M A TE RI A L S C H A RAC TE RI ZA T ION 6 0 ( 2 00 9 ) 1 1 9 1–1 2 0 1

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Tutorial review

Tutorial on x-ray microLaue diffraction

Gene E. Ice⁎, Judy W.L. Pang

Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN 37831-6118, USA

AR TIC LE D ATA ABSTR ACT

Article history: MicroLaue diffraction combines the oldest x-ray diffraction method–Laue diffraction–with the
Received 1 May 2009 most modern x-ray sources, optics and detectors. The combination can resolve complex
Received in revised form materials into single-crystal-like submicron volumes. This unique ability to nondestructively
6 July 2009 map crystal structure at and below a sample surface, with high spatial and strain resolution
Accepted 21 July 2009 can address long-standing fundamental issues in materials science. For example, the three-
dimensional evolution of mesoscale structure and the self organization of defects can be
Keywords: observed nondestructively to understand the origins of inhomogeneous grain growth,
X-ray deformation and fracture.
Microbeam © 2009 Elsevier Inc. All rights reserved.
Laue
Diffraction
Deformation
Grain growth
Fracture

1. Introduction—Brief History of ability is particularly timely because it provides direct compar-

MicroLaue Diffraction
In 1912, there was serious debate within the scientific commu-
nity over both the nature of x-rays and the nature of crystals
[1]. These debates were conclusively settled when, guided by
Max von Laue's insight that crystal lattice dimensions were
ideal for generating interferences in x-rays, Friedrich and
Knipping produced the world's first Laue patterns. These early
experiments set the stage for our current understanding of
crystal structure, the nature of x-rays and ultimately the be-
havior of materials. Now almost a century later, Laue diffraction
is poised for a second revolution with the potential to unlock
some of the most important and long-standing mysteries of
materials science. This new revolution is based on the addition
of unprecedented spatial and angular resolution, which allows
for nondestructive characterization of local crystal structure
with submicron three-dimensional (3D) resolution. This new
isons with–and guidance for–emerging theoretical models of
fundamental processes essential to modern technology, includ-
ing grain growth, inhomogeneous deformation and fracture.
Driving this second revolution is the development of ultra-
brilliant x-ray synchrotron sources. Synchrotron x-ray sources
are now some 14 orders of magnitude more brilliant (photons/
s/mm2/mrad2/eV) than conventional sources. This high bril-
liance has opened new scientific frontiers in biology, geology,
chemistry and materials science, and allows for intense
submicron x-ray beams capable of producing Laue patterns
in milliseconds. In addition to the availability of intense x-ray
sources, microLaue diffraction has also benefited from the
development of advanced x-ray optics, efficient x-ray area
detectors and powerful computational capabilities with new
data analysis strategies.
The importance of spatially-resolved diffraction has long
been recognized [2]. Both electron beam and laboratory-based

⁎ Corresponding author.
E-mail address: IceGE@ornl.gov (G.E. Ice).

1044-5803/$ – see front matter © 2009 Elsevier Inc. All rights reserved.
doi:10.1016/j.matchar.2009.07.006
1192 M A TE RI A L S C H A RAC TE RI ZA T ION 6 0 ( 2 00 9 ) 1 1 9 1– 1 2 0 1
x-ray microdiffraction efforts predate the widespread avail-
ability of synchrotron radiation and continue. For example,
electron-backscattering diffraction (EBSD) is now a critical tool
in materials science [3], and provides a rapid method of ana-
lyzing surface crystal structures which can be extended to 3D
analysis by systematically removing surface layers [4,5]. In
addition, heroic laboratory experiments with x-ray microdif-
fraction predate synchrotron sources and continue to inspire
and provide important information about materials [6–11].
Within this context, microLaue diffraction provides unprece-
dented flexibility to study complicated 3D crystal structures
nondestructively, with little sample preparation, and with Q
resolution only possible in special cases with electron diffrac-
tion methods.
A major milestones toward modern microLaue diffraction
was a spatially-resolved Laue measurement on a white beam
topography line at the National Synchrotron Light Source
circa 1987 [12]. Using a 25 μm-Ø laser-drilled pinhole in Pt,
Rebonato et al. [12] mapped changes in the elastic strain
distribution near a single-crystal Mo notch during a tensile
experiment. This demonstration experiment used a simple
knife-edge to localize the Laue spots and a solid-state detector to
determine spot energy. Even this early approach demonstrated
the ability of microLaue measurements to precisely determine
changes in local lattice parameters and to relate elastic strain
maps to the local boundary conditions. Also, while similar to
lab-based experiments by Weismann and co-workers [6–8], the
measurements were made with 100× smaller beams.
Around 1990 these and related results came to the attention
of Walter Brown at Bell Laboratories who invited Gene Ice to
discuss how such techniques might be adapted to study elastic
strains in microelectronic interconnects. At the time, elastic
strains were known to influence interconnect reliability, but no
direct measurements were possible because actual intercon-
nect material was buried under an oxide passivation layer.
From their discussions a complete picture emerged that in-
cluded the essential elements needed to efficiently map elastic
strains in thin films: (1) achromatic microfocusing optics, (2) an
efficient area detector; (3) a precision sample stage; and (4) an
insertable monochromator to characterize the energy of one or
a few Laue spots. This basic suite of instrumentation was later
realized in a demonstration project on the MHATT-Cat beam-
line 7-ID at the Advanced Photon Source (1998) and later on
the dedicated APS station 34-ID-E (2000). Resolution in the
third dimension was added through an insight by Bennett
Larson [13]. Larson et al. adapted beam profiling techniques
used to measure the incident beam size and diffracted beam
ray tracing techniques under development by Stewart Stock
and others to create a simple but powerful way to localize Laue
diffraction along the incident x-ray beam. This technique was
called differential aperture microscopy [13].
Of course during this period of time parallel and related
efforts were underway around the world. Early microdiffrac-
tion experiments at Daresbury [14], the Photon Factory [15,16],
the NSLS [17,18], and the ESRF [19,20] demonstrated the
importance of localized x-ray diffraction information from
materials. At the ALS, experiments aimed at a microLaue
capability began around 1997 with a proof-of-principle experi-
ment in 1998. The microLaue station 7.3.3 at the ALS
championed by Howard Padmore and J. Patel–with a virtually
identical instrumentation philosophy to 34-ID-E–came on line
in 1999. Early results from beamline 7-ID and station 34-ID-E at
the APS, as well as the results from 7.3.3 at the ALS justified
the optimism of the early supporters with unexpected
observations of deformation in electronic interconnects [21]
and with a conclusive picture of grain growth mechanisms in
high-temperature superconductor (RABiTS) films [22].
Based on these and a growing number of exciting results,
microLaue instruments have now been commissioned at the
Pohang Synchrotron [23], the Swiss Light Source (X05LA) [24],
and the Canadian Light Source (VESPERS) [25] with other in-
struments planned for the Australian Light Source [26], SOLEIL
[27], PETRA III and elsewhere. In addition, in 2007 the Ad-
vanced Light Source moved microLaue experiments to a new
more powerful beamline 12.3.2 [28].
2. Underlying Physics of MicroLaue Diffraction
2.1. Laue Diffraction from Perfect Crystals
As Laue guessed in 1912, the atomic lattice in crystals creates
constructive and destructive interferences in the scattering of
x-rays from the crystal atoms. It is well known, for example
that a monochromatic x-ray beam of wavelength λ efficiently
reflects off crystal planes with spacing d, when the crystal is
rotated to satisfy the Bragg condition:
2dsinh = nk: ð1Þ
Here θ is the angle between the incident beam and a real-
space set of parallel atomic planes defined by the crystal
lattice. Here we note that the real space planes are defined as
described below according to the real-space lattice, but do not
necessarily intersect real atoms. Efficient scattering results
from constructive interference of the weak scattering from
thousands of atomic planes within the crystal. What is often
less appreciated is that between the conditions for efficient
scattering, the crystal lattice causes destructive interferences
and scattering away from the Bragg condition is typically
weaker than from an amorphous sample with the same atoms.
Indeed for good crystals, the chance of satisfying the Bragg
condition with an arbitrary crystal orientation and a mono-
chromatic beam is small.
The beauty of Laue diffraction is the automatic selection of
those monochromatic wavelengths from continuous spectra
that satisfy the Bragg condition and the reflection of those
wavelengths into angles that are determined by the shape and
orientation of the unit cell. The ability to determine crystal
orientation quickly and with minimum sample preparation
continues to make Laue diffraction a useful tool even today.
Schematically the main elements of Laue diffraction can be
understood with a generalized Ewald Sphere construction. As
illustrated in Fig. 1, constructive interference for a real space
lattice occurs under specific conditions related to the x-ray
wavelength and to the crystal orientation with respect to the
incident beam. For more details see for example reference [29]
or any general text on x-ray diffraction. The three dimensional
orientation/wavelength conditions set up a reciprocal space
lattice and if the momentum transfer, kf–ki, for a scattering
direction intersects a reciprocal lattice point, then the crystal
 M A TE RI A L S C H A RAC TE RI ZA T ION 6 0 ( 2 00 9 ) 1 1 9 1–1 2 0 1
Fig. 1 – Two-dimensional Ewald sphere diagram generalized
to show the reciprocal space volume probed by a
polychromatic beam with maximum and minimum
wavelengths λmax and λmin. Note that for a given diffraction
direction in real space, the intensity is a radial integral
through reciprocal space weighted by the spectral density
distribution between λmax and λmin. The parallel planes
responsible for a reciprocal latticepoint, hkl, are defined by
the intersection of the nearest-neighbor planes with the
real-space unit cell vectors (inset on top right).
reflects efficiently. With monochromatic beams, the set of all
possible momentum transfers is a sphere called the Ewald
Sphere. Curiously, it was Ewald whose mathematical investi-
gation of electromagnetic waves in a space-lattice helped
stimulate Laue's speculation about interferences of x-rays
passing through crystals.
As shown in Fig. 1, the Ewald sphere for a wavelength λ
always passes through the (0,0,0) reciprocal lattice point (small
angle scattering) and may or may not pass through another
reciprocal lattice point depending on the crystal orientation.
However, if a continuum with a sufficient range of wave-
lengths is directed onto a crystal, then a volume of reciprocal
space is sampled, and multiple constructive interference con-
ditions (Laue spots) are satisfied. Each constructive interfer-
ence, represents a particular wavelength and a particular set
of parallel crystal planes (Fig. 1 insert top right). The crystal
planes that contribute to each reflection are defined by the
index, hkl, which specifies the intercept of the next parallel
plane with the real-space lattice vectors. For an hkl plane that
passes through the origin in real space, the next parallel plane
in the system of planes intercepts along the a1 lattice direction
at a1/h, along the a2 lattice direction at a2/k and along the a3
lattice direction at a3/l (Fig. 1 upper right inset). The plane
normal for a Laue reflection → n hkl, is determined by the in-
cident beam direction (− j) and the real-space scattered beam
direction →r hkl [29],
Yr +j
Y
n hkl = Yhkl : ð2Þ
j rhkl + jj
For a cubic lattice, the inter-plane spacing is d = a0 =
pffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
h2 + k2 + l2 , and the plane spacing for any set of planes can
be determined experimentally through Braggs law if the angle
of diffraction and the wavelength of the diffraction x-rays are
known (Eq. (1)).
1193
This represents the basic theory of Laue diffraction as it is
typically practiced. Almost always the Bragg plane directions
are the main interest with conventional Laue diffraction. The
remaining complexity is that to understand the orientation
of a crystal, the Bragg plane identity or index, hkl, must be
determined. Experienced researchers can look at the symme-
try around a reflection and guess the index of the reflection.
In addition, a number of programs exist for determining the
index based on the angles between reflections (see for exam-
ple reference [30]).
With microLaue diffraction the addition of submicron spa-
tial resolution opens up a number of exciting possibilities.
Spatial resolution perpendicular to the beam direction is
created by achromatic focusing optics— typically Kirkpatrick–
Baez mirrors. With thin films, this allows for small volumes to
be studied directly (Fig. 2a). Thin film research with microLaue
diffraction is unique in its ability to nondestructively study
thin layers below the surface of a sample and to relate the
crystallography of the substrate to the crystallography of the
overlying layers.
With bulk samples the penetrating nature of x-rays probes
along an extended volume in the sample. The Laue patterns
from subgrain volumes along the beam are superimposed at
the detector, but can be resolved by passing an absorbing wire
near to the sample surface and then ray tracing back to the
beam axis (Fig. 2b). With this differential aperture micro-
scopy, completely novel materials characterization becomes
possible. For example, grain boundaries, phase boundaries
and other interfaces can be mapped in 3D by comparing the
point-to-point Laue patterns from small volumes and map-
ping how the Laue patterns change within larger volumes.
In addition, to good spatial resolution, the use of small probe
beams and high-resolution x-ray sensitive area detectors allows
for precision measurements of the angles between Laue spots.
Changes in inter-spot angles, compared with the angles in
unstrained materials can be used to determine the deviatoric
strain tensor (shape of the unit cell). Four linearly independent
reflections determine the unit cell shape, and the energy of any
one of the four reflections can be used to determine the unit cell
volume (full strain tensor). Beyond the local elastic strain, local
rotations of the Laue patterns, can for the first time, be used to
determine the Nye Tensor which results from unpaired dis-
locations, and is of fundamental interest to theoretical models
of crystal plasticity [31]. Below we briefly outline how microLaue
Fig. 2 – (a). With a focused microbeam, thin films can be
studied with submicron transverse resolution. (b). A wire can
be used to decode the overlapping Laue patterns from
volumes along the incident probe beam.
1194 M A TE RI A L S C H A RAC TE RI ZA T ION 6 0 ( 2 00 9 ) 1 1 9 1– 1 2 0 1
patterns can be used to determine information about the local
elastic strain (stress) and the local dislocation content. This
formalism is based on Fig. 1, which shows that in a Laue ex-
periment, each pixel intensity at the 2-D detector records a
radial line integral through reciprocal space weighted by the
incident beam spectra.
2.2. Laue Diffraction from Imperfect Crystals
2.2.1. Elastic Strain
Elastic stress is one of the key driving forces for mesoscale
materials evolution and single crystal strain can be used as a
monitor of stress through the compliance matrix [32]. Ul-
timately local elastic stress can be determined by deviations
from the unstrained unit cell parameters of subgrain crystal
volumes. Methods for determining the unit cell parameters
from monochromatic automated diffractometer experiments
on single crystals have been famously derived by Busing and
Levy [33]. Their formalism finds that 3 linearly independent
reflections determine the 3 parameters required for crystal-
lographic orientation and the 6 parameters of the unit cell: a,
b, c, α, β, γ. Following a similar formalism, Chung and Ice [30]
show that four Laue reflections (λ unknown) determine the
3 crystallographic orientation parameters and the unit cell
shape: a/c, b/c, α, β, γ. Once the unit cell shape is known, the
unit cell parameters can be determined with the additional
information of the energy of one reflection. The components
of the second-rank elastic strain tensor, εij, (deviatoric or full)
can be determined from the transformation matrix T that
maps unstrained to strained vectors, [30]
 
eij = Tij + Tji =2  Iij where Ameas = TA0 :
It is important to note that although elastic strain distorts
the angles between reflections, with a constant strain tensor
throughout the sampled volume, the sharpness of the Bragg
spots will not be changed. However, if the elastic strain tensor
Fig. 3 – Various dislocation types have distinct effects on the observed Laue diffraction pattern. Here we compare modeled
streaking of three of 12 most likely slip systems in an FCC alloy with experimental measurement of an Ir weld.
changes within the volume probed (strain gradients), then the
angular distortions are not uniform and the reflections must
be blurred. A strain tensor gradient can therefore cause blurring
and streaking of the Bragg peaks. In general, the strain tensor
(either deviatoric or total) at each point inside a sample can
therefore be determined by 3D spatially resolved microLaue
diffraction. Strain gradients can then be calculated by differ-
ential geometry. There is however another very common
cause of Laue spot streaking: dislocations.
2.2.2. Dislocations and MicroLaue Patterns
In many materials, Laue streaking due to unpaired disloca-
tions is common and dominates over the influence of elastic
strain gradients. Dislocations are line defects that interrupt
the periodicity of the crystal lattice and introduce long-range
rotations between sections of the crystal lattice. The rotation
axis depends on the kind of dislocation. The size of the mea-
sured rotations depends on the density of unpaired or geo-
metrically necessary dislocations and on the volume sampled.
Because the character of Laue pattern streaking changes with
dislocation type (Fig. 3) and because the commonly activated
dislocations are known for most materials, 3D spatially-
resolved blurring of Laue patterns can be fitted to models to
evaluate the most likely slip systems in a local volume [34–36].
In principle, it is also possible to derive information about the
total dislocation density by observing longitudinal blurring of
the Laue reflections [34–36]. However these are much more
difficult experiments and have not yet been attempted. In real
materials, inhomogeneities in dislocation density and elastic
stresses are interrelated, and can arise either because of the
geometry of loading or because of inhomogeneous deforma-
ð3Þ tion in the materials.
Although modeling can lead to insights into the activated
dislocations, there are assumptions involved because real
materials have a complex distribution of various dislocation
kinds. However, microLaue diffraction can unambiguously de-
termine the local Nye (dislocation) tensor and can even
 M A TE RI A L S C H A RAC TE RI ZA T ION 6 0 ( 2 00 9 ) 1 1 9 1–1 2 0 1
determine this in the presence of an elastic strain gradient.
This capability has been demonstrated in a series of beautiful
experiments by Larson, El-Azab et al., [31] and is of great
importance because of the central role the Nye tensor plays in
emerging theories of size-dependent plasticity. Formally, the
Nye tensor αij, is determined by measurements of local lattice
curvature κ and elastic strain tensor gradients.
aij = jji  ðjii ÞIij  eijk Ak elj :
The curvature tensor κ and the elastic strain gradient
components can be determined by mapping the local crystal-
lographic orientation and elastic strain in three dimensions.
As mentioned above, the development of strain gradient
plasticity theories [37,38] represent an effort to bridge the gap
between classical plasticity and dislocation theory and to ac-
count for size-dependent plasticity. Considering different mod-
els of geometrically necessary dislocations of constant density,
GNDs, Gao [38] related effective strain gradient η to the density
of GNDs, n+. In many cases plastic strain and dislocation den-
sity heterogeneity within the crystal lattice can precipitate the
organization of defects and the presence of local lattice rotations
changes the diffraction conditions and causes redistribution of
intensity of each Laue spot. In this way, Laue images collected
using synchrotron x-ray microbeams are sensitive to the hier-
archical distribution of dislocations.
3. Implementation of Polychromatic
Microdiffraction
Although Laue diffraction is inherently a rather simple char-
acterization method, the extension to submicron-spatial resolu-
tion with <0.01° angular resolution requires special equipment
and techniques. This is particularly true for mapping local
crystal structure and defects in 3D. A schematic of the geometry
for a generic polychromatic microdiffraction experiment is
shown in Fig. 4. The experiment has six key elements: (1) the
intense source, (2) a nondispersive monochromator that can
be inserted into or out of the polychromatic x-ray beam to pass
either a polychromatic or a tunable monochromatic beam on-
to the sample, (3) a nondispersive focusing system (typically
Fig. 4 – A generic polychromatic microdiffraction system has
six key elements: (1) a brilliant polychromatic x-ray source;
(2) a nondispersive monochromator that can be moved into or
out of the beam; (3) achromatic focusing optics; (4) a precision
sample stage; (5) an x-ray absorbing wire; and (6) an x-ray
sensitive area detector.
1195
Kirkpatrick–Baez Mirrors) that focus either monochromatic or
polychromatic beams to the same spot, (4) the sample with a
precision 3D stage to position the sample; (5) an absorbing wire
that can run through the diffraction pattern to resolve the Laue
diffraction from along the penetrating beam path; and (6) an
x-ray sensitive area detector.
The experiments are typically run at a nominal 2θ scat-
tering angle of 90°, although other options are possible. This
ð4Þ
choice of scattering angles has two advantages: (1) the depth
sampled by the x-rays is maximized at 90°, and (2) the spatial
resolution along the incident x-ray beam from differential
aperture microscopy is best at 90°. One disadvantage of work-
ing at 90° is the lower reflectivity of high-energy reflections
and a transmission geometry is used at the SLS [24].
In a typical experiment the sample is mounted on the
sample stage, and positioned so its surface intersects the beam
near the focus of the nondispersive focusing optics. The initial
sample positioning is done using either a laser position
monitor or a long-distance microscope. After the sample is
positioned, a polychromatic Laue pattern is collected with the
x-ray sensitive area detector. The pattern is indexed with an
automated indexing program using the known unit cell
parameters of the undeformed material. Once the index of
the reflections is determined, then the energies of the reflec-
tions can be estimated. At this point the experimental ap-
proach depends on the kind of sample that is being studied
and the kind of information that is required. The white beam
measurements inherently provide the deviatoric stain tensor
which is sensitive to geometrical distortions of the unit cell
shape but not to hydrostatic strain. If deviatoric strain is
sufficient, then the sample can be mapped in two dimensions
by simply moving the sample under the focused beam. If three-
dimensional information is required, then at each position of
the sample, the wire is moved through the diffraction pattern
(wire scan) and the shadow of the wire on the diffraction
pattern is used to triangulate backward the measured intensity
at the detector. This “differential aperture microscopy meth-
od” determines the local Laue pattern generated at each sub-
grain volume along the incident beam.
For even more detailed information, scanning energy
methods can be used to determine the absolute strain tensor.
For example, if the energy of even one Laue reflection is de-
termined, then the deviatoric strain tensor can be set on an
absolute scale and the full strain tensor is determined. Nat-
urally in order to make such measurements, both wire scans
and monochromator energy scans are needed in addition
to two-dimensional samples scans. These measurements are
therefore very time consuming and even with the fastest area
detectors can only be used over restricted 3D volumes.
4. Example Applications of MicroLaue Diffraction
MicroLaue diffraction has widespread applicability both to stud-
ies of fundamental materials physics and to applied studies of
specific materials systems. For example, microLaue diffraction
has been used to understand unanticipated deformation pro-
cesses in electronic interconnect materials during electromi-
gration [21]. Other examples include fundamental studies of
1196 M A TE RI A L S C H A RAC TE RI ZA T ION 6 0 ( 2 00 9 ) 1 1 9 1– 1 2 0 1
dislocation patterning in Cu single crystals [39] that allow direct
comparison to plasticity simulations; studies of 3D grain growth
mechanisms that test the impact of grain boundary curva-
ture and defect refinement [40]; measurements of elastic stain
distributions in anomalous Sn grain growth leading to Sn
whiskers in Pb-free solders [41]; and measurements of hetero-
epitaxial grain growth on surfaces with specific implications of
high-temperature superconductor films on textured substrates
[22]. In general the unique power of polychromatic microdif-
fraction is to observe 3D crystal structures nondestructively
and with sufficient spatial and angular resolution as to test
theories of mesoscale evolution driven by inhomogeneous
strain, plasticity, or defect distributions. We describe below
four experiments that illustrate the how microLaue and related
methods can contribute to our understanding of inhomoge-
neous deformation and elastic strain distributions. We proceed
from polycrystal samples with complicated grain boundary
networks to bi-crystals and ultimately to single crystal samples.
As the starting complexity of the sample decreases, in many
ways the sophistication of theory must increase to account for
more subtle processes that break sample symmetry.
4.1. Subgrain Rotations Near the Free surface of
Polycrystalline Materials
An example of unexpected complexity in local subgrain lattice
rotations during deformation, is a uni-axial tension experi-
ment by Pang et al. that followed local lattice rotations near the
surface of a polycrystalline Ni sample [42]. This nondestructive
microLaue study provides new insights into mesoscale defor-
mation inhomogeneity in polycrystalline materials. The aver-
age grain size of the Ni sample was ~100 μm. Microbeam-Laue
diffraction reveals pronounced Laue streaking after 15% strain
(Fig. 5a). The plastic response of the material in each grain can
be explained by the formation of a cell wall structure to relax
the stress field induced during pulling.
After deformation, depth-resolved Laue images were con-
structed below the free surface of a single Ni grain with the
­
grain surface normal almost parallel to [2 33] and with loading
­
direction approximately in [11 2] direction. Distinct streaking
of the Laue spots is observed to ~25 μm below the sample
surface. The depth-integrated Laue image is given in Fig. 5a.
The depth-resolved Laue images identify the contribution of
Fig. 5 – a) Experimental Laue images from a grain A of a
polycrystalline Ni sample after 15% of strain; b) detailed
features of the Laue streak corresponding to the boxed region
in a).
the Laue streaks at various depths of the samples. Fig. 5b
shows a small region of the Laue pattern, corresponding to the
boxed region in Fig. 5a. In the near-surface region only one set
of very-long streaks is present which is replaced by a second
set of streaks about 12–15 μm below the surface. Each set of
streaks is related to a certain (predominant) dislocation den-
sity tensor and indicates that at least two regions with dif-
ferent slip systems and different strain gradient direction are
present in the probed volume [43].
The streak profiles were used to determine the orientation of
eigenvectors and eigenvalues of the dislocation density tensor
from the streaks profiles of the experimental Laue pattern at
each region. The predominant slip systems corresponding to
the dislocation density tensor were determined by least square
fitting. To understand the shape of the experimental Laue
images and to check the sensitivity of the Laue image to
different possible slip systems, Laue patterns were simulated
with different slip systems. As Ni is face-centered cubic, slip
systems comprised of dislocation movements with the distor-
tion direction, Burger's vector b // h110i and corresponding glide
planes [111], and dislocation lines ξ // h112i are considered.
Assuming only one set of slip system is activated in the
near surface region, the direction of the slip system is deter-
­ ­
mined to be b // [011 ] and ξ // [21 1]. A change in the slip
direction was observed at around 15 μm where splitting of the
streaks were noted as illustrated in Fig. 5. The split indicates
that more than one slip system was activated. It is not possible
to determine the exact number of activated slip systems from
the experiment. Instead the minimum number of slip systems
required to explain the observed Laue patterns was assumed.
­
The best-fit set is a combination of two slip systems: b // [011 ]
­ ­ ­ ­
and ξ // [211 ] + b // [01 1] and ξ // [2 11 ]. Comparison between the
simulated and experimental images is shown in Fig. 6. The
addition of one more slip systems at 15 μm is consistent with
the argument that restrictions in the bulk may require more
dislocation activities to achieve rotation.
4.2. Grain Boundary Effects on Local Dislocation Density
Grain deformation is strongly influenced by the crystallographic
orientations of the grain and by the orientation of neighbor
grains, which influences the grain boundary type. Inhomoge-
neous deformation is anticipated at grain boundaries because of
strain incompatibility of neighbor grains, and because the grain
Fig. 6 – a) Experimental and b) simulated Laue patterns
corresponding to the depths 15–25 mm beneath the surface.
 M A TE RI A L S C H A RAC TE RI ZA T ION 6 0 ( 2 00 9 ) 1 1 9 1–1 2 0 1 1197

boundary provides a barrier to dislocation motion. A bicrystal

is the simplest case to explore these processes.
Ohashi, Pang et al. [44] studied the local rotations in a Ni
bicrystal during in situ uniaxial pulling at 0, 12 and 16% plastic
strain. The rotations were characterized with microLaue dif-
fraction. Quantitative information such as lattice rotation and
dislocation density development was obtained with 3D sub-
micron spatial resolution. The sample loading axis was par-
allel to the laboratory x-axis (perpendicular to the incident
beam direction). Diffraction patterns were collected from dif-
ferent sample locations in grains A (left) and B (right) by
translating the sample under the white microbeam. Micro- Fig. 8 – Laue patterns for deformed grains A and B.
Laue patterns were recorded along a line parallel to the sample
loading axis (x) with a varying pitch: 2 μm in the vicinity of
the grain boundary with increasing spacing in regions more
distant (up to 400 μm) from the boundary.
In FCC crystals, typical edge dislocation lines are parallel to
In grain A the orientation of the surface normal before
the directions of <112> with Burgers vectors being parallel to
deformation was almost parallel to [233] with loading di-
­ the directions <110> and corresponding glide planes [111]. We
rection approximately in grain [11 0] direction. In grain B the
note that bending of slip bands parallel to the boundary is
x-axis is close to the [125] direction with surface normal
­ observed in SEM image of the grain B up to a distance of
approximately in the [031 ] direction. Two main phenomena
several micrometers from the boundary.
were observed during this experiment: lattice rotation and
Finite element simulations were performed using the
plastic deformation. The change of lattice orientation as a
method developed by Ohashi [46,47]. For numerical simulations
function of the distance from the boundary is shown in
the dimension of the model was the same as for the sample used
Fig. 7 for both grains A and B. The grain A lattice orientation
in the experiment. The specimen was meshed in non-uniform
changes smoothly as the probe volume approaches the grain
manner in x and y directions which enabled sharp changes of
boundary and reaches higher misorientations than in B
the modeled quantities in the vicinity of the grain boundary and
grain. In grain B strong oscillation in the lattice orientation
specimen surface. Fig. 9a shows the shape of the simulated
are observed. The maximum rotation magnitude is double in
deformed specimen which is slightly bent and twisted. Accu-
grain A compared to grain B (Fig. 7). Plastic activity is also ­
mulation of plastic shear strains on the (111) [101] slip system is
quite different in both grains. In grain A plastic activity is low,
shown in Fig. 9b. Significant contrast is found between grains A
while in grain B zones with high plastic activity are con-
and B. No activity of this slip system is predicted in grain A. The
centrated in shear bands and separated by zones with low
grain boundary region of grain B also shows negligible activity
dislocation density. The length of the grain A remained
whereas the bulk region exhibits large plastic shear strain up to
nearly constant during pulling while grain B mainly accom-
−28%. The anisotropic deformation behavior between the two
modated the total length change of the sample.
Regions with large strain gradients and high density of geo-
metrically necessary (GN) dislocations manifest themselves by
streaking of the Laue spots as observed in a Laue pattern of
deformed grain B shown in Fig. 8. The plastic response [35,45]
of the material in both A and B grains of the bicrystal can
be described by formation of GN and SS (statistically stored)
dislocation population in the material to relax the stress field
induced during pulling.

Fig. 9 – a) The shape of the deformed sample with 10%

nominal strain. Distribution of the normal strain□xx is
Fig. 7 – Misorientations relative to the orientations of the mapped on the deformed shape of the sample; b) distribution
undeformed state for grains A and B of the Ni bicrystal after of plastic shear strain with 10% nominal strain on the (111)
16% plastic strain. [101] slip system at a depth of 0.3 mm beneath surface.
1198 M A TE RI A L S C H A RAC TE RI ZA T ION 6 0 ( 2 00 9 ) 1 1 9 1– 1 2 0 1
grains explains the shape change observed in both the simula-
tion and the experiment.
4.3. Self-assembly of Dislocation Cell Structure in
Single Crystals
Plastic deformation involves the creation and evolution of
large numbers of dislocations and the self assembly of these
dislocations into mesoscale cell structures. Studies have in-
dicated dislocation arrangements in a wide range of materials
are scale-invariant from nanometer to millimeter [48–51]. Dis-
location arrangements in the mesoscopic range have been
inferred from measurements of the spacing between slip lines
and cell walls; and from surface morphology measurements.
MicroLaue diffraction provides a powerful new tool to test
these ideas. With microLaue diffraction, mesoscale structural
evolution can be followed in-situ nondestructively and in 3D.
Consider for example a measurement of spatial correlations
between local crystallographic orientations of deformed Cu
single crystals over the length scale of a micrometer to hun-
dreds of micrometers. The orientation variation within a
deformed single crystal is introduced by non-uniform local
rotation and is related to the local shear stress fluctuation
caused by symmetry-breaking heterogeneity of the deforma-
tion process. From surface studies, a power-law dependence
in the spatial correlations of the variation of local crystal-
lographic orientations is expected.
The Hurst roughness exponent, H, for 8% tensile deformed
Cu crystals with <321>, <111> and <100> axes was measured
parallel to the tensile axis. The Hurst exponent (0 < H < 1) pro-
vides a measure of the fractal dimension of a data series,
where H = 0.5 indicates uncorrelated fluctuations, while higher
values indicate positive point to point correlations and smaller
values correspond to anti-correlated point-to-point fluctua-
tions. Fig. 10 is a color coded map of the direction of the local
<100> crystal axis with respect to the sample co-ordinates
of the measured region. The color variation here indicates
the changes in the direction of the crystal axis along both the
loading direction and depth (z). Both samples show formation
of bands with a bigger effect in the <321> sample.
The H values are plotted in Fig. 11 as a function of depth, z
for all samples. At the surface, all three samples show similar
Fig. 10 – Orientation map of crystal axis <100> for deformed Cu samples with <321> (top) and <100> (bottom) parallel to the
loading axis.
Fig. 11 – Hurst exponents for the Cu samples as a function of z.
H values as observed in surface studies. In addition, in the
<321> sample, H remains nearly constant with depth. How-
ever in the case of the <111> sample, H begins to drop at 5 μm
and continues decreasing until z reaches 10 μm. The H values
for the <100> sample drops continuously until depth increases
to 10 μm with a value of ~0.32.
The observed depth dependence of H may be explained by
the interactions of multiple slip systems in the <111> and
particularly <100> crystals. For the <321> crystal, only one slip
system is activated and rotational changes are presumably
more uniform because the activated glide planes are parallel
and do not interact. The effect of multiple slip system lockups
does not exist at the surface and hence yield a universal H
value [51]. The results show that deformation is different in
the near-surface and bulk regions. Another observation is the
length scale of the self-affined pattern, which is in the order of
20–70 μm. Dislocation patterning terminates well below the
sample length even in the case of single crystals.
These single crystal experiments have important implications
for polycrystal samples; In the case of the Ni polycrystal
experiments [42] individual grains exhibit distinct rotation
patterns and subgrain variations in the rotations as a function
of depth were found after 15% plastic deformation. Clearly in
polycrystal samples with complicated 3D grain boundary net-
works, there are important interactions between defects that
 M A TE RI A L S C H A RAC TE RI ZA T ION 6 0 ( 2 00 9 ) 1 1 9 1–1 2 0 1 1199

simply do not exist on surfaces. Modeling efforts should be

focused in 3D to capture the real bulk behavior of these materials.

4.4. Elastic Strain Example

The experimental tools developed for microLaue diffraction

can be used to extend the technique to study absolute lattice
parameters by scanning the x-ray energy near a Laue spot.
This approach provides precise information on the lattice
parameter (or elastic strain) distribution with submicron spa-
tial resolution and is particularly useful in highly deformed
samples where deviatoric information may be difficult to
measure with high precision.
Consider for example, a commercial carburization treatment
known as Kolsterising ® , which has shown promise
for hardening surfaces of the stainless steel target vessel for Fig. 12 – An indexed Laue image of the Kolsterised stainless
the Spallation Neutron Source against cavitation erosion and steel sample.
pitting caused by the action of pulsed pressure waves in the
liquid mercury target. To understand the mechanism of hard-
ening, and to uncover any factors that might be of concern
for the integrity of a Kolsterised target vessel, a series of anticipated in both the near and long term. One obvious area
characterization tests were conducted on the surface layers of for improvement is in terms of spatial resolution. Optics suit-
Kolsterised austenitic 316LN stainless steel [52]. The findings able for microLaue experiments have been demonstrated with
support most of the manufacturer's claims. The austenite lattice ~24 nm beams [54] which is an order of magnitude smaller in
is enlarged and placed in a state of compressive stress and the linear dimension and two orders of magnitude smaller in area
surface is distorted by the treatment. The Kolsterised layer is not than the most advanced existing device. Even smaller beams
brittle; it is plastically deformable and is quite resistant to are possible. Such small beams will allow for ambitious ex-
cracking during straining. The shallow depth of the hardened periments including in-situ observations of single dislocations
layer will require protection measures to avoid mishandling moving through a lattice.
damage to the layer during installation of a target vessel. Another obvious area with both near term and long term
Formation of supersaturated solid solution by carburization potential is in the use of ultra-fast and energy-resolved area
in the Kolsterised layer naturally expands the lattice and is detectors. As x-ray optics and source continue to improve, it
presumed to be due to absorption of carbon in supersaturated will be possible to generate Laue patterns in fractions of a
solid solution [53]. To explore the depth dependence of the millisecond with 100 nm beams and in milliseconds with
expanded lattice parameter of the austenite in the Kolsterised beams in the tens of nanometers. Area detectors with milli-
layer, microLaue diffraction energy scans were used. A trans- second readout will be required to efficiently utilize the x-ray
verse sample was prepared by cutting perpendicular to the beams. Already an area detector with ~ 100 millisecond read-
surface such that the interface between the Kolsterized layer out has been installed on station 34-ID-E, and a detector with
and the bulk was clearly exposed. To eliminate grain-to-grain ~1 millisecond readout has been tested on station 12.3.2. In
variation the measurements were made on a single large addition the ability to measure x-ray energy will provide for
grain that intercepted the surface. A Laue image with indexed simultaneous collection of reciprocal space volume informa-
reflections obtained by polychromatic beam is shown in Fig. 12. tion. Advanced detectors will be matched with more advanced
The unindexed Laue spots, generally with lower intensity, are differential aperture methods to further accelerate and make
contributed by the minority phases in the alloy and by grains
beneath the surface. Energy scans over a range of ±250 eV
centered at 16.85 keV were carried out to determine the cor-
responding energy for the (353) peak as a function of distance
from the surface. The results are presented in Fig. 13. They
show that the expansion of the austenite lattice parameter is
a maximum at the surface and progressively decreases with
depth, reaching the value of annealed, non-Kolsterised steel at
a depth of ~30 μm. The shape of this profile is similar to the
corresponding hardness–depth profile.

5. Future Directions

Despite major progress over the last decade, microLaue dif- Fig. 13 – Variation of the austenite lattice parameter with
fraction is rapidly evolving with significant improvements depth.
1200 M A TE RI A L S C H A RAC TE RI ZA T ION 6 0 ( 2 00 9 ) 1 1 9 1– 1 2 0 1
routine the collection of 3D submicron-resolved diffraction
information.
Beyond instrumentation, the software currently in use to
collect and analyze microLaue data is still in its infancy. As
the field grows, there is increased demand for user friendly
software and for data analysis in real time to maximize the
experimental productivity of the precious microLaue instru-
ments. International collaborations are underway to standar-
dize and accelerate approaches for reconstruction of Laue
patterns in depth, peak searching, indexing, structure deter-
mination and other critical analysis steps.
Finally, as sample features become increasingly small,
coherent effects will play an ever larger role in the observed
patterns. The use of wide-bandpass and energy-tunable beams
opens up new opportunities for studying ultra-small features
below the diffraction limit of achromatic optics. More details
about future directions in coherent scattering, small beams, fast
detectors and new software can be found in references [55] and
[56].
Acknowledgements
This research is supported by the Division of Materials Science
and Engineering, Office of Basic Energy Science, U.S. Department
of Energy. Research is in part on beamline 34-ID-E which is funded
by the Office of Basic Energy Science, U.S. Department of Energy.
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