Microchim Acta 155, 19–29 (2006)
DOI 10.1007/s00604-006-0502-4
Original Paper
Orientation Imaging Microscopy for the Transmission
Electron Microscope
David J. Dingley

TSL-EDAX and Bristol University, 392 East, 23000 South Draper, Utah 84020, USA
Received May 26, 2005; accepted November 25, 2005; published online June 6, 2006
# Springer-Verlag 2006
Abstract. The resolution limit of Orientation Imaging
Microscopy in the Scanning Electron Microscope is
between 20 nA and 80 nA depending on the basic reso-
lution=beam current performance of the SEM, the sam-
ple atomic number and the level of residual strain
within it. The newer technique of orientation imaging
in the transmission electron microscope, TEM, im-
proves on this resolution limit by a factor of five to ten.
The new technique is based on a novel procedure
for determining the crystallography of separate small
volumes in the sample by examination of a large se-
ries of dark field images. Each image is recorded for a
different diffraction condition. This is achieved by
using a computer to direct the electron beam onto
the same area of the sample so that it covers all direc-
tions within a cone of semi-apex angle 3 degrees.
Analysis of the intensity of the same point in each
of the dark field images permits reconstruction of a
diffraction pattern for that point providing the data
to calculate its crystal orientation. The process is
repeated for each point in the image. The Orientation
Image Micrograph is constructed from the orienta-
tions so determined.
The technique is shown to be capable of producing
orientation micrographs of high spatial resolution for
unstrained samples. For highly strained samples diffi-
culties are encountered in accurately indexing the
complicated diffraction patterns that are observed.

E-mail: djdingley@hotmail.com
Methods to improve the indexing procedures involve
determining the sub-cell structure first from a compar-
ison of patterns from adjacent pixels and then sum-
ming all patterns belonging to a single sub-cell. The
resultant improvement in pattern quality permits more
reliable determination of orientation. Examples of
this procedure are taken from studies of deformed
aluminum.
Key words: Orientation imaging; transmission electron micros-
copy; conical dark field.
Orientation Imaging Microscopy (OIM) [1] is a well
established technique and is described in numerous
publications. An overview of the subject is document-
ed in a series of papers by leading exponents of the
technique in the book, Electron Backscatter Diffrac-
tion in Materials Science [2], where an extensive bib-
liography of the earlier literature can also be found.
OIM is normally associated with the scanning elec-
tron microscope (SEM) and is based on computer
identification and indexing of electron backscatter
diffraction, (EBSD) patterns, Venables [3], Dingley
[4, 5]. The resultant micrographs are produced by
scanning the incident electron beam over the area of
interest in the sample and recording the patterns
sequentially. The resolution limit for the technique
ranges from 20 nm to 80 nm depending on the
resolution=beam current response of the SEM and
the sample atomic number and level of internal strain.
Figure 1 illustrates the dependence of this resolution
20
Fig. 2. High resolution OIM of platinum polycrystal
on the electron beam diameter. Figure 2 illustrates the
resolution limit for the technique achieved so far by
the author. In both Figs. 1 and 2 the sample was poly-
crystalline platinum, the microscope was an FEI
XL30 FEGSEM operated at 30 kV, and the EBSD
equipment and software used was that provided by
TSL. In Fig. 1 the OIM is shaded according to the
crystal direction normal to the sample surface and is
overlaid on a secondary electron image recorded from
the same area. In Fig. 2 the smallest grain resolvable,
marked X, measures 6 nm by 8 nm but it will be
noticed that the grain boundary edges are irregular
and detract from the overall quality.
The extension of Orientation Image Microscopy to
the Transmission Electron Microscope was begun in
D. J. Dingley
Fig. 1. Two OIMs from Platinum
(blue coloration) superimposed on
SEM image recorded at electron
beam diameters 6 nm and 48 nm
respectively
1994 by the research group at TSL and was first pub-
lished by Dingley et al. [6] It is based on a novel
procedure which they describe in detail but is repeated
here as it is still relatively new. Over the past ten years
the basic experimental procedure has remained
unchanged but significant advances have been made
in the computer methods used. Throughout the early
work, the major problems were associated with index-
ing diffraction patterns that had too few reflections
imaged in them. This was overcome by using a digital
recording camera permitting different exposure times
for images recorded at small diffraction angles and
those recorded at large angles. The difficulties remain-
ing are associated with indexing complex diffraction
patterns. These are observed when imaging highly
deformed samples where there may be crystal rotation
through the thickness of the sample. Nevertheless, in
order for the technique to be as robust in determining
orientation images as is currently achieved using the
EBSD technique such patterns have to be analysed
satisfactorily. This paper describes the procedures
investigated to achieve this end.
Basis of the New Method
In an orientation image micrograph the changing crys-
tal orientation of a selected area of the sample is
imaged. To achieve this in the TEM the conventional
methods for measuring the required orientations
would be selected area diffraction, Kikuchi diffraction
or convergent beam diffraction. Selected area diffrac-
Orientation Imaging Microscopy for the Transmission Electron Microscope
tion has a resolution limit of the order of 1 micron and
is thus of no practical use. An OIM could be obtained
however in the TEM by scanning the beam over the
sample and recording the successive Kikuchi or con-
vergent beam patterns in a computer. The procedure is
illustrated in Fig. 3. For the convergent beam and
Kikuchi pattern cases the diffraction area is the size
of the incident probe. Hence high resolution could be
Fig. 3. Schematic of STEM mode of obtaining an OIM in the
TEM
Fig. 4. Formation of dark field images
21
achieved. However as the probe size decreases
towards the nanometer range these patterns are not
always observed especially if the sample is less than
10 nm thick and deformed. Such procedures are thus
unreliable. Furthermore, the time to produce an image
with sufficient data points, 65000 is typical, would be
of the order 2 hours in which time a sample in the
TEM is likely to drift by 100 nm. Convergent beam
patterns and Kikuchi patterns have large intensity gra-
dients across them which are difficult to flatten as
required for subsequent computer analysis. For these
reasons a different approach has been devised.
In the new approach dark field images of the area of
interest are recorded from which the crystallography
of each point in the image is later determined. The
method of forming the dark field image is to tilt the
incident beam so as to direct successive diffracted
beams to pass through the objective aperture. This is
illustrated schematically in Fig. 4 together with
images of the untilted and tilted diffraction patterns
and a comparison between bright field and dark filed
images. Figure 5 shows eight dark filed images
recorded in this way from a twined gold sample.
The diffraction pattern at the center of the figure
shows the diffracted beams used to form the separate
images.
22
Normally to observe the dark field images the dif-
fraction pattern from the area of interest is viewed
first. However, in the new method, the dark field
images are observed first. They are then analysed to
deduce the form of the diffraction pattern that would
have emanated from each corresponding point in the
sample. Experimentally, the dark field images are
recorded using a digital video camera. Each image
is from exactly the same area of the sample and each
recorded at a different beam tilt. The different beam
tilts are produced using a computer to alter the beam
direction as illustrated in Fig. 6. In the figure, the tilt
of the beam from normal incidence is
and the rota-
Fig. 6. Illustration of circular scanning to form a series of dark
filed images
D. J. Dingley
Fig. 5. Eight dark field images from a
gold single crystal
tional angle of the beam is . Each diffraction condi-
tion is thus specified by a specific (
, ) pair.
ranges
typically from 0 to 3 degrees to include diffracted
beams up to 6th order. It is increased in steps of
0.06 degrees.  varies through 360 degrees and is
normally incremented in steps of 4 degrees. Images
are recorded at a magnification sufficient to provide
the resolution required and yet include as large an area
of the sample as possible. Some 5000 images are
recorded at a pixel size of 256256. The total record-
ing time is of the order 15 minutes. It is an experi-
mental requirement that the image remains stationary
throughout the scan process. This entails that the rota-
tion and tilt point of the beam are exactly centered on
the sample. On modern instruments this is not parti-
cularly difficult. The drift of the sample in this time is
less than 10 nm.
Each pixel in the image has a corresponding point
in the sample. A pixel will thus become bright when
the incident beam has a (
, ) value such that it
excites a diffracted beam in the corresponding point
in the sample and that diffracted beam passes through
the objective aperture. Thus an examination of the
dark filed images is made to determine the (
, )
values at which each pixel brightens. This provides
a set of reflections for each point that were excited
during the scan and in turn this allows a reconstruc-
tion of the diffraction pattern that is associated with
them. An image containing 256256 pixels yields
Orientation Imaging Microscopy for the Transmission Electron Microscope
65536 reconstructed diffraction patterns with a spatial
resolution given by the width of the image multiplied
by the magnification and divided by 256.
In practice the varying brightness of a pixel is
plotted in (
, ) space to reconstruct this diffraction
pattern. The process is illustrated in Fig. 7. The pat-
tern shown is a reconstruction from a set of dark filed
images recorded from a superalloy sample. It has all
the appearances of a normal diffraction pattern and
can be analysed in exactly the same way.
Indexing of Reconstructed Patterns
The method adopted for indexing a reconstructed dif-
fraction pattern (RDP) follows the same procedures
developed for automated indexing of regular spot pat-
23
Fig. 7. Illustration of production of recon-
structed diffraction pattern
terns and also borrows from the tried and tested rou-
tines used for indexing EBSD patterns. The method
differs however, in one important respect from the con-
ventional indexing of spot patterns and follows the
principles suggested by Zaefferer [7]. Figure 8 illus-
trates the principle. For diffracted beams to be excited
they must fall on or very close to the Ewald sphere,
that is within about 0.1 degrees of it. The real space di-
rection of this vector is known. It is inclined upwards
from the horizontal by 2 the Bragg angle. The lattice
spacing corresponding to the reflection can be found
through the Bragg equation knowing the electron
wavelength and the angle
at which peak intensity
of the reflection occurs. Possible Miller indices hkl for
this reflection can be found from the lattice spacing
and knowing the crystal parameters for the material.
Fig. 8. Schematic for precise determination
of crystal orientation
24 D. J. Dingley

Fig. 9. (a) Diffraction pattern from gold with detected spots outlined with the search rectangles. (b) Indexed diffraction pattern from gold

Fig. 10. Diffraction patterns from silicon taken

at 1 degree intervals with resultant indexing
overlaid

This is repeated for sets of three reflections found
from the diffraction pattern. The crystal direction,
uvw, normal to the sample, is then found by solving
Eq. (1) for the three hkl values.
u  h þ v  k þ w  l ¼ 2 cosð90 
Þ
sibilities, is fixed. And so forth for the third reflection.
Consistency between first second and third reflections
must be found for acceptance. If a consistent match is
ð1Þ

To start with there is an uncertainty in the specific hkl

value to use. There is also an experimental error in
determining
so that a certain tolerance has to be
allowed in lattice spacing and hence hkl family. We
proceed by fixing the hkl value of the first reflection.
The difference in  values of the first and second
reflections is calculated and a search is made to see
which particular hkl value of the second reflection is
angled from the first by the calculated difference in 
values. And so the second hkl value, or several pos- Fig. 11. RDP from superalloy
Orientation Imaging Microscopy for the Transmission Electron Microscope 25

not found the hkl value for the first reflection is chang- three reflections that can be extracted from the pat-
ed to an alternative if there is one, and the procedure terns. For each consistent combination including the
repeated. The entire process is repeated for all sets of ambiguous cases the calculated uvw is tabulated. The

Fig. 12. RDP from gold with ringed spot originating from the micro twins depicted in the dark field micrograph

Fig. 13. (a) OIM for gold single crystal. Coloration

depicts deviation from {001} crystal direction by up to
7 degrees. (b) Misorientation histogram for trace
across OIM in a
26
uvw that is obtained most frequently is voted the most
likely solution. Determination of the crystal orienta-
tion follows by combining this direction with two
others in the plane of the pattern. The two directions
in the plane of the pattern are found by determining
the crystal directions parallel to two observed reflec-
tions. The indices of these reflections are known; they
correspond to the indexing found for the selected
solution.
The key to satisfactory indexing is the automated
procedure in finding the diffraction spots. A small
rectangular filter is passed through the image of the
diffraction pattern and the intensities falling within it
summed. The rectangles found to accumulate high
intensities are deemed to have fallen on reflections.
A two dimensional Gaussian fit is made to the inten-
sity distribution within these boxes to better find the
position of the peak intensity. Figure 9a shows a dif-
fraction pattern from gold with the detected peaks
numbered and with the search rectangles overlaid.
Figure 9b shows the same pattern after the indexing
routine has chosen the best fit solution.
The precision of the indexing routine is illustrated
in Fig. 10 which shows the resultant indexing of
diffraction patterns from silicon tilted successively
through 1 degree steps.
Fig. 14. Reconstructed diffraction patterns from different regions of a deformed grain
D. J. Dingley
The reconstructed diffraction patterns have spots
larger than those obtained from selected area micro-
graphs. The size is determined by that of the objective
aperture. The spots are also less regular in shape
becoming more extreme in patterns reconstructed
from deformed specimens. In strain free samples how-
ever the patterns can be sharp and contain fine detail
such as Kikuchi lines as illustrated in Fig. 11.
Figure 12 illustrates an interesting result obtained
from the twinned gold sample. The reconstructed dif-
fraction pattern shows one reflection that does not
belong to the matrix diffraction pattern. It is circled
in red and is due to diffraction from a micro twin. The
imbedded twin is circled in the dark field image to the
right. The dark field image formed by imaging a
matrix reflection is shown to the left. The micro twins
are less than 10 nm wide.
Formation of Orientation Images
from Reconstructed Diffraction Patterns
Once the reconstructed diffraction patterns have been
indexed and each orientation measured the data is
fed to the mapping programs developed for imaging
orientation data obtained using EBSD in the SEM.
The OIM for the gold single crystal in Fig. 12 is
Orientation Imaging Microscopy for the Transmission Electron Microscope
Fig. 15. Illustration of incorrect indexing of reconstructed diffraction pattern. The third solution is correct
shown in Fig. 13a. The shading depicts the crystal
orientation normal to the surface. The deepest shade
corresponds to the exact [100] crystal direction. The
brightest shade corresponds to an angular change of
the normal crystal direction of 7 degrees. It is seen
Fig. 16(a and b). (a) Is a bright field image from deformed alu-
minum and (b) a grain map of the same area
27
from the histogram in Fig. 13b that the twins cause
significant local lattice bending.
Mapping Orientation Changes from Highly
Strained Crystals
Most of the previous papers on Orientation imaging in
the TEM have used examples for annealed material
albeit with nano-sized crystals. These cases are simi-
lar to the gold sample illustrated above and do not
Fig. 17(a and b). Improvement in pattern quality on summing
patterns from coherent areas
28
prove a challenge to the technique, that is as long as
there are sufficient spots in the reconstructed pattern.
Whereas poor spot detection was a problem in the
earlier work it has been greatly reduced by using a
digital camera to record the dark field images. The
new camera and associated software permits the expo-
sure time to be increased as the beam deflection angle
increases and so compensates for the fall off of inten-
sity of the dark field image at the larger tilt angles.
The greater challenge has been to produce a robust
indexing procedure for deformed specimens. Some
success has already been published in this area,
Penelle et al. [8]. However there are many cases
where the reconstructed patterns have caused consid-
erable difficulty. Figure 14 contains several RDP
along a fragmented grain in a highly deformed alumi-
num sample. The patterns differ in detail due to the
local lattice bending but contain some spots that are
common between adjoining regions of the grain.
However, the patterns also contain numerous spots
which can not all be indexed as originating from the
same grain or even forming part of the main pattern.
In such cases slight changes in peak detection param-
eters can result in incorrect indexing. This is illus-
Fig. 18(a and b). Show respectively orientation image of de-
formed aluminum and corresponding pole Fig
D. J. Dingley
trated in Fig. 15. To remedy the situation advantage
had been taken of the fact that the pixels within a sub-
cell in the structure produce diffraction patterns that
are similar. Software was developed to sum the recon-
structed patterns for such sub-cells. The units were
identified by testing to see if patterns from adjacent
pixels had either 60%, 80% or 90% reflections in
common. The sub-cells could be as small as 1 or 2
pixels. A ‘grain map’ was constructed from this data
depicting the individual regions where such common-
ality was found. The image corresponding to the sum
of the diffraction patterns within a sub-cell was used
for indexing. One such grain map for the deformed
aluminum sample shown in Fig. 14 is shown in
Fig. 16b. The bright field image of the same area is
shown in Fig. 16a. The grain map shows greater frag-
mentation of the structure than the bright field image.
Figure 17a and b shows the improvement in pattern
quality obtained by summing the patterns within a
sub-cell. Figure 18a and b shows respectively, the
orientation map generated using the averaged pattern
from each sub-cell together with the pole figure repre-
Fig. 19(a and b). Show respectively orientation image of de-
formed aluminum and corresponding pole figure calculated using
different indexing parameters than those used to generate Fig. 18
Orientation Imaging Microscopy for the Transmission Electron Microscope
sentation of the distribution of the {001} plane nor-
mal. Figure 19a and b are the map and pole figures
obtained when using different diffraction peak search
parameters. The results are nearly identical. This indi-
cates an improvement in robustness of the indexing
procedure though the differences between the two
maps imply they are not yet 100% reliable. Further
research in this area is required.
Discussion
Construction of orientation image micrographs using
the transmission electron microscope is a challenging
experimental exercise. The dark field diffraction pro-
cedure adopted above has required developing a cir-
cular scanning procedure to collect dark field images
over a range of (
, ) values as defined in Fig. 6. This
is now a routine operation. Analysis of the dark field
images to extract a diffraction pattern for each pixel in
the image is also routinely achieved and the quality of
these reconstructions can be high, Fig. 11. A method
for reliably indexing spot diffraction patterns was also
needed. Advances in this area have been significant
with the precision of measurements exceeding 1
degree for selected area patterns as demonstrated in
Fig. 10. It is not so high for measurements on recon-
structed patterns because the diffraction spots appear
larger and often irregular. In the case of the twinned
gold crystal shown in Fig. 12 this irregularity was due
to the twin diffraction spots merging with the primary
diffraction pattern. In the case of the pattern from
recrystallised superalloy, Fig. 11, the irregularity
results from the appearance of Kikuchi lines. In the
case of the deformed aluminum it was due to severe
crystal lattice bending.
The resolution of the dark field method was shown
to be better than 10 nm by virtue of imaging the gold
micro twins (Figs. 12 and 13), and because of the
detail in structure revealed in the deformed aluminum
sample (Figs. 16b and 18a).
The construction of orientation image maps from
the reconstructed patterns was shown to be very reli-
able for low strain samples (Fig. 13), but not so
from highly strained samples (Fig. 15). A detailed
examination of the reconstructed patterns from the
deformed aluminum often showed a set of reflections
that could not be indexed together with the matrix
pattern. One explanation is that there are two crystals
through the thickness and the dark field method is
sensitive to reflections coming from both crystals.
29
Procedures whereby RDPs are summed for adjacent
pixels that are detected as having essentially the same
pattern have undoubtedly improved the quality of the
images and enhanced the most prominent diffraction
spots. In this way the peak detection and indexing
routines have a better chance of consistently distin-
guishing the matrix pattern to produce an improved
orientation map. The success of the method is dem-
onstrated by comparing the maps and pole figures in
Fig. 18.
Conclusions
It has been shown that successful automated indexing
of selected area spot patterns can be carried out with a
precision of 1 degree or better. Almost the same pre-
cision can be achieved on indexing reconstructed dif-
fraction patterns. The novel experimental method for
obtaining these reconstructions using a dark field im-
aging procedure has been shown to be very reliable.
The spatial resolution of the technique is better than
10 nm for strain free samples. For samples in high
states of residual stress and extensive crystal lattice
bending, complex diffraction patterns are observed
which are difficult to index. Increased reliability in
indexing such patterns was obtained by summing
the patterns that belong to a coherent volume of the
material. The coherent volumes, that is grains or sub-
grains, were reliably distinguished by comparing the
reconstructed diffraction patterns from neighboring
pixels.
Acknowledgements. The author is deeply indebted to his coworkers
at TSL, (www.EDAX.com), namely Dr. Stuart Wright, and Damian
Dingley for the computer programming and to Mike Tiner and Jeff
Ferrar for much of the data.
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