research papers

Journal of
Applied
First laboratory X-ray diffraction contrast
Crystallography tomography for grain mapping of polycrystals
ISSN 0021-8898

A. King,a* P. Reischig,b,c J. Adrienb and W. Ludwigb,d

Received 10 April 2013
Accepted 11 August 2013 a
Synchrotron Soleil, 91192 St Aubin, France, bUniversité de Lyon, INSA-Lyon, MATEIS CNRS UMR
5510, 69621 Villeurbanne, France, cDelft University of Technology, 2600 AA Delft, The
Netherlands, and dEuropean Synchrotron Radiation Facility, 38043 Grenoble, France. Correspon-
dence e-mail: andrew.king@esrf.fr

The first results of three-dimensional grain mapping using a laboratory

# 2013 International Union of Crystallography
Printed in Singapore – all rights reserved
tomograph equipped with a microfocus W target X-ray tube source, operated
at 90 kV and 350 mA, are presented. Adapted algorithms exploit the
polychromatic radiation spectrum and the projection magnification arising
from the cone-beam geometry. The first map of grain shapes and crystal-
lographic orientations from a titanium sample containing 42 grains is presented
and its validity confirmed by a phase contrast reconstruction of the grain
boundaries. Perspectives are given for the further development of the technique
to accommodate samples with more grains or with greater intragranular
orientation spread.

1. Introduction use of synchrotron radiation, which imposes strong restrictions

The vast majority of metallic and ceramic materials are
polycrystalline, and the interaction between the crystalline
grain structure and various physical processes is increasingly
the subject of study (Bantounas et al., 2007; Herbig et al., 2011;
King et al., 2008; Krupp, 2007; Rolland du Roscoat et al., 2011;
Schaef et al., 2011). The nondestructive three-dimensional
mapping of crystallographic orientation in polycrystals is thus
increasingly important for materials science.
In recent years, several such techniques have emerged.
These include three-dimensional X-ray diffraction microscopy
(3DXRD) (Poulsen, 2004; Schmidt et al., 2008), high-energy
X-ray microscopy (Suter et al., 2006) and diffraction contrast
tomography (DCT) (Johnson et al., 2008; Ludwig et al., 2009;
Reischig et al., 2013). These techniques are characterized by
the use of extended, parallel and monochromatic synchrotron
X-ray beams. Grain shapes, positions and crystallographic
orientations are determined from the shapes, intensity distri-
butions and the positions of diffraction spots recorded on a
high-resolution two-dimensional detector placed close to the
sample.
A related family of techniques uses focused polychromatic
synchrotron radiation (Larson et al., 2002). In these methods,
Laue diffraction patterns recorded on a low-resolution
detector give grain orientations, and spatial resolution is
obtained by scanning the sample and an analyser wire with
respect to the focused beam (‘differential aperture micro-
scopy’). Initially, these techniques used X-ray energies on the
order of 15 keV in reflection geometry to investigate small
sample volumes. Recently, the concept has been adapted to
higher X-ray energies, allowing the investigation of milli-
metre-sized samples in transmission geometry (Hofmann et
al., 2012). All of these X-ray techniques have in common the
on access to instruments, meaning that only limited experi-
mental time is available to scientists.
Electron backscatter diffraction in the scanning electron
microscope allows two-dimensional crystallographic orienta-
tion mapping on surfaces, but can only be extended to three
dimensions using destructive serial sectioning techniques
(Matteson et al., 2002; Rowenhorst et al., 2006; Venables &
Harland, 1973). Recent developments have applied 3DXRD
to electron diffraction in the transmission electron micro-
scope, but this is applicable only to samples of less than one
micrometre in thickness (Lui et al., 2011).
Laboratory X-ray microtomography has become an essen-
tial tool in many materials science institutes (e.g. Limodin et
al., 2009; McDonald et al., 2009). A microfocus X-ray tube
provides a divergent polychromatic X-ray beam, contrasting
with the parallel beam typically used in synchrotron micro-
tomography. The sample is placed close to the source and a
divergent cone-beam geometry is used to project an enlarged
radiograph onto a detector placed some distance away. The
spatial resolution in the image is determined by the source
size, detector resolution, and the ratio between the source–
sample and source–detector distances. The spatial resolution
and field of view are easily adjusted by changing the sample
position. Features generating absorption contrast can be
reconstructed in three dimensions using adapted back-
projection algorithms (Feldkamp et al., 1984). However, only
in some specific cases of multiphase materials can absorption
contrast reveal grain shapes, owing to differences in chemical
composition or density, and even then the grain orientations
are not accessible.
There is thus a clear motivation for a technique that can
exploit diffraction contrast imaging using standard laboratory

1734 doi:10.1107/S0021889813022553 J. Appl. Cryst. (2013). 46, 1734–1740


X-ray sources and equipment, in order that three-dimensional
polycrystalline microstructures can be studied nondestruc-
tively without a synchrotron source. Enabling three-dimen-
sional mapping of grain shapes and orientations with widely
available laboratory equipment will allow more systematic use
of these techniques, important for developing true scientific
understanding of how polycrystals respond to loading, corro-
sion or thermomechanical processing. In this article, we
describe laboratory DCT (Lab-DCT), a new technique that is
performed using a standard laboratory tomograph, and
present the first experimental results obtained.
2. Technique
Lab-DCT is performed using standard laboratory X-ray
tomography instrumentation. A single detector is used to
collect both absorption contrast radiographs in the direct
beam and diffraction spot images. The addition of slits to
define the incident beam is the only hardware modification
necessary to a standard instrument. The projection magnifi-
cation is adjusted so that the image of the sample fills only the
central part of the detector. Fig. 1 shows a schematic diagram
of the experimental setup. As the sample is rotated through
360 around a fixed axis, grains diffract the beam on to the
outer part of the detector. The recorded diffraction spot
images are used to calculate the orientations and positions of
grains, and to reconstruct their three-dimensional shapes. The
direct-beam radiographs are used to produce an absorption
contrast reconstruction of the sample as in regular tomo-
graphy. Figs. 2(a) and 2(b) show examples of the diffraction
spots from a sample and the corresponding direct-beam image.
2.1. Data acquisition
A polychromatic X-ray spectrum from a tube source means
that diffraction events are not observed at discrete angles (2).
Instead, different beam energies are diffracted at varying
diffraction angles as the lattice planes rotate. As the sample is
Figure 1
A schematic view of the Lab-DCT setup. The technique can be
performed in using standard laboratory tomography instrumentation
with minimal modifications. Dimensions shown refer to measurements for
which results are shown.
J. Appl. Cryst. (2013). 46, 1734–1740 A. King et al.
research papers
rotated, diffraction spots precess across the detector in curved
paths. Fig. 3(a) shows the sum of diffraction spot images
recorded during a 15 sample rotation, showing the diffraction
spot paths. The Lab-DCT analysis method described here is
based on identifying these paths of diffraction spots. A
diffraction spot arising from the (hkl) planes of a grain will
appear on one side of the detector and move towards the
sample, to lower diffraction angles and correspondingly higher
beam energies. As the maximum energy in the beam spectrum
is reached, the spot gradually disappears, reappearing on the
other side of the sample after further rotation [scattering from
the ðhklÞ planes]. The spot then moves away from the sample
to higher diffraction angles and lower energies, until it
disappears from the detector. The only exceptions are those
scattering vectors that are close to parallel with the rotation
axis, which may never reach high enough diffraction angles to
exceed the edges of the detector. The spot intensity changes as
a function of angle, according to the incident-beam spectrum,
scattering efficiency, self-absorption by the sample and
Figure 2
(a) Diffraction spot contrasts after processing to remove other
contributions. (b) The simultaneously acquired direct-beam image. The
sample and the outline of the beam are marked in both (a) and (b). The
outline of the grain, which gives rise to the circled diffraction spot, is
marked in (b).
Figure 3
(a) Composite of images for 15 sample rotation, showing lines of spots.
No filtering of the direct beam is used. (b) An enlarged region of (a), with
guide lines marking the spot path and characteristic beam energies, with
(c) an Hf filter and (d) an Er filter applied. Note the increased
background noise due to an incorrect dark current correction. (e) Narrow
bandwidth image produced by dividing image (b) by (c).
 X-ray diffraction contrast tomography for grain mapping of polycrystals 1735
research papers
detector efficiency as a function of energy. The spot behaviour
is illustrated schematically in Fig. 4. Because the spots move as
the sample is rotated, images are acquired at discrete angular
steps in order that the spot images are not blurred. This is in
contrast with the monochromatic synchrotron technique, in
which continuous rotation is necessary to ensure that all parts
of a diffracting grain are observed.
It is important that the beam spectrum contains a suffi-
ciently wide range of energies that diffraction spots arising
from several families of crystal lattice planes can be observed
within the range of solid angle covered by the detector. To best
exploit the projection magnification in the conical beam, the
diffraction angles (Bragg angles, 2) should be similar to the
cone opening angle covered by the detector, favouring the use
of relatively high beam energies (Fig. 1). Because of the
projection magnification, the physical pixel size of the detector
does not limit the spatial resolution as it does in the parallel-
beam case. Using a low-spatial-resolution detector greatly
improves the detection efficiency, particularly for high X-ray
energies, and to some extent compensates for the much-
reduced flux when compared with a synchrotron source. The
technique is therefore particularly well suited to highly
attenuating materials requiring high beam energies for suffi-
cient transmission.
2.2. Data processing
The principles of the data processing are similar to those
used for standard synchrotron DCT, and the initial treatment
here of the images was performed using tools from the stan-
dard DCT processing software (Johnson et al., 2008; Ludwig et
al., 2009; Reischig et al., 2013). A constant dark current is
offset and a moving median background correction applied in
order to remove slowly changing features from the images, to
leave only diffraction spot contrasts (Fig. 2a). The diffraction
spots are segmented from the images and metadata describing
Figure 4
Determination of diffraction geometry from observed data. The spot-
intensity profile is used to determine the centre of the line. The
construction used reveals the scattering vector and a path through the
sample on which the grain must be found.
1736 A. King et al.  X-ray diffraction contrast tomography for grain mapping of polycrystals
the spots stored in a database. The direct-beam image record
is simultaneously treated as a conventional tomographic data
acquisition.
The data analysis is based on using an automatic search
algorithm to identify the paths of spots as they precess across
the detector as the sample rotates. The identification of such
lines containing several spots appears to be robust, provided
that the majority of spots are not affected by overlaps. The
geometry of the diffraction events is determined by analysing
the paths of the spots, as shown in Fig. 4. Two versions of this
analysis have been implemented using MATLAB (version
7.14.0; MathWorks Inc., Natick, MA, USA): a computationally
simple version, in which the spot paths are approximated to
straight lines, and a more advanced analysis in which the true
curved paths are fitted.
(a) Straight lines. For most lattice planes (as an indication,
those giving rise to diffracted beams with angles 2 < 15 , 20 <
 < 160 ), the lines of spots can be treated as straight lines to a
good approximation. Each line of spots, extending from one
side of the detector to the other, is fitted with a straight line in
three dimensions (x and y position in the detector plane as a
function of the sample rotation). The centre point of each line
is then identified by considering the diffraction spot inten-
sities. The centre point can be considered as the sample
rotation angle and detector position at which diffraction
would occur with an angle of 0 . A line drawn from this point
on the detector to the X-ray source must therefore pass
through the diffracting grain, as shown in Fig. 2. The
diffracting plane normal must be perpendicular to this line and
coplanar with the line of diffraction spots. The error implied
by the assumption of straight lines can be estimated by
simulating the paths of a diffraction spot across the detector
for a given experimental configuration. The difference
between the true plane normal and the plane normal calcu-
lated from a straight line fit through the simulated points gives
a measure of the error in each observation. Grain orientations
are found by a best fit to multiple observations of plane
normals, so the final error in orientation should be less than
the error in a single plane normal.
(b) Curved lines. For higher diffraction angles and for
scattering vectors that are nearly parallel to the rotation axis,
the diffraction spot paths become noticeably curved. The path
can be described by considering the direction of the scattering
vector and the position of the grain within the sample. At each
sample rotation angle, the position of the grain in the incident
cone beam defines the incident-beam direction. The directions
of the incident beam and the scattering vector determine the
direction of the diffracted beam, and the hence the diffraction
angle (2) and the wavelength diffracted from the polychro-
matic beam. The intersection of the diffracted beam with the
detector plane defines the spot position. Given a line of
diffraction spot positions, the grain position and the scattering
vector can be fitted using a suitable least-squares algorithm.
In either case, the ðhklÞ family for each reflection is iden-
tified using the profile of diffracted intensity as a function of 2
in each line. By considering the beam spectrum (in the data
presented here, this exhibited a clear maximum around the
J. Appl. Cryst. (2013). 46, 1734–1740

tungsten K lines at 58.0 and 59.3 keV), the ðhklÞ family of
each line was identified. Each line of spots therefore reveals
the orientation and the ðhklÞ type of a set of lattice planes, and
a path through the sample on which the grain must lie. This
information is equivalent to that obtained from a Friedel pair
of spots in the monochromatic and parallel-beam synchrotron
technique, and so the standard DCT grain-indexing algorithm
(Indexter) can be used to determine grain positions and
crystallographic orientations (Ludwig et al., 2009; Reischig et
al., 2013).
2.2.1. Image formation and reconstruction. The three-
dimensional shapes of the individual grains are reconstructed
from the indexed diffraction spot images. Both the direct-
beam radiograph and the diffraction spot images are enlarged
by the conical projection. The interaction of the polychromatic
cone beam with the parallel lattice planes results in diffraction
spot images which are mirrored along the scattering direction,
and magnified astigmatically, as illustrated schematically in
Fig. 5. Similarly, the outline of the grain that gives rise to the
diffraction spot circled in Fig. 2(a) is marked on Fig. 2(b). The
shapes of the grain and the spot illustrate the mirroring along
the scattering direction. The inverse transform, correcting the
inversion and astigmatism, is applied before using a cone-
beam geometry simultaneous iterative reconstruction tech-
nique (SIRT) algorithm to reconstruct the three-dimensional
grain shapes (Palenstijn et al., 2013). The individual grain
reconstructions are assembled to produce a full three-dimen-
sional map. Postprocessing morphological dilation is used to
fill any unassigned voxels in the grain map (Johnson et al.,
2008). A similar cone-beam (SIRT) algorithm is used to
reconstruct the absorption contrast volume of the sample from
the direct-beam radiographs.
3. Results
3.1. Sample
The sample used for this first proof of concept measurement
was a ‘dog bone’-shaped tensile test sample with a 0.4 mm
gauge diameter. The material used was the metastable
research papers
microfocus X-ray generator with a tungsten transmission
anode and an accelerating voltage of 90 kV and a current of
350 mA. The effective source size under these conditions has
been measured as 3–4 mm. The detector is a PaxScan 2520 V
from Varian Medical Systems, which uses a CsI scintillator and
amorphous silicon architecture. It has a physical pixel size of
0.127 mm and a field of view of 1920  1536 pixels and was
located 577 mm from the source. The sample was placed
23 mm from the source, giving an effective pixel size of 5 mm.
Images were binned 2  2 to increase sensitivity, doubling the
effective pixel size to 10 mm. A set of manual slits was placed
between the source and sample to define the size of the direct
beam. The conical beam geometry implies that the slit opening
was about 350 mm in order to obtain a beam size of about
700 mm at the sample position. These dimensions used for this
particular sample are indicated in Fig. 1.
In all, 720 radiographs were recorded covering 360 in steps
of 0.5 . The exposure time for each image was 10 s, giving a
total acquisition time of around 2 h. Images were processed as
described in x2, and 17 919 diffraction spots were segmented
from the images. Lines of spots were identified automatically
and fitted using straight lines. Taking the example of a plane
normal inclined at 45 to the rotation axis, the error involved
in assuming straight lines for this experimental configuration
was estimated to be less than 0.5 . A total of 538 lines of
diffraction spots were used to produce geometrical informa-
tion for the grain-indexing step. Spot images were treated as
described in x2 and used as projections to reconstruct the grain
shapes.
3.3. Reconstruction
Fig. 6 shows the grain map reconstructed using Lab-DCT.
Grains have been coloured according to their orientation,
expressed as Rodrigues’ vectors and mapped into a red–
green–blue colour space. The map consists of 42 grains with an
average diameter of 170 mm. The same volume of the sample
-titanium alloy Ti21S (Dey et al., 2007). Previous DCT
investigations using the same material have shown that it has
low mosaicity, with an intragranular orientation spread of
0.05–0.15 per grain. A heat treatment of 24 h at 1063 K was
used to precipitate a layer of -titanium on the grain bound-
aries. The  and  phases have sufficiently different densities
that they can be distinguished using phase contrast tomo-
graphy (PCT), allowing the grain shapes (although not their
crystallographic orientations) to be reconstructed using
established techniques (Cloetens et al., 1997). In this way, the
accuracy of the Lab-DCT grain reconstruction can be vali-
dated, using the method described by Ludwig et al. (2009).
This approach has the advantage of being nondestructive and
of providing the complete three-dimensional grain shapes for
verification.
Figure 5
3.2. Method Diffraction spot image formation in polychromatic, cone-beam geometry
creates projections that are astigmatically magnified and inverted along
Measurements were performed using a Phoenix X-ray the scattering direction. The letter ‘G’ is chosen as a suitably
v|tome|x laboratory tomograph at INSA de Lyon, using a asymmetrical shape for illustration.

J. Appl. Cryst. (2013). 46, 1734–1740 A. King et al.  X-ray diffraction contrast tomography for grain mapping of polycrystals 1737
research papers
was imaged using synchrotron PCT measurements at beam-
lines ID11 and ID19 of the ESRF. These volumes were
rescaled and aligned to the Lab-DCT grain map. Sections
through the grain map and the PCT reconstruction are shown.
It can be seen that all large grains are reconstructed and that
the reconstructed grain shapes are realistic. Marked in the
images is a grain boundary that was not decorated by the
-titanium phase. Inspection of the Lab-DCT grain map shows
that this is a low-angle grain boundary (6.8 intergranular
misorientation; note the similar colours of the two grains). The
main sources of error in the reconstruction appear to arise
from small partial grains at the surface of the sample that have
been subdivided when the sample was cut from a larger piece
of material.
4. Discussion
The method presented here has been demonstrated using a
sample with low mosaicity and relatively large grains. It is
useful to discuss several factors that relate to the application
of the technique to more general materials for scientific
applications and to the use of polychromatic laboratory
sources for this type of measurement.
4.1. Application
To be a useful scientific tool, Lab-DCT should be capable of
mapping of the order of one thousand grains in a sample. This
should be easily achieved, as the 42-grain sample mapped here
was far from the condition where diffraction spot overlap
would become limiting. Thus, several hundred grains in a scan
should be possible, and one thousand grains can be mapped by
scanning several adjacent volumes. It should be noted that
relatively few images are required compared with the
synchrotron technique (5–10 times fewer) and hence it is
Figure 6
The reconstructed grain map, compared with the PCT reconstruction showing the grain boundaries that was used for validation purposes. In the DCT
reconstruction colour represents crystallographic orientation.
1738 A. King et al.  X-ray diffraction contrast tomography for grain mapping of polycrystals
reasonable to split the acquisition over several scans. Under
these conditions, the scattering power of a grain is propor-
tional to the grain volume. Therefore, smaller-grained samples
will require longer exposure times or more intense sources. If
the sample size can be reduced as well as the grain size, the
sample can be positioned closer to the X-ray source, providing
greater flux density and stronger magnification. In this case,
exposure time would be expected to scale as the inverse of the
grain diameter.
4.2. New laboratory sources
Currently, the acquisition time for a data set is limited by
the integration time required to form usable diffraction spot
images given the available X-ray flux. In future, developments
of liquid jet anode laboratory sources may provide this
increase (Hemberg et al., 2003). Current designs offer an order
of magnitude increase in flux compared with equivalent solid
anode sources, but have not yet been optimized for the very
small source sizes required for cone-beam projection micro-
scopy [Excillum JXS-D1 Metal Jet Source Data Sheet 2011-10-
10 (downloaded 23 July 2013); http://www.excillum.com/
images/pdf/JXS-D1_2011-10-10.pdf].
4.3. Effects of polychromaticity
The polychromaticity of the beam limits the described
approach to samples exhibiting small lattice deformations, as
these lead to an irregular distortion of the diffraction spots.
Nevertheless, if the lattice deformations are small enough, the
advantages of using a polychromatic instead of a monochro-
matic beam are twofold. Firstly, spots from a given lattice
plane and grain precess across the detector, diffracting
different X-ray energies at each rotational angle of the sample.
This increases the number of available projection images per
grain, which improves the orientation and shape reconstruc-
J. Appl. Cryst. (2013). 46, 1734–1740

tion accuracy. Secondly, diffraction occurs simultaneously
from the entire grain volume, even though the incident angle
varies across the grain in the conical beam. In the case of a
monochromatic conical beam, only partial grain volumes
would be visible at any given rotation angle. As mentioned
previously, to obtain sharp diffraction spot images stepwise
rotation is used as opposed to continuous rotation with a
monochromatic beam.
The current grain-reconstruction algorithms are based on
backprojection and assume no mosaic spread within grains. In
the example given, a grain has an angular size seen from the
source of about 0.5 (170 mm grains, 23 mm from the source).
For the diffraction spots to be reasonable projections, the
intragranular orientation spread should be much less than this,
i.e. 0.1 per grain. This limits the technique to materials with
very low mosaicity. This argument does imply that the
problems of mosaicity can be mitigated by moving the sample
closer to the source, increasing the angular extent per grain,
until the overlap between spot images on the detector
becomes a limitation.
To achieve better reconstructions, it will be necessary to
incorporate subgrain misorientation into the reconstruction
algorithms as discussed by Schmidt et al. (2008) and Suter et al.
(2006). Grain volumes and centres of mass can, nevertheless,
still be obtained from less perfect samples. The data processing
route presented is also applicable to data acquired using other
polychromatic radiation sources, including cold or thermal
neutrons and polychromatic or broadband monochromatic
synchrotron beams.
4.4. Filtering to reduce bandwidth
An alternative route for the control of excessive mosaicity,
or to allow greater numbers of grains to be treated in a single
scan by reducing spot overlap, is to use filtering to create a
pseudo-monochromatic data acquisition at the energy of the
tungsten K lines. This technique was described by Webster et
al. (1986) for coherent and Compton scattering experiments.
Filters are chosen with absorption edges just above and below
the K line energy. Ideally, erbium and ytterbium would be
used. For trial purposes erbium (Er K edge 57.5 keV) and
hafnium (Hf K edge 65.4 keV), both 0.25 mm thick, were used.
The filters have essentially the same attenuation effect, except
in the immediate vicinity of the absorption edge. Therefore,
when an image acquired using one filter is divided by an image
acquired using the other filter, all contributions are removed
with the exception of those arising from energies between the
two absorption edges, a window of about 4 keV if Yb and Er
are used (i.e.
E/E = 7%). Thus most spot overlaps can be
removed. Fig. 3(b)–3(e) show trial data illustrating this
process. In the images shown, an error in the calibration of the
dark current has produced increased background noise in one
of the acquisitions, reducing the final image quality. Note this
approach has the drawback that two consecutive scans must be
performed and that the filters reduce the incident flux, and
therefore must be expected to cost a factor of four in acqui-
sition time. In the case of spot overlap due to a large number
J. Appl. Cryst. (2013). 46, 1734–1740 A. King et al.  X-ray diffraction contrast tomography for grain mapping of polycrystals
research papers
of grains, it might be more effective to reduce the vertical
beam height and hence the volume of material sampled.
However, a sample with a large number of grains in a cross
section might require this approach.
5. Conclusions
Lab-DCT is a new technique enabling the reconstruction of
the grain structure of polycrystals using standard laboratory
tomography instrumentation with minimal modifications. The
technique and the data processing route are described. The
algorithms described are also applicable to other experiments
using polychromatic radiation, including neutron and
synchrotron X-ray sources, and future laboratory X-ray
sources. The first grain map derived from experimental data is
presented. The validity of the reconstructed grain shapes has
been confirmed by imaging the same region of the sample
using synchrotron PCT to image a second crystallographic
phase precipitated on the grain boundaries. It is hoped that by
allowing grain mapping experiments to be performed using
laboratory equipment, the new technique will enable
researchers to make more compete studies of the influence of
crystallographic microstructure on material behaviour and
properties.
James Marrow, Oxford University, is acknowledged for
suggesting a laboratory-based DCT technique in 2007, prior to
the developments shown here. The majority of this work was
carried out while AK was employed at the ESRF, Grenoble.
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