metals

Article
A New Electron Backscatter Diffraction-Based
Method to Study the Role of Crystallographic
Orientation in Ductile Damage Initiation †
Behnam Shakerifard 1, *, Jesus Galan Lopez 1,2 and Leo A. I. Kestens 1,3
1 Materials Science and Engineering Department, Faculty 3mE, Delft University of Technology, Mekelweg 2,
2628 CD Delft, The Netherlands; j.galanlopez@tudelft.nl (J.G.L.); Leo.Kestens@UGent.be (L.A.I.K.)
2 Materials innovation institute M2i, Elektronicaweg 25, 2628 XG Delft, The Netherlands
3 EEMMECS department, Metals Science and Technology Group, Faculty of Engineering and Architecture,
Ghent University, Technologiepark Zwijnaarde 903, 9052 Ghent, Belgium
* Correspondence: b.shakerifard@tudelft.nl or behnam.shakerifard@gmail.com; Tel.: +31-15-27-822-02
† This paper is an extended version of our paper published in the 18th International Conference on Textures of
Materials (ICOTOM 18), St George, UT, USA, 5–10 November, 2017.




Received: 19 October 2019; Accepted: 6 January 2020; Published: 12 January 2020


Abstract: The third generation of advanced high strength steels shows promising properties for
automotive applications. The macroscopic mechanical response of this generation can be further
improved by a better understanding of failure mechanisms on the microstructural level and
micro-mechanical behavior under various loading conditions. In the current study, the microstructure
of a multiphase low silicon bainitic steel is characterized with a scanning electron microscope (SEM)
equipped with an electron backscatter diffraction detector. A uniaxial tensile test is carried out on
the bainitic steel with martensite and carbides as second phase constituents. An extensive image
processing on SEM micrographs is conducted in order to quantify the void evolution during plastic
deformation. Later, a new post-mortem electron backscatter diffraction-based method is introduced to
address the correlation between crystallographic orientation and damage initiation. In this multiphase
steel, particular crystallographic orientation components were observed to be highly susceptible
to micro-void formation. It is shown that stress concentration around voids is rather relaxed by
void growth than local plasticity. Therefore, this post-mortem method can be used as a validation
tool together with a crystal plasticity-based hardening model in order to predict the susceptible
crystallographic orientations to damage nucleation.

Keywords: steels; bainite; crystallographic orientations; ductile failure; void initiation.

1. Introduction
Advanced high strength steels (AHSSs) and, in particular, the third generation of AHSSs with
bainitic matrix have shown remarkable potential for automotive applications [1,2]. Complex multiphase
bainitic steels with second phase constituents martensite and retained austenite are promising
candidates to reach an optimum balance between strength, ductility, and formability [3–9]. Developing
bainitic steels with enhanced properties would enable weight reduction of the car body, thus reducing
fuel consumption and pollution and saving energy. Studying the micro-mechanical behavior and
damage micro-mechanisms of such multiphase steels is essential for developing a bainitic microstructure
with improved properties. In multiphase steels, it has been well reported that microstructural
heterogeneities, such as different phases with various mechanical contrast, play a significant role in the
partitioning of stress (and/or strain) during plastic deformation [10–13]. Hence, at the microstructure

Metals 2020, 10, 113; doi:10.3390/met10010113 www.mdpi.com/journal/metals

Metals 2020, 10, 113 2 of 11

level, these local deformation incompatibilities may induce void formation at the critical moment in
Metals 2019, 9, x FOR PEER REVIEW 2 of 11
order to dissipate the local plastic work.
The role of the second phase (i.e., martensite) and its morphology (size, shape, and distribution) in
ductile damage initiation in dual phase steels has been extensively studied by advanced experimental
at the microstructure level, these local deformation incompatibilities may induce void formation at the
and crystal
critical plasticity-based
moment modelling
in order to dissipate the techniques [14–18]. Moreover, in polycrystalline materials,
local plastic work.
the anisotropic
The role ofresponse
the second of each
phase individual crystallographic
(i.e., martensite) orientation(size,
and its morphology to stress
shape,(and/or strain) is another
and distribution) in
important
ductile damage initiation in dual phase steels has been extensively studied by advanced[19]
factor that needs to be considered in damage initiation mechanisms. Jia et al. have shown
experimental
forand
a duplex
crystalstainless steel that,
plasticity-based at high macroscopic
modelling stresses,
techniques [14–18]. when allin
Moreover, grains in both constituent
polycrystalline materials,phases
the
deform plastically,
anisotropic response the of
role of individual
each the crystallographic orientation
crystallographic anisotropy
orientation to stresson(and/or
stress–strain
strain) is partitioning
another
is important
more pronouncedfactor thatthan
needstheto be considered
phase in damage
contrast. The roleinitiation mechanisms. Jiaorientation
of crystallographic et al. [19] have onshown
damage
for a duplex stainless steel that, at high macroscopic stresses, when all grains in
initiation at relatively high levels of plastic deformations was also observed on metal–matrix [20], rigidboth constituent phases
deform
fiber plastically,
composites [21],the
asrole
wellofasthe
in crystallographic orientation
an austenitic stainless steelanisotropy
under theon stress–strain
cyclic loading partitioning
condition [22].
is more pronounced
Eventually, in multiphase thanpolycrystalline
the phase contrast. The role
materials, the of crystallographic
simultaneous effectorientation on damage
of phase contrast, with
initiation at relatively high levels of plastic deformations was also observed
various morphologies, and crystallographic orientation on damage initiation is a frequent topic of on metal–matrix [20], rigid
fiber composites [21], as well as in an austenitic stainless steel under the cyclic loading condition [22].
investigation [15,22–24].
Eventually, in multiphase polycrystalline materials, the simultaneous effect of phase contrast, with
In the current study, firstly, a comprehensive and quantitative microstructural characterization
various morphologies, and crystallographic orientation on damage initiation is a frequent topic of
is performed using a scanning electron microscope (SEM) equipped with an electron backscatter
investigation [15,22–24].
diffraction
In the (EBSD)
current detector. Second,
study, firstly, a quantitativeand
a comprehensive analysis on void
quantitative distribution and
microstructural its correlation
characterization is to
theperformed
macroscopic usingstrain is conducted.
a scanning electron This enables to(SEM)
microscope understand
equipped at which
with an macroscopic strain level
electron backscatter
damage
diffraction (EBSD) detector. Second, a quantitative analysis on void distribution and its correlationtotothe
initiates in the microstructure. In this research work, particular attention is given
crystallographic
the macroscopicorientation aspect of damage
strain is conducted. initiation,
This enables while theatmechanical
to understand phase contrast
which macroscopic and its
strain level
morphological
damage initiates aspectin is
thereported elsewhere
microstructure. Inby Shakerifard
this et al. [18].
research work, An EBSD
particular analysis
attention is employed
is given to the to
crystallographic
observe orientation
the orientations aroundaspect
the of damage
initiated initiation,
voids. while the
Afterwards, mechanical
textures phase contrast
are calculated and its
and compared
morphological aspect is reported elsewhere by Shakerifard
in order to study the correlation between damage and crystallographic orientation. et al. [18]. An EBSD analysis is employed
to observe the orientations around the initiated voids. Afterwards, textures are calculated and
2. compared
Materialsin
and Methods
order to study the correlation between damage and crystallographic orientation.

The bainitic
2. Materials andsteel used in the current study has a low silicon content. The chemical composition
Methods
is shown in Table 1. The 1 mm thick sheet of cold rolled ferritic–pearlitic steel is annealed above the
The bainiticin
Ac3 temperature steel
theused in the
Vatron current study
Annealing has a low
Simulator silicon content.
® (Vatron, The chemical
Linz, Austria), and composition
quenched toisthe
shown in Table 1. The 1 mm thick sheet of cold rolled ferritic–pearlitic steel is annealed above the Ac3
bainite holding temperature of 450 ◦ C for the holding time of 120 s. Following bainite transformation,
temperature in the Vatron Annealing Simulator® (Vatron, Linz, Austria), and quenched to the bainite
the material is quenched to room temperature. The annealing cycle of the developed bainitic steel is
holding temperature of 450 °C for the holding time of 120 s. Following bainite transformation, the
depicted in Figure 1.
material is quenched to room temperature. The annealing cycle of the developed bainitic steel is
depicted in Figure 1.
Table 1. Chemical composition of the studied bainitic steel (wt.%).

Elements Table 1. Chemical

C% Mn% composition
Si% ofCr%
the studied bainitic steel
Al% P%(wt.%). S% N%
Steel Elements
0.215 C%1.96 Mn%0.10
Si% Cr%
0.61 Al%0.020P% 0.007
S% N%
0.0027 0.005
Steel 0.215 1.96 0.10 0.61 0.020 0.007 0.0027 0.005

Figure Schematic
1. 1.
Figure Schematicillustration
illustration of
of the annealingcycle
the annealing cycleused
usedtotodevelop
developthethe bainitic
bainitic steel.
steel.
Metals 2020, 10, 113 3 of 11

In order to analyze the microstructure of this bainitic steel, as reported by Shakerifard et al. [9],
samples are prepared by the standard metallographic steps of grinding, diamond polishing, and polishing
with colloidal SiO2 . A scanning electron microscope FEI® (SEM-Quanta FEG 450, FEI, Hillsboro, OR,
USA) equipped with EBSD detector is employed to characterize the microstructure of the samples prior
to and after tensile testing. EBSD maps are recorded with a step size of 0.05 µm and post processed
with the EDAX-TSLOIM AnalysisTM software.
The investigated steel consists of a bainitic matrix with two main second phase constituents of
martensite and carbide. However, two types of martensites are observed: (i) auto-tempered martensite
(ATM) and (ii) MA islands, which are composed of isolated martensite blocks (M) with a negligible
fraction of retained austenite (A) between the martensite laths [18]. The EBSD technique is employed
to quantify the grain size and fraction of bainite and martensite (ATM and MA) separately. For this
purpose, the grain average image quality (GAIQ) parameter, directly correlated to the sharpness of
the Kikuchi pattern, is used in order to distinguish these two constituents [14,15,25]. This is possible
because the martensite phase demonstrates a lower IQ parameter compared with bainite, as a result of
intrinsic distortion in the martensitic crystal structure, and higher dislocation density compared with
bainite. Grains are defined with a minimum number of five pixels and a misorientation threshold of
five degrees. The grain size is measured based on the linear intercept method and by averaging lines
along both the rolling and normal directions (RD and ND) for each phase.
The fraction of MA islands is measured separately from the total martensite (ATM and MA)
fraction by a specific etching method. Initially, the surface of the samples is activated by ethanol, which
is quickly followed by Klemm etchant (50 mL saturated aqueous sodium thiosulfate, 1 g potassium
metabisulfite) color etching. Later, ten backscatter electron (BSE) images, which provide an enhanced
contrast between matrix and MA islands compared with secondary electron images, are captured
from the sample and binarized into black and white images. In addition, the fraction of MA islands is
measured by image processing.
Uniaxial tensile tests are performed at room temperature with strain rates of 2 × 10−5 and 8 × 10−3 s−1
in the elastic and plastic regions of the tensile curve, respectively, in order to examine the tensile
properties of the bainitic steel. Tensile tests are carried out based on the DIN EN 6892-1 standard using
a Zwick Z100® tensile machine (ZwickRoell AG, Fürstenfeld, Austria). Dog-bone specimens with a
width and gauge length of 6.25 and 25 mm, respectively, are loaded along the rolling direction (RD).
Two tests are performed, and elongations are measured by the extensometer. Additionally, two tensile
tests are interrupted in the uniform and non-uniform regions, respectively, in order to investigate the
evolution of damage within the microstructure at various strain levels.
Tasan et al. [16] have conducted an extensive study on various techniques for the quantification of
voids evolution during plastic deformation. They have reported that microscopic techniques such
as 2D SEM and 3D X-ray micro-tomography (XµT) provide significant information regarding the
strain levels and the involved micro-mechanisms in damage initiation and evolution compared with
mechanical-based techniques. The possible drawback of the 2D SEM technique is an underestimation
in damage quantities, where voids may smear-out by mechanical polishing. Lai et al. [26] have
demonstrated that the advantage of the SEM-based technique is its high resolution and its ability to
detect smaller voids compared with XµT. However, as reported by Landron et al. [27,28], the XµT can
provide 3D visual information with regard to growth characteristics of individual void.
In the current study, the quantification of voids is performed by a high resolution FEG-SEM Nova
600 (FEI, Hillsboro, OR, USA). The evolution of voids as a function of the plastic strain is studied on
the RD–ND section in the middle width of the fractured tensile samples. Two variables are considered
to quantify the evolution of voids: (i) the void number density (VD) and (ii) the void area fraction
(VAF) in the 2D section of microscopic observation. The VD indicates the nucleation activity of voids
during plastic deformation, while VAF includes void growth in addition to nucleation. This SEM-based
technique provides the possibility to visualize the dispersion of the voids within the microstructure.
True plastic strain εlongitudinal values are calculated in equally distanced intervals from the fracture
Metals 2019, 9, x FOR PEER REVIEW 4 of 11
Metals 2020, 10, 113 4 of 11

surface based on the normal (𝜀thickness ) and transversal strains (𝜀transveral ) using optical microscopy
surface based on the normal (εthickness ) and transversal strains (εtransveral ) using optical microscopy
images and the following equations:
images and the following equations:
𝐴00
A
ε𝜀fracture
fracture==ln
ln , (1)
(1)
A
𝐴𝑓f
t𝑡f𝑓 𝑤
w𝑓f
εlongitudinal (εthickness
𝜀longitudinal==−−(𝜀thickness++ε𝜀 ) )==lnln +
transveral
transveral + ln
ln ,, (2)
(2)
t𝑡00 𝑤
w00
where𝐴A
where 00is is
thethe initial
initial cross-section
cross-section areaarea
of theoftensile
the tensile and 𝐴𝑓 and
samplesample is theAfracture
f is the surface
fracturearea
surface area
(measured
(measured by optical microscope image) in Equation (1). The
by optical microscope image) in Equation (1). The 𝑡0 , 𝑡𝑓 , 𝑤0 , and 𝑤0𝑓 are t , t , w
f the , and w
0 thickness f are the thickness
and width values andof
width
the values
tensile sampleof the tensile
prior and sample priortest,
after tensile andrespectively.
after tensile Atest, respectively.
field of approximatelyA field1ofmm approximately
2 is examined

1 mm 2 is examined by running an automated image acquisition software to capture over 1000 SEM
by running an automated image acquisition software to capture over 1000 SEM micrographs. The SEM
micrographs.are
micrographs The SEM micrographs
captured are captured
with a magnification with ahaving
of 4000×, magnification
a width and of 4000×,
heighthaving
of 1024a×width and
884 pixels,
height of 1024
respectively. × 884settings
These pixels, provide
respectively. These
a pixel settings of
resolution provide
31 nma andpixelenable
resolution of 31 the
to detect nm micro-voids
and enable
to detect @ (R2017(a), MathWorks, Natick,
within thethe micro-voids within
microstructure. Matlabthe microstructure.
@ (R2017(a), MatlabNatick,
MathWorks, MA, USA) and ImageJ@ software MA, USA)(1.5
and ImageJ @ software
1P, NIH, WA, USA) with(1.5 1P, NIH,
specific image WA, USA) with
processing specificisimage
algorithm used toprocessing algorithm
stich and study is used to
all micrographs.
Astich
voidand
sizestudy all is
criterion micrographs. A void
defined in which sizevoids
all the criterion is than
larger defined
0.1 µmin which all theare
2 (≈33 pixels) voids larger than
counted.
0.1 µm2 (≈33 pixels) are counted.
3. Results and Discussion
3. Results and Discussion
3.1. Microstructure Characterization
3.1. Microstructure Characterization
The microstructures of the low Si bainitic steel are shown in Figure 2. The bainitic steel reveals a
The microstructures of the low Si bainitic steel are shown in Figure 2. The bainitic steel reveals a
bainitic matrix in which small carbides are observed, whereby isolated MA islands are also observed
bainitic matrix in which small carbides are observed, whereby isolated MA islands are also observed within
within the bainitic matrix. Table 2 quantitatively illustrates the microstructural variations of the bainitic
the bainitic matrix. Table 2 quantitatively illustrates the microstructural variations of the bainitic steel.
steel.

Figure
Figure2.2.Scanning
Scanningelectron
electronmicrographs
micrographs ofof the
the bainitic steel under
bainitic steel under consideration:
consideration: (a)
(a)SEM
SEMmicrograph
micrograph
ofofthe
themicrostructure
microstructureetched
etchedbybyKlemm;
Klemm;(b)
(b)SEM
SEMmicrograph
micrograph ofof
the microstructure
the microstructure etched
etchedbyby
Nital; (c)
Nital;
image
(c) image quality map and the fraction of retained austenite is negligible (<1%). The rolling directionis
quality map and the fraction of retained austenite is negligible (<1%). The rolling direction
along thethe
is along horizontal axis
horizontal and
axis andthe
thenormal
normaldirection
directionisis along
along the vertical axis.
the vertical axis. ATM,
ATM,auto-tempered
auto-tempered
martensite;
martensite;SEM,
SEM,scanning
scanningelectron
electronmicroscope.
microscope.
Metals 2019, 9, x FOR PEER REVIEW 5 of 11
Metals 2020, 10, 113 5 of 11

Table 2. Microstructural variables of the bainitic steel.

Table 2. Microstructural variables of the bainitic steel.
Sample Phases Grain Size (m) Fraction (%) Block Size (m) Cementite Size (m)
Sample BainitePhases 1.44  0.01
Grain Size (µm) Fraction
Bal (%) Block Size
- (µm) Cementite Size
- (µm)
Bainitic MA Bainite -1.44 ± 0.01 3.4  1.7
Bal 0.7  0.35
- - -
steel CementiteMA - -  1.0
3.6 3.4 ± 1.7 0.7 ±
- 0.35 -  0.04
0.07
Bainitic steel
ATMCementite
1 0.5  0.1 -  1.8
4.8 3.6 ± 1.0 -- 0.07 ± 0.04
-
ATM1 0.5 ± 0.1 4.8 ± 1.8 - -
1 Auto-tempered martensite (ATM) phase was exposed by Nital etchant and quantified by the
1
Auto-tempered martensite (ATM) phase was exposed by Nital etchant and quantified by the subtraction of whole
subtraction of whole martensitic region measured by electron backscatter diffraction (EBSD) from
martensitic region measured by electron backscatter diffraction (EBSD) from MA regions.
MA regions.
3.2. Tensile Test
3.2. Tensile Test
The tensile curve and mechanical properties of the material are depicted in Figure 3. The engineering
The tensile curve and mechanical properties of the material are depicted in Figure 3. The
tensile curve of the material demonstrates the small non-uniform region, which implies that the steel
engineering tensile curve of the material demonstrates the small non-uniform region, which implies
could not accommodate considerable elongation beyond the uniform plastic domain. The localized
that the steel could not accommodate considerable elongation beyond the uniform plastic domain. The
necking behavior (cf. Figure 4) of the material also confirms the small post-necking region of the
localized necking behavior (cf. Figure 4) of the material also confirms the small post-necking region of
tensile curve.
the tensile curve.

Figure 3.
Figure 3. Engineering
Engineering stress
stress and
and elongation curve with
elongation curve with corresponding
corresponding tensile
tensile properties.
properties.

3.3.Damage
3.3. DamageAnalysis
Analysis

3.3.1.Quantitative
3.3.1. QuantitativeAnalysis
AnalysisofofVoids’
Voids’Evolution
Evolution
Figure44demonstrates
Figure demonstratesthe the RD–ND
RD–ND cross
cross section
section at half
at half widthwidth
of theoffracture
the fracture tensile
tensile sample sample
before
and after image processing. The size of the voids and their shape fully correspond to theirreal
before and after image processing. The size of the voids and their shape fully correspond to their real
geometry. ItItisisobserved
geometry. observed that
that voids
voids are
are only
only present
present atat the
the neck
neck region
region ofof the
the fractured
fracturedtensile
tensilesample.
sample.
Voids are
Voids are distributed
distributed heterogeneously
heterogeneously and and more
more densely
densely present
present inin the
the vicinity
vicinityof ofthe
thefracture
fracturesurface.
surface.
The microstructural observation of the interrupted tensile sample at the elongation
The microstructural observation of the interrupted tensile sample at the elongation of 5%, reported of 5%, reported
elsewhereby
elsewhere byShakerifard
Shakerifard et et
al.al. [18],
[18], confirmed
confirmed the the absence
absence of void
of void formation
formation duringduring the uniform
the uniform plastic
plastic deformation.
deformation. In contrast
In contrast to this to this bainitic
bainitic martensitic
martensitic steel,
steel, for for ferritic
ferritic and martensitic
and martensitic dualdualphasephase
(DP)
(DP) steels, it has been reported that voids can nucleate in the early stage of plastic
steels, it has been reported that voids can nucleate in the early stage of plastic deformation prior to deformation prior
to necking
necking [29].[29].
It is observed in Figure 5 that VD and VAF parameters increase with the plastic deformation.
The exponential trend of these two damage-related parameters demonstrates a sudden increase at
the strain level of 74%. The localized necking behavior of the fracture tensile sample close to fracture
surface (cf. Figure 4) resulted in higher stress triaxiality, and thus increases VAF significantly.
 Metals2019,
Metals 2020,9,10, 113 PEER REVIEW
x FOR 6 6ofof1111

Figure 4. Roughly 1000 contiguous high-resolution SEM micrographs (each ≈ 27 × 32 µ m2); (a) after
stitching all SEM micrographs and (b) image processed, whereby voids are magnified 50× with respect
to matrix pixels for enhanced visualization.

It is observed in Figure 5 that VD and VAF parameters increase with the plastic deformation. The
exponential
Figure4.trend
Figure of these
4.Roughly
Roughly 1000 two
1000 damage-related
contiguous
contiguous parameters
high-resolution
high-resolution SEM demonstrates
SEM micrographs
micrographs a sudden
(each ≈ increase
≈ 27 ×× 32
32 µm at after
µ m22);); (a)
(a) the
afterstrain
level stitching
of 74%. all
stitching The localized
allSEM
SEM necking
micrographs
micrographs andbehavior
and (b) imageof
(b)image the fracture
processed,
processed, tensile
whereby sample
voids
voids close to50×
are magnified
are magnified fracture
50× withrespect
with surface (cf.
respect
Figure 4) resulted
totomatrix
matrixpixels in higher
pixelsfor stress
forenhanced triaxiality,
enhancedvisualization.
visualization. and thus increases VAF significantly.

It is observed in Figure 5 that VD and VAF parameters increase with the plastic deformation. The
exponential trend of these two damage-related parameters demonstrates a sudden increase at the strain
level of 74%. The localized necking behavior of the fracture tensile sample close to fracture surface (cf.
Figure 4) resulted in higher stress triaxiality, and thus increases VAF significantly.

Figure
Figure 5.
5. Quantitative
Quantitativeanalysis
analysisof
ofvoids’
voids’evolution
evolution as
as aa function
function of
of true
true plastic
plastic strain.
strain.

3.3.2.Crystallographic
3.3.2. CrystallographicOrientation
OrientationAspect
AspectofofVoid
VoidInitiation
Initiation
Theindividual
The individualrole roleofofmartensite
martensiteas asaahard
hardphase
phase and and its
its topological
topological impact on micro-mechanisms
micro-mechanisms
ofofvoid
voidinitiation
initiationininductile
ductilefailure
failure inin this
this bainitic
bainitic multiphase
multiphase steel steel has been reported in in detail
detail byby
ShakerifardetFigure
Shakerifard et
al.al. 5.
[18]. Quantitative
[18].
TheyThey havehaveanalysis
shownshown of voids’
that that evolution
in
in this this steel
steel as agrade
grade function
voidsvoids of true
nucleate plastic
nucleate
at the atstrain.
the interface
interface of bainiteof
bainite
and and martensite
martensite (B/M). This (B/M).showsThistheshows
effectthe effect of mechanical
of mechanical phase between
phase contrast contrast between
B and M B(soft andand
M
3.3.2. Crystallographic
(soft phase,
and hard Orientation
phase, respectively), Aspect
which of Void Initiation
hard respectively), which leads to leads
stress toandstress and partitioning.
strain strain partitioning.At anyAtmomentany moment when
when incompatibilities
incompatibilities
The individual reach reach
rolea of
critical a critical level,
level, voids
martensite as a hard voids
nucleate nucleate
phaseinand order in order to
to locally relax
its topological locally
impact relax
the on
sharp the sharp stress
stress gradients
micro-mechanisms
ofgradients
amongvoid soft among
and hard
initiation insoft and hard
phases.
ductile phases.
Although
failure Although
the
in this effect ofthe
bainitic effectphase
second
multiphase of steel
second hasphase
beenconstituents
constituents and their in
reported and
topologytheir
detail is
by
topology isthe
significant,
Shakerifard significant,
et role
al. [18]. the role
They haveofshown
of crystallographic crystallographic
orientation
that in thisinorientation
gradeinvoids
the evolution
steel theofevolution
stress
nucleate of
atstress
(and/or) (and/or)
the strain ofstrain
is inevitable.
interface is
bainite
Ininevitable.
and this regard,
martensite In this regard,
in(B/M).
order inshows
order to
to investigate
This theinvestigate
the role of
effect the role of crystallographic
of mechanical
crystallographic contrastorientation
phaseorientation Binand
void
in void initiation,
between Minitiation,
33 voids
(soft and
33 voids
were
hard phase, were
analyzed analyzed
locally by
respectively), locally
the by the
EBSD
which EBSD to technique.
technique.
leads The
stress and The
method method
strain of capturing
ofpartitioning.
capturing Atorientations
orientations
any moment of of grains
grains
when is
is depicted
depicted schematically
schematically in in Figure
Figure 6. 6. Figure
Figure 6b 6b particularly
particularly reveals
reveals the
the procedure
procedure
incompatibilities reach a critical level, voids nucleate in order to locally relax the sharp stress gradients of
of capturing the
the local
local
surrounding
surrounding
among soft and orientations
orientations
hard phases. ofofgrains
grains around
around
Although theaaeffect
void. This
void. This
of rectangular
rectangular
second area has facesand
phase constituents with
with approximately
approximately
their topology is
threetimes
three timesthe
significant, therole
short
short and
ofand longdiameters
long diameters
crystallographic ofaatypical
of typical
orientation void
in void
the (approximating
of stressthe
(approximating
evolution void
void by
(and/or) by an
an elliptical
strain elliptical area
area
is inevitable.
with
with
In this a major
a major
regard,and and minor axis).
minortoaxis).
in order This method
This method
investigate the role is used
is of
used consistently
consistently for
crystallographic for all 33 of
all 33 of the
orientation the studied
studied
in void voids.
voids. 33 voids
initiation,
were analyzed locally by the EBSD technique. The method of capturing orientations of grains is
depicted schematically in Figure 6. Figure 6b particularly reveals the procedure of capturing the local
surrounding orientations of grains around a void. This rectangular area has faces with approximately
three times the short and long diameters of a typical void (approximating the void by an elliptical area
with a major and minor axis). This method is used consistently for all 33 of the studied voids.
Metals 2020, 10, 113 7 of 11
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Metals2019, 9,9,x xFOR
2019, FORPEER
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Figure 6. Schematic representation of orientation selection on an overlapped image quality and inverse
Figure6.
Figure Schematic representation
6. Schematic representationofoforientation
orientationselection on an
selection onoverlapped image
an overlapped quality
image and inverse
quality pole
and inverse
pole figure map; (a) complete region of analysis, (b) region selected around the void with faces
figure
pole map; (a)
figure map; complete
(a) to region
complete of analysis,
region (b) region
of analysis, selected around the void with faces approximately
approximately equal three times the void diameter; (b)
andregion selected
(c) remaining around
region the void
of analysis. Thewith faces
rolling
equal to three times
approximately equal the
to voidtimes
three diameter;
the and diameter;
void (c) remaining
and region
(c) of analysis.
remaining The
region of rolling direction
analysis. The is
rolling
direction is along the horizontal axis and the normal direction is along the vertical direction.
along the horizontal axis and the normal direction is along the vertical direction.
direction is along the horizontal axis and the normal direction is along the vertical direction.
Owing to severe plastic deformation and distortion of the crystal lattices in the vicinity of the
Owing to severe plastic deformation and distortion of the crystal lattices in the vicinity of the
Owing
voids, to pattern
a poor severe quality
plastic was
deformation and distortion
normally observed. of the crystal
Only orientations withlattices in the index
a confidence vicinity of the
above
voids, a poor pattern quality was normally observed. Only orientations with a confidence index above
voids, a poor
0.1 are used pattern quality
for further was Later,
analysis. normally
the observed.
orientationOnly orientations
distribution with
function a confidence
(ODF) index
is calculated above
from
0.1 are used for further analysis. Later, the orientation distribution function (ODF) 2is calculated from
0.1approximately
are used for further
131,000 analysis. Later, the
void neighboring orientation
pixels (with andistribution function
equivalent area (ODF)
of ~642 is 2calculated 33
μm surrounding from
approximately 131,000
voids). The calculated
void
3D-ODF
neighboring
of 33 voids
pixels (with
using(with
MTEX
an equivalent area of ~642 µm surrounding
approximately 131,000 void neighboring pixels ansoftware
equivalent(5.1.1,
areaChemnitz,
of ~642 μmGermany)
2 [30] is 33
surrounding
33shown
voids).
in The calculated
Figure 3D-ODF of 33
7 and3D-ODF
denominated voids using MTEX software (5.1.1, Chemnitz,
space. Germany) [30] is
voids). The calculated of 33asvoids
the void-ODF
using MTEX(VODF) using the
software Euler
(5.1.1, Chemnitz, Germany) [30] is
shown in Figure 7 and denominated as the void-ODF (VODF) using the Euler space.
shown in Figure 7 and denominated as the void-ODF (VODF) using the Euler space.

Figure 7. Three-dimensional (3D) void orientation distribution function (ODF) (3D-VODF). Three 𝜑2
sections (𝜑2 = 15°, 45°, and 75°) consist of the dominant components with regard to voids orientations.
Figure 7.
Figure Three-dimensional (3D) void orientation
7. Three-dimensional orientation distribution
distributionfunction
function(ODF)
(ODF)(3D-VODF). Threeϕ2𝜑2
(3D-VODF).Three
2 ==15°,
sections (ϕ ◦
15 three◦
,45°,
45 ,and
and ◦
75 )consist
consist
sections
Figure(𝜑 7 2shows 75°)
sections of 𝜑2 of=of15°,
the 45°,
the dominant
dominant components
components
and 75°, with
with regard
which exhibit regardto
tovoids orientations.
voidscomponents
the dominant orientations.of
VODF. In the neck region of the fracture tensile sample where voids are present, the orthorhombic
Figure
Figure 77shows
showsno three
three sections
sections of
exists,of ϕ2thus
𝜑 = 15 ◦ 45◦ , and 75◦ , which exhibit the dominant components
the,45°,
sample symmetry longer and 2 = 15°, Eulerand 75°, is
space which exhibit
confined intothe
0 < dominant
𝜑1 < 360° and components
0 < 𝜑2 , 𝛷 of
of
VODF.VODF. In the
In the neck
< 90° (triclinic neck region of
regioncondition).
symmetry the fracture
of the fracture tensile
Figuretensile
8c shows sample
sample where voids
whereofvoids
the texture are present,
are present,
the regions with nothe orthorhombic
thevoids,
orthorhombic
which
sample
sample symmetry
will besymmetry
denominated no longer
no longer exists,
here asexists, and thus
and
the no-void-ODF thus the
the Euler space
Euler
(NVODF). space
The isis confined
confined
NVODF into
reveals <
<𝜑 ϕ1 <<360°
into a00 smoother 360 ◦ and 0 < ϕ ,
and 0 < 𝜑2 ,2 𝛷
distribution,
1
<Φwhich
< 90 ◦ (triclinic symmetry condition). Figure 8c shows the texture of the regions with no voids, which
90° is because
(triclinic of the fact
symmetry that regions
condition). Figure with
8c no showsvoidsthehave moreofdispersed
texture the regions orientations compared
with no voids, which
will
withbe denominated
regions selected here
around as the no-void-ODF
voids (cf. Figure (NVODF).
6c). The
will be denominated here as the no-void-ODF (NVODF). The NVODF reveals a smoother distribution, NVODF reveals a smoother distribution,
whichIn
which isSection
is because
because of the
3.3.1,
of the fact
it was that
that regions
factillustrated regionsthat, with
prior
with no
notovoids have
havemore
the necking
voids moredispersed
point at elongation
dispersed orientations
of 5% (𝑒𝑢 =compared
orientations 5%), no
compared
with regions selected
microstructural
with regions selected around
voidsaround voids (cf.
were initiated
voids (cf. Figure
inFigure
the tensile6c). sample. Therefore, the deformation texture of the
6c).
material
In at the3.3.1,
InSection
Section ultimate
3.3.1, ititwas
wastensile strength
illustrated
illustrated (UTS)
that,
that, prior
prior point, which
totothe
the is denominated
necking
necking here as the
pointatatelongation
point elongation ofofuniform
5% = 5%),
5%(𝑒(eu= ODF
𝑢 5%), no
(UODF), cf. Figure 8a, can be considered as a reference texture
microstructural voids were initiated in the tensile sample. Therefore, the deformation texture of of
no microstructural voids were initiated in the tensile sample. from
Therefore, which
the voids
deformationwill nucleate.
texture the
Furthermore,
the material at the
the neck-ODF
ultimate will bestrength
tensile considered, (UTS) cf.point,
Figure 8d, which
which is is calculated
denominated herebyas merging
the the
uniform
material at the ultimate tensile strength (UTS) point, which is denominated here as the uniform ODF
textures
ODF of VODF
(UODF), and NVODF,
cf. Figure 8a, can which means it includes
be considered all the texture
orientations
fromofwhich
void neighboring grains
(UODF), cf. Figure 8a, can be considered as as a reference
a reference texture from which voids
voids willwillnucleate.
nucleate.
and void
Furthermore, the distant grains.
the neck-ODF It
neck-ODF will needs to
will be be emphasized that this method is a post-mortem analysis, which
Furthermore, be considered,
considered, cf. cf. Figure
Figure 8d, 8d, which
which isiscalculated
calculatedby bymerging
mergingthe the
implies of
textures that
VODFall orientations
and NVODF, related
whichto the
means VODF it and NVODF
includes all theare derived from
orientations of the
voidtensile sample after
neighboring grains
textures of VODF and NVODF, which means it includes all the orientations of void neighboring grains
its fracture.
and void distant Therefore,
distant grains.it It is needs
It not obvious which interface was initially at the origin of the void nucleation.
and void grains. needs to to be
be emphasized
emphasized that that this
thismethod
methodisisaapost-mortem
post-mortemanalysis,analysis,which
which
The rectangular region of interest around voids includes all the potentially susceptible orientations
implies that
implies that all
all orientations
orientations related related to to the
the VODF
VODF and
and NVODF
NVODF are
are derived
derived from
from the
thetensile
tensile sample
sample after
after
from which voids might have been initiated. Therefore, this rectangular geometry also includes the
its fracture. Therefore, it is not obvious which interface was initially at
its fracture. Therefore, it is not obvious which interface was initially at the origin of the void nucleation. the origin of the void nucleation.
The rectangular
The rectangular region region of of interest
interest around
around voids voidsincludes
includesall allthe
thepotentially
potentiallysusceptible
susceptibleorientations
orientations
from which voids might have been initiated. Therefore, this rectangular geometry also includes the
 Metals 2020, 10, 113 8 of 11
Metals 2019, 9, x FOR PEER REVIEW 8 of 11

from which voids might have been initiated. Therefore, this rectangular geometry also includes the
grainsthat
grains thatwere
wereindirectly
indirectlyinvolved
involvedin inthe
the void
void initiation
initiation process
process byby providing
providing thethe local
local constraint
constraintto to
the void nucleation
the void nucleation process. process.
Thevisual
The visualcomparison
comparisonofofthe theVODF
VODFand andNVODF
NVODF withwith respect
respect to
to the
the neck-ODF
neck-ODF reveals
reveals that
thatthat
that
the NVODF more closely resembles the texture observed in the necked
the NVODF more closely resembles the texture observed in the necked region (neck-ODF). However,region (neck-ODF). However,
bythe
by thecomparison
comparisonbetweenbetweenthe theVODF
VODFand andNVODF
NVODFwith with the
the UODF,
UODF, itit appears
appears that
that the
the VODF
VODF better
better
resembles the UODF. In order to further investigate the resemblance of the VODF and UODF textures,
resembles the UODF. In order to further investigate the resemblance of the VODF and UODF textures,
ofϕ𝜑22 == 15
thecontour
contourmapsmapsofofVODF
VODFare areoverlaid
overlaid with
with the
the UODF
UODF at ◦ ◦ ◦
the at the
the three
three sections
sectionsof 15°,, 45
45°,, and
and 75
75°,,
cf.cf.Figure
Figure9.9.TheThecontour
contourmapsmapsrepresent
representthe theVODF,
VODF, while
while the
the gradient
gradient maps
maps in in the
the backgrounds
backgrounds
represent the UODF, and the black arrows indicate the main components of the VODF. Figure
represent the UODF, and the black arrows indicate the main components of the VODF. Figure 99also
also
reveals that, for the ϕ = 15 ◦ and 75 ◦ sections, the VODF closely resembles the
reveals that, for the 𝜑2 = 15° and 75° sections, the VODF closely resembles the UODF, as shown earlier
2 UODF, as shown earlier
forthe
for the𝜑ϕ 2=
2 = 45°
◦ section, cf. Figure 8a,b.
45section, cf. Figure 8a,b.

Figure8.8.𝜑2ϕ2= =45
Figure 45◦section
sectionofofODFs
ODFsofof the
the steel
steel at
at two various
various deformation
deformation levels;
levels; (a)
(a) uniform
uniform
deformationunion
deformation unionODF
ODF(UODF)
(UODF)(calculated
(calculatedfrom
from 796,000
796,000 data points), (b) post uniform
uniform VODF
VODF(131,000
(131,000
datapoints),
data points),(c)
(c)post
postuniform
uniformno-void-ODF
no-void-ODF(NVODF)
(NVODF) (460,000
(460,000 data
data points),
points), and (d) necking
necking or orpost
post
uniform ODF consist of the merged ODFs in
uniform ODF consist of the merged ODFs in b and c. b and c.

Thetexture
The texturesimilarity
similaritybetween
betweenthe
theUODF
UODFandand VODF
VODF can
can be
be understood
understood byby considering
considering the
the stress
stress
relaxationprocesses
relaxation processesininthe
themicrostructural
microstructurallevel.
level. According
According toto Figure
Figure 5,
5, voids
voids are
are nucleated
nucleated atat aahigh
high
rate at the strain level of approximately 74% and, knowing that voids act as stress concentrators,one
rate at the strain level of approximately 74% and, knowing that voids act as stress concentrators, one
mayexpect
may expectthat
thatthe
thelocal
localstress
stresspeaks
peakscan
canbe
berelaxed
relaxed further
further either
either by
by plastic
plastic deformation
deformation of
of the
the grains
grains
surrounding a void and/or by further void growth. However, it is observed in Figure 9 that, upon void
initiation, the local stress relaxation is rather controlled by the void growth mechanism than local
 Metals 2020, 10, 113 9 of 11

Metals 2019, 9, x FOR PEER REVIEW 9 of 11

surrounding a void and/or by further void growth. However, it is observed in Figure 9 that, upon
void initiation, the local stress relaxation is rather controlled by the void growth mechanism than local
plasticity inside the grains. This mechanism acts as a preferred local stress relaxation process as the
plasticity inside the grains. This mechanism acts as a preferred local stress relaxation process as the
VODF clearly resembles the UODF texture. However, it is also apparent that the components of the
VODF clearly resembles the UODF texture. However, it is also apparent that the components of the
VODF and UODF do not correlate one to one, which can be explained either by further plasticity after
VODF and UODF do not correlate one to one, which can be explained either by further plasticity after
void initiation at the neighboring grains around voids or including orientations that are not directly
void initiation at the neighboring grains around voids or including orientations that are not directly
involved in void initiation. In addition, a void represents a free surface trapped in the bulk of the
involved in void initiation. In addition, a void represents a free surface trapped in the bulk of the
material that has appeared in order to relax the stresses at the microstructural level. However, once it
material that has appeared in order to relax the stresses at the microstructural level. However, once it
has nucleated, the competitive role between the local hardening and free surface growth determines
has nucleated, the competitive role between the local hardening and free surface growth determines the
the major contribution of these two mechanisms on local stress relaxation, which is an energetically
major contribution of these two mechanisms on local stress relaxation, which is an energetically driven
driven process. As void growth seems to be the main mechanism of local stress relaxation around voids,
process. As void growth seems to be the main mechanism of local stress relaxation around voids,
the dominant components of the VODF can be considered as susceptible orientations to void
the dominant components of the VODF can be considered as susceptible orientations to void nucleation.
nucleation.

Theoverlapped
Figure9.9.The
Figure overlappedVODF VODF(contour
(contourmapmap with
with arrows indicating dominant
dominant components)
components) and
and
UODF (color gradient map) of the material at two different
UODF (color gradient map) of the material at two different deformationdeformation levels (UODF
(UODF at
at 5%
5% and
and VODF
VODF
𝜑2ϕ=2 15°,
= 15(b)
≥74%); ◦ , (b) ϕ = 45◦ , (c) ϕ = 75◦ .
atat≥74%); (a)(a) 𝜑2 =245°, (c) 𝜑2 = 275°.

4. Summary and Conclusions

4. Summary and Conclusions
In this research, a new EBSD-based method was used to study the role of crystallographic
In this research, a new EBSD-based method was used to study the role of crystallographic
orientation in void nucleation. In this regard, the microstructure of the fractured tensile sample in
orientation in void nucleation. In this regard, the microstructure of the fractured tensile sample in the
the vicinity of the fracture surface, where voids were concentrated, was measured by EBSD. Later,
vicinity of the fracture surface, where voids were concentrated, was measured by EBSD. Later, ODFs
ODFs were calculated based on their relative locations with respect to voids: (i) the crystallographic
were calculated based on their relative locations with respect to voids: (i) the crystallographic
orientations of the grains surrounding 33 voids were selected and represented by the void-ODF,
orientations of the grains surrounding 33 voids were selected and represented by the void-ODF, (ii)
(ii) whereas the regions away from the voids represented the no-void-ODF (NVODF). It was observed
whereas the regions away from the voids represented the no-void-ODF (NVODF). It was observed that
that the VODF more closely resembles the UODF. The post-mortem crystallographic orientation
the VODF more closely resembles the UODF. The post-mortem crystallographic orientation analysis
analysis around voids revealed that, after void initiation, the local stress relaxation process is rather
around voids revealed that, after void initiation, the local stress relaxation process is rather dissipated
dissipated by void growth than by further local plastic deformation. In other words, it can be concluded,
by void growth than by further local plastic deformation. In other words, it can be concluded, that upon
that upon void initiation, orientations around voids may not go through significant rotations. This can
void initiation, orientations around voids may not go through significant rotations. This can be
explained by the hardening saturation process of grains at certain macroscopic strain level due to
Metals 2020, 10, 113 10 of 11

be explained by the hardening saturation process of grains at certain macroscopic strain level due
to plasticity prior to damage initiation. Consequently, the increased macroscopic deformation until
failure does not lead to considerable orientation change in the VODF components. Therefore, the major
components of the uniform ODF at the onset of necking correspond to ODF observed in the vicinity of
voids (the VODF).

Author Contributions: Methodology, B.S. and L.A.I.K.; Resources, B.S.; Supervision, J.G.L.; Visualization, B.S.;
Writing—original draft, B.S.; Writing—review & editing, L.A.I.K. All authors have read and agreed to the published
version of the manuscript.
Funding: This work has been conducted in the framework of the BaseForm project, which has received funding
from the European Union’s Research Fund for Coal and Steel (RFCS) research programme under grant agreement
#RFCS-CT-2014-00017.
Acknowledgments: The authors would like to acknowledge Tata Steel, IJmuiden (The Netherlands), for providing
the material in the current study. Special thanks to Frank Hisker for providing the tensile test results.
Conflicts of Interest: The authors declare no conflict of interests.

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