Micron 75 (2015) 110

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Micron
journal homepage: www.elsevier.com/locate/micron

Using transmission Kikuchi diffraction to study intergranular stress

corrosion cracking in type 316 stainless steels
Martina Meisnar a, , Arantxa Vilalta-Clemente a , Ali Gholinia b , Michael Moody a ,
Angus J. Wilkinson a , Nicolas Huin c , Sergio Lozano-Perez a
a
University of Oxford, Department of Materials, Parks Road, OX1 3PH Oxford, UK
b
University of Manchester, School of Materials, Grosvenor Street, M1 7HS Manchester, UK
c
AREVA, Dpartement Mtallurgie et Corrosion, Section Corrosion et Tenue des Matriaux, Centre Technique France, France

a r t i c l e i n f o a b s t r a c t

Article history: Transmission Kikuchi diffraction (TKD), also known as transmission-electron backscatter diffraction
Received 13 March 2015 (t-EBSD) is a novel method for orientation mapping of electron transparent transmission electron
Received in revised form 20 April 2015 microscopy specimen in the scanning electron microscope and has been utilized for stress corrosion
Accepted 20 April 2015
cracking characterization of type 316 stainless steels. The main advantage of TKD is a signicantly higher
Available online 27 April 2015
spatial resolution compared to the conventional EBSD due to the smaller interaction volume of the
incident beam with the specimen.
Keywords:
Two 316 stainless steel specimen, tested for stress corrosion cracking in hydrogenated and oxygenated
Transmission Kikuchi diffraction
TKD
pressurized water reactor chemistry, were characterized via TKD. The results include inverse pole gure
Intergranular stress corrosion cracking (IPFZ) maps, image quality maps and misorientation maps, all acquired in very short time (<60 min)
SCC and with remarkable spatial resolution (up to 5 nm step size possible). They have been used in order to
316 stainless steel determine the location of the open crack with respect to the grain boundary, deformation bands, twinning
Scanning electron microscope and slip. Furthermore, TKD has been used to measure the grain boundary misorientation and establish a
SEM gauge for quantifying plastic deformation at the crack tip and other regions in the surrounding matrix.
Transmission electron backscatter Both grain boundary migration and slip transfer have been detected as well.
diffraction
2015 Elsevier Ltd. All rights reserved.
t-EBSD
Grain boundary migration
Grain boundary misorientation

1. Introduction
Stainless steel alloys such as SUS316 are widely used for
applications in nuclear power plants because of their excellent per-
formance in high-temperature and corrosive environments (Arioka
et al., 2006a). For decades, they have been commonly used as the
main constituents of structural components in the primary circuit
of Pressurized Water Reactors (PWRs) and Boiling Water Reac-
tors (BWRs) (Karlsen et al., 2010). However, despite their corrosion
resistance, these materials have shown susceptibility to intergra-
nular stress corrosion cracking (IGSCC) after long service periods
(Terachi et al., 2008; Arioka et al., 2007).
Hence, for at least two decades stress corrosion cracking (SCC)
in stainless steels has been the focus of increasing research efforts
(Andresen, 2013; Arioka, 2013; Dietzel and Bala Srinivasan, 2011;
Corresponding author. Tel.: +44 01865 273700; fax: +44 01865 273789.
E-mail address: martina.meisnar@materials.ox.ac.uk (M. Meisnar).
Kain, 2011; Lynch, 2011; Shoji et al., 2011; Staehle, 2010; Das
et al., 2009; Lozano-Perez et al., 2009a; Couvant et al., 2007;
Terachi et al., 2007). However, there is still only limited under-
standing of the mechanisms underlying SCC and there is no general
model for the initiation and propagation of SCC yet (Bruemmer
and Thomas, 2010; Guerre et al., 2007; Vaillant et al., 2004; Scott
and Le Calvar, 1993). Most studies are complicated by the fact
that there are several parameters potentially simultaneously inu-
encing the occurring crack initiation and propagation processes,
including water chemistry, temperature and matrix composition
(Terachi et al., 2007; Lozano-Perez et al., 2009b; Arioka et al., 2006b;
Terachi and Arioka, 2006; Langevoort et al., 1984).
These previous SCC propagation studies have focused on the
oxide structure and chemistry, the crack morphology and the
matrix surrounding the crack tip, such as changes in the local matrix
composition and deformations. These features have been studied
using a variety of electron microscopy (EM) methods, including
scanning electron microscopy (SEM), auger electron spectroscopy
(AES), transmission electron microscopy (TEM) (Kruska et al., 2011;

http://dx.doi.org/10.1016/j.micron.2015.04.011
0968-4328/ 2015 Elsevier Ltd. All rights reserved.
2 M. Meisnar et al. / Micron 75 (2015) 110
Lozano-Perez and Gontard, 2008; Lozano-Perez and Titchmarsh,
2003; Lozano-Perez et al., 2004; Olszta et al., 2011) as well as
NanoSIMS (Lozano-Perez et al., 2008a,b). To complement these
mechanical and chemical studies of SCC, higher resolution charac-
terization from a crystallographic point of view (such as orientation
mapping) is also necessary.
There is limited information on the relationship between SCC
crack propagation and crystallographic features in the sample sur-
rounding the crack tip. This includes the misorientation of the
grains on either side of the crack, the plastic deformation before,
around and ahead of the crack tip as well as the existence of defor-
mation structures such as twinning, slip and deformation bands.
Comparing these features in different types of SCC specimen (with
regard to water chemistry, temperature or matrix composition)
may provide signicant new insights with respect to the propa-
gation of SCC.
This work represents a novel study of crystallographic features
in two different types of samples, tested in hydrogenated and oxy-
genated PWR primary water chemistry, utilizing a new method of
high-resolution orientation mapping: transmission Kikuchi diffrac-
tion (TKD) or sometimes also known as transmission-electron
backscatter diffraction (t-EBSD). The samples were chosen because
they manifest two different types of crack propagation. It is shown
that, with this novel technique, high-resolution crystallographic
data can be easily acquired which may contribute to solving
some remaining questions about the SCC crack propagation pro-
cess (such as the impact of plastic deformation around the crack
tip).
2. Material
The material used for this study was type 316 (reactor grade)
stainless steel. Two different types of specimen were characterized:
type 316 tested under oxygenated PWR water conditions, provided
by AREVA; and type 316 tested under hydrogenated PWR water
conditions, provided by INSS. Both steels exhibited SCC after auto-
clave testing. The compositions of each alloy are listed in Table 1.
Specimen 316INSS underwent solution treatment followed by
water quenching and uni-directional cold-rolling to a thickness
reduction of 20%. The SCC test (CGR) was performed at the INSS
(Japan) laboratories using a pre-cracked 1/2 CT specimen in the
TS direction in an autoclave under constant load (30 MPa m1/2 ).
The sample was exposed to a testing environment of simulated
PWR water chemistry (hydrogenated water: 500 ppm B + 2 ppm Li,
+30 cm3 -STP/kg-H2 O DH2 ) for 700 h at 360 C. More information
about the standard methods for stress corrosion cracking testing
can be found on the American Society of Testing and Materials
website (www.astm.org).
Specimen 316AREVA was a reverse U-bend specimen with a
shot-peened surface and was tested at the AREVA Laboratories
in France. The specimen was exposed to a PWR primary water
chemistry in shutdown conditions with increased oxygen content
(oxygenated conditions: 10 ppm O + 1200 B + 2 ppm Li) for 1500 h
at 345 C.
The cross-sectioned surface of both samples was ground with
SiC paper and polished with 1-m diamond suspension. Mirror-
nish was achieved by nal treatment (15 min) with colloidal silica.
Subsequently, the bulk specimens were screened with an opti-
cal microscope and the SEM to locate the crack tips. These crack
tips have then been lifted out in situ in plan-view orientation
in a focused ion beam (FIB) instrument. The lift-outs were then
mounted on TEM Cu grids and thinned to electron transparency
(<100 nm). Before the actual TKD acquisition, the TEM foils were
plasma cleaned for 5 min (Fishione 1020 plasma cleaner). Initial
TEM observations were made with a JEOL 2100 LaB6 TEM and
EELS spectra were acquired with a JEOL ARM200F (cold-FEG gun,
200 kV).
3. TKD methodology
For decades, electron backscatter diffraction (EBSD) has been
a very important and commonly used tool for the gathering
of crystallographic data for many materials scientists (Dingley,
2004; Schwartz et al., 2009). Like many other techniques, recent
progress in nano-science has required orientation mapping to
improve in terms of spatial resolution. However, reports sug-
gest that EBSD appears to have reached its threshold at around
50100 nm, depending on the analyzed material (Keller and Geiss,
2012; Trimby, 2012; Zaefferer, 2011).
In 2012, Keller et al. rst reported of a new technique called
transmission-electron backscatter diffraction (t-EBSD) or later also
known as transmission Kikuchi diffraction (TKD) which uses the
scanning electron microscope (SEM) with a conventional EBSD
detector to perform orientation mapping on electron transparent
TEM foils (Keller and Geiss, 2012). While the exact same hard-
ware as for EBSD was used, the TKD setup changed slightly with
regard to the specimen position. The EBSD software accounts for
this by adapting the pattern recognition algorithm. The TKD geom-
etry is derived from the basic EBSD setup with the main difference
being the specimen position and its orientation with respect to
the SEM column. Instead of the 70 tilt of the sample toward the
EBSD camera, the TEM foil (mounted on a standard TEM Cu grid) is
almost horizontal (max. 10 tilt) with respect to the incident elec-
tron beam. Due to this setup and the thin TEM foil, the interaction
volume of the electron beam with the sample is minimized in TKD.
This is because of the sample thickness and the fact that the cone
of the incident electron beam in EBSD is much larger due to the tilt
angle of 70 which increases the interaction volume [as shown via
Monte Carlo simulations in Keller and Geiss (2012)]. Hence, the lat-
eral resolution is therefore signicantly improved (Trimby, 2012).
In addition, the almost-horizontal mounting of the sample reduces
the need for dynamical focus or tilt correction.
The ideal thickness of the TEM foil for TKD depends on the mate-
rial composition; good quality results have been achieved at under
100 nm thickness (Rice et al., 2014). In the rst years of application
of this technique, it has become apparent that the quality of TKD
patterns is very much dependent on the thickness of the specimen,
which also has a strong effect on the achieved spatial resolution.
Therefore, TEM sample preparation is key for the successful and
reliable data acquisition via TKD (Suzuki, 2013).
The TKD patterns originate from the volume very close to the
bottom surface of the sample (Trimby, 2012). No additions to the
common EBSD system are necessary: the Kikuchi patterns are
recorded with the EBSD camera and the (for TKD slightly adapted)
EBSD software is responsible, as usual, for orientation mapping.
There is a general consensus from researchers applying TKD to
the characterization of a variety of materials that this technique
offers a signicant improvement in spatial resolution (Keller and
Geiss, 2012; Trimby, 2012; Rice et al., 2014; Brodusch et al., 2013;
Trimby and Cairney, 2014; Trimby et al., 2014; Babinsky et al.,
2014). The authors concur that in most cases that the advantages
offered by this improved resolution outweighs the extra effort of
having to prepare electron transparent TEM foils.
In this study, all TKD maps were collected using a Zeiss Merlin
FEG-SEM and an eFlashHR Bruker EBSD detector system. An accel-
erating voltage of 20 kV and a probe current of 3 nA were used.
Reports (Trimby, 2012) suggest that in thicker sample regions 30 kV
works best, but the used specimens were very thin (6080 nm) and
20 kV produced sufciently good pattern quality. The TEM foil was
mounted on a special Bruker TKD sample holder with an intrinsic
 M. Meisnar et al. / Micron 75 (2015) 110 3

Table 1
Chemical content of the alloys used in this study (wt%), provided by INSS Japan and AREVA France.

Alloy Fe Cr Ni C Si Mo Cu Mn P S

316AREVA Bal. 17.52 12.31 0.023 0.488 2.45 0.132 1.73 0.025 0.008
316INSS Bal. 16.54 11.00 0.047 0.045 2.07 n.a. 1.42 0.024 0.001

software and misorientation (MO) line proles have been extracted

manually.
Uncertainty estimation has been provided for all MO proles.
The utilized TEM lamellas may vary slightly in thickness across
the entire area and due to heavy deformation in the sample noise
and statistical errors have arisen, especially visible in the MO pro-
les. The standard deviation has therefore been calculated for every
prole around the plateau area, based on the average uctuation
around the extracted plateau value.

4. Results

Fig. 1. Image of SEM chamber in measurement ready position with TKD sample
holder (left); EBSD detector (right) and electron pole piece (top).
specimen tilt of 45 . The stage has been tilted in the opposite sense
to 35 in order to achieve a net tilt of 10 .
Fig. 1 shows the sample-detector geometry inside the SEM
chamber. The sample is mounted at a net angle of 10 with ref-
erence to the horizontal and the working distance is 7.5 mm. The
EBSD detector has been inserted from the right-hand side and is fac-
ing upwards slightly (4 ) to collect the incoming electrons exiting
the bottom sample surface. The detector distance to the specimen
is 12 mm. All these parameters were recommended by Bruker, the
manufacturer of the EBSD/TKD instrumentation and software.
All TKD maps have been collected in 1 h with a step size
of 11 nm (note the increased resolution with respect to conven-
tional EBSD) and TKD pattern resolution of 160 120 pixels. A total
area of 3.2 m 2.4 m was recorded. The data were subsequently
analyzed with Esprit 1.9.4 version, the Bruker orientation map-
ping software. Inverse pole gure (IPFZ) maps, image quality maps
and misorientation maps have been created automatically by the
The two samples selected for this study have been initially char-
acterized by TEM (JEOL 2100, LaB6 lament, 200 kV) in order to
detect interesting features and to determine the location of the
crack tip as well as oxides in the crack opening. STEM images of both
FIB-prepared TEM lamellae are illustrated in Fig. 2 (a: 316AREVA,
b: 316INSS).
Noticeably, the crack opening in 316AREVA appears much larger
than in 316INSS. At the crack tip, the opening measures 600 nm for
316AREVA and 150 nm for 316INSS (as illustrated in Fig. 2).
The oxygenated water chemistry is known for the enhanced
dissolution of matrix material at crack anks and the crack tip com-
pared to the hydrogenated PWR typical water chemistry (Arioka
et al., 2007, 2008; Yamada et al., 2009). This behavior could be a
potential explanation for the dimensional difference of the crack
openings observed in 316AREVA (oxygenated, Fig. 2a) and 316INSS
(hydrogenated, Fig. 2b), although it is also expected that stresses
are higher in the reverse U-bend specimen.
After the initial screening of the samples via TEM, TKD mea-
surement has been performed as described in the previous section.
Fig. 3 shows the IPFZ-, image quality- and the average misorienta-
tion (misorientation will be henceforth abbreviated MO) maps of
the crack tip area in both samples.
As in conventional EBSD, inverse pole gure (z direction) maps
(IPFZ) in Fig. 3a and d shows the existence of different grains with
different crystallographic orientations by appearing in different

Fig. 2. STEM dark eld images acquired with JEOL 2100 at 200 kV; (a) 316AREVA TEM lamella, SCC test under (oxygenated) BWR conditions, crack tip opening 600 nm; (b)
316INSS TEM lamella, SCC test under (hydrogenated) PWR conditions, crack tip opening 150 nm; dashed lines indicate the location of the grain boundary (GB).
4 M. Meisnar et al. / Micron 75 (2015) 110

Fig. 3. TKD maps: (a) 316AREVA Inverse Pole Figure in z direction (IPFZ) map: different color represents a difference in crystallographic orientation (legend above); (b)
316AREVA image quality map: contrast arises form crystallographic defects or differences in crystallographic orientation; (c) 316AREVA average MO map: the brighter the
region the higher is the average MO; (d) 316INSS IPFZ map (legend above); (e) 316INSS image quality map; (f) 316INSS average MO map.

colors (colors according to the orientation triangle for fcc austen-
ite; a legend for both IPFZ maps is displayed above Fig. 3a and d,
respectively). In addition, large oxide particles in the open crack
in 316INSS (in Fig. 3d) have also been indexed due to the excel-
lent spatial resolution of this method. Fig. 3a shows a similar grain
pattern along the crack anks with a lateral translation along the
grain boundary (GB) of 200 nm. This indicates a crack opening
mechanism that may have involved shear strain.
Similarly, based on low contrast in the band identication,
image quality maps were generated (Fig. 3b and e) and show some
darker areas as regions of high defect density in the material. This
includes deformation bands, twinning and slip bands as well as the
open crack advancing between the two grains and the grain bound-
ary itself. The deformation history of the samples (cold rolling or
reverse u-bending) indicates that the bands intersecting the grain
boundary are deformation bands.
Finally, Fig. 3c and f illustrates the average misorientation (MO)
where each pixel represents the MO value in this pixel with regard
to all (averaged) neighboring pixels. A color temperature scale (dark
blue to red) has been applied. Ultimately, regions with high MO
average appear brighter (green, yellow, red) than those areas in
the sample with low MO average (light and dark blue).
It can be observed in 316INSS (Fig. 3f) that the region ahead
of the crack tip with a high density of defects such as deformation-
and slip bands appears as region with high MO average, specically
where the slip bands intersect with the grain boundary. As will be
seen next, deformation in the crack tip region is very localized in
this sample. Fig. 3c shows high average MO in the bottom grain
close to the crack ank just before the crack tip. This zone of ele-
vated lattice rotation indicates a high level of plastic deformation
and its presence reinforces the previous suggestion of a crack open-
ing mechanism that involved the sliding of the two grains against
each other (which would result in elevated lattice rotation at the
crack tip).
In addition, misorientation-to-reference (MOTR) maps have
been generated (an option available in the software). Here, each
 M. Meisnar et al. / Micron 75 (2015) 110 5

Fig. 4. Misorientation to reference MOTR maps and misorientation proles along the GB ahead of the crack tip; (a) MOTR map in 316AREVA, white line: location of MO
prole, 0: origin of MO prole; (b) MO prole in 316AREVA, GB MO 4 1.2 ; (c) MOTR map in 316INSS; (d) MO prole in 316INSS, GB MO 29 1.5 .

pixel has a global MO value with regard to a single reference
point within the entire map. Each value within the map represents
the MO from the reference point to the respective pixel. Therefore,
the MO from one point in the map to another can be measured,
revealing for instance the grain boundary misorientation.
In the rst instance, the MOTR maps (316AREVA: Fig. 4a,
316INSS: Fig. 4c) were used to measure the MO between the
two grains adjacent to the open crack by acquiring MO proles
(316AREVA: Fig. 4b, 316INSS: Fig. 4d) from one grain to the other.
The origin (0) of the MO prole is the point of reference for each
pixel along the prole as well as for the entire MOTR map. Since
there is only little change in MO in one grain, but presumably high
change from one grain to the other, the MO proles exhibit a surge
at the location of the grain boundary.
The MO prole for 316AREVA (Fig. 4b) indicates that there is
only 4 1.2 MO between the two grains (the low MO is also the
reason for an apparently noisier prole), whereas the MO prole
in 316INSS (Fig. 4d) jumps from 0 in the top grain to a plateau of
29 1.5 in the bottom grain.
MO prole measurements have been repeated for both samples
at different locations across the grain boundary leading away from
the crack tip with very similar results each time.
The nal step in this characterization of SCC specimen via TKD
was the establishment of a method to measure the plastic strain
at different locations in the sample by utilizing the (indirect) rela-
tionship between the measured MO and plastic deformation of the
crystal lattice. This relationship stems from the fact that the misori-
entation relates to plastic strain gradients originating from lattice
curvature (Lehockey et al., 2000). Such strain gradients are very
likely to occur near crack tips in a constrained volume. It should be
stressed at this point that all misorientation values are relative and
plastic strain has not been quantied.
Fig. 5a shows a MOTR map of the 316INSS sample and the loca-
tions of a number of MO proles acquired in the top and the bottom
grain at different distances from the crack tip. While the misorien-
tation between the two grains has been previously determined as
29 1.5 (Fig. 4d), the current MO proles are used to determine
the MO within a single grain from the crack tip outwards into the
surrounding matrix.
MO proles 1 and 2 have been acquired at the crack tip in the
sample and are shown in Fig. 5b and c. After exhibiting a sudden rise
starting from the origin (close to the crack tip), the MO remains at
a certain value for the remaining distance of the prole. A gradient
of MO is apparent, indicated by the rising MO values over a certain
distance, and suggests substantial lattice deformation in that region
(which henceforth will be called the plastic zone).
The two parameters that have been extracted from the MO pro-
les are the distance from the origin at which the MO reaches

Table 2
MO prole values for Fig.5a. The plastic zone refers to the distance from the origin of the misorientation prole within which there is a misorientation gradient present. The
II component refers to the plastic zone component perpendicular to the crack.

No. Grain Plastic zone (nm) Angle ( ) II plastic zone (nm) Plateau ( )

1 Bottom 100 40 76.6 2.8 0.8

1a Bottom 200 40 153.2 2.9 0.75
1b Bottom 200 40 153.2 2.9 0.8
1c Bottom 25 40 19.15 2 0.9
1d Bottom 25 40 19.15 2 0.85
1e Bottom 20 40 15.32 1.2 0.5
1f Bottom 100 40 76.6 3 0.9
2 Top 120 30 60 1.4 0.6
2a Top 200 30 100 1.4 0.6
2b Top 170 30 85 2.4 0.95
2c Top 400 30 200 4.5 1.2
2d Top 550 30 275 7 1.2
2e Top 50 30 25 4.2 1.15
2f Top 100 30 50 4 1.0
6 M. Meisnar et al. / Micron 75 (2015) 110
Fig. 5. MO proles in 316INSS sample: (a) local MO map, location of MO proles 1
(white line, origin: white square), 1a1f (white dashed lines), MO proles 2 (black
line, origin: black dot) and 2a2f (black dashed lines); (b) MO prole1 (solid line:
raw data, dashed line: tted data): MO reaches plateau of 2.8 0.8 at 100 nm
after the origin; (c) MO prole 2: MO reaches plateau of 1.4 0.6 at 120 nm
after the origin; note: MO proles measured at different angles from GB; II-value
has been calculated for each prole and corresponds to the actual distance from the
GB (see Table).
the plateau (the length of the plastic zone; bottom grain: 100 nm,
top grain: 120 nm) and the relative matrix rotation (in degrees) at
which the plateau is reached (bottom grain: 2.8 0.8 , top grain:
1.4 0.6 ). While in both grains the MO reaches a plateau after
similar distances from the origin, the MO plateau values are very
different (twice as high in the bottom grain compared to the top
grain). However, the MO proles have been acquired at different
angles from the horizontal (grain boundary orientation), in order to
avoid intersection with deformation bands, and therefore, II-values
(normal to the GB, in order to get an actual comparable distance
from the crack tip, grain boundary or open crack) have been calcu-
lated via basic trigonometry in order to be comparable. The results
of these calculations for all MO proles are shown in Table 2.
MO proles 2c2f in the top grain show elevated plateau values
compared to the MO values around the crack tip, probably because
of the high density of deformation bands in that region. Remark-
ably, MO proles 1a and 1b (taken at the crack anks of the bottom
grain) show a much larger plastic zone than the proles taken at or
ahead of the crack tip. This leads to the conclusion that the strain
might be much more localized at the crack tip and ahead of it than
at the crack anks. Fig. 6 shows a MOTR map in 316AREVA, indi-
cating the location of 6 MO proles extracted from the crack anks
as well as the top grain ahead of the crack tip at different distances
from the crack tip.
Notably, the MO plateau values decrease the further away the
proles were acquired from the crack tip. MO prole 3 (Fig. 6e) was
taken at the crack tip and exhibits a plateau at 3.5 1.2 , whereas
MO prole 6, acquired at a distance of 4 m from the crack tip,
plateaus at 1.5 0.5 (Fig. 6h). As in 316INSS (Fig. 5b and c), the
region of plastic deformation can be extracted from the MO proles
by determining the length over which the MO gradient extends,
although here, MO proles 46 are already perpendicular to the
grain boundary. Due to that, only the II-value of MO proles 13
had to be calculated. While the plastic region in MO proles 3 and
6 extends over the rst 200 nm, MO prole 4 shows a shorter region
of plastic deformation (100 nm). In contrast, MO prole 5 reaches
the rst plateau after 200 nm (at 1.8 0.6 ) but exhibits another
MO gradient between 900 and 1100 nm (due to the bending of
the deformation bands), ending at a plateau of 2.5 0.7 .
In addition, the plastic zones at both crack anks of 316AREVA
have been determined. Fig. 6a shows the location of MO prole
1 (top grain) and MO prole 2 (bottom grain) in 316AREVA. Both
proles were acquired with the same angle to the horizontal and
therefore the distances are directly comparable. These measure-
ments show, that the plastic zone in the top grain extends much
further (500 nm) than in the bottom grain (20 nm).
Finally, Fig. 7 shows the comparison of a STEM bright eld image
with the MOTR map of the crack tip in the 316INSS sample and the
respective elemental EELS SI maps.
The STEM image in Fig. 7a shows the boundary between the
upper and the lower grain very clearly due to diffraction contrast.
The grain boundary extends from the left edge of the image in a
straight line until reaching close vicinity to the crack tip. Instead of
continuing straight however, the grain boundary advances into the
bottom grain on a path along the interface of the matrix with the
open crack, revealing that grain boundary migration has occurred.
This is clearly visible in the MOTR map (Fig. 7b) due to the con-
trast resulting from the misorientation between the two grains. In
instances, where the diffraction contrast is not as perceptible as in
the present STEM image (due to specimen tilt for example), TKD
is perhaps the most suitable method for studying grain boundary
migration ahead of SCC crack tips.
Furthermore, Fig. 7d (EELS SI map of OK edge) shows that grain
boundary migration has taken place ahead of the oxidation front
of the crack tip. The region through which the GB has passed is
enriched in Ni (Fig. 7c, EELS SI map of Ni L edge), but Fe and Cr
depleted (Fig. 7e and f, EELS SI maps of Fe and Cr L edge). While
most of this region is also depleted in O, there is a thin nger of Cr
oxide (see O and Cr map) protruding into the Ni-rich region.
5. Discussion
In this study, two specimen exhibiting SCC have been analyzed
via the novel TKD technique which allows orientation mapping
with remarkable spatial resolution.
First of all, the occurrence of IGSCC can easily be veried via TKD
IPFZ maps (Fig. 3a and d), as they highlight the different crystal-
lographic orientation of the two grains. In addition, intergranular
oxide particles can be easily indexed via TKD. It has been previ-
ously established that crystalline oxide particles in open SCC cracks
are usually Fe-rich magnetite or spinel oxides (Bruemmer and
Thomas, 2010; Lozano-Perez et al., 2009b, 2012; Olszta et al., 2012;
Staehle, 2007). In TKD, they appear as particles of certain crystal-
lographic orientation in the IPFZ maps and can be easily located
and distinguished from each other. The misorientation of the oxide
particles and the surrounding matrix can also be easily measured
with this method. This is particularly important in measuring the
 M. Meisnar et al. / Micron 75 (2015) 110 7

Fig. 6. MO proles at crack anks and ahead of the crack tip in 316AREVA; (a) MOTR map indicating the locations of MO proles 1 (top grain) and 2 (bottom grain), the crack
tip region and MO prole 3 at the crack tip (top grain); (b) GB region ahead of crack tip, location of MO proles 46 (top grain); (c) MO prole 1 (plastic zone extends over
500 nm); (c) MO prole 2 (plastic zone extends over 20 nm); (eh) MO proles 36, decreasing MO plateau value with increasing distance from crack tip.

crystallographic relationship between the individual oxide parti-
cles to the grains on either side of the crack and identifying trends
in the oxide particles misorientation and proximity to the parent
grain. In this study, no epitaxial relationships were found, which
suggests an outer oxide growth enhanced by precipitation from
ions in solution.
In addition, TKD has shown to be very effective for the identi-
cation of defects in the material. Image quality maps (Fig. 3b and e)
are constructed based on the index-ability of the Kikuchi pattern in
each pixel. Regions of higher defect density are harder for the soft-
ware to index and therefore appear as darker regions in the image
quality map (Wright and Nowell, 2006). Hence, it is possible with
TKD to acquire high-resolution maps of defects and locate the SCC
crack tip, deformation bands, twinning and slip in the sample.
For example slip transfer (Guo et al., 2014), is a phenomenon
frequently observed in IGSCC research and is straight-forward to
detect in the TKD image quality maps. The slip bands ahead of the
open SCC crack in 316INSS (Fig. 3e) intersect the grain boundary and
protrude into the neighboring grain, however at a slightly different
angle. It was also highlighted that deformation bands intersect-
ing grain boundaries can create regions of high local deformation
(Fig. 3f). TKD image quality maps are very well suited for this
type of research and are as such extremely effective for an initial
high-resolution study of defects surrounding SCC crack tips before
commencing with methods such as TEM.
Moreover, grain boundary misorientation ahead of the crack
tip has also been measured in both samples (Fig. 4). The notion
that there is a connection between intergranular SCC crack propa-
gation and the MO of the grain boundaries the crack propagates
along, is a prominent theory within the SCC research commu-
nity (Bruemmer et al., 2012, 2013; Baik et al., 2012; Britton and
Wilkinson, 2012; Gertsman and Bruemmer, 2001; Lynch, 2013;
Lozano-Perez, 2008a,b; Raja and Shoji, 2011). In particular, West
et al. have established that there is a connection between slip trans-
fer and other grain boundary parameters (e.g. Schmid and Taylor
factor) and SCC susceptibility of certain GBs (West et al., 2012).
Increasing grain boundary inclination and decreasing Schmid fac-
tor lead to the highest normal stress on the grain boundary, making
it more susceptible to cracking. In addition, their ndings suggest
that cracking is more likely along grain boundaries, which exhibit
discontinuous slip. It should be noted that although slip trans-
fer through the cracked grain boundary was observed in 316INSS
(Fig. 3e), there was enough slip incompatibility to create areas
of localized deformation at the intersection of deformation bands
with the grain boundary (Fig. 3f).
Within this study, TKD has been discovered as a method where
the determination of the grain boundary MO is particularly easy
to achieve. It has been determined, that the grain boundary MO in
316AREVA is 4 1.2 and 29 1.5 in 316INSS. Low-angle grain
boundaries as in 316AREVA are unusual for IGSCC, but there are
many other factors inuencing SCC crack propagation that could
be the reason for propagation along this particular grain boundary.
For example, due to the high level of deformation this sample was
exposed to previous to the SCC test (reverse U-bend and surface
8 M. Meisnar et al. / Micron 75 (2015) 110

Fig. 7. Illustration of grain boundary migration in 316INSS; (a) STEM bright eld image recorded with JEOL 2100 at 200 kV; diffraction contrast between the two grains (b)
local misorientation map recorded via TKD: the contrast between grain 1 and grain 2 results from the different crystallographic orientations of the two grains; (cf) EELS SI
maps acquired via JEOL ARM200 at 200 kV (0.7 eV energy resolution, 5 nm pixel size).

shot-peening), the high stress concentration and defect densities
at the GBs makes them susceptible to intergranular SCC. Additional
data has to be acquired in order to make a more general statement
about the dependence of SCC crack propagation on grain boundary
MO, which can now be easily accomplished with TKD.
Furthermore, grain boundary migration, a phenomenon that has
recently been discussed with respect to intergranular SCC (Lozano-
Perez et al., 2014; Schreiber et al., 2014), can clearly be identied
via TKD. The evolution of a grain boundary, often under stress and
corrosion-enhanced diffusion, by traveling short distances through
the crystal and simultaneous growth of one grain at the expense of
the other is known as grain boundary migration. This phenomenon
is possibly enhanced in the vicinity of dislocations or lattice defor-
mations and has been discovered close to SCC crack tips several
times (Lozano-Perez et al., 2014; Schreiber et al., 2014).
Finally, it has been shown how MO proles were used to deter-
mine the plastic zone reaching from the crack tip outwards into
the matrix (Fig. 5). At the crack tip in sample 316INSS, the plastic
zones were measured in MO proles 1 and 2 and extend over a
very similar distance in both grains. However, their nal MO value
(the plateau) is very different (top grain: 1.4 0.6 , bottom grain:
2.8 0.8 ). Therefore, it can be concluded that the lattice deforma-
tion is approximately twice as high in the bottom grain compared
to the top grain.
In the top grain, the plateau values were higher in the region of
high deformation band (DB) density, which may be an indicator for
high stress concentration. In the bottom grain, the plastic zone was
much more localized at the crack tip and ahead of it, compared to
the measurements at the crack ank.
The acquisition of MO proles in the top grain of sample
316AREVA (Fig. 6) showed that the plateau value of the MO
decreases with increasing distance away from the crack tip along
the GB. The extent of the plastic zone at the crack tip region was
also much bigger than in the 316INSS sample. Comparison of the
 M. Meisnar et al. / Micron 75 (2015) 110
MO proles at the crack anks in 316AREVA yielded a much larger
plastic zone in the top grain than in the bottom grain. As dis-
cussed previously, metal dissolution plays an important role in
the oxygenated water chemistry of the oxygenated environment.
Therefore, we can expect that the crack anks we see in 316AREVA
(Fig. 6a) are not the original crack anks present at the beginning of
the SCC test and part of the plastic zone might have been dissolved
since then. However, this seems to only apply to the bottom grain,
which exhibits a much smaller plastic zone. A possible conclusion
could be that the bottom grain has been preferentially dissolved.
In general, comparing the zone of plastic deformation at the
crack tip in both samples, it appears that the MO gradient extends
over a smaller distance (100 nm) in 316INSS than in 316AREVA
(200 nm). Both specimens are not directly comparable in terms
of the governing SCC mechanisms due to different test con-
ditions (water chemistry and form of pre-existing stress), but
the differences in crack opening and morphology can be corre-
lated to a different oxidation and mechanical response of the
alloys.
Regardless of the form of pre-existing stress (cold-rolling for
316INSS and reverse U-bend for 316AREVA), the plastic strain
around the crack tip seems to be much more localized in 316INSS
than in 316AREVA. In addition, it has been observed that a much
larger portion of the crack ank was dissolved in 316AREVA during
the SCC test. In contrast, the crack anks in 316INSS appear to have
been maintained to a very high degree. This suggests that the inu-
ence of oxidation and plastic deformation on crack propagation in
both samples might not be the same. It is known that materials
exposed to oxygenated water chemistry (as 316AREVA) are much
more prone to metal dissolution due to oxidation than materials
exposed to PWR primary water (like 316INSS). Therefore, it could be
proposed that the governing factor in SCC propagation in 316AREVA
might have been a mixture of dissolution and plastic deformation.
In contrast, the plastic zone around the crack tip in 316INSS is much
more localized and hence plastic deformation appears to have been
the major contributor to the SCC process. However, at this stage
further study is required to conrm the validity of these proposed
mechanisms and to propose new insights regarding a general SCC
model.
6. Summary and conclusion
A number of signicant microstructural and micromechanical
features related to SCC have been successfully analyzed via TKD, a
novel high-resolution orientation mapping method based on tradi-
tional EBSD. TKD uses electron transparent TEM lamellae in an SEM
and offers higher spatial resolution than EBSD due to the smaller
interaction volume of the incident beam with the specimen. Tradi-
tional EBSD hard- and software can be used for this technique with
slight changes in the setup.
In this study, TKD has been used to identify and characterize
grain boundary misorientation, grain boundary migration, oxide
particles in the crack opening, deformation and slip bands ahead of
the crack tip as well as the size and degree of plastic deformation
around and ahead of the crack tip.
In conclusion, the application of TKD for characterizing SCC
specimen proved to be very successful for the analysis of some
of the key aspects of SCC and makes it possible to avoid time-
consuming diffraction techniques in order to gain crystallographic
information about the sample. In TKD, a map can be acquired
in 30 min and individual points in the specimen can be ana-
lyzed in a few seconds. TKD is highly recommended for future
SCC research in order to study the inuence of grain orienta-
tion, lattice defects and plastic deformation on the governing SCC
mechanisms.
9
Acknowledgements
The authors are grateful for the support of AREVA (France) and
INSS (Japan) in terms of providing the samples and funding. Finally,
we would like to thank Bruker for supporting the establishment of
TKD at Oxford Materials.
References
Andresen, P.L., 2013. Basic Elements of Initiation and Propagation of SCC in Water-
cooled Nuclear Power Systems.
Arioka, K., 2013. Role of Diffusion of Vacancy in Materials Lead to SCC Initiation.
Arioka, K., Yamada, T., Terachi, T., Staehle, R.W., 2006a. Intergranular stress
corrosion cracking behavior of austenitic stainless steels in hydrogenated high-
temperature water. Corrosion 62, 7483.
Arioka, K., Yamada, T., Terachi, T., Chiba, G., 2006b. Inuence of carbide pre-
cipitation and rolling direction on intergranular stress corrosion cracking of
austenitic stainless steels in hydrogenated high-temperature water. Corrosion
62, 568575.
Arioka, K., Yamada, T., Terachi, T., Chiba, G., 2007. Cold work and temper-
ature dependence of stress corrosion crack growth of austenitic stainless
steels in hydrogenated and oxygenated high-temperature water. Corrosion 63,
11141123.
Arioka, K., Yamada, T., Terachi, T., Miyamoto, T., 2008. Dependence of stress corrosion
cracking for cold-worked stainless steel on temperature and potential, and role
of diffusion of vacancies at crack tips. Corrosion 64, 691706.
Babinsky, K., De Kloe, R., Clemens, H., Primig, S., 2014. A novel approach for
site-specic atom probe specimen preparation by focused ion beam and trans-
mission electron backscatter diffraction. Ultramicroscopy 144, 918.
Baik, S., Olszta, M.J., Bruemmer, S.M., Seidman, D.N., 2012. Grain-boundary structure
and segregation behavior in a nickel-base stainless alloy. Scr. Mater. 66, 809812.
Britton, T.B., Wilkinson, A.J., 2012. High resolution electron backscatter diffraction
measurements of elastic strain variations in the presence of larger lattice rota-
tions. Ultramicroscopy 114, 8295.
Brodusch, N., Demers, H., Gauvin, R., 2013. Nanometres-resolution Kikuchi patterns
from materials science specimens with transmission electron forward scatter
diffraction in the scanning electron microscope. J. Microsc. 250, 114.
Bruemmer, S.M., Thomas, L.E., 2010. Insights into stress corrosion cracking
mechanisms from high-resolution measurements of crack-tip structures and
compositions. Mater. Res. Soc. Symp. Proc. 1264, 159170.
Bruemmer, S.M., Olszta, M.J., Toloczko, M.B., Thomas, L.E., 2012. Linking grain bound-
ary microstructure to stress corrosion cracking of cold rolled alloy 690 in PWR
primary water. NACE Int. Corrosion Conf. Ser. 7, 59125927.
Bruemmer, S.M., Olszta, M.J., Toloczko, M.B., Thomas, L.E., 2013. Linking grain
boundary microstructure to stress corrosion cracking of cold-rolled alloy 690
in pressurized water reactor primary water. Corrosion 69, 953963.
Couvant, T., Legras, L., Pokor, C., Vaillant, F., Brechet, Y., Boursier, J.M., et al., 2007.
Investigations on the mechanisms of PWSCC of strain hardened austenitic
stainless steels. Canadian Nuclear Society 13th International Conference on
Environmental Degradation of Materials in Nuclear Power Systems, 1., pp.
499514.
Das, N.K., Suzuki, K., Ogawa, K., Shoji, T., 2009. Early stage SCC initiation analysis of
fcc Fe-Cr-Ni ternary alloy at 288 C: a quantum chemical molecular dynamics
approach. Corrosion Sci. 51, 908913.
Dietzel, W., Bala Srinivasan, P., 2011. Testing and evaluation methods for stress cor-
rosion cracking (SCC) in metals. In: Raja, V.S., Shoji, T. (Eds.), Stress Corrosion
Cracking: Theory and Practice. , 1st edition. Woodhead Publishing, pp. 133166.
Dingley, D., 2004. Progressive steps in the development of electron backscatter
diffraction and orientation imaging microscopy. J. Microsc. 213, 214224.
Gertsman, V.Y., Bruemmer, S.M., 2001. Study of grain boundary character along
intergranular stress corrosion crack paths in austenitic alloys. Acta Mater. 49,
15891598.
Guerre, C., Raquet, O., Herms, E., Marie, S., Le Calvar, M., 2007. SCC crack growth
rate of cold-worked austenitic stainless steels in PWR primary water conditions.
Canadian Nuclear Society 13th International Conference on Environmental
Degradation of Materials in Nuclear Power Systems, 1., pp. 676699.
Guo, Y., Britton, T.B., Wilkinson, A.J., 2014. Slip band-grain boundary interactions in
commercial-purity titanium. Acta Mater. 76, 112.
Kain, V., 2011. Stress corrosion cracking (SCC) in stainless steels. In: Raja, V.S., Shoji,
T. (Eds.), Stress Corrosion Cracking: Theory and Practice. , 1st edition. Woodhead
Publishing, pp. 199244.
Karlsen, W., Diego, G., Devrient, B., 2010. Localized deformation as a key precursor to
initiation of intergranular stress corrosion cracking of austenitic stainless steels
employed in nuclear power plants. J. Nucl. Mater. 406, 138151.
Keller, R.R., Geiss, R.H., 2012. Transmission EBSD from 10 nm domains in a scanning
electron microscope. J. Microsc. 245, 245251.
Kruska, K., Lozano-Perez, S., Saxey, D.W., Terachi, T., Yamada, T., Smith, G.D.W., 2011.
3D atom-probe characterization of stress and cold-work in stress corrosion
cracking of 304 stainless steel. 15th International Conference on Environmen-
tal Degradation of Materials in Nuclear Power Systems-Water Reactors, 2., pp.
891898.
10 M. Meisnar et al. / Micron 75 (2015) 110
Langevoort, J.C., Fransen, T., Geilings, P.J., 1984. On the inuence of cold work on
the oxidation behavior of some austenitic stainless steels: High temperature
oxidation. Oxidation Met. 21, 271284.
Lehockey, E., Lin, Y., Lepik, O., 2000. Mapping Residual Plastic Strain in Materials
Using Electron Backscatter Diffraction., pp. 247264.
Lozano-Perez, S., 2008a. A guide on FIB preparation of samples containing stress
corrosion crack tips for TEM and atom-probe analysis. Micron 39, 320328.
Lozano-Perez, S., 2008b. Novel characterization of stress corrosion cracks. J. Phys.:
Conf. Ser. 126.
Lozano-Perez, S., Gontard, L.C., 2008. Understanding stress corrosion cracking with
electron tomography. Microsc. Microanal. 14, 642643.
Lozano-Perez, S., Titchmarsh, J.M., 2003. TEM investigations of intergranular stress
corrosion cracking in austenitic alloys in PWR environmental conditions. Mater.
High Temp. 20, 573579.
Lozano-Perez, S., Titchmarsh, J.M., Jenkins, M.L., 2004. TEM characterization of stress
corrosion cracks in 304SS. Inst. Phys. Conf. Ser. 179, 233236.
Lozano-Perez, S., Kilburn, M.R., Yamada, T., Terachi, T., English, C.A., Grovenor, C.R.M.,
2008a. High-resolution imaging of complex crack chemistry in reactor steels by
NanoSIMS. J. Nucl. Mater. 374, 6168.
Lozano-Perez, S., Schrder, M., Yamada, T., Terachi, T., English, C.A., Grovenor, C.R.M.,
2008b. Using NanoSIMS to map trace elements in stainless steels from nuclear
reactors. Appl. Surf. Sci. 255, 15411543.
Lozano-Perez, S., Saxey, D., Terachi, T., Yamada, T., Cervera-Gontard, L., 2009a. 3-D
characterization of SCC in cold worked stainless steels. 14th International Con-
ference on Environmental Degradation of Materials in Nuclear Power Systems
Water Reactors, 2., pp. 926934.
Lozano-Perez, S., Yamada, T., Terachi, T., Schrder, M., English, C.A., Smith, G.D.W.,
et al., 2009b. Multi-scale characterization of stress corrosion cracking of cold-
worked stainless steels and the inuence of Cr content. Acta Mater. 57,
53615381.
Lozano-Perez, S., Kruska, K., Iyengar, I., Terachi, T., Yamada, T., 2012. Understand-
ing surface oxidation in stainless steels through 3D FIB sequential sectioning. J.
Phys.: Conf. Ser. 371.
Lozano-Perez, S., Dohr, J., Meisnar, M., Kruska, K., 2014. SCC in PWRs: learning from
a bottom-up approach. Metall. Mater. Trans. E 1, 194210.
Lynch, S.P., 2011. Mechanistic and fractographic aspects of stress-corrosion crack-
ing (SCC). In: Raja, V.S., Shoji, T. (Eds.), Stress Corrosion Cracking: Theory and
Practice. , 1st edition. Woodhead Publishing, pp. 178.
Lynch, S.P., 2013. Mechanisms and kinetics of environmentally assisted cracking:
current status, issues, and suggestions for further work. Metall. Mater. Trans. A:
Phys. Metall. Mater. Sci. 44, 12091229.
Olszta, M.J., Schreiber, D.K., Thomas, L.E., Bruemmer, S.M., 2011. Electron microscopy
characterizations and atom probe tomography of intergranular attack in alloy
600 exposed to PWR primary water. 15th International Conference on Environ-
mental Degradation of Materials in Nuclear Power Systems-Water Reactors, 2.,
pp. 14221435.
Olszta, M., Schreiber, D., Thomas, L., Bruemmer, S., 2012. High-resolution crack imag-
ing reveals degradation processes in nuclear reactor structural materials. Adv.
Mater. Process. 170, 1721.
Raja, V.S., Shoji, T., 2011. Stress Corrosion Cracking Theory and Practice. Woodhead
Publishing, Cambridge, UK.
Rice, K.P., Keller, R.R., Stoykovich, M.P., 2014. Specimen-thickness effects on trans-
mission Kikuchi patterns in the scanning electron microscope. J. Microsc. 254,
129136.
Schreiber, D.K., Olszta, M.J., Bruemmer, S.M., 2014. Grain boundary depletion and
migration during selective oxidation of Cr in a Ni-5Cr binary alloy exposed to
high-temperature hydrogenated water. Scr. Mater. 89, 4144.
Schwartz, A.J., Kumar, M., Adams, B.L., Field, D., 2009. Electron Backscatter Diffraction
in Materials Science, 2nd edition. Springer.
Scott, P.M., Le Calvar, M., 1993. Some Possible Mechanisms of Intergranular Stress
Corrosion Cracking of Alloy 600 in PWR Primary Water., pp. 657667.
Shoji, T., Lu, Z., Peng, Q., 2011. Factors affecting stress corrosion cracking (SCC) and
fundamental mechanistic understanding of stainless steels. In: Raja, V.S., Shoji,
T. (Eds.), Stress Corrosion Cracking: Theory and Practice. , 1st edition. Woodhead
Publishing, pp. 245272.
Staehle, R.W., 2007. Critical analysis of tight cracks. Canadian Nuclear Society 13th
International Conference on Environmental Degradation of Materials in Nuclear
Power Systems, 3., pp. 18771957.
Staehle, R.W., 2010. Approach to Predicting SCC of Fe-Cr-Ni Alloys.
Suzuki, S., 2013. Features of transmission EBSD and its application. JOM 65,
12541263.
Terachi, T., Arioka, K., 2006. Characterization of oxide lm behaviors on 316 stainless
steels in high-temperature water inuence of hydrogen and oxygen consider-
ations for initiation of SCC. In: NACE International Corrosion Conference Series,
pp. 0660810660810.
Terachi, T., Yamada, T., Chiba, G., Arioka, K., 2007. Inuence of cold work on IGSCC of
316 stainless steel in hydrogenated high-temperature water. In: NACE Inter-
national Corrosion Conference Series, pp. 076051076059.
Terachi, T., Yamada, T., Miyamoto, T., Arioka, K., Fukuya, K., 2008. Corrosion behavior
of stainless steels in simulated PWR primary water-effect of chromium content
in alloys and dissolved hydrogen. J. Nucl. Sci. Technol. 45, 975984.
Trimby, P.W., 2012. Orientation mapping of nanostructured materials using
transmission Kikuchi diffraction in the scanning electron microscope. Ultrami-
croscopy 120, 1624.
Trimby, P.W., Cairney, J.M., 2014. Transmission kikuchi diffraction in the scanning
electron microscope: orientation mapping on the nanoscale. Adv. Mater. Pro-
cess. 172, 1315.
Trimby, P.W., Cao, Y., Chen, Z., Han, S., Hemker, K.J., Lian, J., et al., 2014. Characterizing
deformed ultrane-grained and nanocrystalline materials using transmission
Kikuchi diffraction in a scanning electron microscope. Acta Mater. 62, 6980.
Vaillant, F., Boursier, J., Rouillon, Y., Couvant, T., Amzallag, C., Raquet, O., 2004. Stress
Corrosion Cracking of Cold Worked Austenitic Stainless Steels in Laboratory
Primary PWR environment, 490. American Society of Mechanical Engineers,
Pressure Vessels and Piping Division (Publication) PVP, pp. 5163.
West, E.A., McMurtrey, M.D., Jiao, Z., Was, G.S., 2012. Role of localized deformation
in irradiation-assisted stress corrosion cracking initiation. Metall. Mater. Trans.
A: Phys. Metall. Mater. Sci. 43, 136146.
Wright, S.I., Nowell, M.M., 2006. EBSD image quality mapping. Microsc. Microanal.
12, 7284.
Yamada, T., Terachi, T., Miyamoto, T., Arioka, K., 2009. Crack growth behav-
ior of welded and cast stainless steels in hydrogenated and oxygenated
high-temperature water. 14th International Conference on Environmental
Degradation of Materials in Nuclear Power Systems Water Reactors, 1., pp.
684689.
Zaefferer, S., 2011. A critical review of orientation microscopy in SEM and TEM. Cryst.
Res. Technol. 46, 607628.