm lithography, subset size: 9 µm
26 2013 Ghadbeigi [89] Dual-phase steel Plasticity In situ DIC with SEM, uniaxial tensile tests, – Plastic deformation of martensitic
et al. GS: 5–20 µm RT, etched two-phase microstructure (Nital), islands,
(ferrite) grid size: 16 and 8 pixels – Crack initiation at interface boundaries
and crack growth towards interior of
martensitic islands
27 2013 Han [90] Dual-phase steel Plasticity Ex situ DIC with SEM, uniaxial tensile tests, – Ferritic/martensitic phase boundaries
RT, combined with EBSD, FIB grid, grid size: no preferred locations for strain
40 µm partitioning
– High strain localizations caused by
morphology of surrounding
microstructure either than by
orientation or type of interface
28 2013 Joo et al. [91] Dual-phase steel Plasticity Ex situ DIC with SEM, uniaxial tensile test, – Quantitative analysing of plastic
Grain size: 1– RT, Ag nanodot pattern, subset size: deformation of martensitic islands on a
3 µm 20 pixels to 8 pixels submicron scale
(martensite)
29 2013 Brenne et al. [92] Ti–6Al–4V Plasticity Ex situ DIC with OM, uniaxial tensile and – Relationship between microstructure,
Additive cyclic loading and four-point bending test, no geometry and mechanical behaviour of
manufactured additional pattering, subset size: cellular structures
– Prediction of areas of damage initiation
under all loading conditions by DIC
30 2013 Gioacchino [93] Austenitic steel Plasticity Ex situ DIC with SEM, uniaxial tensile test, – Necessity of submicron resolution in
et al. RT, combined with EBSD, speckle pattern: order to catch up the strain
gold nanosized dots, subset size: 0.25 µm localizations related to slip bands
(continued)
403
Table A.2 (continued)
404

No. Year Author References Material Research field Method Topic + outcome
31 2013 Kammers [94] Aluminium Plasticity In situ DIC with SEM, tensile tests, RT, – High flexibility of patterning technique
et al. (AA1100), self-assembled gold nanoparticles (15– for metallic, non-metallic materials,
Ni-Cr superalloy 350 nm) complex specimen geometries and
SiC delicate test material
– High spatial resolution of DIC
32 2013 Kurtovic [95] Aluminium Plasticity In situ DIC with CLSM, uniaxial tensile tests, – Strong strain localization in AA5054,
et al. laminates of RT, top view and side view DIC homogenized in AA6014layers
AA6014 and – PLC effect occurring in ufg pure
AA5054 (ufg) AA5054 suppressed by laminates with
AA60124
33 2013 Marteau et al. [96] IF steel Plasticity In situ DIC with SEM, uniaxial tensile tests, – Plastic deformation of martensitic
Dual-phase steel RT, combined with EBSD, microgrid, subset grains
size: 40 pixels – Strain heterogeneities independent of
grain orientation, shape and size
34 2013 Na et al. [97] Martensitic steel Plasticity In situ DIC with SEM, uniaxial tensile tests, – Strain localization in the vicinity of
combined with EBSD, subblock boundaries
35 2013 Patriarca [98] FeCr steel Plasticity In situ DIC with OM, uniaxial tensile tests, – Direct quantification of capability of
et al. RT, airbrush speckle pattern, subset size: GB to transmit or block dislocation
glide by strain fields across GB
36 2014 Ramazani [99] Dual-phase steel Plasticity In situ DIC with SEM, uniaxial tensile tests – Cracking of martensite as main failure
et al. and three-point bending tests, combined with mechanism
EBSD, combined with XFEM calculations, – Good agreement with XFEM results
speckle pattern
37 2014 Kimiecik [100] NiTi SMA Plasticity In situ DIC with SEM, uniaxial tensile tests, – Large strain heterogeneities within
et al. RT, combined with EBSD, self-assembling individual grains regarding mean strain
gold nanoparticles, subset size: 30 pixels or strain range
– No clear dependence on grain
orientation or grain size
(continued)
Appendix
Table A.2 (continued)
No. Year Author References Material Research field Method Topic + outcome
Appendix

38 2015 Eskandari [101] TWIP steel Plasticity In situ with OM, uniaxial tensile tests, RT up – Strain localization bands correlated
et al. GS: 40 µm to 400 °C, speckle pattern using black Cobalt with formation of e-martensite (RT) or
oxide particles, subset size: 20 pixels twinning (400 °C)
39 2015 Chow et al. [102] Aluminium alloy Plasticity Ex situ DIC with OM, uniaxial tensile test, RT, – Simultaneous estimation of elastic
(AA 5052) combined with XRD, speckle pattern, subset strains by XRD and total strain fields
GS: 5–20 mm size: 340 µm by DIC at grain scale
– Determination of uncertainties for total
strain and elastic strains to be
±4  10−4 and ±3  10−5,
respectively
40 2015 Gioacchino [103] Austenitic steel Plasticity Ex situ DIC with SEM, uniaxial tensile test, – Evolution of plastic strain linked to the
et al. RT, combined with EBSD, speckle pattern: development of lattice curvature
gold nanosized dots, subset size: 0.17 µm
41 2015 Stinville [104] Ni-base Plasticity In situ DIC with SEM, uniaxial tensile tests, – Maximum strain at twin boundaries
superalloy (René RT, combined with EBSD and TEM, etched – High dislocation densities in highly
88DT) microstructure, subset size: 21 pixels localized slip bands
GS: 26 µm
42 2016 Pina et al. [105] Vermicular Plasticity In situ DIC with SEM, uniaxial tensile tests, – Mechanical anisotropy of vermicular
graphite iron graphite particles
43 2016 Jiang et al. [106] Ni-base Plasticity Ex situ DIC with SEM, bending tests, RT, – Measurement of total and elastic
superalloy combined with HR-EBSD, SiO2 particle deformation using HR-DIC and
Mar002 (single (250 nm) pattern, subset size: 100 pixels HR-EBSD
crystal) – Evaluation of small elastic lattice
curvature adjacent to slip bands and
residual stress across slip bands
44 2016 Wang et al. [107] Ni single crystal Plasticity In situ DIC with OM, miniature loading stage, – Determination of displacement fields
(99.999%) CMOS camera using B-spline transformations
(continued)
405
Table A.2 (continued)
406

No. Year Author References Material Research field Method Topic + outcome
45 2012 Besnard et al. [108] Non-specified High-speed In situ DIC with stereo high-speed camera – Stereo correlation technique to analyse
deformation imaging, speckle pattern necking during high-speed
deformation
46 2008 Bartali et al. [109] Duplex steel Fatigue In situ DIC with OM, uniaxial fatigue tests, – Accommodation of cyclic plastic strain
GS: 10 µm RT, cylindrical specimen with shallow notch, first by austenitic followed by ferritic
(asuetnite) and etched microstructure, subset size: 32 pixels grains
10  50 µm – Strain localizations indicator for crack
(ferrite) initiation
– Crack initiation at ferrite/ferrite GB
followed by crack growth into
austenitic neighbouring grains
47 2009 Bartali et al. [110] Duplex steel Fatigue In situ DIC with OM, uniaxial fatigue tests, – Cyclic plastic slip in austenite on at
GS: 10 µm RT, cylindrical specimen with shallow notch, least two slip systems controlled by the
(austenite), etched microstructure, combined with EBSD Schmid factor
30 µm (ferrite) and interferometric profilometry, subset size: – In ferritic grains more than two slip
32 pixels systems, not Schmid factor controlled
48 2009 Niendorf [111] IF steel (ufg) Fatigue In situ DIC with OM (Keyence, long focus), – Fatigue-induced damage evolution in
et al. speckle pattern ufg IF steel
– Influence of grain shape on overall
stress state
49 2013 Abuzaid et al. [112] Hastelloy X Fatigue Ex situ DIC with OM, uniaxial fatigue tests, – Influence of shielding and transmission
GS: 50 µm RT, combined with EBSD, speckle pattern, on the formation of strain localizations
subset size: 4.7 µm near GB
– Enhanced strain localization prior to
fatigue crack initiation
50 2017 Guan et al. [113] Ni CMSX4 Fatigue Ex situ DIC with SEM, three-point bending – HR-DIC in order to quantify to
single crystals tests, RT, combined with EBSD, combined quantify the developing strain fields
and MAR002 with crystal plasticity modelling, SiO2-particle and the strain localization in both
oligocrystals pattern (150–250 nm), subset size: single and oligocrystals
GS: 3000 µm
Appendix

(continued)
Table A.2 (continued)
No. Year Author References Material Research field Method Topic + outcome
Appendix

51 2006 Lagattu et al. [72] TiAl Fracture In situ DIC with OM, pre-cracked CT – Strain localization around crack tip
mechanics specimen, fatigue tests, RT, speckle pattern,
two different mesh sizes
52 2011 Sangid et al. [114] Ni–Co alloy Fracture In situ DIC with OM, uniaxial tensile tests and – Identification of dislocation-mediated
mechanics fatigue crack growth tests, combined with plasticity as deformation mechanism
EBSD, speckle pattern, subset size. 130 pixels near crack tip
– Improved fatigue growth resistance
53 2014 Schäfer et al. [115] Ni-base Fracture In situ DIC with SEM, tensile and cyclic – Elastic and plastic strain fields around
superalloy mechanics loading of pre-cracked specimen, natural stage-I crack
CMSX-4 microstructure – Measurement of plastic zone size
54 2016 Ahadi et al. [116] NiTi Fracture Ex situ DIC with OM, fatigue tests on – Grain size dependence of fracture
GS: 1.5 µm– mechanics pre-cracked CT specimens, RT, Si particle toughness and crack growth resistance
10 nm speckle pattern, combined with IR-TG – Reduction of grain size results in
decrease in KIc and transformation
zone in front of the crack tip
55 2016 Mao et al. [117] C/SiC composite Fracture In situ DIC with OM, three-point bending with – In situ monitoring of nucleation and
mechanics SENB specimen, high temperatures 1600 °C), growth of crack in a SENB specimen
high-temperature resistant speckle pattern, under bending
subset size: 29 pixels
56 2003 Soppa et al. [118] Al/Al2O3 Modelling In situ DIC with SEM, uniaxial tensile tests, – Change of strain pattern due to
composite and RT, combined with FE simulations, e-beam interface cracks
(AA6061) parameter lithography, subset size:
identification
57 2006 Besnard et al. [119] Aluminium alloy Modelling In situ DIC with OM, uniaxial tensile test, RT, – Strain localization in PLC bands
(AA5005) and speckle pattern, subset size: 16–4 pixels
parameter
identification
(continued)
407
Table A.2 (continued)
408

No. Year Author References Material Research field Method Topic + outcome
58 2007 Heripré et al. [120] Zircomium, Modelling In situ DIC with OM and SEM, uniaxial – Multiscale coupling of morphology
Titanium and tensile tests, combined with EBSD, combined and texture of a microstructure with
aluminides parameter with FEM modelling, gold grid, grid step size: results of mechanical strain field
identification 2 µm, grid thickness: 300 nm analysis
– Finite element calculations based on
the microstructure determined
experimentally compared with the DIC
calculated strain fields
59 2008 Avril et al. [121] Steel Modelling In situ DIC with OM using two high-speed – Identification of elastic-visco-plastic
and CCD cameras, uniaxial tensile loading, RT, constitutive parameters
parameter speckle pattern, subset size: 21 pixels – Combination of full-field
identification measurements with virtual field
method
60 2008 Zhao et al. [122] Al-oligocrystal Modelling In situ DIC with OM, uniaxial tensile loading, – Significant influence of grain topology
and RT, combined with EBSD, CWLM, and FEM and microtexture on strain
parameter simulation, speckle pattern heterogeneities
identification – Surface roughening related to macro
strain localization and intra-grain
interaction
61 2010 Saai et al. [123] Al-Bi crystal Modelling In situ DIC with OM and IR-TG, speckle – Combination of DIC and IR-TG during
and pattern, subset size: 10 pixels tensile test
parameter – Calculation of strain fields and local
identification heat sources
(continued)
Appendix
Table A.2 (continued)
No. Year Author References Material Research field Method Topic + outcome
Appendix

62 2014 Tasan et al. [124, 125] Dual-phase steel Modelling In situ DIC with SEM, uniaxial tensile tests, – Initiation of plasticity in regions with
(DP600, DP800) and RT, combined with EBSD and FEM larger ferrite grain size and lower local
GS: 8 and 5 µm parameter simulation, SiO2 particles martensitic fractions
(ferrite) and 3 identification – Importance of martensite distribution
and 2 µm on strain heterogeneities
(martensite) – Integrated computational materials
engineering approach for designing of
advanced DP steels
63 2014 Lim et al. [126] Ta-oligocrystals Modelling In situ DIC with SEM-EBSD, uniaxial tensile – Comparison of CP-FEM results with
and tests combined with CP-FEM simulations, EBSD and HR-DIC
parameter speckled with copper powder (300 nm), subset – Good agreement in crystallographic
identification size: 9.7 µm rotations between experiments and
model
64 2016 Kasvayee [127] Cast iron Modelling In situ DIC with OM, tensile tests, RT, – Strain localizations between graphite
et al. (GJS-500-2) and combined with FEM, pit etching particles
parameter (HCl + H2O2 + H2O) + GB etching (5% – Good agreement of DIC and FEM
identification Nital) concerning shear bands between
graphite particles, differences in the
magnitude of strain
65 2002 Chasiotis [128] Multi-user Elastic In situ DIC with AFM, uniaxial tensile tests, – New tensile tester for MEMS
et al. MEMS (MUMS) properties combined with FE simulation, scanning area – Determination of Young’s modulus
5  5 µm up to 20  20 µm and tensile strength of MEMS via
load-displacement curves in
combination with AFM surface
recordings
66 2005 Cho et al. [129] Amorphous DLC Elastic In situ DIC with AFM, uniaxial tensile tests, – Anisotropic displacement fields at
MEMS properties notched specimen, scanning area 15  15 µm ultra-high stress concentrations
– Determination of Young’s modulus
and Poisson ratio
(continued)
409
Table A.2 (continued)
410

No. Year Author References Material Research field Method Topic + outcome
67 2007 Cho and [130, 131] Polycrystalline Elastic In situ DIC with AFM, uniaxial tensile tests, – Highly inhomogeneous axial
Chasiotis Si-Films properties 2–2.5 µm thick freestanding specimens, displacement fields for specimen
surface measurement areas: 1  2 µm2 up to domains smaller than 5  5 µm2
5  15 µm2, subset size: 300 nm – Importance of polycrystalline
anisotropy in NEMS
68 2010 Han et al. [132] Glass Elastic In situ DIC with AFM, double cleavage – Determination of nanoscale stress
properties compression test, RT, intensity factors
– Out-of-plane displacement at the free
surface in front of crack tip
69 2009 Korsunski [133] TiN PVD coating Residual FIB-DIC, hole drilling, Pt depth hole pattern – Agreement between FIB-DIC results
et al. on WC/Co stresses and FE predictions
substrate – Residual stress evaluation at the
submicron scale
70 2011 Sebastiani [134] CrN coating on Residual FIB-DIC, incremental ring-core milling (1 µm – Providing of criteria for proper
et al. steel stresses RCM), Pt depth holes pattern selection of pillar size and proper
elastic constants
71 2013 Krottenthaler [135] Carbon coating Residual FIB-DIC, H-bar milling, Pt nanoparticles as – H-bar milling suitable geometry for
et al. on different stresses pattern contrast reliable residual stress estimation using
substrate FIB-DIC
materials (steel, – Determination of compressive residual
Al) stresses in hydrogenated amorphous
carbon coatings
72 2014 Salvati et al. [136] Residual FIB-DIC, ring-core milling, combined with FE – Strain redistribution at the surface of
stresses simulations the central part of the ring-core milled
area
73 2015 Korsunski [137] Residual FIB-DIC, different types of FIB milling – Reliable estimation of residual stress
et al. stresses error bounds and confidence limits
(continued)
Appendix
Table A.2 (continued)
No. Year Author References Material Research field Method Topic + outcome
Appendix

74 2016 Salvati et al. [138, 139] Silicon Residual FIB-DIC in combination with FEM – Determination of FIB-induced strain
stresses – Evaluation of lower bound pillar radius
for stress evaluation (1 µm)
75 2007 Lenoir et al. [140] Argillite Volumetric Digital volume correlation (DVC) with – Onset of shear strain localizations
strain microCT, triaxial testing
measurements
76 2008 Bay et al. [141] Metallic foam Volumetric Digital volume correlation (DVC) with –
strain microCT, spherical indentation
measurements
77 2011 Jandejsek [142] Bone Volumetric Digital volume correlation (DVC) with –
et al. Aluminium foam strain microCT, uniaxial compression, combined
measurements with FEM
78 2013 Mostavi et al. [143] Poly-granular Volumetric Digital volume correlation (DVC) with –
graphite strain microCT, short-bar chevron notched specimen
measurements
411
412

Infrared thermography: State of the art (Table A.3).


Table A.3 Chronological overview of the application of infrared thermography (IR-TG) starting from 2000 including classification of the research field
No. Year Author References Material Research field Method Topic + outcome
1 2001 Louche et al. [144] Steel (S355MC) Plasticity TG-camera (Agema 880 sw), – Low amplitude thermal front with
GS: 50 µm tensile tests, RT, DIC constant velocity related to Lüders
band propagation
– Thermal and kinematic
measurements similar results
2 2004 Yang et al. [145] Bulk metallic glasses Plasticity/ TG-camera (Indigo Phoenix), – Different shear band mechanisms
Fatigue MWIR, focal plane array during tensile and fatigue
320  250 pixels2, tensile tests specimens
(RT), fatigue tests (R = 0.1), – Temperature decrease during shear
band propagation
– Instantaneous melting at failure
3 2005 Ranc et al. [146] Aluminium alloy (4% Plasticity TG-camera, focal plane array – PLC instabilities in a Al-Cu alloy
copper) 320  240 pixels2, tensile test – Estimation of band width, band
(RT) velocity and strain increment caused
by PLC band formation
4 2008 Ranc et al. [147] Ti alloy (TiAl4V) Plasticity Pyrometer, dichroic mirrors, – Initiation of adiabatic shear bands
beam splitter, Torsion, dynamic – Multiple formation of adiabatic
torsion tests shear bands followed by interaction
and annihilation of shear bands
5 2009 Bouzakher et al. [148] Fe-based metallic glasses Plasticity TG-camera (Flir), focal plane – Investigation of mechanical damage
(Fe78–Si10–B12) array, 120  160 pixels2, MWIR, processes at edge-notch region of
tensile tests, SEM, AFM large ribbon metallic glass
6 2009 Guzman et al. [149] Al alloy (AA6082), Mg Plasticity TG-camera (Thermosensoric), – Synchronisation of mechanical,
alloy focal plane array, 384  288 electronic and thermal time
pixels2, MWIR, quasi-static and intervals
dynamic (SHPB) compression
tests
(continued)
Appendix
Table A.3 (continued)
No. Year Author References Material Research field Method Topic + outcome
Appendix

7 2009 Kim et al. [150, 151] FeMnAlC Plasticity TG-camera (Cedip), tensile tests, – Jerkey flow at higher strain levels
DIC – Formation and propagation of PLC
bands
– Velocity of PLC bands decreases
with time and true strain
– PLC effect caused by DSA due to
interaction of dislocations with C-V
complexes
8 2011 Delpueyo et al. [152] SMA (Cu-Al-Be) Plasticity TG-camera, (Cedip), focal plane – Calculation of heat sources and
Single crystal array, MWIR amplitude of temperature oscillation
– Martensitic microstructure related to
two thermomechanical couplings:
(i) thermoelastic coupling in the
austenite and (ii) thermocoupling
related to martensitic phase
transformation
9 2011 Lee et al. [153] Multiphase TRIP steel Plasticity TG-camera, tensile tests – Occurrence od Lüders effect
(Fe-0.05C-6.5Mn-1.5Si), depending on grain size
ufg – Correlation between IR images and
local strain maps
10 2012 Saed-Akbari [154] TWIP steels Plasticity TG-camera (InfraTec), focal – Significant temperature variation in
et al. (Fe–C–Mn, Fe–C–Mn– plane array, MWIR, tensile tests, front of propagating PLC bands
Al) −40 °C, RT, 100 °C – Analysis of the stress—
GS: 3, 25, 80 µm instantaneous strain rate—space
– Precise adjustment of combination
of deformation parameters and
chemical compositions
11 2004 Boulanger et al. [155] Dual-phase steel (DP60) Fatigue TG-camera (Cedip SW), – Dissipative and thermoelastic effects
64  128 pixels2, 250 Hz frame – Dependence of dissipation on
rate, space resolution: testing frequency and stress
amplitude
413

(continued)
Table A.3 (continued)
414

No. Year Author References Material Research field Method Topic + outcome
0.2 mm/pixel, load-controlled
fatigue tests (R = −1, R = 0)
12 2006 Xue et al. [156] Martensitic steels (AISI Fatigue TG-camera, 320  240 pixels2, – Mean temperature increase related
52100, 42CD) and cast lateral resolution 0.17 mm/pixel, to damping behaviour of material
iron (GS51) ultrasonic fatigue tests (20 kHz) – Dependent both on amplitude and
rate of cyclic loading
– Sharp temperature increase when
crack propagation starts
13 2007 Berthel et al. [157] Dual-phase steel (DP600) Fatigue TG-camera (Cedip), focal plane – Heterogeneous distribution of heat
array, 64  120 pixels2, 250 dissipation from the beginning of
images/s, spatial resolution deformation
0.13 mm/pixel, fatigue tests – Distribution time independent and
stress range/load ration until fatigue
crack initiation
14 2008 Xue et al. [158] Cast iron (GS51) Fatigue TG-camera (Mercury), focal – Detection of fatigue damage
plane array, 320  240 pixels2, processes by IR-TG
frame rate 12.5 Hz, ultrasonic – Temperature evolution related to
fatigue tests (20 kHz) heat dissipation process
15 2008 Ranc et al. [159] Titanium alloy Fatigue Pyrometric measurements, – Temperature exceed 1100 °C within
Ti–6Al–4V Torsion Kolski split Hopkinson adiabatic shear bands
bar – Heterogeneity of temperature within
bands
16 2008 Pastor et al. [160] Aluminium alloy AA2024 Fatigue TG-camera (Cedip), focal plane – Application of in-house filtering
array, 320  240 pixels2, MWIR, method to the heat diffusion
low cycle fatigue tests, two equation in order to assess
different specimen geometries occurring heat sources
17 2009 Wagner et al. [161] Al alloys (AlSi7Mg0.6, Fatigue TG-camera (Cedip), focal plane – Dependence of temperature increase
AlSi5Cu3Mg); array, 320  240 pixels2, MWIR, and dissipated energy on applied
Steels (AISI 4240, AISI ultrasonic fatigue tests, SEM stress level
5120)
Appendix

(continued)
Table A.3 (continued)
No. Year Author References Material Research field Method Topic + outcome
Appendix

– Crack initiation about 92% of


fatigue life
18 2009 Maquin et al. [162] Steel (rolled), aluminium Fatigue TG-camera (Cedip), focal plane – Methodology for measurement of
array, 160  120 pixels2, 350 Hz small amounts of dissipated heat
frame rate, fatigue tests during cyclic loading below yield
stress
19 2011 Doudard et al. [163] Dual-phase steel Fatigue TG-camera (Jade), focal plane – Identification of heat sources from
array, 320  356 pixel2, MWIR thermal images
– Self-heating test
20 2011 Favier et al., [164, 165], Copper, CuZn, a-Iron Fatigue TG-camera, ultrasonic fatigue – Energy dissipation even at stress
Phung et al. tests amplitudes below the “slip band
threshold”
– Correlation between dissipated
energy and quantity of slip
markings
21 2010 Jones et al. [166] Al alloys Fracture Lock-in thermography – Quantification of crack closure and
mechanics other crack shielding mechanisms
22 2011 Ranc et al. [167] Theoretical work Farcture Thermomechanical model for – Heterogenous temperature field in
mechanics mode I crack the plastic zone in front of a crack
tip
– Effect of dissipation at the crack tip
on the stress intensity factor
23 2012 Fedorova et al. [168] Ti alloy (Ti6Al4V) Fracture TG-camera (Cedip), focal plane – Calculation of the dissipated heat at
GS: mechanics array, 320  256 pixels2, fatigue the crack tip
crack propagation tests – Method for determination of
J-integral or stress intensity factor
from dissipated energy
(continued)
415
Table A.3 (continued)
416

No. Year Author References Material Research field Method Topic + outcome
24 2011 Vives et al. [169] Cu-Zn-Al SMA Plasticity TG-camera (Cedip), resolution – Undercooling during reversed
Single crystal 80 µm/pixel, 100 Hz frame rate martensitic transformation
25 2012 Dunand et al. [170] NiTi SMA Plasticity TG-camera (Flir), 50 Hz frame –
rate, acoustic emission
measurements, cyclic
pseudoelastic loading
26 2013 Bagavathiappan [171] Monitoring – Civil engineering, electrical
et al. components, deformation
monitoring, inspection of
machineries
27 2013 Blanche et al. [172] Copper (GS: 25 µm) Fatigue TG-camera, VHCF, flat specimen – 1D heat diffusion model
28 2013 Basu et al. [173] Magnesium alloy AZ31B Machining TG-camer (Flir), combination – Observation of the deformation
processes with EBSD and XRD zone during machining
29 2013 Phung et al. [174] Copper Fatigue IR measurements of temperature – Increase in dissipation with number
and intrinsic dissipation during of cycles, but no slip markings were
VHCF, in combination with formed
EBSD and AFM
30 2013 Krewerth et al. [175] Aluminium alloy Fatigue TG-camera (Infratec), 640  320 – Detection of internal, surface and
AlSi7Mg1 pixel2, VHCF, correlated multiple crack initiation
fractography
31 2014 Bär et al. [176] High-alloy steel Fatigue TG-camera (Cedip), E-mode: – Dissipation of energy in front of a
thermoelastic effect, D-mode: crack tip independent on the size of
dissipated energy, SENB plastic zone
specimens
32 2014 La Rosa et al. [177] Carbon steel C40 Plasticity TG-camera (Flir), 320  240 – Determination of fatigue limited by
Austenitic steel AISI 304 pixels2, acoustic emission, tensile either thermography or acoustic
tests, fatigue tests emission
(continued)
Appendix
Table A.3 (continued)
No. Year Author References Material Research field Method Topic + outcome
Appendix

33 2015 Blanche et al. [178] Copper Fatigue TG-camera (Flir), 512  640 – Proposal of heat diffusion models
pixel2, VHCF for estimation of dissipated energy
34 2015 Ranc et al. [179] Theoretical work Thermomechanics Orthogonal decomposition of – Partial derivatives of heat diffusion
measured thermal fields equation
– Spectral solution of diffusion
problem
– Estimation of heat sources via heat
equation
35 2015 Charkaluk et al. [180] Theoretical work Thermomechanics Thermomechanical couplings at – Intragranular coupled analysis of
grain scale strain and temperature full-field data
– Thermomechanical confirmation of
early microplasticity
36 2015 Wang et al. [181] Ni single crystal Plasticity TG-camera (Cedip), 320  240 – Radiometric artefact of temperature
(99.999%) pixel2, 120 Hz frame rate, tensile fields due to pronounced surface
tests, RT slip topography
37 2015 Krewerth et al. [182] 42CrMo4 Fatigue TG-camera (Infratec), 640  320 – Full-surface view thermography
pixel2, VHCF, correlated – Subsurface crack initiation detected
fractography by IR-TG
38 2016 Canzar [183] EN-GJS-400-18LT Fracture Experimental method and finite – Estimation of the plastic zone in
mechanics element simulation, CT front of the crack tip
specimens, combination with DIC – Dissipated energy along crack path
39 2016 Charbal et al. [184] Theoretical work Thermomechanics Application of DIC for distortion – Integrated DIC
measurements of IR images – Improvement of recording IR
images
40 2016 Torabian et al. [185] Dual-phase steel (DP600) Fatigue VHCF, R = −1 – Abnormal temperature evolution for
r > 247 MPa
– Thermally activated deformation
mode
– A thermal deformation mode of
ferritic phase
417

(continued)
Table A.3 (continued)
418

No. Year Author References Material Research field Method Topic + outcome
41 2016 Torabian et al. [186] Dual-phase steel (DP600) Fatigue VHCF, R = −1, self-heating tests – Determination of dissipated energy
per cycle
– Dissipated energy per cycle equals
quadratic function of the stress
amplitude
42 2016 Vshivkov et al. [187] Stainless steel (AISI 304) Fatigue Cyclic loading, f = 10 Hz, – Study of thermoelastic effect
Titanium alloy R = −0.1, different stress – Study of fatigue crack growth
concentrators
43 2015 Huang et al. [188] C-Mn steel Fatigue TG-camera (Cedip), 320  240 – Differences in temperature evolution
pixel2, different content of free for steels with different free solute
solute atoms content
44 2016 Ancona et al. [189] Martensitic steel, Fracture Two TG-cameras (Flir, – Amplitude and phase of the thermal
Austenitic steel mechanics Deltatherm), 640  512 pixel2, component
320  256 pixel2, cyclic loading, – Correlation of heat sources to plastic
f = 13 Hz, R = 0.1, CT deformation and crack closure
specimens
45 2016 Crupi et al. [190] Theoretical work Fatigue VHCF – Modelling of surface and
undersurface crack initiation and
related temperature evolution
46 2016 Delpueyo et al. [191] Aluminium alloy AA5052 Plasticity TG-camera (Cedip), 147 Hz – Evolution of PLC bands
frame rate, tensile test, RT – Calorimetric signature of type A and
type B bands
47 2016 Sharkev et al. [192] Titanium (GS: 20 µm and Plasticity TG-camera (Flir), 640  512 – Differences in temperature evolution
200 nm) pixel2, 115 Hz frame rate, tensile for coarse grained and ufg material
tests, RT
48 2016 Krupp et al. [193] Martensitic steel Fatigue TG-camera (ImageIR), in – Formation of protrusion bands
combination with SEM and – Pile-up of protrusion bands at prior
EBSD, FIB, VHCF at 20 kHz and austenite grain boundaries
HCF at 95 Hz
(continued)
Appendix
Table A.3 (continued)
No. Year Author References Material Research field Method Topic + outcome
Appendix

49 2016 Meneghetti and [194] Theoretical work Fatigue Estimation of specific heat energy – Two-dimensional thermal and
Ricotta per cycle in a small volume at the structural problem
tip of a propagating crack
50 2017 Yan et al. [195] Aluminium alloy Plasticity TG-camera (Infratec), 320  240 – Different temperature evolutions in
pixel2, tensile tests, HCF tests, specimens parallel or perpendicular
parallel and transversal to rolling to the rolling direction
direction
51 2017 Torabian et al. [196, 197] Dual-phase steel Fatigue Self-heating measurements, – Main dissipation mechanisms:
VHCF, flat specimens to-and-fro glide of edge dislocations
419
420

Fully-coupled full-field measurements: State of the art (Table A.4).


Table A.4 Chronological overview of the application of fully-coupled full-field measurements starting from 2000
No. Year Author References Material Research field Method Topic + outcome
1 2007 Favier et al. [198] NiTi SMA Plasticity IR-TG + DIC, two specimen surfaces, two – Macroscopic deformation
(thin-wall tubes) cameras (CCD + TC), uniaxial tensile tests, RT, instabilities related to
subset size DIC: 10 pixels localized deformation bands
2 2008 Bodelot et al. [199, 200, Austenitic Plasticity IR-TG + DIC, one specimen side, two cameras – First fully-coupled full-field
201] stainless steel (CCD + TC), dichroic mirror, uniaxial tensile kinematic and thermal
(316L) tests, RT, combined with EBSD, special coating measurements at grain scale
GS: 240 µm for IR and DIC, subset size DIC: 16 pixels on the same area of interest
(104 µm), subset size TG: 3 pixels (90 µm) – Difficulties to link up the
strain localizations with
thermal fields
3 2010 Chrysochoos [78] Steel, Plasticity IR-TG + DIC, two specimen sides, two cameras – Influence of dissipated energy
et al. polycrystalline (CCD + TC), tensile tests, RT and thermocoupling
polymer, single mechanisms on stress-strain
crystalline response
CuZnAl SMA
4 2010 Dumoulin [202] High-strength Plasticity IR-TG + DIC, one specimen side, two cameras – Estimation of heat sources,
et al. steel (CCD + TC), tensile tests, RT, numerical studies stored and dissipated
energies
– High reproducibility of local
and global behaviour
5 2010 Saai et al. [123] Al-Bi crystal Plasticity IR-TG + DIC, one side, two cameras – Heterogeneities of strain and
(CCD + TC), combined with FE modelling, temperature fields caused by
grain orientations and grain
interactions
– Better agreement of
experimental and numerical
results for strain fields than
for thermal fields
Appendix

(continued)
Table A.4 (continued)
No. Year Author References Material Research field Method Topic + outcome
Appendix

6 2011 Bodelot et al. [203] Austenitic Plasticity IR-TG + DIC, two specimen sides, tow cameras – Experimental observation of
stainless steel (CCD + TC), dichroic mirror, uniaxial tensile heat dissipation caused by
(316L) tests, RT, combined with EBSD, subset size DIC: strain heterogeneities
GS: 240 µm 16 pixels (104 µm), subset size TG: 3 pixels – Thermomechanical coupling
(90 µm) at grain scale
7 2011 Seghir et al. [204] Austenitic Plasticity IR-TG + DIC, two specimen sides, two cameras – Simultaneous determination
stainless steel (CCD + TC), dichroic mirror, uniaxial tensile of local strain and
(316L) GS: tests, RT, high emissivity for TG and speckle temperature fields at grain
130 µm pattern for DIC, combined with EBSD and FE scale
modelling – Dislocation density based
thermo-elasto-visco-plastic
model
8 2012 Maynadier [205] NiTi SMA Plasticity IR-TG + DIC (IRIC), one specimen side, TC, – Simultaneous thermal and
et al. uniaxial tensile tests, RT, electropolished surface kinematic full-field
with fine black speckle pattern, subset size: 12 measurements
pixels – Uncertainty of local strain
field same order as usual DIC
– Uncertainty of thermal field
<0.03 K
– Measurement of local and
thermal fields caused by
MPT of SMA
9 2012 Toussaint [206] Carbon-black Plasticity IR-TG + DIC, two specimen sides, two cameras – Complex thermomechanical
et al. filled rubber (CCD + TC), cyclic loading, RT behaviour of elastomeric
materials
10 2012 Delpueyo [207] Cu-Al-Be SMA Plasticity IR-TG + DIC, two specimen sides, two cameras – Good agreement between
et al. (CCD + TC), loading–unloading tests strain and heat maps
– Different strain fields during
loading and unloading
(continued)
421
Table A.4 (continued)
422

No. Year Author References Material Research field Method Topic + outcome
11 2014, Martinez [208, 209] Carbon-black Plasticity IR-TG + DIC, two specimen sides, two cameras – Measurement of heat sources
2015 et al. filled rubber (CCD + TC), cyclic loading, RT at the crack tip
12 2014 Montanini [210] Brass, Thermal Heating experiments, TC of MWIR, – Dual emissivity speckle
et al. thermoplastic expansion pattern
glass fibre – Determination of thermal
reinforced expansion coefficients by
composite IR + DIC
13 2015 Li et al. [211] Aluminium alloy Plasticity IR-TG + DIC, two specimen sides, two cameras – Constrained DIC and IR data
AA1050 (CCD + TC), tensile tests with partial unloadings, processing methods
RT – Characterization of local
themomechanical variables
for each grain
14 2015 Wang et al. [212] Aluminium alloy Thermoelastic IR-TG + DIC, two specimen sides, two cameras – Compensation of motion
stress analysis (CCD + TC), cyclic loading, RT, specimen with within IR images based on
notch or hole DIC
– Improvement of the accuracy
of thermoelastic stress
analysis
15 2016 Wang et al. [213] Al-oligocrystal Plasticity IR-TG + DIC, two specimen sides, two cameras – Observation of pronounced
GS: > 10 mm (CCD + TC), black carbon (TG) and airbrush out-of-plane deformation of
speckle pattern (DIC), combined with oligocrystals
interferometric profilometry – Correlation of out-of-plane
deformation with thermal and
kinematic fields
– Correlation of strain
heterogeneities with
microstructure
(continued)
Appendix
Table A.4 (continued)
No. Year Author References Material Research field Method Topic + outcome
Appendix

16 2008 Chrysochoos [214, 215] Dual-phase steel Fatigue IR-TG + DIC, two specimen sides, two cameras – Estimation of deformation
et al. (DP600) (CCD, TC) cyclic loading, incremental step tests, energy and dissipated energy
RT per cycle
17 2014 Plekhov et al. [216] Ti alloy Fatigue IR-TG + DIC (IRIC), one specimen side, TC, – Calculation of heat
(Ti-4.2Al-1.6Mn) uniaxial cyclic loading, RT, thin layer of dissipation at the crack tip
amorphous carbon on polished specimen surface – Shape of the plastic zone in
front of the crack tip
18 2016 Ahadi et al. [116] NiTi SMA Fatigue IR-TG + DIC, uniaxial cyclic loading with – Grain size dependence of
GS: 1.5 µm– pre-cracked CT specimens, two specimen sides, fracture toughness and crack
10 nm two cameras (CCD + TC), silicon micro particles growth resistance
(DIC), candle fume (TG) – Reduction of grain size
results in decrease in KIc and
transformation zone in front
of the crack tip
19 2011 Chan et al. [217] Ni Plasticity IR-TG + DIC, two specimen sides, two cameras – Interdependence of heat
(GS = 30 µm) (high-speed CCD and TC), tensile deformation, generation and strain
and RT localization
electrodeposited – 30 µm: decreasing trend of
Ni (GS = 30 nm) heat convertion
– 30 nm: increasing trend of
heat conversion
20 2001 Guduru et al. [218] Maraging steel Fracture IR-TG + DIC, two specimen sides, two cameras – Failure mode transition from
C300 mechanics (high-speed CCD and TC), impact test on crack opening to shear band
pre-cracked specimens, coherent gradient sensing formation
– Non-uniform temperature
distribution along shear band
(continued)
423
Table A.4 (continued)
424

No. Year Author References Material Research field Method Topic + outcome
21 2011 Silva et al. [219] Aluminium alloy Thermoelastic IR-TG + DIC, single camera setup, uniaxial cyclic – Contrast conditions both for
AA 2024 stress analysis loading, specimens with noth or hole IR and DIC
– Influence of specimen
movement
22 2011 Badulescu [86] Aluminium Mechanics TG-camera (Cedip), focal plane array, 320  240 – Calculation of heat sources
et al. GS: centimetre pixels2, MWIR, tensile tests, DIC, fully-coupled and strain maps
full-field measurements, crystal plasticity FEM – Agreement of heat source
distribution on local strain
increments
– Estimation of stored energy
of individual grains
23 2012 Seghir et al. [220] Austenitic Thermomechanics See (9), combined with FE modelling – Energy storage within
stainless steel material during plastic
(316L) GS: deformation
130 µm – Estimation of the local
heterogeneities of stored
energy
24 2012 Seghir et al. [221] Austenitic Thermomechanics See (9, 10), combined with EBSD – Crystallography-based
stainless steel projection technique of
(316L) GS: temperature and
130 µm displacement fields on
polynomial basis
25 2013 Seghir et al. [222] Austenitic Thermomechanics See (9, 10) – Determination of errors for
stainless steel the fully-coupled full-field
(316L) GS: kinematic and thermal
130 µm measurements
– Decomposition of
measurements in the Eulerian
and Lagrangian parts
Appendix
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Index

A Brass (Bs)-type shear bands, 32


Accumulative Roll Bonding (ARB), 381 Broadband sensors, 136
Accuracy, 307 Burgers vector, 11
Acoustic emission, 116
Acoustic Emission (AE) measurement method, C
The, 115 Carbon diffusion, 359
Activated slip systems, 211 Chi-square ðv2 Þ distribution, 124
Activation energy, 358 Chromium and nickel equivalents, 85
Activity, 118 Classification, 148
Adaptive Sequential k-means (ASK) algorithm, Close-packed planes and directions, 11
150 Clustering, 148
Adiabatic shear bands, 32 Complementary in situ investigations, 248
Advanced high-strength steels, 71 Confocal laser scanning microscope, 103
AE amplitudeUp , 118 Confocal microscopy, 103
AE data acquisition, 139 Conjugate system, 20
AE instrument, 138 Considére criterion, 26
AE sensor, 135 Continuous AE, 313
Airbrush technology, 159 Continuous signals, 117
Al-alloyed TWIP, 73 Co-planar system, 20
Allotrope modifications, 52 Copper (C)-type shear bands, 32
a′-martensite, 53 Correlation algorithm, 164
Asymptotic SRS, 40 Correlation coefficient, 166
Austenite, 47 Cottrell effect, 34
Austenite-stabilizing, 53 Critical resolved shear stress, 19
Auto-correlation functions, 120 Critical slip system, 20
Average frequency, 119 Critical strain for the onset of twinning, 82
Critical true strain, 358
B Cross-Correlation (CC) algorithm, 164
Background noise, 144 Cross-slip, 15
Back-stress, 22 Cross-slip system, 20
Bain, 48 Crystallographic orientation, 27, 211
Bain transformation, 55 Cumulated plastic strain, 282
Band Contrast (BC) maps, 211 Cyclic loading, 209
Biaxial loading, 210
Body force, 130

© Springer Nature Switzerland AG 2020 435


A. Weidner, Deformation Processes in TRIP/TWIP Steels,
Springer Series in Materials Science 295,
https://doi.org/10.1007/978-3-030-37149-4
436 Index

D Forward stress, 22
Data categorization and cluster analysis, 147 Fourier transformation, 143
Data reduction and factor analysis, 146 Frank partials, 15
Deformation bands, 24 Full-field measurement, 157
Deposition of particles, 160 Fully-coupled full-field, 157
Descriptive statistics and time-series analysis, Fully-coupled, full-field measurements, 101
142
Detectability of AE, 132 G
Dichroic mirrors, 362 c-martensite, 53
Digital image correlation, 157 General description of AE time series in time
Direct c to e transformation, 60 domain, 141
Direct e to a′ transformation, 61 Gibbs free energy, 50
Discrete Fourier transformation, 143 g-matrices, 211, 257
Dislocation, 9 Green’s functions, 130
Dislocation density, 22 Grid technology, 160
Dislocation glide, 11
Dislocation lack yield point, 34 H
Displacement fields, 157 Habit plane, 47
Displacement mapping, 163 Hall–Petch effect, 75
Displacement mapping functions, 163 Hall–Petch relationship, 22
Displacive movement, 47 Hart criterion, 26
Dissimilarity, 149 Heaviside function, 130
Double-ended slip bands, 28 High-alloy Fe–16Cr–6Mn–xNi–0.05C, 205
Double slip, 20 High-alloy TRIP steels, 84
Drift distortions, 308 High austenite stability, 323
Driving force, 84 Highly distorted, 235
Duration, 119 High-manganese TWIP, 73
Dynamic strain aging, 33 High-resolution TEM, 212
High-speed cameras, 104
E Hits, 117
Edge dislocations, 9 Hsu-Nielsen source, 136
Electron Backscattered Diffraction (EBSD), h-type criterion, 26
210 Hydrostatic pressure, 231
Electron Channelling Contrast Imaging
(ECCI), 210 I
Elevated temperatures, 250 Image of deformed state, 159
Energy E (or power) of the AE signals, 127 Image pattern contrast, 158
Energy of AE, 119 Incubation period, 282
e-martensite, 53 Indirect c–a′ transformation via e-martensite,
Etching technique, 161 62
Extrinsic stacking fault, 13 Infrared–thermography, 157
In situ cyclic experiments, 250
F In situ experiments, 99
Facet, 161 In situ SEM testing, 366
Fast Fourier transformation, 141 In situ tensile tests, 250
Faulted austenite, 235 Instantaneous SRS, 40
Fe–16Cr–6Mn–3Ni–0.05C, 241 Instrumentation, 135
Fe–16Cr–6Mn–6Ni–0.05C, 221 Integrated Computational Materials
Fe–16Cr–6Mn–9Ni–0.05C, 238 Engineering (ICME), 368
Ferrite-stabilizing, 52 Interrupted monitoring, 100
Fine-grained material, 378 Intrinsic stacking fault, 13
First-order phase transition, 47 Invariant shear systems, 302
First-order shape functions, 163 Inverse pole figure colouring could, 211
Forest dislocations, 34
Index 437

K Non-thermoelastic MPT, 50
Kaiser effect, 153 Normal distribution, 121
Kernel average misorientation, 211 Normalized CC, 164
Kinematic displacement, 157 Normalized PSDF, 128
Kolmogorov–Smirnov, 129 Normalized SSD, 164
Kullback–Leibler divergence, 149 Number of counts, 119
Kurdjumov–Sachs, 48
Kurdjumov–Sachs transformation, 56 O
Kurtosis, 121 Olson–Cohen model, 66
Optical microscopy, 102
L Orientation relationships, 48
Laminates, 381
Large-chamber SEM, 111 P
Lateral resolution, 309 Parametric, 149
Lomer-Cottrell-lock, 13 Partial dislocation-mediated twins, 279
Long-distance (or long focus) microscopes, Partial dislocations, 12
104 Persistent slip bands, 24
Long-pass filters, 362 Persistent slip markings, 29
Low-alloyed multiphase TRIP steels, 74 Phase map, 211
Lowest austenite stability, 241, 328 Piezo-electric sensors, 136
Lüders bands, 24 Pile-up, 22
Lüders effect, 33 Pitsch OR, 270
Lüders strain plateau, 36 Planar-biaxial loading, 219
Planar glide, 15
M Plastic deformation, 7
Macroscopic strain localizations, 340 Poisson distribution, 122
Magnetic measurements, 213 Pole mechanism, 17
Magnitude of shear s, 276 Portevin–Le Chatelier bands, 24
Martensite, 47 Portevin–Le Chatelier effect, 33
Martensite variants, 59 Power spectral density functions, 120
Martensitic phase transformation, 47 Pre-amplifier, 135
Martensitic start temperature, 51 Primary slip system, 19
Mean free path of dislocations, 22 Probability density functions, 120
Mean square values, 120 Pronounced TRIP effect, 338
Measure of distance, 149 Pronounced TWIP effect, 335
Mechanical loading devices, 110
Mechanical stress-strain hysteresis loops, 281 Q
Median frequency fm , 127 Quasi-hydrostatic high-pressure deformation,
Medium austenite stability, 326 210
MgO partially stabilized ZrO2, 379 Quasi in situ, 100
Micro bands, 32
Micro shear bands, 32 R
Microstructural characterizations, 210 Random data, 120
Miniaturized loading devices, 109 Random (stochastic) processes, 120
Mobile dislocations, 34 Real-time, 100
Multiple slip, 20 Real-time in situ experiments, 100
Multivariate random time-series process, 140 Reference image, 159
Reference subset, 161
N Resolution, 307
Nishiyama–Wassermann, 48 Resolution of the localized strains, 309
Nishiyama–Wassermann transformation, 59 Resonant, 136
Nomarski interference contrast, 102 Response function, 117
Non-parametric, 149 Rigid body translation, 163
Non-supervised, 148
438 Index

S Stress-assisted MPT, 207


Scanning electron microscopy, 102, 210 Stress-strain curve, 7
Schmid factor, 19 S-type criterion, 26
Schmid’s law, 19 Sub-lDIC, 256
Scratch testing, 375 Subpixel accuracy, 166
Screw dislocations, 9 Substitutional or interstitial atoms, 39
Search field, 162 Sum of Squared Difference (SSD) algorithm,
Second-order shape functions, 163 164
Self-accommodation, 303 Supervised, 148
Serrated plastic flow, 37 Suzuki effect, 34
SF tetrahedron, 13
Shape functions U and V, 163 T
Shape memory materials, 382 Temporal evolution, 313
Shear bands, 24 Texture, 94
Shear deformation mechanism, 60 Thermal fields, 157
Shear plane, 15 Thermal loading devices, 110
Shear strain amplitude, 31 Thermodynamic, 73
Shockley partial dislocations, 12 Thermoelastic MPT, 50
R3 boundary, 16 Threshold-based data acquisition, 139
Similarity, 148 Threshold-less, 313
Single crystalline material, 377 Top-down, 370
Single-ended slip band, 28 Top-down approach, 369
Single-phase TWIP, 74 Total number of hits N, 117
Skewness, 121 Total strain amplitude, 282
Slip bands, 24 Transducer, 116
Slip line, 28 Transfer function, 117
Slip system, 19 Transition from TRIP to TWIP effect, 336
Sources of AE, 130 Transmission Scanning Electron Microscopy
Specimen coordinate system, 286 (t-SEM), 212
Spectral analysis, 143 Transformation-induced plasticity, 71
Spontaneous, 207 Transient signals, 117
Stacking fault, 13 TRIP-assisted steels, 83
Stacking-fault energy, 14 TRIP effect, 72
Standard CC, 164 TRIP matrix composites, 379
Standard SSD, 164 T-type criterion, 26
Stationary and propagative strain localizations, Twin boundary, 16
24 Twin bundles, 277
Steel with highest and medium austenite Twin direction, 15
stability, 322 Twin-free grains, 82
Steel with lowest austenite stability, 322 Twinned grains, 82
Stereographic projection, 286 Twinning, 15
Stereographic standard triangle, 19 Twinning-induced plasticity, 71
Strain error fields, 308 Twinning systems, 16
Strain fields, 157 Twin plane, 15
Strain hardening, 21 TWIP effect, 72
Strain-hardening curves, 23 Two-step shear mechanism, 58
Strain-induced martensitic transformation, 51
Strain-induced MPT, 207 U
Strain localizations, 24 Ultrafine-grained microstructure, 378
Strain rate, 40 Undercooling, 51
Strain-rate sensitivity, 40 Uniaxial cyclic loading, 217
Strain softening, 25 Uniaxial monotonic loading, 209
Stress-accommodating systems, 303 Uniaxial quasi-static loading, 213
Stress-assisted, 51
Index 439

V X
Variant selection, 59 X-ray diffraction, 212
Volume fraction of twins, 82
Z
W Zero-normalized CC, 164
Welch function, 144 Zero-normalized SSD, 164
Wiener–Khinchin theorem, 129 Zero-order shape functions, 163

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