Strains, planes, and EBSD

in materials science
Electron back scatter diffraction (EBSD) has made an impressive impact
on the characterization of materials by directly linking microstructure and
crystallographic texture to provide very rich and quantitative datasets which
in many instances have forced us to rethink how microstructure should be
defined and analyzed. In this article we try to first give a very basic idea of
how an EBSD map is obtained and what the data produced is like. We then
give a brief history detailing some of the more major steps in developing the
technique to what it is today. Finally, we explore two advanced and exciting
technique areas of strain mapping and 3D microscopy and demonstrate
how the EBSD technique continues to evolve to tackle new applications and
bolster our materials characterization toolbox.
Angus J. Wilkinson* and T. Ben. Britton
Department of Materials, University of Oxford, Parks Road, Oxford, OX1 3PH, UK
*E-mail: angus.wilkinson@materials.ox.ac.uk

Electron backscatter diffraction (EBSD) allows crystallographic
information to be obtained from small volumes of material in a
scanning electron microscope (SEM) which provides versatility in
mapping orientation, crystal type, and perfection over a wide range
of step sizes making it a powerful microstructural characterization
tool. EBSD maps are formed by moving a focused probe of electrons
point by point across a grid of positions on the surface of a bulk
sample in a scanning electron microscope. At each point, some of
the electrons backscattered from the sample are collected by a
detector comprising a scintillator screen coupled generally by a
lens, but sometimes by a fiber optic bundle, to a photon sensitive
imaging detector, typically a charge coupled device (CCD) camera,
to form an electron backscatter diffraction pattern. The scintillator
is generally 30 to 40 mm in size and held close enough to the sample
so as to subtend a relatively large angle (60 to 70). The sample
is generally highly tilted (60 to 80) toward the detector, as is
depicted schematically in Fig. 1, to increase the quality of the pattern
obtained. Each pattern consists of many bands of raised intensity
that span across the screen. The bands, termed Kikuchi bands, appear
at first glance to have parallel straight edges but in fact the edges are
slightly curved and are the hyperbola formed by the intersection of
Kossel diffraction cones with the plane of the detector. An example
pattern from a CCD based detector is shown and compared to
examples from earlier technologies and simulations in Fig. 2. Most
importantly the centers of the bands are straight lines and mark
the projections onto the detector screen from the point-like volume
illuminated by the incident electron beam of the diffracting planes
within the crystal.
Patterns are transferred from camera to the computer for indexing
and determination of crystal orientation, as detailed in Fig. 3. Briefly, the

3 66 SEPTEMBER 2012 | VOLUME 15 | NUMBER 9 ISSN:1369 7021 Elsevier Ltd 2012. Open access under CC BY-NC-ND license.
 Strains, planes, and EBSD in materials science
Fig. 1 Schematic diagram showing the experimental set-up for EBSD observations.
Hough transform algorithm is used to convert the nearly straight bands
from lines to points which can be more easily located. With knowledge
of the experimental geometry, the peak locations can be converted to a
table of interplanar angles and compared with look up tables of expected
angles for the phases present within the sample.
With modern systems, pattern capture and indexing can be performed
very rapidly (many 100s of patterns per second) and when combined
with precise scanning of the electron beam, a detailed mapping of the
sample crystallography (crystal type, crystal orientation, pattern quality
etc.) can be obtained. These maps provide rich measurements of the
sample microstructure.
Fig. 4 outlines the major stages in the process of characterizing a
sample using EBSD. No technique provides suitable information without
adequate specimen preparation. For EBSD, standard metallographic
processes of sectioning, grinding and polishing are the starting point but
additional care must be taken to ensure that the final polishing steps
leave the sample surface free of any sectioning damage, as the EBSD
pattern is generated from a very thin surface layer (~40 nm) of material.
Polishing with colloidal silica, chemical etching, electro-polishing, ion
milling, and plasma etching are all methods that have been shown
to work in various material systems 1-3. If the sample is etched an
assessment of microstructure uniformity using an optical microscope
is often time well spent. Once the sample is in the SEM chamber, it is
sensible to have a quick manual interactive point and click survey of the
sample to assess the quality of patterns being obtained, as at this point
if the patterns are of poor quality, the preparation steps may need to be
revisited. Secondary and/or back scattered electron imaging can be used
to guide selection of the initial area and step size to use. Furthermore, if
the measured crystal orientations need to be related to some external
macroscopic direction (e.g., extrusion direction, rolling direction, growth
direction) then care needs to be taken to align the sample correctly with
REVIEW
the axes of the microscope and EBSD detector. This may seem obvious
but it is sometimes overlooked or rather poorly performed in the rush to
get on to rather more interesting parts of the operation.
In practice, there is no one way of correctly setting up an EBSD scan
as the parameters used depend on many competing factors including the
nature of the sample and the information that is required. For instance, if
the main aim is to measure the overall crystal texture with little regard
for the grain size and morphology, then it is sensible to use a relatively
coarse step size so as to quickly asses many grains within the sample. In
other situations such as an analysis of the path taken by a fatigue crack
and assessing damage in the surrounding lattice, then it would be sensible
to choose a smaller step size and a slower and more accurate use of the
pattern capture and peak detection algorithms (i.e., increased resolution
in the Hough transform and longer exposure times) to realize an increase
sensitivity in the measurement of intragranular misorientation.
For samples which are entirely unknown at the outset, it is generally
useful to run a rather quick map with widely spaced measurement
points, or a line scan, to get an estimate of the grain size and to visualize
the microstructure morphology before deciding on settings for more
detailed work.
For all these applications, assessment of how representative a
given dataset might be should be made. For example if the grain size
distribution is known to be unimodal and the average grain size is the only
requirement then we agree with Humphreys4 and Randles5 guidance
that a minimum of 200 grains should be sampled, with at least ~10
points across a grain, i.e., 100 points per grain so that a relatively modest
map of 20 000 points results, with the step size set at approximately
a tenth of a first guess at the grain size. If the grain size distribution is
required, rather than just the average, then a similar but slightly more
elaborate assessment of the size of the required dataset can and should
be made. Similar assessment of the size of datasets required to establish
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 REVIEW Strains, planes, and EBSD in materials science
(d)
(a) (b)
(c) (e)
Fig. 2 Electron backscatter patterns: (a) High angle diffraction pattern from lead
sulphide captured by Alam et al.6 on film, (b) picture of monitor showing pattern
obtained using SIT camera with BBC micro-computer graphics overlay indicating
indexing15, (c) EBSD obtained using a current day CCD-based EBSD detector, (d)
kinematic and (e) dynamical simulations of EBSD patterns from Si101.
sub-grain size, texture, phase fractions in multiphase materials can also
guide quantitative measurement of microstructure with EBSD5, just as it
does with other techniques.
An example of the information available from an EBSD dataset is
shown in Fig. 5, in this case from a Ti-15wt%Mo alloy. The first map
(Fig. 5a) distinguishes regions of the high temperature retained bcc
phase in blue, from the low temperature hcp phase in red. We find that
~20 % of the phase has transformed to . Some information concerning
the crystal orientations is revealed in Fig. 5b in which the color of every
point depends on the crystal pole along the surface normal direction,
through the color-key provided for each phase. This makes it clear that
there are several grains within the field of view and within a particular
grain there are one or more colonies of lathes with similar orientations.
Here mapping of the orientation data makes it clear that changes in
lathe crystallography are linked to changes in the alignment of the
long axis of the lathe (noting that we are looking at a 2D cross section
from a 3D microstructure). We can also see that phase has formed on
many of the grain boundaries. Looking in more detail at the crystal
orientations of the in relation to the parent grains we can see that the
Burgers orientation relationship is obeyed:
This type of information can be obtained very quickly using EBSD and
commercial EBSD software packages provide many of the analysis tools
that are required. Repeating this process for a larger area with a finer step
size could be used to examine quantitative metrics such as sample macro
368 SEPTEMBER 2012 | VOLUME 15 | NUMBER 9
and micro texture (separating alpha and beta phases automatically), beta
grain size, lath morphology and intergranular misorientations. Two very
useful reviews of strategies for EBSD analysis and quantitative analysis of
microstructure have been given by Randle5 and Humphreys4 respectively.
A brief history of EBSD
In 1954 Alam, Pashley and Nicholson6 recorded onto EM film patterns
which we now call EBSD patterns (see Fig. 2a) and observed that the
pattern contrast was greatest when the sample was inclined so that
the beam was incident within ~20 30 of the surface plane. They also
noted that the part of the pattern at low take-off angles gave the highest
contrast which was at best 15 %. Todays EBSD experiments adopt
geometries that are in accord with these earliest observations with 20
between the sample surface and incident beam routinely used.
In the 1970s Venables and co-workers7-9 implemented the technique
on a VG STEM operated in conditions more usual for an SEM and recording
patterns on film either directly exposed to electrons within the chamber
or using an externally mounted film camera coupled to a scintillator
screen within the microscope chamber. Significantly they showed how
the patterns could be used to measure the orientations of micro-crystals
selected with the scanned beam in the SEM and gave a detailed error
analysis estimating the orientation accuracy to be 0.5 to 1 very similar
to todays measurements8.
Dingley who had been working on micro-Kossel diffraction10-12 picked
up the EBSD technique and pushed it forward by using a low light level
ISIT camera to view the scintillator and overlaying the video output from
this with graphics from a BBC micro-computer allowing a significant
increase in the rate of pattern indexing and orientation measurements13-15.
An example pattern from this type of set up is shown in Fig. 2b. This is one
of the very earliest attempts at integrating capture of video information
at a microscope to enable quantitative on-line analysis. Pattern indexing
methods were improved so that minimal user input of only 3 zone axes
positions were required to index and calculate orientations for patterns
from cubic crystals14, non-cubic crystals16 and full automation of the
analysis set as a clear goal very early on. The main materials science
challenge EBSD was aimed at in these early days was in grain boundary
characterization, a theme that continues to this day, and in particular
identifying any significant special properties associated with low CSL
boundaries, e.g.17-19. Other topics that were explored were possibilities for
phase identification including combining EBSD with local chemistry from
EDX20. A further notable study by Baba-Kishi and Dingley21-23 attempted
to distinguish between different space and point groups from symmetry
elements and systematic reflections in EBSD, again a topic that has
been returned to more recently with much greater image analysis and
computing power available now24.
The next big advance in the method came with automation of the
band detection step which finally allowed the whole process of pattern
collection and indexing to be undertaken without user intervention.
By adding in computer control of the SEM beam position it was then
a relatively simple task to implement EBSD orientation mapping. The
Yale group of Adams, Wright, and Dingley (on sabbatical from Bristol)25,26
first implemented a Burns algorithm for band detection but moved to
the modified Hough transform which the Ris group (Krieger Lassen, Juul
 Strains, planes, and EBSD in materials science REVIEW

Fig. 3 Overview of EBSD indexing procedure showing pattern capture through to determination of crystal orientation.

Jensen and Conradsen) had shown to be successful27-29. Both groups had
successfully implemented automated EBSD mapping by the early 1990s.
Goehner and Micheal30 showed that phase discrimination is possible
by comparing measured interplanar angles to those expected from the
known crystallography for each of a wide range of possible phases held in
a database. The problem to be overcome here is in reducing the number
of possible phases to a manageable level either through knowledge of
local chemistry or by the primitive lattice volume.
Application areas
EBSD has now been used for many aspects of materials characterization
including characterization of grain boundary types, establishing epitaxial
relationships between layers on substrates in metal, semiconductor
and superconductor systems, characterizing texture and its changes
during deformation and annealing in metal alloys and geological
samples, establishing links between grain size and texture components
during deformation and annealing, contributing to determination of
grain boundary energy through thermal grooving, and ex situ and in
situ experiments on grain boundary mobility. Although long, this list
is not exhaustive and so we have decided to explore in detail only the
following two aspects of strain measurement and three dimensional
characterization. We have selected these aspects as we feel they are
currently undergoing considerable development (and of course are of
significant interest to the authors).

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 REVIEW Strains, planes, and EBSD in materials science
Strain measurement
Early work with EBSD concentrated on annealed structures however
there has always been interest in applying EBSD to deformation studies.
Initial attempts followed earlier work with ECP patterns, e.g.31-34 in
using the blurring of the EBSD patterns to assess the level of cold work.
These methods are not as well established as for peak broadening of
XRD and/or neutron diffraction and results have not be quantified in
terms of dislocation densities but instead calibration samples are used
to read across pattern blurring parameters to equivalent plastic strains.
Applications were to superalloys in creep35, Al36 and Al-SiC MMCs37, 38,
and distinguishing between deformed and recrystallized grains29. Since
automated EBSD mapping has been available pattern quality has not
been used so much for deformation studies in any quantitative sense.
Instead plastic deformation studies have concentrated on use of
intragranular misorientations which result from the residual dislocations
accumulated during plastic straining. Various empirical metrics have
been suggested and again in some cases calibration samples have been
used to read across from these parameters to equivalent plastic strain.
Methods exist to estimate a lower bound on the dislocation density either
by a physically motivated minimization of dislocation line energy or a
computationally convenient minimization of the square of the densities
of the different dislocation types39,40. Being physically based this approach
is also being used by the X-ray synchrotron41,42 and extensively within the
micromechanical modeling43-45 communities. Grand challenges within the
materials science and engineering communities will benefit from the use of
a common physically based framework such as the Nye tensor to compare
and combine results across these differing and complementary techniques.
Accurate analysis of elastic strain, or lattice parameters, from
measurement of Kikuchi band edge positions though Braggs law has
largely proved unsuccessful, despite some success with ECP46, primarily
because Kikuchi lines of sufficiently high order are not present47,48. Goehner
and Micheal49 have explored the use of HOLZ rings for lattice parameter
determination but found limited sensitivity for strain measurement
and these rings are quickly removed by plastic deformation and so the
method would not be very general.
The most successful form of elastic strain measurement to date has
been performed by measuring changes in interplanar angles and therefore
determination of the deviatoric components of the elastic strain tensor.
This can be performed using cross-correlation functions to determine
small shifts in the patterns compared to a reference pattern obtained
from the crystal in a known strain state. The approach can be found in the
early work of Troost et al.50 and Wilkinson48,51,52. The method was improved
notably by Wilkinson Meaden and Dingley53-56 with the geometry altered
from an initial cumbersome long camera length-low capture angle set-
up to the more conventional large capture angle set-up while retaining
a sensitivity of ~10-4. Several other groups have now implemented this
method or modifications of it57-61 or are using a commercial version62-66 *.
In this approach one pattern is used as a reference and small shifts
are measured for a number of regions of interest (ROI) dispersed across
the wide capture angle of the EBSD pattern. In common with various
other image analysis applications the shifts are determined automatically
using cross-correlation analysis and sensitivities of a few hundredths of
a pixel can be obtained, although this depends on the pattern quality.
370 SEPTEMBER 2012 | VOLUME 15 | NUMBER 9
These pattern shift and their systematic variation across the screen can
be related back to the magnitude and nature of lattice strain variation
and lattice rotation relative to the reference pattern51-55,60,67-69. The strain
sensitivity of ~10-4 can be thought of as measurement of shifts to a few
hundredths of a pixel compared to sample to screen distances of a few
hundred pixels. Two of the most recent improvements in the method
have been firstly to increase the number of ROIs used in the analysis and
move to an robust iterative fitting analysis to reduce the effects of outlier
shift measurements on the resulting strain and rotation analysis67, and
secondly to use a remapping of the test pattern to remove the larger
lattice rotations which cause errors in the smaller elastic strains68,69.
The most significant remaining challenge for strain mapping is the
so-called reference pattern problem. In many circumstances there is a
location on the sample from which a strain free reference pattern can be
obtained with the crystal in the required orientation (e.g., far field from
the deformed area of interest). However there are many more where this
is not the case and so the measured strains represent variations from
an unknown strain state at the position at which the reference pattern
was obtained. One route to overcoming this is to use simulated patterns
for the reference as suggested by Kacher et al.57, although many of the
specifics in the approach used by Kacher et al. have been criticized mainly
due to the lack of fidelity in the simple simulations used and the lack of
certainty over the detector geometry and aberrations70, 71.
An alternative to cross-correlation analysis, that does not rely on a
reference pattern, has been suggested by Maurice and Fortunier72 who
use the 3D-Hough transform as a means of increasing the precision of
band center positions, and thus interplanar angles, compared to the
standard Hough transform. Assessment of simulated patterns suggested
a sensitivity of 2 10-4, but factors such as noise and asymmetry of
the Kikuchi band profiles are likely to significantly increase errors for
measurements on real patterns which have yet to be reported.
Applications of the cross-correlation analysis have been to both
functional and structural materials. Early measurements were reported
for SiGe alloys grown as unrelaxed blanket films on Si substrates in plan
view48, 51, 52 and in cross-section54, 55. Work on SiGe/Si systems patterned
with mesas has provided good agreement between EBSD measurements
and elasticity theory60, 73, 74. Further validation of the EBSD method has
been provided by the group at NIST who have compared EBSD results with
micro-Raman65 and AFM66 measurements near wedge indents in Si. They
assessed the stress sensitivity of the EBSD measurements to be ~10 MPa.
Good agreement between EBSD and micro-Raman has also been given
by Tomita et al.64 for strained Si on insulator and SiN/Si systems. Ishido
et al.62 have examined cross-sections of GaN structures including a 5 nm
AlN/25 nm GaN multilayer for which they give a line scan within which
the 50 repeats of the multilayer can be distinguished indicating that good
spatial resolution can be achieved. Speller et al.75 have recently widened
the scope of cross-correlation EBSD studies by using it to map changes in
c/a ratio with chemistry obtained from EDX in the iron containing FeySe1-
x
Tex superconductor. Applications to structural metallics began with single
crystals including fatigue crack tips in superalloys54, and tensile cracks in
tungsten76 or single grains of polycrystals including mapping strains and
dislocation densities near indents in Fe40 and Ti45, phase transformation
induced strains in martensitic steels58,77 and thermally and mechanically
 Strains, planes, and EBSD in materials science
Fig. 4 Flow chart indicating significant steps in a typical EBSD observation.
induced strain localization near hard inclusions in a superalloy78,79. The
method has also been applied to polycrystalline Ti-6Al-4V deformed in
uniaxial tension at room temperature80 and by hot rolling81 in studies
aimed at determining dislocation densities using the Nye tensor. Ojima
et al.63 have recently reported the first in situ deformation of a polycrystal
coupled with the cross-correlation EBSD method which successfully
demonstrates that grains with <100> along the tensile axis tend to
continue increasing in elastic strain beyond the applied stress level at
which <110> aligned grains tend to show a saturated elastic strain. These
generalities are in agreement with volume averaged behavior seen for the
same alloy using neutron diffraction, but the EBSD shows significant grain
to grain variation which presumably depends on the local neighborhood.
To illustrate the data available from the cross-correlation based analysis
we will examine the elastic strains and rotations measured near a Vickers
hardness indent in (001) Si. Fig. 6 (upper left) shows the misorientations
REVIEW
near the indent measured by conventional Hough transform analysis
along with a wireframe showing the crystal orientation. The indent was
made with a load of 50 gF, which was large enough to generate radial
cracks which radiate out from the center along the indent diagonals
which are aligned with the [110] and [1-10] direction corresponding to
horizontal x1 and vertical x2 axes. EBSD measurements were made on a
JEOL JSM 6500F FEG-SEM at a beam energy of 15 keV, a beam current of
~16 nA and a sample tilt of 70. EBSD patterns were recorded at the full
~1k 1k pixel 12 bit deep resolution of the peltier cooled CCD camera
and saved to hard disk for batch-wise off-line analysis using CrossCourt3
software. The data acquisition rate was approximately 1 pattern/sec with
the camera gain kept low so as to achieve good signal to noise and the
50 50 m area was mapped at a step size of 1 m in approximately
half an hour.
Two data quality parameters are used to assess the dataset (lower left
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 REVIEW Strains, planes, and EBSD in materials science

(a)

(b)

Fig. 5 Example EBSD data obtained from Ti-15%Mo. Inserts show raw diffraction patterns which are successfully indexed to determine crystal orientation and phase (a).
The resultant data set can be separated into maps showing alpha and beta phase orientations (b) shown here with respect to the sample normal. In this alloy, the Burgers
orientation relationship is seen easily, as shown for the colony/parent beta grain insert, which relates the basal plane (0001) and an <11-20> type lattice direction in the
hexagonal phase, with a {110} plane and a <111> type lattice direction in the beta phase.

of Fig. 6). The geometric mean of the normalized cross-correlation peak
heights shows low values for regions within the indent due to shadowing
effects from the topography of the sample and pattern blurring from the
extensive deformation. The mean angular error describes the difference
between measured pattern shifts and back calculations of pattern shifts
based upon the best fit solution for the strain and rotation tensor. There is
generally strong correlation between regions with low cross-correlation
peak height and large mean angular errors. Thresholds can be used to
remove the poorer quality data from subsequent analysis. In this instance
patterns generating a cross-correlation peak height of less than 0.3 or a
mean angular error of greater than 10-3 rads were removed from other
maps. All components of the strain and lattice rotations are determined,
and these are shown in pictorial tensor layout in Fig. 6. The lower parts
of the tensors are not shown as the strain tensor is symmetric (i.e.,
Ij
= ji mirror across lead diagonal) and the rotation tensor is antisymmetric
(i.e., ij= - ji mirror across lead diagonal and swap sign).
The 11 strain along the horizontal axis is seen to be compressive above
and below the indent and tensile to the left and right with the magnitude
of the strains falling significantly with distance from the center of the
indent. For the 22 strain this is swapped so that the compressive regions
are to the left and right while the tensile strains occur above and below
the indent. This is in accord with expected compressive radial and tensile
hoop strains that should develop. The in plane 12 shear strains are also
consistent with this and show clear positive and negative lobes at 45
to the horizontal. The lattice rotation 23 about the horizontal axis shows
positive and negative rotations above and below the indent that result
from the uplift of material surrounding the indent, to account for the
materials volume displaced from the indent impression itself. A similar
effect is seen for the 31 rotation about the vertical x2 axis. Abrupt changes
in lattice rotation are accommodated by opening displacements caused
by the radial cracks; this is most clearly demonstrated in 12 rotations
(about the surface normal) which are generally of smaller magnitude.
This is expected for mode I cracks loaded in tension and has also been
seen for cracks in single crystal tungsten76. This relatively simple test case
gives an indication of the completeness of the quantitative data available
from EBSD strain mapping.
3D microscopy
The development of automated data collection in three dimensions using
EBSD has opened up an exciting field of materials characterization. Two

372 SEPTEMBER 2012 | VOLUME 15 | NUMBER 9

 Strains, planes, and EBSD in materials science REVIEW

(a)

(b)

(c)

Fig. 6 Information obtained from a high angular resolution EBSD map of a 50gF micro hardness indent in single crystal silicon. Upper left shows the crystal misorientations
with an overlay indicating the how the crystal is oriented. Lower left gives the two data quality parameters: mean angular error (lower is better) and cross-correlation
peak height (normalized to between 0 and 1 with 1 best). To the right are shown the elastic strain (top) and lattice rotation (bottom) tensors. These are displayed as
pictorial tensors with a map shown for each non-zero component in the upper part of the tensor with the symmetry operator needed to populate the lower part also
indicated.

dimensional information obtained from surface sections of materials,
can be descriptive for an elegantly designed experiment. However,
in many cases additional information regarding the structure and
connectivity of microstructural units in the third dimension would add
significant value by reducing our reliance upon assumptions required
to extend our observations to describe microstructures completely.
Data obtained with 3D EBSD can be used to populate models with
realistic microstructural information, for example with finite element
or fast Fourier transform based crystal plasticity modeling82-84.
For these data sets, the advantage of EBSD over other methods of
observation (e.g., optical or secondary electron image acquisition) is
that crystalline materials can easily be segmented and characterized
using orientation information. In many cases this provides greater
contrast than simply relying on electron (or ion beam) channeling
contrast or the use of etchants to reveal microstructural features. In
addition, orientation information combined with simple rules regarding
microstructural connectivity can be utilized to improve the fidelity of
the 3D reconstruction. Furthermore, the EBSD analysis can easily be
extended using energy dispersive spectroscopy85.
Production and successful exploitation of 3D EBSD involves three
major steps: data acquisition; model generation; and quantitative
analysis.
Data acquisition is performed by successively removing layers from
a block of material and observation of the newly revealed surface. Any
preparation route that produces a surface suitable for the successful
generation of high quality diffraction patterns can be used. Mechanical
polishing and focused ion beam machining are the two leading
routes.
Mechanical routes utilize readily available equipment but require
many man hours to observe multiple slices. Material removal rates are
high, which limits the minimum slice thickness (>1 m) but potentially
allows sampling of large volumes of material. In addition, precise
calibration of the thickness of the layer removed is difficult and can
introduce uncertainty into the data reconstruction step. Time can be
saved if orientation information is not required for every slice, instead
recording optical micrographs of an etched surface for every slice and
orientation maps for every nth slice can be used86. Uchic and co-workers
are currently developing a system which integrates mechanical
polishing, SEM operation and EBSD acquisition with robotic interchange
to aid automation87. Such a system should make data acquisition using

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 REVIEW Strains, planes, and EBSD in materials science
mechanical routes significantly less demanding and greatly increase
the quality and size of the available 3D datasets.
In contrast, dual beam SEM-focused ion beam (FIB) instruments
are expensive but recent developments in automation and instrument
stability have made data acquisition much simpler. Data is acquired
by moving the sample into a position suitable for EBSD observation,
scanning the top surface, moving the sample into a position suitable
for milling and removing a thin layer. This is repeated for as many slices
as the user requires (or time allows). Slices as thin as ~50 nm can be
successively removed, making the analysis of submicron grain sizes
possible88.
However, the sampling volume attainable by this route is significantly
smaller due to limited material removal rates. Furthermore, as the EBSD
camera capture angle is relatively large, the volume of material that
must be removed for each slice typically must be larger than the area
scanned (or else edges of the pattern can become shadowed). A specimen
geometry used is a mechanically polished sharp right angle. This can be
used either to cross section a bulk material or removal of material from a
standard cross section. For example, Zaafarani and co-workers used this
geometry to sample the deformation flow fields beneath nanoindention
impressions in copper revealing the full 3D character of the deformation
field, which compared well with their finite element prediction 89.
Alternatively, if significantly large volumes are required, it may be more
efficient to manufacture a protruding finger-like specimen, which can
be gradually shortened to remove each slice87, 90. This geometry reduces
EBSD pattern shadowing, waterfall and re-deposition artifacts as each
free surface remains as a protrusion.
Knowledge of the microstructure and the eventual use for the
data obtained is essential to make decisions regarding slice thickness
and EBSD step size. For both of these acquisition routes, the choice
of slice thickness is determined at the lower end by the limits of the
sectioning technique and at the upper end by the speed (and accuracy)
of the material removal process. The choice of EBSD step size is largely
dependent on the data acquisition speed available; here the use of a
fast camera capturing several hundred patterns per second can be
desirable, either enabling larger areas to be scanned or a finer step size
to be chosen.
The combination of step size and slice thickness defines the size and
shape of the unit voxel (volume pixel) in the final map. The area scanned
combined with the thickness of each slice and the number of slices
viewed defines the volume of material sampled.
Choice of voxel size and shape and the volume of material sampled
is dependent on the nature of the experiment performed. In general,
this is a combination of both the amount of instrument time available,
the fidelity of the data required, the nature of the problem studied and
the amount of effort required. For example, in order to analyze the
nature of grain boundary planes within a material it is necessary to
obtain many slices within each grain in order to accurately trace the
grain boundary plane region (as a general rule of thumb Groeber et al.
suggest at least 10 slices per grain86 which is similar to the suggestion of
Humphreys et al. for 2D EBSD noted previously4). Yet, if the distribution
of grain orientations in a 3D volume or the generation of a mesh for
finite element modeling is required, then a significantly lower sampling
374 SEPTEMBER 2012 | VOLUME 15 | NUMBER 9
frequency is necessary, thus sampling a larger volume of material, which
may ensure that a representative volume element is sampled.
Once several slices have been obtained, reconstruction of the 3D
model must be performed. Firstly, the data that has been acquired will
not be a perfect representation of the sampled material: successive
removal will not consistently reproduce rectangular sections (due to a
misalignment during the mill step); there will be optical distortions in
the electron microscope; each slice will be misaligned with respect to its
neighbors; there will be mis-indexed points; and finally, we do not have a
continuous description of the microstructure (i.e., approximating curved
lines on grain boundaries as a staircase).
Careful data acquisition will reduce the magnitude of the sample
mis-alignment and optical distortions (yet they will always be present).
Generally the use of a suitable fiducial marker of a known shape (i.e.,
a milled circle or cross for FIB polishing or a series of hardness indents
for mechanical polishing) can be combined with image correlation
to reposition the sample well between each slice. In addition, these
features could be imaged to produce a distortion free micrograph (e.g.,
using a travelling optical microscope or normal incidence SEM) to assess
the presence of optical distortions91. Subsequently a suitable correction
could be applied, e.g. using an affine transformation86, to ensure that the
appropriate data cube is reconstructed.
Physical alignment of the fiducial markers results in close alignment
of each successive slice. Typically, alignment of the slices prior
to reconstruction of the data cube is still required. A high quality
reconstruction can be performed by aligning not only microstructure
features, such as grain boundary triple points, but also local crystal
misorientations between voxels in neighboring slices. One strategy
suggested by Groeber and colleagues, is to allow iterative realignment
of the slices in the form of translations in x and y (but in theory it could
also include any potential misalignment such as sample tilt) in order
to reduce the total misorientation in the cube86. Clearly, care must be
taken in dealing with poorly indexed points and grain boundary regions.
Correction of poorly indexed points can be performed in a similar fashion
to convention 2D clean up routines, but now may include information
gained from voxels in neighboring slices.
At this point we have a data stack that consists of voxels which are
well alignment spatially with respect to each other but they may not
yet represent the microstructure as fully as our interrogation requires.
For example if the morphology of the individual grain boundary
planes is important, then the apparent stepped nature of the interface
inherited from the discrete sampling strategy must be addressed. For
this application, neighboring voxels of significantly different orientation
could be segmented from the data stack. Subsequently for each neighbor
voxel a marching cubes algorithm can be utilized to transform the
rectangular faceted voxel into a series of triangular facetted polygons92.
Finally additional smoothing of the microstructure can be performed as
required.
One example of 3D-EBSD obtained from FIB-SEM tomography is
shown in Fig. 7, courtesy of Groeber and co-workers (described in detail
elsewhere87, 90, 93-95). Here a polycrystalline nickel superalloy sample has been
examined with FIB-SEM tomography and 3D EBSD with voxel size of 250
250 250 nm3. Fig. 7a shows a reconstruction of the 3D data cube after
 Strains, planes, and EBSD in materials science
Fig. 7 Three dimensional reconstructions of microstructure obtained from a nickel
superalloy (IN100): (left) after alignment and application of marching cubes;
(middle) after grain boundary smoothing; (right) selected grains from the 3D
model. The material volume analyzed measured 50 m by 50 m by 50 m, with
EBSD maps acquired after 250 nm FIB slices. Figure courtesy of Groeber, Rollett
and colleagues86, 90.
initial alignment of consecutive slices, allowing for small shifts in the EBSD
maps for each slice to minimize total misorientation between neighbors,
and then application of a marching cubes algorithm to render triangular
facets. In order to analyze the nature of grain boundary planes, the grain
boundaries have been smoothed to reduce alias induced roughening
caused by discreet nature of voxel sampling. Qualitative analysis via
rendering of particular grains in the volume showing Fig. 7c hints at some
of the quantitative metrics that can be explored with in such a data cube,
such as grain volumes, misorientation and other metrics which have two
dimensional counterparts90. Data of this type can be used to measure five
parameter grain boundary plane distributions, which includes not only
four parameters from standard 2D EBSD, grain boundary misorientation
(axis 2, angle 1) and surface trace (1) but in addition the subsurface
grain boundary plane inclination94.
While FIB-SEM or mechanical section routes of 3D EBSD provides a
wealth of data on volumes of material at an intermediate length scale,
resolution of the technique is limited by the probe size (~20 nm) and
slicing and reconstruction ability at smaller length scales. Analysis of truly
nanocrystalline materials of very fine detail in microstructures is therefore
difficult and TEM experiments on these materials may be more suitable96
and are certainly complementary.
At larger length scales the total analyzed volume of material and the
sampling resolution is limited primarily by experiment time and instrument
stability. Recent advancements in 3D X-ray diffraction (XRD) microscopy
provide similar information non-destructively with limited resolution97,98.
One advantage with these techniques is that although 3D-XRD
experiments are difficult to perform, the technique is fundamentally non-
References
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REVIEW
destructive and thus in addition to sampling larger volumes of material, in
situ dynamical information can be obtained.
Summary and outlook
EBSD has come from being a very specialist technique being used in a small
number of physics laboratories to a mainstream materials characterization
tool. Potential of the technique to solve real materials problems was
recognized near the outset and these end goals have always driven its
development. In this field, technique development had been strongly
associated with two aims: (i) looking for general solutions so that the tool
can be rolled out easily from a specific initial problem to wide range of
related ones and (ii) automation so the statistically significant datasets
can be obtained for quantitative assessment of material microstructure.
This has led to the powerful tool we have today with a vast range of
applications which continues to expand.
We have picked strain mapping and 3D microscopy as two areas which
demonstrate that technique development is currently very active and to
demonstrate the pace at which substantial advances have been achieved.
In addition, we note that the work of Winkelmann on development of
dynamical diffraction simulations99-101 and detailed analysis of the energy
distributions contributing to Kikuchi bands within EBSD patterns102 is another
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We may also see some developments in detector technology over
the next decade. We already see two competing trends in EBSD either
attempting to go faster which has driven down pattern resolution, or to
obtain as much detail in the pattern as possible which drives down speed.
More sensitive detectors would be of benefit in both cases. It seems very
likely new detector strategies being developed for X-ray and TEM may also
lead to improved EBSD detectors.
EBSD has come a long way but the journey is far from over.
Acknowledgements
We gratefully acknowledge funding from EPSRC (EP/E044778/1, EP/
G004676/1, and EP/H018921/1). We have enjoyed continuing discussions
of the EBSD technique with Prof David J Dingley (University of Bristol) and Dr
Graham Meaden (BLG Productions Ltd). We are grateful to Prof Tony Rollett
(Carnegie-Mellon University) and Dr Michael Groeber (Wright-Patterson
Air Force Base) for sharing and discussing 3D EBSD data with us. We also
thank Dr Aimo Winkellman for his insight into the physics of EBSD pattern
formation and simulation code used for Fig. 2e.
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