Electron Diffraction Analysis

Diffraction image analysis 2

Diffraction analysis
Diffraction image calibration .......................................................3
Find center of symmetry.............................................................9
Diffraction image indexing ..........................................................9
Diffraction image measurement ...............................................14
Snap function ...........................................................................15
EDiff0606
 Electron Diffraction Analysis • Electron Diffraction Analysis

Electron Diffraction Analysis

Diffraction image Electron diffraction offers important information regarding the microstructure
analysis for TEM of crystalline substances. This TEM investigation method is especially im-
applications portant, because very small parts of samples containing very fine structures
can be examined. TEM not only offers options for diffraction, but also for
high resolution acquisition of the same part of the sample.
The Electron Diffraction Analysis add-in enables the automatic indexing,
evaluation, measurement, and analysis of diffraction images.

Diffraction button bar

After installing the Electron Diffraction Analysis add-in, the Diffraction button
bar becomes available and enables you to have access to all of the functions
of the add-in.

Calibrate, pg. 3
Find Center of Symmetry, pg. 9
Definition of Structure and Indexing, pg. 9
Measure, pg. 14
Snap Function, pg. 15

This is how you show the Diffraction button bar should it not be visible:
1) Open the Special menu.
2) Select the Edit Button Bars... command.
3) Select the check box in front of the Diffraction entry located in the But-
ton bars list.
4) Close the dialog box by clicking OK.

Installing add-in
2

Should your current software configuration not offer the Diffraction button
bar, you must follow these steps in order to activate the add-in:
1) Open the Special menu.
2) Select the Add-In Manager... command.
3) Select the check box in front of the Electron Diffraction Analysis entry
located in the Available add-ins list.
4) Click the Close button.
 Diffraction image calibration

Diffraction image calibration

Click this button located in the Diffraction button bar in order to calibrate the current diffraction
pattern. A diffraction pattern is automatically calibrated correctly after acquisition when using re-
mote compatible TEMs. The proper calibration is required for indexing and measuring a diffrac-
tion pattern.

1) Load the diffraction pattern you would like to calibrate into the active im-
age buffer or acquire a diffraction image.
This diffraction pattern of
monocrystalline aluminum
has not been calibrated. The
scale bar depicted therefore
shows the unit "Pixel"
(image points).

2) Click the Snap Function button located in the Diffraction button bar
when wanting to apply this function (see pg. 15). The button appears
clicked if the snap function has been activated.
3) Click the Calibrate button located in the Diffraction button bar.
" The Calibration of the diffraction pattern dialog box is opened.

3
 Electron Diffraction Analysis • Diffraction image calibration

Enter lattice spacing 4) In order to be able to calibrate a diffraction pattern, you must know at
least one pair of reflexes in the diffraction pattern, respectively the Mill-
er indices of at least one diffraction ring, as well as the corresponding
lattice spacing.
Enter the lattice spacing for the reflex and its counterpart into the
d-spacing field.
Example calculation If you want to calibrate a diffraction pattern of mono-crystalline aluminum,
you can use the (200) lattice planes for the calibration. You will need the fol-
lowing information to be properly able to specify the lattice spacing:
• Miller Indices
For aluminum, you can use h=2, k=0 and l=0.
• G-value(s)
Aluminum only has one g-value a=0,405 nm.
• Formula used to determine the lattice spaces dhkl
The formula for aluminum is:
a
d hkl = ---------------------------------
2 2 2
h +k +l
The specified values for aluminum result in a lattice spacing of 0,205 nm.
0, 405nm 0, 405nm
d 200 = ----------------------------------- = ------------------------- = 0,2025 nm
2 2 2 2
2 +0 +2
Note Note that you must enter the distance in "real space" into the d-spacing field.
Enter the value 0,202 (nm) for aluminum if you would like to apply the reflex
pair [002] and [002] for the calibration.
Set the unit 5) [nm] is offered as a unit by default. You can change this unit however
you like. To do so, click the Set Unit... button.
In the Set Unit dialog box, select the Å (Angström) entry from the Basic
unit list, if the lattice spacing is to be specified in Angström.
Find Center of Symmetry 6) Enter the camera length used to acquire the current diffraction pattern
into the Current field located in the Camera Length Calibration group.
The camera length is always in [mm].
The camera length is not necessary for the calibration of a single dif-
fraction pattern. It is, however, saved as additional information together
4

with the diffraction pattern. Therefore, the diffraction pattern will still be
properly calibrated even if you do not know the camera length.
Enter the camera length 7) Select the Apply to camera length check box to add the current camera
length to the Available list. The camera length is added to the list as
soon as the calibration has been successfully completed by clicking the
OK button.
Calibrate 8) Click the Calibrate button.
" The mouse pointer jumps into the active image.
9) Position the pointer onto the center of the first reflex, e.g., the [002] re-
flex and click the mouse using the left mouse button.
Position the pointer onto the center of the opposite reflex, in this case
[002], and confirm with the left mouse button.
 Diffraction image calibration

The blue line connects both

reflexes which will be
utilized for the calibration, in
this case [002] and [002].

You should select a reflex

pair which is located as far
as possible from the primary
beam. The larger the cali-
bration distance, the higher
the calibration accuracy.

10) Click OK to close the dialog box and to conclude the calibration.
11) Use the [Shift + F4] shortcut to show the scale bar in the image. If the
diffraction pattern has been correctly calibrated, the scale bar's unit is
a reciprocal length unit, i.e., 1/nm.
This diffraction pattern of
monocrystalline aluminum
has been calibrated. There-
fore, the unit of the scale bar
has a reciprocal length, e.g.,
"1/nm".

The center of the diffraction

pattern is marked by a little
red circle in the image over-
lay.

Save calibrated 12) Use the File > Save As... command to save the diffraction image as a
diffraction patterns file.
A calibrated diffraction pattern should be saved in the TIF file format.
Only then is the calibration data preserved.
 Electron Diffraction Analysis • Diffraction image calibration
Selecting the
viewport
manager view
Note
The magnifier in the view-
port manager on the left
magnifies the image section
under the current position of
your mouse (right).
6
Automatically calibrating diffraction patterns during acquisition
System requirements
Activating remote
control
Optimizing work environment
Your image analysis program offers you a magnifier which enables you to
set the reflex center onto large images rather accurately. You will find the
magnifier in the viewport manager located above the image manager. Click
on the last button to get a list with the possible Navigator, Magnifier and
Viewports views. Select the Magnifier view.
Select the automatic zoom factor for the image in the image window. The
entire diffraction pattern will now be shown in the image window. The mag-
nifier view in the viewport manager shows a magnified section of the image
beneath the current position of your mouse. The current position of your
mouse is shown by a cross hair in the magnifier. You can set the magnifier's
zoom factor. To do so, click the image in the viewport manager with the right
mouse button and select the desired zoom factor from the context menu.
You can move the image under the magnifier's cross hair with the arrow
keys of your keyboard during calibration. Use the arrow keys to set a point
as accurately as possible.
If your diffraction patterns are to be automatically calibrated during acquisi-
tion, your microscope must be able to be controlled by your image analysis
program. This may not be possible with some systems.
You can activate the remote control in the Image > Configure Input > Mag-
nification tab. Choose your microscope from the Device list and select the
Remote > On check box.
 Automatically calibrating diffraction patterns during acquisition

If your system is remote

compatible, the current
magnification will be trans-
ferred from your micro-
scope. The Magnification
field is automatically filled
out; you are no longer re-
quired to manually enter the
magnification.

You will find the name of

your microscope in the De-
vice list.

Testing remote control
In order to test the remote control, activate the Image > Configure Input >
Magnification tab. Here, click the Read button. The current microscope mag-
nification will now be read out and displayed in the Magnification field.
To test whether or not your system can read out camera lengths, switch your
microscope to diffraction mode and acquire a diffraction pattern. Doubleclick
the image buffer which contains the diffraction pattern in order to open the
Image Information dialog box. Check to see if the camera length is listed in
the transferred microscope information located in the Microscope tab.

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 Electron Diffraction Analysis • Diffraction image calibration

If your system is remote

compatible, you will find the
additional Microscope tab in
the image information. This
tab lists a range of informa-
tion which can be automati-
cally read out from your
microscope during image
acquisition.

This is how you automatically execute a calibration

In order to be able to calibrate the input channel for the acquisition of diffrac-
tion patterns, you must acquire and calibrate a diffraction pattern for each
camera length. To do so, you must know a reflex and its counterpart or the
Miller indices of a diffraction ring, as well as the corresponding lattice spac-
ing.
1) Click the Calibrate button located in the Diffraction button bar.
" The Calibration of the diffraction image dialog box is opened.
8

2) Enter the lattice spacing for the reflex and its counterpart into the
d-spacing field.
3) Enter the current camera length into the Current field located in the
Camera Length Calibration group.
4) Select the Apply to camera length check box.
This step is absolutely necessary to calibrate the input channel
and not only the current diffraction pattern.
5) Click the Calibrate button.
6) First click the left mouse button on the first reflex and then on the sec-
ond reflex you want to use for the calibration.
7) Close the dialog box by clicking OK.
8) Carry out the calibration on all the camera lengths.
9) Now, acquire a diffraction pattern with any camera length.
" The acquired diffraction pattern is automatically calibrated correctly.
10) If you want to index or measure the diffraction pattern, click subse-
quently the Find Center of Symmetry button.
 Find Center of Symmetry

Note Please note that the calibration data for the camera lengths are saved to-
gether with the input channel. If you are using another input channel for the
acquisition of the diffraction pattern, the already calibrated camera lengths
are no longer available.

Find Center of Symmetry

Click this button located in the Diffraction button bar to automatically find the center of symmetry
of the current diffraction pattern. The identification of the center of symmetry is a requirement for
the indexing and measurement of a diffraction pattern.

Note If you use the Calibrate command to calibrate a single diffraction pattern, the
center of symmetry is usually determined during the calibration. In this case,
you do not need the Find Center of Symmetry command.
Showing the center of The center will be marked by a little red circle. The circle is
symmetry located in the diffraction pattern's overlay, so that you can fade
it in or out as much as you like.

This is how you define the center of symmetry in a diffraction

pattern
1) Activate the image buffer containing the diffraction pattern whose cen-
ter of symmetry you would like to locate.
2) Click the Find Center of Symmetry button located on the Diffraction but-
ton bar.
Center of symmetry has " If a center has been located, you will receive a message accordingly.
been located " If you are not satisfied with the located center, you can now define
the center anew. To do so, simply click once on the appropriate
center of symmetry using the left mouse button.
Center of symmetry has If your image analysis program could not locate any center of symmetry, you
not been located will receive a message accordingly. You can now manually define the center
of symmetry via a simple mouse click.

Diffraction image indexing 9

Click this button located in the Diffraction button bar in order to index the current diffraction pat-
tern.

In a diffraction pattern, every reflex or diffraction ring is assigned to a partic-

ular set of parallel lattice planes. Your image analysis program helps you to
find the correct set of parallel lattice planes.
You can only then automatically index a diffraction pattern, if the following
requirements have been fulfilled:
• The diffraction pattern has been correctly calibrated.
• The center of the diffraction pattern has been properly defined.
• You know the crystal structure and the parameters of the lattice.
 Electron Diffraction Analysis • Diffraction image indexing
This is how you automatically index a diffraction pattern
Define structure
To index a diffraction
pattern, you must know the
crystal structure and the
lattice parameters. Enter the
appropriate values into the
Define crystal tab.
In the upper right you can
see the diffraction pattern of
a monocrystalline sample; in
the lower right, the diffrac-
tion pattern of a polycrystal-
line sample.
10
Index reflexes
1) In the image buffer, activate the diffraction pattern you would like to in-
dex.
2) Click the Snap Function button located in the Diffraction button bar
when wanting to apply this function (see pg. 15). The button appears
clicked if the snap function has been activated.
3) Click the Definition of Structure and Indexing button located on the Dif-
fraction button bar.
" The Indexing dialog box opens.
4) Enter the appropriate values for the current diffraction pattern into the
Define crystal tab.
5) Select the Single crystal option if the current diffraction pattern shows
individual diffraction reflexes.
Select the Polycrystalline material if the current diffraction image con-
tains rings.
6) For aluminium, select for example the entries Cubic and Face centered
(F) from the Crystal type group.
" The lattice parameters are automatically adapted to the selected
lattice type. Thus, one does not require three different g-values for
all of the lattice types. In the dialog box, only the fields that must be
filled out for the selected lattice type can be edited.
For example, there is only a single g-value (a) for the "face-cen-
tered cubic" lattice type. Angles α, β and γ are always 90°.
7) Enter the g-values. Aluminum has only one g-value (a = 0,405 nm).
8) Activate the Indexing diffraction pattern tab.
 Diffraction image indexing

Use the Indexing diffraction

pattern tab to identify the
reflexes or diffraction rings.
The tab also offers
additional settings which
have an impact on the out-
put of the values.

In the upper right you can

see an indexed diffraction
pattern of a monocrystaline
sample; in the lower right, of
a polycrystalline sample.
The intensity of the poly-
crystalline diffraction dia-
gram has been reduced so
that the indexing is more
legible for printing purposes.

9) Click the Auto-indexing button to start the automatic indexing. Your

image analysis program will then search for the highest intensities in
your diffraction pattern and then determine the appropriate Miller indi-
ces.
Note You will receive a message accordingly if the automatic indexing should not
have been successful. You can then either increase the sensitivity or man-
ually define the basis vector.
Save diffraction pattern 10) The diffraction pattern should be saved in the TIF file format. All of the
crystal parameters which you have set for the definition of structure will
automatically have been saved together with the image.

11
11) Load the image to be able to view the crystal parameters again. Click
the Definition of Structure and Indexing button again. The Define
crystal tab now shows the structure parameters of the current diffrac-
tion pattern.

Indexing a diffraction image via basis vectors

Should the automatic indexing not be successful, you can also manually
index a single crystal diffraction pattern by defining the basis vectors.
1) In the image buffer, activate the diffraction pattern you would like to
index.
2) Click the Definition of Structure and Indexing button located on the
Diffraction button bar.
3) Enter the appropriate values for the current diffraction pattern into the
Define crystal tab.
4) Activate the Indexing diffraction pattern tab.
5) Click the Define g-vectors button.
" The mouse pointer moves to the image window. The start point of
the first g-vector is automatically the primary beam.
 Electron Diffraction Analysis • Diffraction image indexing

6) Position the mouse pointer onto a reflex which you are sure to be able
to identify and click the left mouse button.
" The Select reflexes dialog box will be opened. All of the reflexes are
listed in the dialog box which can be theoretically located near the
clicked position in the diffraction pattern. If you can not find the
reflex which you want to use for calibration, you should recheck the
entries for the crystal structure in the Define crystal tab or re-cali-
brate the diffraction pattern.
7) Enter the Miller indices for the first basis vector or select the appropri-
ate Miller indices from the dialog box's list. Confirm the first basis vector
by clicking OK.
8) Define the rest of the basis vectors.
" All of the reflexes of the current diffraction pattern will be reindexed
with the defined basis vectors.
Two basis vectors are suffi-
cient enough to clearly de-
fine the lattice for a face-
centered cubic lattice.
You define the basis vectors
by clicking two known
reflexes. If the diffraction
pattern has been correctly
calibrated, the clicked reflex,
in this case [111], will be of-
fered in the Select reflexes
dialog box.

Display and output options

You have several possibilities to alter the display or export of the indexing.
You will find the display and export options on the Indexing diffraction pat-
tern tab located in the Indexing dialog box.
When altering a display or output option, you should subsequently click the
Refresh button in order to be able to view the altered settings in the current
diffraction pattern.
Image overlays The identified indexes will now be written to the image overlay. You can
12

imagine the overlay as being a transparent foil which is placed over the
image. Because of this, the image is not altered by the indexing, but rather
only supplemented in the image overlay. In addition, you can always hide or
delete the image overlay. To do so, use the functions of the Overlay button
bar.
In the Standard button bar, click the Overlay Button Bar button to show the
Overlay button bar. To display or hide the overlay of an image, use the Layer
button, for example.
The image overlay only then remains separate from the image, if you have
saved the image in TIF format. All other image formats do not support such
an image overlay. For this reason, the image overlay is automatically burned
into the image when saving the image in another image file format.
Note You should not permanently burn the overlay into the image. The overlay will
then become a permanent part of the image. The image information which
was located below the drawing object, are lost when burning.
Diffraction patterns often have a bit depth of 16 bits and cannot be burned
 Diffraction image indexing

into 16-bit images. Therefore, 16-bit images must be converted automatical-

ly into 8-bit images prior to burning. This conversion, however, results in the
irreversible loss of image information.
You will find the display and
export options on the Index-
ing diffraction pattern tab
located in the Indexing
dialog box.

Color Select one of 16 possible colors from the Display color palette. This color
then solely effects the color of the labeling when indexing a diffraction
image.
Labeling size You can alter the font with which the reflexes are to be indexed. Open the
Special > Preferences > View tab. Enter the desired font into the Overlay >
Pen size field.
Export to image Select the Show indices in Overlay check box to show all of the Miller indices
overlay in the overlay of the diffraction pattern.
Clear the Show indices in Overlay check box, so that only the position of the
located diffraction reflexes, respectively rings are shown in the diffraction
pattern's overlay instead of the Miller indices.
Select the Show only basis vectors check box to show only Miller indices
which belong to the basis vectors. This button is not available when working
with polycrystalline material.
Export to sheet Select the Results to sheet check box to create a sheet in addition to the in-
dexing. The sheet is created as soon as you click on one of the following but-
tons: Auto-indexing, Define g-vectors, or Refresh.
The status of the Lattice spacing [nm] and Reciprocal lattice spacing [1/nm]
determines which values are to be transferred to the output sheet.

13
Note In doing so, an already existing sheet will be overwritten. If you would like to
maintain the sheet, save it as a file using the File > Save As... command be-
fore creating the next sheet.
The sheet contains all of the
located Miller indices and
the lattice spacing, respec-
tively the reciprocal lattice
spacing pertaining to them.
 Electron Diffraction Analysis • Measuring diffraction images

Measuring diffraction images

Click this button located in the Diffraction button bar to measure the current diffraction pattern.
It is possible to measure distances and angles on a diffraction pattern. The origin for each of
the measurements is automatically the primary beam, respectively the center of symmetry.

You can only then measure a diffraction pattern, if the following require-
ments have been fulfilled:
• The diffraction pattern has been correctly calibrated.
• The center of the diffraction pattern has been properly defined.
This is how you measure the radius of a diffraction ring or the
distance between the primary beam and a reflex
1) Click the little arrow located next to the Measure button and select the
desired measurement functions. In this case, select the Distances
entry.
" The mouse pointer moves to the image window.
2) Position the pointer onto the diffraction reflex or onto any point on the
diffraction ring and click the left mouse button. The primary beam is
automatically the start point of the measurement.
" The first distance to be measured is shown in the image overlay.
Select the distances you
want to measure directly on
the image. The origin for
each of the measurements
is automatically the primary
beam, respectively the
center of symmetry.

The results are listed in the

measurement display. You
will find the measurement
display in the Measure-
ments tab located in the im-
age manager. Click the icon
14

with the caliper rule located

in the image manager, to
bring the measurement dis-
play to the foreground.

3) Repeat the last steps for each measurement you want to execute.
4) Click the middle mouse button or the [Esc] key to end the measure-
ment.
5) Use the File > Save As... command to save the image together with the
measurement as one file. The image should be saved in the TIF file for-
mat.
 Snap Function

Display and output options

Exporting The measured values are displayed in color in the image's overlay. In addi-
measurement tion, all measurement functions create an entry in the measurement display.
results These measurement results remain linked to the image even after the image
has been saved. You can export the measurement results to a sheet any
time.
To do so, click the Create Measurement Sheet button located in the mea-
surement button bar. Use the Measure > Measurements Bar command to
show the Measurements button bar.
Measurement label If you are measuring an indexed diffraction pattern, it is usually disturbing if
the measurement results are also written to the image overlay.
Use the Special > Preferences... command. Select the Show labels > None
option located in the Measure tab. You will now only see the measurement
object in the image overlay.
Color If you are making measurements on the diffraction pattern, you determine
the colors of the measurement objects in the Special > Preferences > Mea-
sure tab.
Labeling size You can alter the font with which the reflexes are to be indexed. Open the
Special > Preferences > View tab. Enter the desired font into the Overlay >
Pen size field.

Snap Function
Click this button in the Diffraction button bar to activate or deactivate the snap function. The but-
ton appears clicked if the snap function has been activated.

Some of the functions used for the analysis of diffraction patterns require
you to define a reflex on the diffraction pattern via mouse click. The accuracy
of all the results depends on how well the reflex's center has been hit. The
snap function assists you.
If the snap function is active, you simply have to click in the vicinity of a dif-
fraction reflex or ring. Your image analysis program then automatically
searches for a diffraction reflex or ring located in the vicinity of your mouse

15
click.
 Index

A
Activate remote control 6
Automatic calibration 8

C
Calibrate 3

D
Definie crystal structure 10
Diffraction button bar 2
Display and Export Options, Indexing 12
Display and Export Options, Measuring 15

F
Find center of symmetry 9

I
Image overlays 13
Indexing 9
Indexing via basis vectors 11
Install 2

M
16

Measure 14

S
Saving diffraction pattern 11
Snap Function 15

T
Test remote control 7