Materials Science & Engineering A 674 (2016) 171–177

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Spatial correlation between local misorientations and nanoindentation

hardness in nickel-base alloy 690
Rickard R. Shen a,n, Valter Ström b, Pål Efsing a,c
a
Department of Solid Mechanics, KTH Royal Institute of Technology, Teknikringen 8D, Stockholm SE-100 44, Sweden
b
Department of Materials Science, KTH Royal Institute of Technology, Brinellvägen 23, Stockholm SE-100 44, Sweden
c
Ringhals AB, Ringhalsverket, Väröbacka SE-432 85, Sweden

art ic l e i nf o a b s t r a c t

Article history: Misorientation increases with plastic strain in metals, and this observation has been used as an empirical
Received 3 May 2016 assessment of plastic strain in recent years. The method has been validated for a sample area corre-
Received in revised form sponding to a 100 mm  100 mm square, but on the micrometer scale misorientations no longer seem to
13 July 2016
correlate with plastic strain. Misorientations are however not dependent on plastic strain but rather on
Accepted 29 July 2016
dislocation density, which means it should also be related to hardness. Therefore, we have in this work
Available online 30 July 2016
compared maps of predicted hardness calculated from misorientation determination with maps of actual
Keywords: hardness measured by nanoindentation.
EBSD It was shown that the predicted and measured hardness maps do indeed correlate spatially in nickel-
Nanoindentation
base Alloy 690, although the measured values have a significantly smaller hardness variation. This is
Local misorientation
explained by a presumably high and uniform density of statistically stored dislocations, which contribute
Hardening
Plasticity to hardness but do not affect the misorientation determination from electron backscatter diffraction.
Nickel based superalloys Thus local misorientation can be used to qualitatively map the local effective plastic strain distribution,
for example to identify regions of increased hardness.
& 2016 Elsevier B.V. All rights reserved.

1. Introduction
In recent years electron backscatter diffraction (EBSD) has been
used to characterize changes in polycrystalline metals that result
from plastic deformation [1–12]. Specifically the change in mis-
orientations, i.e. the change in crystal lattice orientation between
different points in the material, has become popular to focus on. A
scalar misorientation quantity can be defined in different ways,
and the most common methods have been summarized in litera-
ture [13]. No matter how misorientations are defined though,
when averaged over a larger area they tend to increase with
average plastic strain, and this empirical observation has allowed
the use of EBSD for plastic strain estimation.
This misorientation based plastic strain assessment technique
has been validated for quantification of plastic strain using a
sample area corresponding to roughly a 100 mm  100 mm square
[1,2]. Spatial variations in local misorientation values can be seen
on a micrometer scale as well, and attempts at correlating these
local misorientations with strain measurements based on digital
n
Corresponding author.
E-mail addresses: rshen@kth.se (R.R. Shen), valter@kth.se (V. Ström),
pal.efsing@vattenfall.com (P. Efsing).
image correlation (DIC) have been performed, although with un-
satisfactory results in copper [14,15] and aluminum [16].
Sasaki et al., however, discussed that DIC measures the actual
strain, while misorientations between neighboring points reflect
the local dislocation density, and that these two quantities do not
necessarily correlate on a micrometer scale [15]. They illustrated
that plastic deformation can accumulate where dislocations had
passed through, but that misorientations only increased where
dislocations accumulated. Misorientations may thus be closer re-
lated to effective plastic strain, which is a measure of strain hard-
ening, i.e. dislocation density buildup, rather than plastic strain,
which is a measure of geometric shape change.
Polycrystalline metals are plastically inhomogeneous at the
microscopic size scale, thus an inhomogeneous hardness dis-
tribution can be expected as the material deforms. As such, maps
of local hardness would be relevant for processing and monitoring
degradation of materials where local material properties are im-
portant, e.g. recrystallization, stress corrosion cracking (SCC) and
fatigue.
If misorientations do indeed correlate with effective plastic
strain, it can be used as a tool to predict the hardness profile.
Therefore, nanoindentation hardness mapping has been used in
this work as a means to investigate the correlation with those
predicted by misorientation mapping.

http://dx.doi.org/10.1016/j.msea.2016.07.123
0921-5093/& 2016 Elsevier B.V. All rights reserved.
172 R.R. Shen et al. / Materials Science & Engineering A 674 (2016) 171–177
An inherent uncertainty with the misorientation technique is
that misorientations are in principle only dependent on the in-
homogeneous straining, which induces geometrically necessary
dislocations (GNDs), whereas the total dislocation density also
consists of statistically stored dislocations (SSDs), which are in-
duced by homogeneous straining [17]. Since homogeneous strains
do not contribute to misorientations, but do contribute to strain
hardening, misorientation distribution does not necessarily reflect
the local hardness distribution accurately on the micrometer size
scale, which necessitates a clarification of the actual relation be-
tween misorientation and hardness.
In practice, strains on a larger scale are often estimated from
misorientation maps (acquired with EBSD), which suggests that a
verified extension of this method to the micrometer scale would
constitute a significant advance.
In this work we have shown the existence of a correlation be-
tween local hardness and local kernel average misorientation
(KAM) which appears useful, but since deformation mechanisms
can differ between materials, and even for the same material if
deformation temperature or rate is significantly changed, we
cannot a priori infer that the findings in this work are generally
applicable.
2. Experimental
2.1. Test material
Alloy 690, a solution strengthened high chromium nickel-base
alloy with a face-centered cubic (FCC) crystal structure, was used
in this work. It is highly ductile, has significant strain hardening,
and deforms by dislocation slip at the temperature and strain rates
involved in this work.
The material used in this work came from a tube that has been
characterized in a previous work [18]. In the as-delivered condi-
tion, the microstructure consisted of an austenitic matrix phase,
fine intergranular M23C6 carbides, and large intragranular Ti(C,N)
precipitates. This particular tube was chosen for having shown a
homogeneous microstructure. The chemical composition of this
tube is given in Table 1.
In order to minimize the overall dislocation density in the
material, it was recovery heat treated at 1050 °C for 4 h and slowly
cooled down to room temperature inside the furnace. This heat
treated material has been considered as being free from effective
plastic strains in this work. The heat treatment caused the average
grain size, measured by the intercept method, to increase from
around 50 mm to 70 mm. The Ti(C,N) precipitates remained un-
changed, but the intergranular M23C6 carbides had changed from a
semi-continuous network of fine carbides to coarse and discreet
ones, but were still located exclusively at the grain boundaries. No
intragranular M23C6 carbides were observed either before or after
the heat treatment.
Cylindrical uniaxial tensile specimens were manufactured from
the heat treated material along the tube's axial direction. The
nominal diameter was 5.00 mm, and the gauge length was
12.55 mm. All specimens were strained at room temperature using
a servo-hydraulic testing machine at a strain rate of approximately
3
10 4 s 1, with strain, ε, defined as the logarithmic strain as
Table 1
Composition of the alloy 690 tube.
Element Ni Cr Fe C Si
Weight-% Bal. 29.5 10.0 0.020 0.28
ε = ln( L/L 0), (1)
where L0 was the length of a region before deformation, and L is
the current length. The specimens were unloaded before failure
and retained a plastic strain, εp, of 0.029, 0.062, 0.087, 0.116 and
0.144 respectively. The heat treated material exhibited a yield
strength of 273 MPa.
2.2. Prediction of local effective plastic strains
Material from both the unstrained and strained specimens was
used to prepare specimens for EBSD. The material was carefully
sectioned along a plane normal to the tube's axial direction using a
Struers Accutom-5 precision cut-off machine. The sampled mate-
rial was mounted in conductive resin and ground using SiC paper,
followed by polishing using diamond paste. Final polishing was
performed using 0.06 mm colloidal silica.
An EBSD system from HKL Technology was used within a LEO
1530 Gemini field emission scanning electron microscope (SEM) to
obtain crystal orientation maps on the sampled materials. The
accelerating voltage was set to 15 kV, and the aperture was opened
to 120 mm. The working distance differed slightly between sam-
ples, but was between 8–10 mm. On each specimen, an area of
610 mm  460 mm was mapped using a square grid with step
length 0.9 mm. HKL software was used for acquisition of the or-
ientation maps and phase identification, but in-house scripts were
used for post-processing of the orientation data. The indexing
rates for the specimens were between 98.0–99.9%, and no cleanup
of non-indexed points was performed.
An orientation smoothening filter proposed by Kamaya was
applied to each orientation map [19]. This filter is essentially a
grain-wise moving average of the orientation, and tends to in-
crease the precision in the orientation map at the cost of a slight
loss of spatial resolution. A square kernel of 3  3 data points was
used for the moving average. A grain was defined as a region en-
closed by boundaries containing more than 10 points, and a
boundary was defined between two neighboring points when the
misorientation between them exceeded 5°. This threshold was in
general high enough to allow deformation-induced misorienta-
tions, but low enough to identify grain boundaries.
Each point in the EBSD map is directly connected to four
neighboring points, and diagonally connected to four additional
points. In this work, KAM with a kernel consisting of only the four
closest neighboring points was used to assign a scalar value to
each point, representing its local misorientation level. The KAM
were lognormally distributed, and the average KAM, KAMave, over
a sampled region was calculated as
⎡ N ⎤
1
KAMave = exp⎢ ∑ ln( KAML, i)⎥,
⎢⎣ N ⎥⎦
i=1 (2)
where KAML, i is the local KAM at point i, and N is the number of
points in the sampled area. Such an average was calculated for
each of the specimens with different level of strain. As shown in
Fig. 1, KAMave increased approximately proportionally with uni-
axial plastic strain, and a linear function was fitted through the
data points to serve as a calibration curve. The level of mis-
orientation uniformity in the specimens was assessed by splitting
the full sampled area into 15 subregions of the same size. Their
Mn P S N Ti Al
0.31 0.007 0.001 0.040 0.35 0.18
 R.R. Shen et al. / Materials Science & Engineering A 674 (2016) 171–177
Fig. 1. Average KAM increased approximately proportionally with increasing
plastic uniaxial strain.
respective standard deviations of average misorientation are re-
presented by the error bars in Fig. 1.
Such a calibration curve is normally used to estimate the plastic
strain averaged over a sampled area. However, in our situation we
use the same relation to estimate local effective plastic strain from
local misorientation.
2.3. Prediction of local hardness
By performing hardness indentation, additional strains would
be introduced into the surface in addition to the pre-existing ones.
Tabor showed that an additional effective plastic strain of 0.08 was
representative for Vickers indenters [20]. A Berkovich tip, used for
nanoindentation in this work, has the same equivalent cone angle
and thus the same representative strain. Tabor further showed
that a material's hardness, H, can be approximated to
H = 3⋅σf ,
where sf is the material's flow stress when the additional strain
from the indentation is taken into account to the pre-existing
strains.
The flow stress as a function of effective plastic strain, εep, was
obtained by performing a uniaxial tensile test in the same way as
for the pre-strained materials, but all the way to failure. Fig. 2
shows that Ludwigson's equation [21]
Fig. 2. A material model was fitted to the curve in order to extrapolate the hard-
ening behavior to strains beyond necking. Tabor's relation was verified using
Vickers hardness tests.
173
n1
σf = K1⋅εep (
+ K2⋅exp n2εep , ) (4)
where K1, n1, K2 and n2, are fitting parameters, matched well to the
stress-strain curve up to necking, which occurred at around 0.37
strain.
By adding the strain from the indentations to the effective
plastic strain map that was predicted based on the local mis-
orientations, Eqs. (3) and (4) were used to predict the hardness
distribution over the surface.
This approach, at least on a larger size scale, is supported by the
work of Overman et al. [3]. They showed that hardness in Alloy
690 can be linked to average misorientation through Tabor's re-
lation, under the assumption that average misorientation is pro-
portional to plastic strain. A similar verification in this work using
Vickers hardness tests on the pre-strained samples is shown in
Fig. 2. A load of 295 N was used for these indentations, with a 20 s
dwell time.
2.4. Nanoindentation
The EBSD specimen with material subjected to 0.144 plastic
strain was selected for nanoindentation since it exhibited the lar-
gest variation in intra-grain misorientation. Extra care was taken
during the grinding of the specimens to keep the top and bottom
surfaces of the specimen parallel to ensure compatibility with the
nanoindentation. Ti(C,N) precipitates, naturally present in the
material and visible on the as-polished surface, were used as na-
vigation markers to find the region previously mapped by EBSD.
Nanoindentation was performed at several chosen sites within
the region already mapped by EBSD. The indents were made using
a Nano Indenter IIs (Nano Instruments in Oak Ridge, Tennessee),
fitted with a Berkovich tip. Indentations were made with a loading
rate of 0.05 mN/s until a nominal depth of 150 nm was reached.
The load was then held constant for a dwell time of 20 s. The
subsequent unloading was also set to a rate of 0.05 mN/s. At each
site where the hardness was mapped, the indents were placed
along three parallel rows 2.6 mm apart, with a 2.6 mm center to
(3) center spacing.
The projected contact areas of the indents were measured in a
JSM-7800F field emission SEM. The images were acquired using an
accelerating voltage of 15 kV and a working distance of around
10 mm. All contact area determinations in the SEM micrographs
were made solely by one of the authors in order to avoid com-
parison inaccuracies from subjective interpretations. These SEM
images were also used in conjunction with the EBSD data to de-
termine the exact location of the indents relative the EBSD map.
Fig. 3. Example of an SEM image of indents used for measuring the indent contact
area.
174 R.R. Shen et al. / Materials Science & Engineering A 674 (2016) 171–177

Fig. 4. A small region of the predicted hardness map is shown with a) the indent locations in a grain, b) the comparison between the measured and predicted hardness
profiles, and c) the indentation order.

3. Results and discussion
The indents were roughly of the same size, and pile up was ob-
served for all indents. An example of an SEM image of indents is
shown in Fig. 3. The indent spacing is short, and was intentionally set
shorter than that recommended by ASTM E2546-15 [22]. This was a
carefully chosen balance between the requirement of a high spatial
resolution and being able to measure the projected indent area with
sufficient precision. As a consequence each indent has most likely
been affected by the previous indent and the previous row of in-
dents. This should theoretically cause a systematic increase in the
hardness values of the first row, and a larger systematic increase in
both subsequent rows. While the accuracy of the measured absolute
hardness values can certainly be questioned, the systematic nature of
the error still allows an unambiguous statement of the spatial
hardness profile. A similar reasoning was used by Marra to study the
hardness profile near grain boundaries of Alloy 690 [23].
The indent locations of a hardness map placed within a selected
grain is shown in Fig. 4 along with a comparison between the measured
and the predicted hardness values in this region, and the order of indent
placement. The trends in the predicted hardness profile correlated well
with those in the measured one. Both profiles agreed on a diagonal
band of higher hardness on the right side, lower hardness near the
upper corners, and hardness values in-between on the lower left side.
The two sets of hardness maps however showed a significant
difference in relative variance. The highest measured hardness
values were roughly a factor 1.2 of the lowest ones, while the
prediction indicated that the same factor is around 3 in the same
area. The hardness prediction did not account for crystal orienta-
tion or for the indent size effect (ISE), but both of these affect the
hardness by a multiplicative factor. Since the crystal orientation is
roughly constant within a grain, and the ISE was kept constant by
only making indents of the same size, the errors from these two
sources would only affect the absolute hardness values, but not
their trends in spatial distribution or their degree of relative var-
iance. The large discrepancy in relative variance in hardness thus
shows that the method for estimating effective plastic strains is
not fully applicable at the microstructural size scale.

Fig. 5. A region with a) indents crossing a twin boundary, b) the comparison between the measured and predicted hardness profiles in this region with the twin boundary
marked by the diagonal line, and c) the indentation order with excluded points in gray.
 R.R. Shen et al. / Materials Science & Engineering A 674 (2016) 171–177
Fig. 6. A region with a) the locations of two sets of indents marked out, b) the comparison between the measured and predicted hardness profiles in the set lying within one
grain, d) the comparison of the set crossing a grain boundary, and c) and e) the indentation order of respective map with excluded points in gray. The grain boundary is
marked by a diagonal line.
Similar results can be seen in another region shown in Fig. 5,
where the indents were placed across a twin boundary. Indents
placed directly on grain boundaries and twin boundaries were
excluded so that all results are representative of the matrix. Again,
the spatial trends in hardness were captured by the prediction,
and again, there was a significant difference in the relative var-
iance in predicted and measured hardness.
Another two sets of maps are shown in Fig. 6. The set of indents
shown in Fig. 6b) was placed within one grain. This set again showed
a spatial correlation in the trends between the measured and the
predicted hardness maps, along with the same large difference in
relative variance. However, the set of indents shown in Fig. 6d), which
was placed across a grain boundary, shows a very different result. The
hardness profile on the left side of the grain boundary showed similar
results as the previously shown maps, but the right side did not. The
measured hardness was consistently high on the right side of the
grain boundary, and did not show the softer region further away from
the grain boundary as the predicted map had shown.
While the change in crystal orientation across the grain
boundary could explain a jump in absolute hardness, it cannot
account for the discrepancy in the trends between the predicted
and measured hardness. Interestingly though, the discrepancy in
Fig. 6d) is instead an observation where the hardness prediction
fails, and a further study appears motivated for a better under-
standing. The uniform level of measured hardness suggests that
the total dislocation density may be more uniform than what is
expected based on the KAM distribution, which would imply a
175
Fig. 7. The band contrast is relatively uniform in the grain on the right side.
higher background SSD density. This is supported by a map of the
EBSD pattern band contrast showing a relatively uniform band
contrast in the right grain, which is shown in Fig. 7.
Band contrast is a value calculated by the HKL EBSD software as
a way of quantifying the image quality of the EBSD pattern, which
deteriorates with increasing dislocation density. While this has
been proposed as an alternative method for plastic strain esti-
mation [24], it has not attracted a wide spread usage due to its
sensitivity to many other factors aside from dislocation density,
including crystal orientation. The pattern quality can at times
differ significantly even across a low angle boundary, which makes
the method challenging to use on the micrometer scale.
To better understand the overall higher hardness in the right
side of Fig. 6d), this region was re-mapped by EBSD after na-
noindentation. A shorter EBSD step length of 0.2 mm was used, and
a KAM map is shown in Fig. 8, which was calculated using points
0.9 mm from the kernel center like the previous maps.
The result shows that the local misorientations around the
indents on the right side are higher and extends further. As
176 R.R. Shen et al. / Materials Science & Engineering A 674 (2016) 171–177
Fig. 8. An indented region was re-mapped to assess the deformation field around
the indents. The cubes represent the crystal orientations in the two grains.
expected, overlaps in indent deformation fields are evident in
many cases, but do not appear to explain the overall higher
hardness of the right side alone. The first indents were laid in the
bottom right of Fig. 8 and show limited overlap, yet still exhibited
high hardness values. The overall higher hardness on the right side
is more likely to be explained by a different crystal orientation
with respect to the loading, or the previously discussed elevated
background SSD density.
The significantly smaller variations in the measured hardness
compared to the predicted hardness observed in all maps could be
explained by the presence of a relatively high and uniform SSD
density in the background. This can be interpreted as a significant
portion of the plastic strain being homogeneous, and that this
homogeneous portion of the plastic strain is roughly spatially
uniform. This would dilute the effect of GND density variations on
the total dislocation density. Since hardness is a function of the
total dislocation density, the relative variation of measured hard-
ness would be small, but still follow the same trends as the GND
density. Misorientations on the other hand are only based on the
GND part of the total dislocation density, and thus effective plastic
strain-, and hardness-, predictions based on local misorientations
would show a much larger relative variance, and thus the method
should not be used for quantification of local hardness.
The generally good spatial correlation found in this work be-
tween misorientations and hardness, and the lack of correlation
between misorientation and local plastic strain observed in other
works [14–16], suggests that plastic strain and effective plastic
strain are not synonymous at the micrometer scale. While these
previous works have shown that it is inappropriate to use local
misorientations for assessment of local plastic strain on the mi-
crometer scale, the results in this work show that local mis-
orientations are still useful for obtaining a qualitative map of the
effective plastic strain.
It should nonetheless be pointed out that misorientations and
plastic strain are related through the storage of dislocations. A
different strain rate, temperature or material may change the de-
formation mechanism and thus potentially change the outcome.
Therefore, our results with clear spatial correlation between pre-
dicted and measured hardness, for this material and deformation,
suggest further studies for a broader applicability.
4. Conclusions
It was found that the predicted hardness distribution based on
local KAM correlated well with the spatial trends in measured
hardness using nanoindentation in most cases in the nickel-base
Alloy 690 material tested in this work. The KAM-based method
however vastly overestimated the variation in hardness, and for
example suggested a ratio of 3 between maximum and minimum
hardness where the measured hardness only exhibited a ratio of
1.2. This could be explained by the presence of a high and uniform
level of SSD density in the background, which would dilute the
effect of variations in GND density. Since misorientations depend
on the GND density, and hardness on total dislocation density,
both methods would still show the same spatial trends. Thus local
KAM can give a good indication of the qualitative hardness profile,
or effective plastic strains, across the surface. Using the macro-
scopic relationship between misorientations and strains to quan-
tify local hardness or strain on the micrometer scale is however
discouraged. Future work on other materials, strain rates and
temperatures are nonetheless required to clarify how far the re-
sults of this work extend.
Acknowledgments
We are grateful and for the funding provided from Vattenfall,
Fortum and Eon/Uniper and for the material used in this work
provided by the Electric Power Research Institute (EPRI). We also
wish to acknowledge Dr. C.F.O. Dahlberg for his assistance with the
in-house EBSD post processing script, and M. Öberg and K.
Lindqvist for their help with the uniaxial tensile testing.
Appendix A. Supplementary material
Supplementary data associated with this article can be found in
the online version at http://dx.doi.org/10.1016/j.msea.2016.07.123.
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