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User’s Guide

EFTEM
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EFTEM

Getting Started with EsiVision 5


EFTEM
THE ESI METHOD ....................................................................5
THE IMAGE EELS METHOD ..................................................11
THE PARALLEL EELS METHOD ...........................................16

Electron Energy Loss Spectra 19

The Spectrum Document .............................................19


Printing EELS spectra .................................................22
Graph Information ........................................................25
Image Information ........................................................30

The Graph menu 31

LABELS, SET... .......................................................................31


SET SPLIT GAIN.. ...................................................................32
MODIFY SPLIT GAIN... ...........................................................33
ZEROLOSS CALIBRATION... .................................................34
INTEGRATION ........................................................................35
BACKGROUND SUBTRACTION... .........................................36
FOURIER-LOG DECONVOLUTION .......................................40

The EFTEM menu 41

EELS ATLAS ...........................................................................39


1103AEFTEM

Set Elements Labels... .......................................................42


Auto Scaling... ....................................................................43
Peak Identification... ..........................................................45
Display Zeroloss ................................................................46
ESI .........................................................................................49
ESI Options ........................................................................50
Acquisition... ......................................................................52
Define series... ...................................................................58
EFTEM •

Quality Check... ................................................................. 60


R-Map ................................................................................ 61
Drift Correction... ............................................................... 63
Save Series... .................................................................... 65
Load Series... .................................................................... 66
Analyze... ........................................................................... 67
Presentation... ................................................................... 69
Overview ........................................................................... 71
Combine Images... ............................................................ 73
IMAGE EELS .......................................................................... 75
Image EELS Options ......................................................... 76
Acquisition... ...................................................................... 78
Define Series ..................................................................... 84
Quality Check .................................................................... 86
Drift Correction... ............................................................... 86
Save Series... .................................................................... 88
Load Series... .................................................................... 90
Analyze... ........................................................................... 91
ESI Mapping... ................................................................... 97
PARALLEL EELS .................................................................. 102
Parallel EELS Options ..................................................... 102
Acquisition... .................................................................... 104
Wide Range Acquistion... ................................................ 110
Calibration... .................................................................... 118
Show Calibration Data... .................................................. 121
Intensity Profile... ............................................................. 121
SERIAL EELS ACQUISITION... ............................................ 124
Serial EELS Options ...................................................... 125
QUANTIFICATION................................................................. 133
Element ratio... ................................................................ 133
Ratio Image... .................................................................. 138
SPECIMEN THICKNESS ...................................................... 141
From Spectrum... ............................................................. 141
From Image... .................................................................. 142
Interactive... ..................................................................... 146
MICROSCOPE PARAMETER... ........................................... 147
SET ENERGY-LOSS... ......................................................... 148
OPTIONS... ......................................................................... 148
EFTEM

EFTEM
Definition EFTEM is the acronym for Energy Filtering Transmission Electron
Microscopy, an analytical technique that makes use of the characteristic
electron energy loss in solids. An energy-filtering TEM can be used to record
energy-filtered images as well as energy-loss spectra:
• An electron energy-loss spectrum is achieved when plotting the
number of electrons against the corresponding energy loss.
• An energy-filtered image is formed by electrons with one
characteristic energy loss.
What does EFTEM The commands of the EFTEM menu provide you with different methods for
provide? recording and analyzing spectra and energy-filtered images. Depending on
your configuration, you may not be able to use all functions of the EFTEM
menu described here. For example, the Serial EELS functions can only be
used when an IEEE-interface is installed.
What do you find in this This manual describes the commands of the EFTEM menu and some
manual? special features of EFTEM images and spectra.
Spectrum EsiVision includes the Graph Processing module. This is a special module
for displaying and processing one-dimensional data files.
Remote Control The remote control of the microscope is needed for a lot of operations, e. g.,
for the automatic acquisition of ESI- or Image EELS series. Therefore, make
sure that you have selected a logical input channel which supports the
remote control.
How to... How to switch on the remote control:

1) Choose the Image > Set Input... command.


" The Set Input dialog box offers a list of all input channels available.
2) Select the desired input and click the Configure... button.
" The Configure Input dialog box is opened. The properties of the
selected input can be defined on several tabs.
3) Click the Magnification tab.
EFTEM • EFTEM

4) Select the type of microscope you use from the Device list box, e. g.,
’LEO 912’.
" The Remote group will be enabled.
5) Select the On check box to switch on the remote control.
" The Read button will appear in the Remote group.
" Click the Read button to transfer the current magnification from the
microscope to EsiVision via remote control.
6) If you get the error message ’The magnification cannot be read.’:
Click the Set COM port... button.
" The Set Remote COM Port dialog box is opened.
7) Select another COM port from the list and close the dialog box by
clicking OK.
8) Close the dialog box by clicking OK.
9) Restart EsiVision.
Note Please note: If you switch off the remote control in the input, the system will
not notice this change until you restart EsiVision.
4
Getting Started with EsiVision

Getting Started with EsiVision


The ESI method
Use the ESI (energy spectroscopic imaging) method for acquiring a highly
resolved element distribution image of you specimen. During the ESI
acquisition, energy filtered images are acquired below and at an element
specific ionization edge. Structures containing the element become brighter
as the selected energy loss is raised and passes the ionization edge of this
element.

Background approximation methods


Explanation of the The energy-loss spectrum corresponding to one image pixel is shown below
diagram (below) schematically. After recording an image at an energy loss ∆E with a slit width
dE the gray value of the image pixel corresponds to the integrated intensity
S(∆E). The net signal SN is characteristic of a particular element and is
calculated by subtraction of the extrapolated background intensity from the
signal S(∆EMAX).
Schematic electron energy-
loss spectrum. For
calculating an element
distribution image, at least
two images at different
energy positions are
necessary. The resulting
image contains element-
specific information only.

5
2 window method The following methods are available for background extrapolation:
The 2 window method requires two images. One image is to be recorded at
an energy loss just below the ionization edge (∆EW1), the second one at the
maximum intensity of the ionization edge (∆EMAX). The net signal SN is
calculated via a pixel-by-pixel subtraction or multiplication of the two images.
The image at ∆EW1 can be multiplied by a factor to consider the decrease
in background intensity with increasing energy loss. This method can only
be applied under the assumption that the background intensity of all image
pixels is decreasing by the same factor.
Variations in the local specimen thickness, crystalline orientation or the
amount of elastic scattering in large angles due to local differences in the
chemical compound can result in a different background of every image

related topics
ESI, Analyze... 67
EFTEM • The ESI method

pixel. This can be taken into account by recording further background


images at slightly different energy values and performing the background
subtraction routine on every single image point.
3 window power law Use the 3 window power law, if the energy dependence of the background
intensity is undisturbed throughout a sufficient energy interval by, e. g.,
ionization edges at lower energy losses or by electron - electron interaction
in the low-loss region. Three images are needed: two below the edge (∆EW2
and ∆EW1) and one at maximum intensity (∆EMAX). The background below
the ionization edge is extrapolated pixel-by-pixel from the signals S(∆EW2)
and S(∆EW1) according to the power law A ∆E-r and subtracted from the
edge signal S(∆EMAX) to obtain the net element distribution. You may also
divide the edge signal by the background signal to get the jump ratio of the
ionization edge.
3 window exponential An exponential or linear decrease of the background intensity can
law sometimes prove to be useful. Both methods (3 window exponential law and
3 window linear law 3 window linear law) require two images below the ionization edge (∆EW2
and ∆EW1) and one at the maximum intensity of the ionization edge
(∆EMAX).
3 window white line An additional method is particularly suitable in case of ionization edges that
are shaped like a ‘white line’. The 3 window white line method works with
images at ∆EMAX situated directly on the white line and two images recorded
below and beyond the white line at ∆EW1 and ∆EWL, respectively. The
background is interpolated linearly. The so-called ‘white lines’ are ionization
edges which are sharply peaked at the ionization threshold (e. g., Fe L2,3,
Ca L2,3, Gd M4,5).
multi window The multi window methods result in the addition of three background-
corrected images. The images are typically recorded just below the
ionization threshold (∆EIO) and with the energy window at ∆EIO + dE and
∆EIO + 2dE (dE = slit width). Provided the slit width is large enough, most of
the ionization edge intensity will contribute to the element distribution image.
The functions for fitting the background intensity correspond to the functions
of the same name provided with the 3 window methods.
Required ESI images for the
different background Method required ESI images
6

approximation methods
2 window ∆EW1, ∆EMAX
3 window ∆EW2, ∆EW1, ∆EMAX
3 window white line ∆EW1, ∆EMAX, ∆EWL
multi window ∆EW2, ∆EW1, ∆EIO1, ∆EIO2, ∆EIOz
all possible windows ∆EW2, ∆EW1, ∆EIO1, ∆EIO2, ∆EIO3,
∆EMAX, ∆EWL
The ESI method

Meaning of the different


energy windows ESI image Meaning
∆EW2, ∆EW1 position of the 1st or 2nd window below the edge
(∆EW2 < ∆EW1 < ∆EIO ).
The images are used for extrapolation of the
background intensity.
∆EMAX position of maximum intensity of the ionization edge
with a width of the energy window dE = 15 eV
∆EWL position of the 2nd window beyond a white line
∆EIOi, i=1-3 positions of three energy windows beyond the
ionization edge used for the multi-window method

Before acquiring an ESI series


These are the important assumptions for a successful analysis of ESI-
series:
Position the energy slit Position the energy slit exactly, before recording a new ESI-series.
1) Set the energy loss to zero on the microscope.
2) Turn on the spectrum mode.
3) Adjust the desired slit width to define the energy window.
4) Place the energy slit with the zeroloss peak lying at the center of the
energy window.
5) Choose the desired energy window by adjusting the energy selection
slit width on the microscope.
6) Now return to the image mode.
Note For more detailed information, look up ‘Zero-Loss imaging’ in the instruction
manual of your microscope.

Energy resolution All images of an ESI-series are to be recorded with the same energy-slit
width.
Image intensity All images of an ESI-series are to be recorded using exactly the same
acquisition conditions. This means that neither the exposure time in the
camera control nor the illumination of the microscope are to be changed

7
during acquisition.
To display a 16-Bit image on a monitor a display-LUT is needed. The
display-LUT assigns the 216 gray values of the image to the 256 gray values
the monitor can display. If you use an automatic gain display, the display-
LUT of each image is different. Therefore, the absolute brightness of two 16-
bit images cannot be compared on the monitor. Please keep this in mind if
you check the images visually. The system, of course, uses the absolute
gray values for calculating the resulting energy loss spectrum.

How to define an input channel for ESI acquisition


It is assumed that you are using a slow-scan CCD-camera. There is at least
one valid input for the camera on the microscope. This input is properly
calibrated.
1) Select the Image > Set Input... command.
2) Select an input that is already defined for the camera on the
microscope.
3) Click the Duplicate Channel button.
EFTEM • The ESI method

" A new entry with the same settings will be added to the list of
available input channels. The name of the entry is ’Name of the
duplicated input + 1’.
4) Click the Configure Input button to define the properties of the input
channel.
5) Click the Info tab.
6) Enter the name of the input into the Channel field, e. g. ’ESI Acqusition’.
7) Select a suitable icon from the Symbol list. There are special icons for
EFTEM channels available.
Remote Control 8) Click the Magnification tab.
9) Choose your microscope - e. g., LEO 912 - from the Device list.
10) Select the On check box in the Remote group to switch on the remote
control.
" The Magnification list will become inactive.
" A Read button will appear next to the check box.
11) Click the Read button to check the remote control.
" The current magnification is read in via remote control.
12) If you get an error message because the remote control does not
respond:
Click the Set COM port... button and select another COM port from the
’LEO 912’ COM port list. You have to restart EsiVision to activate your
change.
Online shading 13) Click the Input tab to set the image acquisition parameters.
correction 14) Select the Offset check box in the Shading correction group to
automatically subtract the camera’s offset image during acquisition.
15) Select the Gain check box to automatically divide every acquired image
by the camera’s gain image.
16) Select the Display tab.
17) Select the Activate check box in the Automatic gain display group.
" The display-LUT for 16-bit images is now optimized for each
snapshot. Please keep in mind that due to the automatic gain
display, the absolute image intensity cannot be judged by the
appearance of the image on screen. To get an impression of the
8

absolute image intensity, add a palette bar to the image. To do so,


use the Image > Scale Bar > Properties... command. Select the
Palette bar check box.
Online histogram 18) Select the Online histogram check box to be able to supervise the gray-
value distribution during image acquisition.

" The histogram window will be automatically opened during image


acquisition.
" In addition, the average gray value of the image will be displayed.
" You can use the online histogram to optimize the offset and gain at
the camera.
The ESI method

Binning Mode 19) Select the Format tab to choose a suitable binning mode for ESI image
acquisition.
20) Select an image format that uses 2x2 binning from the Image format
list. This binning mode ensures an optimum sensitivity of the camera at
the cost of the spatial resolution.
21) Confirm these settings with OK.
22) Close the Set Input dialog box.
Define the input as 23) Use the EFTEM > Options... command.
standard camera for 24) Click the ESI tab.
ESI acquisition 25) Choose the defined input channel from the Camera > Preferred list.
26) Close the dialog box by clicking OK.

How to acquire an ESI-image series


You would like to create an element distribution image of iron.
General ESI settings 1) Use the EFTEM > Options... command to define general settings for
ESI acquisition.
" It is not necessary to set or check these options before every ESI
series acquisition.
2) Select the ESI tab in the EFTEM Options dialog box.
3) Select the Align with live mode check box in the Camera group.
Before you start the 4) Position the energy slit on the microscope.
ESI acquisition 5) Ensure that the first image buffers do not contain important images.
" 10 is the maximum number of images belonging to an ESI image
series (all possible window method including the high contrast
image (HCI image) and additional blacklevel correction).
2 is the minimum number of required image buffers (2 window
method without HCI and blacklevel correction).
Setting the acquisition 6) Use the EFTEM > ESI > Acquisition... command to set or check all
parameters acquisition parameters.
" The ESI Acquisition dialog box is opened.
" The first image buffer is activated. Be aware that the contents of the
image buffer will be deleted.

9
" The system switches to live mode.
Now you should expose the detector, i. e., depending on the
camera in use, put the TV adapter into the ray path or lift the final
screen. When using a LEO 912, the final screen and the camera
shutter will be controlled automatically.
" The energy loss on the microscope is automatically set to the
energy loss ∆EMAX, the maximum intensity of the currently selected
ionization edge.
7) Click the Periodic Table... button to choose a predefined set of
parameters linked with iron.
" The Element selection dialog box is opened. The dialog box
contains the complete periodic table of elements.
8) Click the Fe button and confirm with OK.
" The Element field displays the abbreviation of iron, Fe.
" The Scheme list offers three parameter sets. The most probable
one is activated (Fe-L3_Atlas).
related topics
ESI, Acquisition... 52
Position the energy slit 7
EFTEM • The ESI method

" The energy range of the displayed spectrum diagram changes to


500-900 eV.
9) Enter the actual energy slit width (in eV) in the Slit width field.
10) Choose the 3 window entry from the Method list.
" All required energy windows for applying the 3 window method are
displayed in the spectrum diagram.
11) Change the proposed energy values by clicking on the energy window
in the spectrum diagram and moving the diagram cursor with a
depressed mouse button to the desired energy.
" As soon as you click on the diagram, the energy loss on the
microscope will be also be set to the lowest energy-loss value.
Adjusting the exposure 12) Check image intensity of the ESI series, at least for the first and the last
time image of the series. To do so, click the green energy window in the
diagram to change the energy loss on the microscope. Check the
image intensity and the online histogram.
If the intensity is too low, enlarge the exposure time using the plus
button in the Camera Control. Do not enlarge the illumination aperture
because this may lead to a specimen drift. Never use an automatic
exposure time. The exposure time must be the same for each image of
the ESI-series.
13) Select the HCI check box and insert the desired energy for recording
the high contrast image, e. g., enter the value 0 to record an elastic-
filtered image.
Acquiring the ESI 14) Start the acquisition by clicking OK in the ESI Acquisition dialog box.
image series " The ESI image acquisition is completely automated. Message
boxes inform you on the ongoing procedure.
" You should not alter the camera settings in any way during
acquisition.
" For the 3 window method, the element Fe and the L3 edge, the
acquisition of the ESI-series will continue, e. g., with the following
messages announcing the serial number of the image and the
present energy window:
Acquiring Image 1: 718,5 eV
Acquiring Image 2: 690 eV
10

Acquiring Image 3: 660 eV


Acquiring HCI Image
" Depending on the selected HCI-energy loss, the intensity range of
the high contrast image can exceed the intensity range of the actual
ESI-series considerably. Consequently, you are prompted to adjust
the image brightness on the microscope.
15) Adjust the intensity of the HCI image and confirm the message with OK.
" The acquisition of the ESI image series is finished.
Position of the ESI " The sequence of images in the image buffers is fixed. They are
images in the image sorted according to their energy loss, starting with the lowest
buffers energy value in image buffer 1. The HCI image is always the first
image.
Name of the ESI images " The image buffers are named automatically so that the image title
consists of the element symbol (e. g., Fe), the symbol of the
ionization edge (e.g. L) and a serial number.
16) Use the EFTEM > ESI > Save series... command to save the ESI-
series on disk.
The Image EELS method

The Image EELS method


What is Image EELS?
Definition An Image EELS series consists of several images at different energy-loss
values. The Image EELS submenu provides functions for an automatic
recording of an Image EELS series acquired with a predetermined energy
increment.
Recommended energy- Because the acquisition of an image EELS series produces a large amount
loss range of data, the investigated energy range should usually be restricted to the
structure of interest in the spectrum, e. g., the energy region containing
particular ionization edges. For example, if the iron and nickel
concentrations of a specimen are investigated, an energy loss range of 660-
1140 eV covers the L-edges of both elements.
Application The Image EELS method is particularly suited for detecting very low element
concentrations inside arbitrarily-shaped specimen structures. You may also
create images showing chemical bonding.
Image EELS series can be utilized to generate spectra or element-
distribution images.
Spectra of arbitrarily- The spectra from an Image EELS series are calculated from user-defined
shaped regions image regions. The regions of interest can be of arbitrary shape and need
not be connected. For creating a spectrum, the arithmetical mean (of all gray
values of defined regions) is determined for each image of the series. The
mean gray value is assigned to the energy loss of the corresponding image.
The resulting energy losses and gray values are displayed as a spectrum.
All spectra-processing functions provided by the Graph menu can be
applied to the image EELS spectra afterwards.
Using the image EELS
method you can record a
sequence of energy-filtered
images and extract spectra
of arbitrarily-shaped regions

11

Element-distribution An ESI series can be easily extracted from an image EELS series. Use the
images electron energy-loss spectra to find the suitable energy positions before and
after the ionization edge of interest. You may combine a set of successive
images to improve the signal to noise ratio.

related topics
ESI, Load Series... 66
Image EELS, Acquisition... 78
Image EELS, Analyze... 91
Image EELS, ESI Mapping... 97
EFTEM • The Image EELS method

Before acquiring an image EELS series


These are the important assumptions for a successful analysis of image
EELS series:
Position of the energy Position the energy slit precisely before recording a new image EELS series.
slit 1) Set the energy loss to zero on the microscope.
2) Turn on the spectrum mode.
3) Adjust the desired slit width to define the energy window.
4) Place the energy slit with the zeroloss peak located at the center of the
energy window.
5) Choose the desired energy window by adjusting the energy selection
slit width on the microscope.
6) Return to the image-mode.
Note For more detailed information, look up ‘Zero-Loss imaging’ in the instruction
manual of your microscope.

Energy resolution All images of an image EELS series are to be recorded with the same
energy slit width. The slit width for an image EELS series should be rather
small in order to increase the energy resolution of the spectrum.
Image intensity All images of an image EELS series are to be recorded using exactly the
same acquisition conditions. This means that neither the exposure time in
the camera control nor the illumination of the microscope are to be changed
during the acquisition.
To display a 16-Bit image on a monitor, a display-LUT is needed. The
display-LUT assigns the 216 gray values of the image to the 256 gray values
the monitor can display. If you use an automatic gain display, the display-
LUT of each image is different. Therefore, the absolute brightness of two 16-
bit images cannot be compared on the monitor. Please keep this in mind if
you check the images visually. The system, of course, uses the absolute
gray values for analyzing the image.
Acquisition conditions All images of an image EELS series are to be recorded with the same
camera gain, i. e., you are not allowed to have the brightness and contrast
of the images automatically adjusted by the camera.
Online-Shading Be sure that shading effects are corrected. You can usually make use of the
12

correction online-shading correction provided by the input channel. To switch on the


online-shading correction, open the Image > Configure Input > Input tab.
Select both check boxes in the Shading correction group.
Clipping To decrease acquisition time, it is recommended to make use of the input’s
clipping function. Use the Image > Configure Input > Format tab to clip any
image pixels that extend outside the defined frame.
Increase the number of The maximum number of image buffers is usually restricted to 64. To
image buffers acquire an image EELS series it may be necessary to increase the number
of available image buffers. Use the Special > Preferences... command.
Activate the Image tab and enter the number of image buffers needed into
the Available image buffers field. The maximum number of image buffers is
200.
The Image EELS method

How to define an input channel for image EELS acquisition


It is assumed that there is at least one valid input for the camera on the
microscope. This input is properly calibrated.
The following step by step instructions describes only the input settings
relevant for image EELS acquisition.
1) Select the Image > Set Input... command.
2) Select an input that is already defined for the camera on the
microscope.
3) Click the Duplicate button.
" A new entry with the same settings will be added to the list of
available input channels. The name of the entry is ’Name of the
duplicated input + 1’.
4) Click the Configure... button to define the properties of the input
channel.
Remote Control 5) Click the Magnification tab to switch on the remote control.
6) Choose your microscope - e. g., LEO 912 - from the Device list.
7) Select the On check box in the Remote group.
" A Read button will appear next to the check box.
8) Click the Read button to check the remote control.
" The current magnification is read in via remote control.
Online shading 9) Click the Input tab to set the image acquisition parameters.
correction " The controls of this tab will depend on the type of framegrabber
and/or camera being used - significant divergence from what is
described here is thus possible.
10) Select the Shading correction > Offset check box in the Shading
correction group to automatically subtract the camera’s offset image
during acquisition.
11) Select the Gain check box to automatically divide every acquired image
by the camera’s gain image.
Online histogram 12) Select the Display tab.
13) Clear the Activate check box in the Automatic gain display group.
" When using automatic gain display, you may misjudge the actual

13
image intensities.
14) Select the Online histogram check box to be able to supervise the gray-
value distribution during image acquisition.

" The histogram will be automatically inserted during image


acquisition.
" In addition, the average gray value of the image will be displayed.
The percentage amount refers to the maximum-possible gray
value. The maximum-possible gray value will depend on the
camera.
EFTEM • The Image EELS method

" You can use the online histogram to optimize offset and gain at the
camera.
Binning 15) Select the Format tab to utilize the binning option of the camera.
Binning is used to combine the charge collected by several adjacent
CCD pixels, and is designed to reduce noise and improve the signal-
to-noise ratio. Keep in mind that the binning mode reduces the spatial
resolution of the CCD-camera. The XY-calibration of the input is still
valid when you use a binned mode.
16) From the Image format list select a 4x4 binning mode.
17) Confirm these alterations with OK.

How to acquire an image EELS series


You would like to investigate a specimen containing both iron and cobalt.
The energy-filtering microscope in use can be controlled by EsiVision via the
remote control.
General image EELS 1) Use the EFTEM > Options... command to define general settings for
settings image EELS acquisition.
" It is only necessary to set or check these options once and not
before every image EELS series.
2) Select the Image EELS tab in the EFTEM Options dialog box.
3) Select the Align with live mode check box in the Camera group.
Before you start the 4) Position the energy slit on the microscope.
image EELS 5) Position the specimen structure you want to investigate at the center of
acquisition the monitor or at the center of the final fluorescence screen.
6) Make sure that the image manager does not contain important images.
Setting the acquisition 7) Use the EFTEM > Image EELS > Acquisition... command to set or
parameters check all acquisition parameters.
" The Image EELS Acquisition dialog box is opened.
" The first image buffer is activated. Be aware that the contents of the
image buffer will be deleted.
" The system switches to the live mode.
" The energy loss on the microscope is automatically set to the
14

energy loss ∆EMAX, the maximum intensity of the currently selected


ionization edge.
" Now you should expose the detector, i. e., depending on the
camera in use, put the TV adapter into the ray path or raise the final
screen. When using a LEO 912, the final screen and the camera
shutter will be controlled automatically.
8) Click the Periodic Table... button to choose a predefined set of para-
meters linked with iron.
" The Element selection dialog box is opened. The dialog box
contains the complete periodic table of elements.
9) Click the Fe button and confirm with OK.
" The Element field displays the abbreviaton for iron: Fe.
" The Scheme list offers three parameter sets. The parameter set
you used last is activated.
" The spectrum diagram indicates the complete energy range of the
image EELS series by a green area.

related topics
Image EELS, Acquisition... 78
The Image EELS method

10) Enter the actual energy slit width (in eV) into the Slit width field.
11) Enter the desired interval between two successive images in the
Energy increment field. The energy increment may as well be smaller
than the energy slit width in order to smooth the resulting energy loss
spectrum.
12) Click the Element label... button to indicate the relevant ionization
edges of the two elements of interest - iron and cobalt.
" The Set element labels dialog box is opened - which provides you
with the periodic table of elements.
13) Click the Clear all button in the Set element labels dialog box to delete
element labels that have already been defined. Select the Fe and Co
buttons and confirm with OK.
" The ionization edges of iron and cobalt are indicated in the
spectrum diagram of the Image EELS Acquisition dialog box.
14) If necessary, change the proposed START and STOP values by
clicking on the corresponding energies in the spectrum diagram and
moving the diagram cursor (with a depressed mouse button) to the
energy desired.
" The current energy losses are displayed below the spectrum
diagram, e. g., START = 635.00 eV.
" To obtain an image EELS series for both elements you have to
increase the proposed STOP energy loss so that the cobalt L3
ionization edge is also included.
" The energy loss on the microscope will be also be changed
simultaneously.
" The number of images in the image EELS series (Frames required)
and the acquisition time for the whole series (Time required) are
immediately updated.
Adjusting the exposure 15) Check image intensity of the image EELS series, at least for the first
time and the last image of the series and on the ionization edge.
If the intensity is too low, enlarge the exposure time using the plus
button in the Camera Control. Do not enlarge the illumination aperture
because this may lead to a specimen drift. Never use an automatic
exposure time. The exposure time must be the same for each image of

15
the ESI-series.
16) Enter the energy loss of the two high contrast images (acquired before
and after recording the image EELS series) into the HCI at field.
" All images, including the HCI images, are acquired without
changing gain and offset at the camera or illumination on the
microscope. The energy loss of the high contrast image should
therefore be in the same energy range, i. e., do not use a zeroloss
image as high contrast image.
Acquiring the image 17) Begin acquisition by clicking on the OK button in the Image EELS
EELS series Acquisition dialog box.
Warning You should not alter the camera settings in any way during acquisition.

Memory check " Because acquisition time is considerable, the system will auto-
matically check whether the image EELS series can be finished
successfully. In cases where present storage capacity would be
exceeded by the total number of images required, the acquisition
procedure will be aborted with an error message. The maximum
possible number of images will be indicated to you.
EFTEM • The Parallel EELS method

Number of image buffers " The system reserves all required image buffers. If there are not
enough image buffers available, you will get an error message. You
may either increase the number of available image buffers or
increase the energy increment.
To increase the number of image buffers, open the Preferences
dialog box via [F8]. Activate the Image tab and enter the required
number of image buffers in the Available image buffers field.
" The image EELS acquisition is completely automated. Message
boxes inform you on the ongoing procedure and enable you to
terminate the acquisition at any time by clicking on the Cancel
button. The energy-loss value of the frame being currently recorded
is displayed in the message box.

Position of the images in " After the image EELS acquisition, the HCI image recorded first is
the image buffers located in image buffer No 1, the HCI image recorded last in image
buffer No 2. The other images of the series are written in the image
buffers beginning at No 3. They are sorted according to their
energy-loss values, beginning with the lowest energy.
Image names " The image buffers are named automatically so that the image title
(e. g. CZFeL001) consists of the initials of the operator name (e. g.
CZ), the element symbol (e. g., Fe), the symbol of the ionization
edge (e. g., L) and a consecutive number using an alphanumerical
notation. The HCI images are indicated by the letter ‘Z’ (e. g.,
CZFeLZ01). The operator name is read out from the microscope’s
sheet film camera.

The Parallel EELS method


16

How to define an input channel for parallel EELS


It is assumed that there is at least one valid input for the camera on the
microscope. This input is properly calibrated.
The only input settings described are those recommended for parallel EELS
acquisition.
1) Select the Image > Set Input... command.
2) Select an input that is already defined for the camera on the
microscope.
3) Click the Duplicate button.
" A new entry with the same settings will be added to the list of
available input channels. The name of the entry is ’Name of the
duplicated input + 1’.
4) Click the Configure... button to define the properties of the input
channel.
Remote Control 5) Click the Magnification tab to switch on the remote control.
6) Choose your microscope - e. g., LEO 912 - from the Device list.
The Parallel EELS method

7) Select the On check box in the Remote group.


" A Read button will appear next to the check box.
8) Click the Read button to check the remote control.
" The current magnification is read in via remote control.
Online shading 9) Click the Input tab to set the image acquisition parameters.
correction " The controls of this tab will depend on the type of framegrabber
and/or camera being used - significant divergence from what is
described here is thus possible.
10) Select the Shading correction > Offset check box in the Shading
correction group to automatically subtract the camera’s offset image
during acquisition.
11) Select the Gain check box to automatically divide every acquired image
by the camera’s gain image.
Binning 12) Select the Format tab to switch off the camera’s binning option. From
the Image format list select a 1x1 binning mode to get the optimum
energy resolution.
13) Confirm these alterations with OK.

How to acquire a parallel EELS


Assumptions You would like to acquire a spectrum of the iron L3 edge. There is calibration
data available for the spectrum magnification used. The energy-filtering
microscope in use can be controlled by EsiVision via the remote control.
Note Please keep in mind that the zeroloss is needed for all quantification
methods. In this case use the EFTEM > Parallel EELS > Wide Range
Acquisition... command to acquire an energy loss spectrum including the
zeroloss peak.
General parallel EELS 1) Use the EFTEM > Options... command to define general settings for
settings parallel EELS acquisition.
" It is only necessary to set or check these options once, not before
every parallel EELS acquisition.
2) Select the Parallel EELS tab in the EFTEM Options dialog box.
3) Select the Align with live mode check box in the Camera group.

17
Before you use this 4) Use the Image > Set Input... command to select a suitable input
command channel for parallel EELS acquisition, if not defined in the Parallel
EELS tab of the EFTEM Options dialog box.
5) Switch on the remote control.
6) Activate an empty spectrum buffer.
7) Activate an empty image buffer.
Setting the acquisition 8) Use a small filter entrance diaphragm to select the specimen area you
parameters on the want to investigate or use the spot / Diff. mode.
microscope 9) To get an optimum energy resolution, use a high magnification, at least
x25,000. The object under investigation should fill the whole area of the
diaphragm.
It is not necessary to switch to the spectrum mode because EsiVIsion
will automatically switch on the spectrum mode when acquiring the
parallel EELS.

related topics
Parallel EELS, Wide Range Acquisition... 110
Remote Control 3
EFTEM • The Parallel EELS method

Setting the acquisition 10) Use the EFTEM > Parallel EELS, Acquisition... command to set or
parameters check all acquisition parameters.
Warning It is not possible to acquire a parallel EELS if no calibration data for the
energy loss dispersion is available. The calibration data depends on the
spectrum magnification, the high voltage and the input channel.

" The Parallel EELS Acquisition dialog box is opened.


" The system switches to the live mode and the camera control is
opened.
" The following settings on the microscope are changed auto-
matically by the remote control:
The energy loss and the spectrum magnification are set in
correspondence with the values of the last parallel EELS.
11) Use the Spectrum magnification slider to enter the desired
magnification of the spectrum.
" The spectrum magnification on the microscope is updated via
remote control.
12) Select the desired element from the Element list or from the periodic
table.
13) Use the EELS image to visually adjust intensity and/or exposure time.
Acquiring the parallel 14) Click OK to start the acquisition of the parallel EELS.
EELS " The following dialog box is opened.
18

" The averaged spectrum is displayed in the spectrum document.


" If the Time integration check box is selected, an averaged linescan
is combined with a time integration. Snapshots will be taken
successively and all the spectra recorded will be averaged.
15) Click the Stop button when you are satisfied with the spectrum.
" The Stop button changes its functionality to Start.
" The OK and Cancel buttons become available.
16) Click OK to finish the acquisition.
" The resulting parallel spectrum is written into the active image
buffer.
" The active image buffer contains the EELS image with the analyzed
ROI in the image overlay.

related topics
Parallel EELS, Calibration... 118
Parallel EELS, Acquisition... 104
Electron Energy Loss Spectra

Electron Energy Loss Spectra


Spectrum Document For displaying and processing of spectra, i. e., one-dimensional data, the
functionality of EsiVision was supplemented by an additional document: the
graph or spectrum document. The spectrum document is always available.
It is located in the document area and contains special buttons for setting
the spectrum display.
Spectrum Buffer Box In the Image Manager there is a second
toolbar referring only to spectrum
documents. The visible toolbar is linked to
the type of the active document. The
image buffer box is displayed when an
image document is active. If a spectrum
document is active the spectrum buffer box
is shown.
Click in the spectrum document to change
from image processing operations to
spectra processing operations.
The elements Src (Source), Dest
(Destination) and Src2 (Source 2) of the
operands box now refer to the
corresponding spectrum buffer. The
destination spectrum buffer is used for all
spectrum operating functions creating a
new spectrum. The Source2 spectrum
buffer is needed for spectrum operations
with two source spectra, e. g. for the
addition of two spectra. The elements of
the icon area (Trash, Disk, Printer) delete,
save and print the spectra which you
drag&drop onto one of the icons. The icons
Mask and Drawer have no function in this
context.

19
The Spectrum Document
To display a spectrum To display a spectrum, activate a spectrum document. Select the spectrum
buffer containing the desired spectrum. The whole spectrum in the active
spectrum buffer is displayed as a diagram in the spectrum document.
To measure Use the mouse to determine the exact coordinates of a plotted data point.
individual Bring the cursor to the diagram’s area. A black line cursor appears, which
spectrum can be moved by moving the mouse sideways. The exact energy loss
points channel and Y-value are given in the status bar of the spectrum document.
You will also be given the next ionization edge for electron energy-loss
spectra.
Information in the status bar
of the spectrum document
EFTEM • Electron Energy Loss Spectra

To change the Click left mouse button in the spectrums diagram. The mouse cursor
XY-scaling in changes its shape to a vertical double-headed arrow. Move the cursor up
the diagram and down to stretch or compress the Y-scaling. Move the cursor to the right
or to the left to stretch or compress the X-scaling.
You may also change the scaling of the spectrum using the buttons of the
Graphs button bar.

Scroll bars You may use the scroll bars located at the right side and at the bottom of the
diagram to shift the spectrum along the axes without a change in the axis
20

scale.
Graphs Button Bar The button bar at the top of the spectrum document is used to change the
displayed X and Y range and to edit spectrum overlays.
X Scale The different buttons are combined into functional groups. The first sets the
scale for the X axis of the spectrum.
Zoom In Click this button to decrease the displayed X range, i. e., to stretch the
spectrum in the X direction.
Zoom Out Click this button to increase the displayed X range, i. e., to compress the
spectrum in the X direction.
To scale the X range up or down, keep the corresponding button pressed.
The command will be repeated automatically at short intervals. While
working with these two scaling operations, the initial X value remains
unchanged.
Scale X Click this button to enlarge any X segment of the displayed spectrum to full
axis size. In the desired spectrum, click on the borders of the desired X value
segment (X-range). The first clicking produces a blue diagram cursor, the
second a green one. Both diagram cursors can be moved using the mouse,
Electron Energy Loss Spectra

keeping the mouse button pressed. The current X position is continuously


shown on the status bar. Rightclick to accept the new scale. As long as the
button remains depressed, the diagram cursors will remain visible and can
be moved using the mouse cursor once again.
Y Scale The second group sets the scale of the Y axis of the spectrum.
Zoom Up Click this button to decrease the displayed Y range, i. e., to stretch the
spectrum in the Y direction.
Zoom Down Click this button to increase the displayed Y range, i. e., to compress the
spectrum in the Y direction.
To scale the Y range up or down, keep the corresponding button pressed.
The command will be repeated automatically at short intervals.
While working with these two scaling operations, the initial Y value remains
unchanged.
Scale Y Click this button to enlarge any Y segment of the displayed spectrum to full
axis size. In the displayed spectrum, click on the borders of the desired
Y value segment (Y-range). The first clicking produces a blue diagram
cursor, the second a green one. Both diagram cursors can be moved with
the depressed mouse button. The current Y position is continuously shown
in the status bar. To accept the new scale, press the right mouse button. As
long as the button remains depressed, the diagram cursors will remain
visible and can be moved by the mouse cursor once again.
Max Y Click this button to stretch the Y range automatically from the minimum to
the maximum Y value of the displayed spectrum segment.
Auto. Max Y Click this button to automatically rescale the displayed Y-range of the
spectrum to the maximum Y value. The scaling is automatically updated
when moving the spectrum in the X-direction by using the scroll bars of the
spectrum document.
Define Display Click this button to zoom up a rectangular area of the current spectrum
Area document. Clicking the button opens the Define Display Area dialog box.
Click the Set button to draw a rectangle into the spectrum. Use the mouse
to resize and move the rectangle to the interesting part of the spectrum.
Click the right mouse button to return to the Define Display Area dialog box.
Alternatively, you may enter the absolute X and Y-limits of the spectrum

21
area in question into the fields of the dialog box. Click the OK button to zoom
the selected area of the spectrum to the whole spectrum window.
Default size Click this button to rescale the spectrum and show the whole spectrum that
the current spectrum buffer contains.
Log X Click this button to change the X-axis scale type from linear to logarithmic
scale.
Log Y Click this button to change the Y-axis scale type from linear to logarithmic
scale.
Delete All Labels Click this button to delete all text labels in the current spectrum.

Window Mode When this button is clicked, all spectrum-processing operations that produce
a new spectrum will affect only the displayed part of the spectrum. In this
case, the result comprises only the X range selected before and the new
spectrum will consist of the corresponding number of channels only.
EFTEM • Electron Energy Loss Spectra

Overlay Functions The remaining elements of the button bar refer to overlay functions. The
display of additional spectra in the spectrum document is termed overlay.
Use the Graph > Overlay Selection... command to define a spectrum as an
overlay. If one or more overlays have been loaded, they are all shown with
the actual spectrum at the same time.
Overlay Mode If this switch is set, the scroll bars and all buttons of the button bar
concerning the axis scale apply to the selected overlay only. This function is
for the optical adjustment of the overlay to the original spectrum for
purposes of comparison. For example, this function may be useful in cases
where one of the spectra has an X or Y offset. After clicking on the Overlay
Mode button, the scale markings of the diagram remain those that are valid
for the original spectrum. However, the Log X and Log Y buttons refer to the
displayed spectrum in its entirety.
In case there are several overlays, use this list to select the active overlay.
The active overlay is affected by the overlay operations explained below.
The color of the spectrum - in brackets following the spectrum name - will be
allocated to the corresponding overlay.
Fit Click this button to adjust the Y scale of the overlay to the scale of the actual
spectrum. This function is a quick and convenient method for the direct
comparison of two spectra whose Y ranges are very different. The highest
Y value of the overlay is adjusted to the maximum Y value of the spectrum
in the displayed X range. You should keep in mind that after clicking this
button the labels of the Y axis refer only to the actual spectrum and no longer
refer to the overlay.

Printing EELS spectra


Use the File > Print... command to print currently-loaded EELS spectra.

You may also As a shortcut, you can use the printer icon in the icon area of the Image
Manager for dragging & dropping.
Spectra and images How to print images and spectra simultaneously.
1) Activate the image document.
2) Use the File > Print... command.
22

" The Print Image dialog box provides you with several general page
layouts.
3) To print spectra and images simultaneously, choose the Multiple
Images/Graphs entry from the Page layout list.
4) To assign images and spectra to the relevant frames, click the Layout...
button.
" The Define Page Layout dialog box is opened.
5) Activate the Multiple Images tab.
" The Preview group displays the predefined pagelayout.
" There is an additional list at the right side of the dialog box. The
Documents list displays all available image and spectrum buffers.
6) Click on the plus sign to display the image buffers in the Documents list.
" When an image buffer contains an image, the image name will be
given.
7) Use the left mouse button to drag the desired image onto one of the
frames.
Electron Energy Loss Spectra

" The image buffer number is now connected with the selected
frame, i. e., when printing, the selected image will be printed at the
selected position.
8) Repeat the last two steps to assign up to six images or spectra to the
frames.
9) Click the Print... button.
" The system returns to the Print Image dialog box.
10) Click OK to start the printing task.
What will happen... • The selected images and spectra are fit into the frames.
• Note that only the spectrum range currently displayed in the spectrum
diagram is printed.
• In this mode the spectra are always printed without the additional
spectra information.
To print images and spectra
simultaneously, choose the
Multiple Images/Graphs
entry from the Page layout
list.

You may, of course, use this


feature to print out multiple
spectra onto one page.

23
EFTEM • Electron Energy Loss Spectra

Assign images and spectra


by a simple drag&drop
operation from the
Documents list to the page
preview.

Printing spectra To print the spectrum of the active spectrum buffer, activate the spectrum
document and use the File > Print... command. You may print the spectrum
information together with the spectrum.
What will happen... • Note that only the spectrum range currently displayed in the spectrum
diagram is printed.
• The page layout of printed spectra is preset and cannot be influenced
by the File > Define Page Layout... command.
Use the Print Graph dialog
box to print out single
spectra along with spectrum
information.
24

Print output Choose the Graph only option to print only the spectrum in the active image
buffer.
Choose the With general info data option to print the information from the
General tab of the Graph Information dialog box below the spectrum. The
general info data comprises the spectrum range, the initial and final values,
Electron Energy Loss Spectra

the number of channels, the data type and a user-defined comment.


Choose the With all available info data option to print the information of
additional tabs (of the Graph Information dialog box) onto a second page.
Using the EsiVision For printing out spectra, you may just as well use the report generator
Report Generator integrated into EsiVison. The EsiVision report generator is for creating
professional, multipage reports. The layout possibilities it offers are of the
highest quality.
How to print spectra via the report generator.
1) Load the desired spectra into the spectrum buffer box.
2) Change the display of the spectrum so that the interesting spectrum
structure is clearly visible. For example, you may switch from a linear
to a logarithmic scaling.
3) Use the File > Report > New... command.
" The New Report > General tab provides you with several
predefined page templates.
4) Select the Normal template.
5) Click OK to create a new blank report.
" The report is opened in its own document window. Additional button
bars are added at the right side of the graphical user interface.
6) In the Report Objects button bar, click the Graph button.
7) Define a rectangular spectrum object on the report page. The size of
the spectrum object determines the sizes of the displayed spectrum.
You may change the size and position of the spectrum any time.
" If more than one spectrum is loaded, the Avalable Graphs dialog
box lists all loaded spectra. Select the desired spectrum from the
list and confirm with OK.
8) Use the File > Report > Save As... command to save the report.
Use the File > Print... command to print out the report.

Graph Information
Use this dialog box to obtain or enter detailed information on the active electron energy-loss spectrum.

25
Definition The Graph Information dialog box contains additional information that is
saved along with the spectrum. The general spectrum information includes
spectrum calibration data, the spectrum name and your comments on the
spectrum. The EELS Data and Microscope tabs contain microscope
information that is transferred from the microscope during the acquisition.
Displaying the Doubleclick on any spectrum buffer within the Image Manager to view
Spectrum Information information on that spectrum - you can also alter this information.
EFTEM • Electron Energy Loss Spectra

Graph Information, General


Available The General tab is available for all graphs and spectra created with the
EsiVision software.
Creating graphs is not restricted to the acquisition of energy loss spectra.
You may, e. g., also measure an intensity profile on an image by using the
command Graph > Measure > Horizontal Intensity. These types of graphs
also have a Graph Information dialog box containing only the General tab.

Title In the Title field, a name for the currently-active spectrum buffer is proposed.
If you enter a new title into the field, the name of the corresponding spectrum
buffer will be changed accordingly.
26

Date The Date field will be automatically read in during the spectrum acquisition.
Graph data The Graph data group provides some useful information on the recorded
spectrum. The information given in this group are read in automatically
during acquisition.
Electron Energy Loss Spectra

Graph Information, EELS Data

Material In the Material or Preparation fields, you can enter specific information
Preparation concerning the analyzed material and the preparation method used for the
specimen analyzed. Entries into these fields are optional.
Microscope The Microscope, Magnification and High voltage fields are automatically
Magnification read in during the spectrum acquisition.
High voltage
Dose rate The default value of the parameters Dose rate, Dose and Specimen Area is
Dose 0.0. The default value of the Specimen Temperature is 293.0 K. You may
Specimen area modify the information if required.

27
Acquisition time The Acquisition time is read out by the remote control. The acquisition time
is the total time needed for the acquisition of a serial spectrum or the total
exposure time for the acquisition of a parallel EELS or wide range parallel
EELS spectrum.
EFTEM • Electron Energy Loss Spectra

Graph Information, Microscope


The Microscope tab contains all parameters referring to the microscope in
use. Some of the parameters are automatically read in by the remote
control. If necessary, you can fill in the remaining values via keyboard or by
selecting the suitable item from the pick lists.

Cathode The Cathode (Tungsten) field value cannot be read in by the remote control.
The predefined value is given in brackets.
Type The Type (Photomultiplier) of the detector and the Scintillator material (-)
Scintillator cannot be read in by the remote control. The predefined values are given in
brackets.
28

EM modes The Illumination mode, Magnification mode, Image mode, BF/DF-mode and
Spectrum mode can be read in automatically. The Detection mode (-)
cannot be read in by the remote control. The predefined value is given in
brackets.
Spectrum mag. The Spectrum mag. can be read in automatically. The Detection area (-)
Detection area cannot be read in by the remote control. The predefined value is given in
brackets.
Apertures The diameters of the different apertures cannot be read in by the remote
control. You have to enter the diameters of the currently set Condensor,
Illumination, Objective, Selector and Spectrum apertures in µm via
keyboard.
Focus The Focus and Defocus parameters cannot be read in automatically by the
Defocus remote control.
Electron Energy Loss Spectra

Graph Information, Stage

X position The Stage tab provides information on the active stage position.
Y position If a stage control interface is available, the listed values will be read in
Z position automatically while recording a spectrum. Otherwise, you have to enter the
Tilt present adjustment via keyboard.
Rotation

29
EFTEM • Electron Energy Loss Spectra

Image Information
Use this dialog box to obtain or enter detailed information on an EFTEM image.

Available The EFTEM Data tab is only added for images acquired by the EFTEM >
ESI > Acquisition... or the EFTEM > Image EELS > Acquisition... command.
The EFTEM Data tab is not added to images acquired by the Image >
Snapshot command.
Definition The Image Information dialog box contains additional image information that
is saved along with the image. Image information includes, among other
things, image calibration data, channel settings, the image name and your
comments on the image. All additional image information can only be saved
using the TIFF format.
How to... There are several ways to open the Image Information dialog box. For
example, use the [Alt+Enter] keystroke to view information on the image
within the active image buffer.
EFTEM Data The EFTEM Data tab is automatically added to the image information of all
images acquired using the EFTEM module.

Image Information, EFTEM Data


Use the EFTEM Data tab (of the Image Information dialog box) to display
information on the energy-filtered image in the active image buffer.
30
The Graph menu

The Graph menu


The Graph menu contains some commands especially developed for
spectrum processing. Theses commands are described in the following.

Labels, Set...
Use the Graph > Labels > Set... command to add and position annotations to the active graph.

Before you use Adjust the display:


the command Change the display of the graph so that the interesting region of the graph
is completely displayed in the graph document.

Label text In the Label text field, enter the text for the annotation. The amount of text is
limited to 116 signs.
Click the Set button to position the text frame in the graph document. Note
that the text frame can only be positioned in the visible part of the graph. You
cannot scroll or zoom the graph while you set the labels.
Anchor text Select the Anchor text check box to position the text frame at a fixed position
of the graph document. The position of the text frame does not depend on
the currently displayed part or zoom factor of the graph. Use this option for

31
general descriptive text referring to the whole graph.
Clear the Anchor text check box to position the text frame at a special
position of the graph. When you shift the graph or change the zoom factor,
the position of the text frame will change accordingly.
Centered text Use the Centered text check box to format the text in the text frame. When
the dialog box is opened, the text frame is indicated in the graph document
by a dotted rectangle.
Clear the Centered text check box to left-align the text in the text frame.
Select the check box to center the text.
Data position Use the features in the Data position group to add a label to a special X-
position of the graph.
Position In the Position field, enter the X-position that belongs to the label. The
dimension of the field depends on the current graph dimension. Click the Set
button to find the X-position interactively. A dashed line connects text frame
and the current X-position. Left-click to confirm the setting and transfer the

related topics
The Spectrum Document 19
EFTEM • Set Split Gain..

value into the Position field.


To move the text label itself, click the Set button next to the Label text field
or click the Align button.
Align Click the Align button to update the position of the text frame. The text will
be shifted horizontally directly above the current X-value in the Position field.
To move the text frame in the vertical direction, click the Set button next to
the Label text field.
Draw line Select the Draw line check box to connect text frame and the X-position by
a line.
Draw arrow Select the Draw arrow check box to connect text frame and the X-position
by an arrow.

Set Split Gain..


Use the Graph > Set Split Gain... command to display a wide range electron energy loss spectrum in a
linear scale. You divide the spectrum into different energy loss regions. Increasing the gain factor of the
high energy loss region enables the simultaneous display of the whole energy loss range.

Setting more than one Each time you use the command, you define one split position. You may call
split position the command several times to divide the spectrum into more than one
energy loss region. In this case you should start with the lowest energy loss,
i. e. the first split position.
Note • The split positions and gain factors are integral parts of the spectrum.
They can only be deleted or modified by using the Modify Split Gain...
command.
• You can split the gain factor only for the spectrum in the active
spectrum buffer. Overlay spectra are not affected.
• After setting a split gain do not use the Max Y button in the spectrum
document to stretch the displayed Y range.
The sample aluminium
energy loss spectrum
simultaneously shows the
plasmon loss region with the
zero and the L-ionization
32

edge. This is only possible


because the intensity of the
higher energy losses are
increased by the factor 200.
Modify Split Gain...

Split position In the Split position field, enter the energy loss where there spectrum should
be divided. Click the Set button to define the desired energy loss position
interactively.
Gain factor Use the arrow button next to the Gain factor field to increase the gain factor
of all energy losses greater than the split position. All intensity values are
multiplied by the selected gain factor. The gain factor is indicated in the
spectrum document.
The minimum gain factor is 2. Possible gain factors are 2, 5, 10, 20, 50, 100
and so forth.
The display of the spectrum is automatically updated when changing the
gain factor.

Modify Split Gain...


Use the Graph > Modify Split Gain... command to edit split positions defined by the Set Split Gain...
command.

Before you use Change the display of the spectrum so that all split positions you would like
the command to modify are visible. For example, click the Default size button in the
spectrum document to display the whole spectrum.

33

Splits The Splits list offers all split positions that are defined for the spectrum.
Choose the split position you would like to modify. All split positions that are
currently not displayed in the spectrum document are grayed.
Split position In the Split position field, the energy loss of the currently selected split
position is shown. Click the Set button to move the split position to another
energy loss.
Gain factor The Gain factor field shows the current gain factor of the selected split
position. Use the arrow button next to the Gain factor field to change the gain
factor of all energy losses greater than the split position.
The display of the spectrum is automatically updated when changing the
gain factor.
Delete Click the Delete button to delete the selected split position. Be sure to adapt
the gain factors of the following split position.
EFTEM • Zeroloss Calibration...

Delete All Click the Delete All button to remove all split positions from the spectrum.

Zeroloss Calibration...
Use the Graph > Calibration > Zeroloss Calibration... command to fix the origin of the energy-loss axis by
identifying the zeroloss channel.

What happens After using the command, the displayed range of the spectrum is auto-
matically changed to [-10 eV - +10 eV]. EsiVision will automatically look for
the first local maximum in the spectrum. A line cursor appears at the
proposed position of the zeroloss.

Zeroloss The Zeroloss field shows the energy loss of the cursor position. Click OK to
set this energy loss to zero. The energy axis of the spectrum will be shifted
by this energy loss.
FWHM The FWHM field shows the Full Width of Half Maximum of the zeroloss peak.
The FWHM value is calculated from the spectrum. Use this value as a
measure for the energy resolution. If the spectrum is not properly zeroloss
calibrated, the value calculated for the FWHM is also wrong.
34
Integration

The calculated value for the


FWHM depends on the
position of the zeroloss. If
the zeroloss position is not
properly set, the FWHM is
wrong as well.

Set Click the Set button to modify the actual zeroloss in the spectrum. Move the
line cursor onto the maximum in the zeroloss peak. The intensity value
indicated on the status bar may help. Leftclick if you have positioned the
energy cursor correctly.
OK Click OK to confirm the settings. The scale of the energy axis will be shifted
by the new zeroloss value. The result is put into the destination spectrum
buffer.

35
Integration
Use the Graph > Measure > Integration command to calculate the integral of a specific spectrum range.
The spectrum range can be defined interactively.

Before you use • Adjust the display:


the command Change the display of the spectrum so that the interesting region of the
spectrum is completely displayed in the spectrum document.
• Correct the background:
If you want to calculate the integral intensity below a specific ionization
edge, use the Graph > Calculation > Background Subtraction...
command. Use the background corrected spectrum as an input for the
Integration command.
What happens 1) After using the command, the mouse jumps into the spectrum
document.
2) Define the lower and upper energy loss of the integration region by
clicking the left mouse button.
related topics
The Spectrum Document 19
EFTEM • Background Subtraction...

" The limits of the integration region are indicated as labels in the
spectrum document. Use the Graph > Labels > Modify... command
to modify or delete the measuring labels.
A measuring sheet containing the integration limits and the
resulting integral intensity is created.
3) Click the right mouse button to finish the measurement (or repeat the
last step to measure another integral intensity).
Accumulate measuring It is possible to accumulate measurements in one output sheet. To do so,
results click on the header of the first column and use the Graph > Measure >
Integration command afterwards. The results are then appended to the
active measurement sheet.
The iron L-ionization edge
was integrated. The
background was subtracted
by using the Graph >
Calculation > Background
Subtraction... command.
36

Background Subtraction...
Use the Graph > Calculation > Background Subtraction... command to subtract the unspecific
background under an ionization edge in an electron energy loss spectrum. The background intensity is
calculated from the spectrum progression before the interesting ionization edge.

Before you use • Adjust the display:


the command Change the display of the spectrum so that the interesting ionization
edge is clearly visible. For calculation, the background of a suitable
energy range before the ionization edge must also be displayed. Adjust
the display so that the ionization edge is approximately located in the
middle of the graph document.
Make sure that no preceding or overlapping ionization edges or other
structures are located within the fitting region.
Background Subtraction...

• Switch to a linear spectrum presentation:


The background subtraction function is not working for logarithmic
spectrum presentation.
What happens After using the command, the background is immediately calculated and
extrapolated by fitting the spectrum before the ionization edge. The energy
range of the spectrum that is used for the background fit is determined by a
lower and upper limit. The proposed lower limit is the lowest energy loss that
is displayed in the graph document. The proposed upper limit is the center
of the displayed spectrum range.
The calculated background curve and the lower and upper limits are drawn
into the graph document.
Use the command in the dialog box to adjust the limits and to change the
background fitting method.
The background below the
cobalt L-ionization-edge is
extrapolated from the
background curve before
the edge. The background is
colored in this example.
The upper and lower limits
of the energy range used to
fit the background are
indicated by line cursors.

37
EFTEM • Background Subtraction...

After subtracting the


background the integral
intensity under the
ionization edge can be
calculated: Use the Graph >
Measure > Integration
command.
Keep in mind that the
intensity value of the low
loss region can become
negative. To restrict the
resulting spectrum to the
displayed energy losses,
click the Window Mode
button in the graph
document button bar before
you call the command.

Use the Background


subtraction dialog box to set
the upper and lower limits
and to change the fitting
method.
38

Assumed function From the Assumed function list, choose the suitable fitting method. After
choosing a new fitting method the background is automatically recalculated
from the spectrum values and indicated in the spectrum document. The
dialog box shows the fitting formula and the computed fitting parameters for
the current spectrum.
The following table gives an overview of the available fitting method. IB is the
background intensity and ∆E the energy loss, A and r are variable
parameters that are calculated during the background fit.
Fitting method Formular Description
Linear I B = A ⋅ ∆E + r The background is approximated by a line.

Power I B = A ⋅ ( ∆E ) r A power law is used. In case there are no overlapping


edges before the interesting ionization edge, the
power law should provide the best results.
Background Subtraction...

Fitting method Formular Description


Exponential r ⋅ ∆E An exponential law ist used.
IB = A ⋅ e
2 point (linear) I B = A ⋅ ∆E + r The line is defined by the two intensities at the
position of the lower and upper energy loss. The
curve progression is not considered. Use this option
to compute background below a white line.
Reference Use the Reference group to define the energy range that is used for the
background fit. The energy range is defined by the lower and the upper limit.
Set Lower Click the Set Lower button to change the position of the first limit. Move the
line cursor to the desired energy loss and click the left mouse button to
recalculate the background and return to the dialog box.
Set Upper Click on the Set Upper button to change the position of the second limit. The
upper limit should be set directly before the interesting ionization edge.
Move the line cursor to the desired energy loss and click the left mouse
button to recalculate the background and return to the dialog box.

39
EFTEM • Fourier-Log Deconvolution

Fourier-Log Deconvolution
Use the Graph > Calculation > Fourier-Log Deconvolution command to remove plural scattering from the
spectrum by the Fourier-Log method. This method can only be applied when the zeroloss is included in
the spectrum. Use the command as preparation before calculating the element ratio.

Before you use Calibrate the zeroloss:


the command Check the position of the zeroloss. If necessary, use the Graph > Calibration
> Zero-Loss Calibration command to adjust the position of the zeroloss.
What happens The resulting spectrum is written into the destination spectrum buffer.
After a Fourier-log
deconvolution (grayed
spectrum) the zeroloss and
peaks by multiple scattering
are removed from the
sample boron spectrum.
Use the Graph > Overlay
Selection... command to
compare the original
spectrum with the
deconvoluted one.
40
The EFTEM menu

The EFTEM menu


The commands of the
EFTEM menu can be
subdivided into several
groups.

The EFTEM menu will become available after installing the EFTEM module.
EFTEM button bar The EFTEM acquisition commands can also be initiated using the EFTEM
button bar:

ESI Acquisition, 52
Image EELS Acquisition, 78
Parallel EELS Acquisition, 104
Wide Range Parallel EELS Acquistion, 110

How to... If your current EsiVision configuration does not include the EFTEM menu,
you’ll need to complete the following steps to activate the module:
1) Open the Special menu.
2) Select the Add-In Manager... command.
"The Add-In Manager dialog box will be opened.
3) Select the EFTEM check box from the list of Available add-ins.

41
4) Click the Close button.
How to... How to turn ‘on’ the EFTEM button bar - if it’s not already displayed:
1) Open the Special menu.
2) Select the Edit Button Bars... command.
"The Edit Button Bars dialog box will be opened.
3) Select the EFTEM check box within the Button bars list.
4) Click OK to close the dialog box.

EELS Atlas, Load Reference Spectra...


Use this command to load reference spectra of the EELS atlas.

Definition The EELS atlas represents a spectrum library whose spectra are at your
disposal chiefly for comparative purposes. The collection includes spectra,
frequently more than one, of almost all elements of the periodic table.
EFTEM • The EFTEM menu

How to use the EELS The spectra of the EELS atlas can be used as reference spectra for the
atlas position and shape of the various ionization edges and can be
superimposed on actual spectra as overlays. You may also display the
spectra in all acquisition dialog boxes for setting the optimum energy loss
windows.
EELS-Atlas-Selection After calling the Load Reference Spectra... command, the EELS-Atlas-
Selection dialog box appears.
The EELS atlas includes
sample spectra of almost all
elements. Click on the
desired elements and click
the Load button to open the
sample spectra.

In the shown example


aluminium has been
selected.

Periodic Table of In the dialog box you will find the complete periodic table of elements. Each
Elements element is represented by its own button. The periodic table offers the
following information:
• Ionization edges below 2500 eV
In addition to the chemical symbol and the atomic number of the
42

elements, you can find the symbol of the ionization edges occurring
within an energy region of 0 - 2500 eV at the button of each switch. If
there are two ionization edges in this energy region, both are listed, the
higher energy at the left, the lower at the right.
The ionization edges in the EELS-Atlas-Selection dialog box are listed
up to 2500 eV, whereas the spectra of the EELS-Atlas cover an energy
region of only 2000 eV.
• Color codes
The ionization edges show different profiles which are divided into five
typical classes represented the coloring of the buttons. The colors
correspond to the profiles schematically displayed at the top of the
dialog box. In cases where there are two ionization edges, the color of
the lower-left corner corresponds to the higher energy, the top-right
corner to the lower ionization energy.
When you select an element by clicking on the corresponding button,
the color of the button will change so that you always have visual
control over the number of elements you have selected.
EELS Atlas, Load Reference Spectra...

• Quick infos
Place the mouse cursor onto an element button to get a quick info
including the complete element name and the number of spectra
available in the EELS atlas.
Load To enable the Load button, click one or several element buttons. After
clicking the Load button, the Load EELS-Atlas file dialog box is opened
where all spectra belonging to the selected elements are listed. This is
where you select which spectra are to be loaded.
Select all By clicking the Select all or Clear all buttons, you can either select or
Clear all deselect all elements.

The Load EELS-Atlas file dialog box


Use this dialog box to select spectra to be loaded from the EELS-Atlas. The first spectrum is loaded into
the currently-active spectrum buffer, the other spectra into the spectrum buffers following the active one.

Available To open the Load EELS-Atlas file dialog box, click the Load button in the
EELS-Atlas-Selection dialog box.

Reference Spectra All spectra of the selected elements are listed in the Reference Spectra list.
To specify the spectrum which should be loaded, click on the entry desired.

43
You may select more than one spectrum: Use the [Shift] key to select a
range of spectra; use the [Crtl] key to select an arbitrary selection of spectra.
The entries in the Reference Spectra list include the element symbol and a
short description of the specimen used to acquire the spectrum. More than
one spectrum is offered for some elements. These spectra can be identified
using consecutive numbers.
For more information on the individual spectra, such as the compound of the
specimen used to record the spectrum or the preparation method, load the
spectrum and then use the Graph Information... command.
How to... How to load a spectrum of the EELS-Atlas:
You would like to load different sample carbon spectra.
1) Activate the desired spectrum buffer.
2) Choose the EFTEM > EELS Atlas > Load Reference Spectra
command.
" The EELS-Atlas-Selection dialog box is opened.
3) Click the Clear all button to clear a previous element selection.
related topics
Graph Information 25
EFTEM • The EFTEM menu

4) Click the carbon button. It is situated in the 4th main group.


" The color of the button will be altered from red to blue.
" The Load button will be enabled.
5) Click the Load button.
" The Load EELS-Atlas file dialog box opens.
" The EELS Atlas offers several spectra of different carbon
specimens. For each spectrum, a short description is given.
6) Select the desired spectra from the list, e. g., the spectrum of graphite
and formvar to see the difference between crystalline and amorphous
carbon.
7) Click OK.
" Both spectra are loaded into successive spectrum buffers.

EELS Atlas, Set Elements Labels...


Use this command to label the ionization energies of the selected elements in the active spectrum
document.

Selecting elements This command opens the Set element labels dialog box which is almost
identical to the EELS-Atlas-Selection dialog box. Use the mouse to click on
all the elements whose ionization energies you want to label in the
spectrum. OK activates the selection and the corresponding labels appear
in the active spectrum.
Apply to all EEL In the Set element labels dialog box select the Apply to all EEL spectra
spectra check box to set the element labels for all currently loaded spectra.
Clear the check box to add the selected element labels only to the spectrum
in the active spectrum buffer.
Quick infos The quick infos of the element buttons show the exact energy loss of the
different ionization edges below 2500 eV. Additionally, the value of the
surface (SP) and volume plasmon loss (VP) is given.
Handling spectra The elements’ labels are treated exactly like other spectrum labels. You may
labels thus use one of the following commands in the Graph menu to modify or
delete element labels:
44

Adding labels Use the Graph > Labels > Set... command to add any kind of annotations to
the spectrum. This may be a comment on the spectrum, the acquisition date
and so on.
Modifying labels Use the Graph > Labels > Modify... command to edit element labels. All
elements label are included in the Labels list of the Modify Labels dialog box.
You may change the label position, add a descriptive text or delete individual
element labels.
Deleting labels Use the Graph > Labels > Delete All command to delete all element labels
in the active spectrum. If you want to delete a special element label use the
Modify Labels... command. Select the element label from the Labels list and
click the Delete button.
Alternatively, click the Delete All Labels button in the button bar of the
spectrum document.

related topics
Labels, Set... 31
EELS Atlas, Auto Scaling...

The boron spectrum of the


EELS atlas has been loaded
into the spectrum
document. The nitrogen and
bor labels are set, indicating
that nitrogen was also
present in the specimen.

EELS Atlas, Auto Scaling...


Use this command to restrict the displayed energy range to the region of a specific ionization edge.

What will happen... After calling the command you can choose the element and its ionization
edge from the periodic table of elements. EsiVision will change the
displayed energy range of the active spectrum accordingly.
Quick infos show the plasmon losses and ionization energies below
2500 eV (for each element). The energy range displayed is computed on the
basis of these ionization energies: e. g., in order to display the K-edge of
aluminum, EsiVision will change the energy range to [1537-1657] eV, i. e.,

45
ionization energy minus 30 eV and plus 90 eV. The Y scale of the spectrum
is also adjusted.
Furthermore, low loss regions with volume and surface plasmon losses can
be displayed.
Note To display the energy region of the zeroloss use the EFTEM > EELS Atlas
> Display Zeroloss command.

How to... How to optimize the spectrum display for a specific ionization edge:
You would like to check whether a spectrum of an iron specimen also
contains oxygen.
1) Activate the spectrum buffer box containing the iron spectrum.
2) Use the EFTEM > EELS Atlas > Auto scaling... command.
" The Auto scaling dialog box is opened providing the complete
periodic table of elements.
3) Click the O-button to optimize the spectrum scaling for the oxygen K-
edge.
EFTEM • The EFTEM menu

" In the Details list you will find all plasmon losses and ionization
edges below 2500 eV for the selected element.
The list will contain only one entry for oxygen.
4) Check the Draw Labels check box to add the label of the selected
element to the spectrum.
5) Click OK.
" The scaling of the spectrum will be adjusted for the optimum display
of the oxygen K-edge.
Because of the huge
dynamic range, the whole
iron spectrum can only be
displayed using a
logarithmic presentation.
Even in the logarithmic
display mode, the oxygen
edge is hardly visible.

Autoscaling optimizes the


display of the oxygen edge.
46
EELS Atlas, Peak Identification...

EELS Atlas, Peak Identification...


Use this command to search for characteristic ionization edges.

Before you use • Calibrate the zeroloss:


the command Check the position of the zeroloss. If necessary, use the Graph >
Calibration > Zero-Loss Calibration command to adjust the position of
the zeroloss.
• Adjust the display:
Change the display of the spectrum so that the interesting ionization
edges are visible. If the peak identification does not lead to the
expected result, vary the displayed energy range.
• Switch to the Window Mode:
Click the Window Mode button in the button bar of the spectrum
document to restrict the peak identification to the displayed spectrum
region.
The iron L-ionization edge
has been automatically
identified. Clicking the Show
button in the Peak
Identification dialog box
enlarges the corresponding
energy region.

47
EFTEM • The EFTEM menu

Elements found The Elements found group lists the five possible elements with suitable
ionization edges for the selected energy range. The check box beside the
most probable element is selected. The exact positions of the corresponding
ionization edges are indicated by an arrow and the element label.
You may clear the proposed check box or select other check boxes to mark
the position of the ionization edges of the other elements.
Show Click the Show button next to a proposed element to optimize the spectrum
display for the selected ionization edge. Click the Reset View button to
return to the original displayed energy range.
Show All Click the Show All button to display the whole spectrum. Click the Reset
View button to return to the original displayed energy range.

EELS Atlas, Display Zeroloss


Use this command to display only the first 60 energy channels of a spectrum. To display the whole
spectrum, click the Default Size button on the button bar in the spectrum document.

Available The EELS Atlas > Display Zeroloss command is only available if the current
spectrum contains the energy loss value 0 eV.
48
ESI

ESI
Use this command to open a submenu which offers commands used for the
acquisition, analysis and file management of ESI series.

Available Most of the ESI commands are only available if a valid ESI image series is
loaded.
Creating valid ESI • Use the ESI > Acquisition... command to acquire a new ESI series and
series apply the ESI commands, e. g., checking the quality of the series or
calculating the element distribution images.
• Use the ESI > Load series... command to load an existing ESI series.
When using this command, the series will automatically be detected as
a valid series from all ESI commands.
Do not load the images in the series using the File > Open... command.
The system will not recognize it as an ESI series - even if you load the
images in the correct sequence.
• Use the ESI > Define series... command to assign single energy-
filtered images to an ESI series. This is necessary when ESI images
were not saved using the ESI > Save series... command.

49

related topics
ESI, Load Series... 66
ESI, Define series... 58
EFTEM • ESI

ESI Options
Use the EFTEM > Options... command to open the EFTEM Options dialog box. Use the ESI tab to define
some general options for the Energy Spectroscopic Imaging method.

Camera Options considered by the ESI > Acquisition... command are specified in the
Camera group. The parameters for image acquisition are set by the active
logical input. For example, you can switch on several online-features, such
as an online histogram or online shading correction.
Preferred Select the name of the input channel that is to be used for the acquisition of
50

ESI image series from the Preferred list. As soon as you call the ESI >
Acquisition... command, the active input channel is replaced by the input
channel specified in this list.
(none) Choose the (none) entry to not automatically change the active input
channel before using the ESI > Acquisition... command.
Note Automated ESI acquisition requires the remote control of the microscope to
set the energy loss (and to switch the beam blanker on and off). When the
remote control is not enabled, the ESI > Acquisition... command is not
available. Defining a preferred input channel only makes sense if all inputs
are also capable of remote control. Otherwise, you have to choose a valid
input channel (via [F6]) before ESI acquisition anyway.
Align with live mode Select the Align with live mode check box to switch on the live mode as soon
as the ESI Acquisition dialog box opens. Use the live image to find the
optimum energy windows and camera settings, e. g., the exposure time. It
is strongly recommended to use the live mode for optimizing the acquisition
parameters.
related topics
ESI, Acquisition... 52
ESI

Preprocessing A series of macro steps can be defined in an input. The macro is performed
Postprocessing before or after image acquisition. Use the Preprocessing or Postprocessing
list to specify at which points of the acquisition process these steps are to be
performed.
For example, you can use the pre- and postprocessing feature to have the
final fluorescent screen automatically raised before acquiring an image and
to have the screen then lowered again afterwards. These steps need not be
performed for every single image of the series.
Always Using the Preprocessing or Postprocessing list, you determine whether the
Never pre- or postprocessing steps are to be performed for every image of the
series (Always), or for no image of the series (Never).
Only first image Preprocessing steps are often useful only for the first image (Only first
Only last image image), e. g., initializing hardware components. On the other hand,
postprocessing steps are often only necessary for the last image (Only last
image), e. g., reset camera settings.
Quality check delay The ESI > Quality Check command toggles through all images of an existing
ESI series. Enter the time in [ms] each image should be displayed on screen
into the Quality check delay field. The default setting is 500 ms. The
maximum possible delay time is 10000 ms (= 10 s); the minimum is 0.
Acquisition delay The ESI > Acquisition... command acquires several images at different
energy loss positions. Enter the time in [ms] the system should wait between
two successive snapshots into the Acquisition delay field. The default setting
is 500 ms. The minimum acquisition delay time is 100 ms; the maximum
10 s (= 10000 ms).
Always calculate The ESI > Analyze... command calculates the raw-element distribution
presentation image. Select the Always calculate presentation check box to automatically
create an additional false-color image from the element distribution image.
The effect is the same as using the ESI > Analyze... command first and the
ESI > Presentation... command afterwards.
Edge enhancement on After acquiring an ESI-series, a drift correction can be necessary. The drift
drift correction is automatically calculated and corrected by the system. If a contrast
inversion occurs during the series, a more sophisticated drift detection
algorithm may be necessary. All images of the series are filtered by an edge
enhancement filter and the drift is calculated on the filtered images series.

51
Select the Edge enhancement on drift correction check box to activate this
calculation method. Note that edge enhancement will slow down the drift
correction. Therefore, you should only select the check box if the usual drift
correction does not lead to satisfying results.

related topics
ESI, Quality Check... 60
ESI, Analyze... 67
ESI, Presentation... 69
EFTEM • ESI

ESI, Acquisition...
Use this command to acquire a new ESI-series in order to produce an element distribution image.

Available The ESI > Acquisition... command is only available if the remote control is
activated.

Warning The acquisition of an ESI-series will overwrite the first image buffers. The
number of image buffers needed depends on the selected background
approximation method, the maximum number is 10.
If one of the first image buffers is write protected, you can either remove the
write protection during the ESI acquisition or stop the acquisition process.
You may also The ESI > Acquisition... command is also available on the EFTEM button
bar.

ESI Options There are some general settings for all ESI image acquisitions. They are
summarized on the ESI tab in the EFTEM Options dialog box.
52

related topics
How to acquire an ESI-image series 9
Remote Control 3
ESI, Acquisition...

Preset settings Upon opening the ESI Acquisition dialog box, the system automatically
loads the parameters which were used for recording the last ESI-series. The
energy loss on the microscope is automatically set to the energy loss
∆EMAX, the maximum intensity of the currently selected ionization edge.
Element Into the Element field, enter the element you wish to create an element
distribution for. Only the international standardized abbreviations are
accepted.
Periodic table... Use the Periodic table... button to open a dialog box showing the periodic
table of elements. To select an element, simply click the desired element
button and confirm your choice by clicking on OK.
The quick info displays the full element name and the ionization edges
below 2000 eV.
Edge The Edge field specifies the ionization edge of the selected element. With
regard to predefined parameter sets, this field is for information only. For
user-defined parameter sets, you can enter the edge type.
Slit width Enter the present slit width of the microscope into the Slit width field. The
energy windows displayed in the spectrum diagram are modified
accordingly. The system does not select the slit width; it has to be done by
yourself.
Scheme The Scheme list offers all available parameter sets for the active element.
This parameter set includes all settings in the dialog box except the display
mode of the spectrum diagram, i. e. - specifically - the element, the number
of images and the energy positions.
Predefined schemes For each element, EsiVision offers at least one predefined parameter set.
The name of a predefined scheme consists of the element symbol (e. g.,
Ca), the symbol of the ionization edge (e. g., L2) and the word ‘Atlas’. A
particular set of energy values is linked to this predefined scheme. To load
a predefined scheme for a specific element, click the Periodic Table...
button.
User-defined schemes To define your own parameter set for an element, type a new name in the
Scheme field. The Edge field will then become an edit field which you can
use to specify the type of the ionization edge and the Delete and Save
buttons will be enabled. After loading a previously saved parameter set, the

53
spectrum diagram is updated immediately.
Save Click the Save button to save the present parameter set for a specific
element. For loading an existing user-defined parameter set, insert the
corresponding element in the Element field. Then all available parameter
sets associated with this element are listed in the Scheme list.
The Save button is only available when a new name is entered in the
Scheme field.
Delete Click the Delete button to delete a previously stored parameter set for a
specific element. To do so, enter the element into the Element field and
select the corresponding parameter set from the Scheme list.
The Delete button is only available if a user-defined parameter set exists for
the active element.
The number of ESI images
needed depends on the
analyzing method chosen.
EFTEM • ESI

Method The Method list offers the available methods for background fittings. Select
the desired one from the list. The selected method determines the number
of images and the position of the energy losses. All energy windows
required by the selected method will be immediately displayed in the
spectrum diagram. The proposed energy values are empirical values
resulting in an optimum background fitting for the selected method, e. g., the
3 window method.
Note The background fitting method selected during acquisition is only a
preliminary choice. You can still use another method when creating an
element distribution image, provided that all necessary images are
available. If you do not want to restrict yourself to one particular method,
select all possible windows. As a result, the ESI series will contain all
necessary images for applying any analysis method.
Example For example, an ESI-series recorded with the 3 window method can be
analyzed by the 3 window linear method as well as by the 3 window
exponential method because both methods require two images below and
one at the maximum of the ionization edge.
On the other hand, it is not possible to use the 3 window white line method
with this ESI series because the image beyond the ionization edge is
lacking.
HCI Select the HCI check box to record an additional High Contrast Image. The
HCI image enables you to identify structures in the element-distribution
image or to correct a possible specimen drift. It is not considered when
calculating the element-distribution image. The HCI image is often recorded
at 250 eV, just below the carbon K-edge, because the reduced contribution
of carbon results in a particularly high image contrast - especially when
investigating biological sections. However, you are allowed to enter another
energy loss, e. g., ∆EMAX in case it is more suitable for the specimen under
investigation.
Note You may also include a zeroloss or elastically-filtered image in the ESI
series. Just take the HCI image at the energy loss 0 eV.

The following information is


indicated in the diagram of
the ESI Acquisition dialog
54

box:
z the energy loss spectrum
of the relevant energy range
(red, blue or magenta
curve).
z the position and the width
of the various energy
windows (green rectangles)
z the current energy loss on
the microscope (blue
triangle at the top of the
diagram)

related topics
Background approximation methods 5
ESI, Acquisition...

The diagram in the dialog box displays a spectrum of the required energy-
loss range. The shown spectrum comprises 400 eV; the starting point
depends on the ionization energy. The Y values automatically range from 0
to the maximum intensity of the displayed energy range.
Show Spectrum Decide which spectrum should be displayed in the diagram in the Show
Spectrum group. You may display all three types of spectra simultaneously
and overlapping, but you cannot switch off all spectra at the same time. If
only one spectrum is left, the corresponding check box is no longer
available. In this case, you have to display a second one before you are
allowed to switch off the spectrum.
Symbolic Select the Symbolic check box to display only a schematic energy-loss
spectrum. The schematic spectrum does not represent the real shape of the
selected ionization edge. Without exception, the ionization edges in the
schematic spectrum show a saw tooth shape with the ionization threshold
energy at ∆EIO1 and the maximum intensity at ∆EMAX. The schematic
spectrum of, e. g., a white line will thus not differ from the schematic
spectrum of, e. g., a delayed edge.
EELS atlas Select the EELS atlas check box to display the spectrum of the EELS atlas
belonging to the selected element and ionization edge. There is precisely
one spectrum available for each element and ionization edge.
Spectrum Select the Spectrum check box to work with your own reference spectra.
The contents of a specific spectrum buffer are displayed in the diagram. The
number of the spectrum buffer has to be specified in the field below the
Spectrum check box. The default spectrum buffer is the active one.
The Spectrum check box is only available if the specified spectrum buffer
contains a valid EELS spectrum. If the specified spectrum does not cover
the whole energy range, only a part of the spectrum will be displayed.
Setting the energy loss Use the mouse to change the given energy-loss values for the ESI image
for the ESI images series directly in the spectrum diagram. Before setting the energies, choose
the element, the ionization edge, and the background-fitting method.
To change the energy of a specific ESI image, you first activate the energy
window by simply clicking on the corresponding green rectangle.
" A blue line cursor appears, the exact energy value is displayed
below the diagram and at the same time updated on the

55
microscope.
To change the energy value, drag the blue line cursor with the depressed
left mouse button to the desired energy position.
" The green-colored columns will trace the diagram cursor. The
associated energy value displayed below the diagram will be
updated continuously.
For the precise positioning of the energy window use the left and right
keyboard arrows.
" The activated energy window will be shifted step by step in the
corresponding direction. The minimal energy increment depends
on the present microscope settings.
Note You are not allowed to move the energy loss ∆EMAX below the ionization
threshold. The default sequence of the energies cannot be changed, e. g.,
∆EW1 cannot be dragged below ∆EW2.
EFTEM • ESI

Setting the energy loss You may also set the energy loss on the microscope via the remote control
on the microscope without changing the energy window position. Use this feature if you are
working in the live mode to get an impression of the image quality. To do so,
activate the blue arrow at the upper part of the diagram. Drag the arrow to
the desired energy position.
" The energy loss on the microscope changes. The positions of the
green areas in the diagram remain unchanged.
Element Label... Click the Element Label... button to indicate certain ionization edges in the
spectrum diagram. A periodic table will be displayed on screen where you
can select the desired elements simply by clicking on the corresponding
element symbols. Use this option to get an overview of the positions of
ionization edges occurring in the selected energy range.
Energy scale Change the displayed energy range of the spectrum diagram in the Energy
scale group.
Element region Select the Element region option to display the energy range around the
selected ionization edge.
Full range Select the Full range option to see the entire energy range covered by the
spectrometer. If Full scale has been selected and the green-colored energy
interval has been shifted out of the energy region, the Element region option
will be disabled. You cannot choose this option until the two regions overlap
again.
You may use the Full range option to check the conditions for acquiring the
HCI images with an energy loss beyond the energy loss range of the image
EELS series.
Camera Control... The Camera Control dialog box is usually not available when a dialog box is
opened. Click the Camera Control... button to activate the Camera Control
dialog box in order to adjust the exposure time. To go back to the Image
EELS Acquisition dialog box just click somewhere on the dialog box.
The layout of the Camera
Control dialog box depends
on the camera type. This is
a typical camera control for
a slow scan CCD camera.
56

Exposure defines how long the camera’s CCD chip is exposed. -


time /+ adjusts the exposure duration in pseudologarithmic
steps.

Use activates/deactivates automatic gain display. No


automatic matter what the actual exposure conditions are, the
gain display image will be displayed contrast-enhanced onscreen.
Histogram All image pixels will be included in the computation of
calculation the current gray-value histogram.
on full This histogram is evaluated for auto gain display.
image
Histogram The gray-value histogram is computed using only
calculation image pixels within a cross-shaped segment of the
on image (each cross segment being just a few pixels in
crosshair width).
ESI, Acquisition...

Histogram The current gray-value histogram is computed based


calculation on image pixels within a frame you have set (Region
on ROI Of Interest).
Set ROI draws a red frame within the image which is positioned
via mouse and is enlarged/reduced (while pressing the
left mouse button). Rightclick to set the frame, which
then disappears from view.
Use fixed activates/deactivates fixed-scale contrast enhance-
scaling ment. The continually updated gray-value histogram
is not evaluated. Fixed gray-value limits are used
instead.
Automati- automatically recomputes the fixed gray-value limits
cally adjust used for the fixed-scale contrast enhancement.
fixed scal-
ing
Manually opens a dialog box where you may manually redefine
adjust the fixed gray-value limits for fixed-scale contrast
fixed scal- enhancement.
ing
OK Click OK to start a fully automatic acquisition of the ESI series. Message
boxes keep you informed on the ongoing procedure. You may terminate the
acquisition procedure at any time by clicking on the Cancel button in one of
the message boxes.

Using an SIT camera


If you use an SIT-camera, the ESI Acquisition dialog box looks slightly
different. The features described below are only relevant for video cameras.
Note All images of an ESI-series are to be recorded with the same gain of the
camera, i. e., you are not allowed to have the brightness and contrast of the
images automatically adjusted by the camera. Do not set the DAGE SIT-
camera to ’manual’ for example.
Test... Click the Test... button to control the positions of the energy windows and
the corresponding image intensities. Click the button to start the test loop.
The button is only available for video cameras.

57
Energy The starting energy value will be the energy
Start/Stop window with the lowest energy loss. Clicking the
Cancel Start button begins the test run and, as a result,
the button changes its functionality to Stop. All
energy values of the ESI series will be sent to
the microscope in turn. When the test loop has
reached the lowest or highest energy value, the
sequence of the test loop will run the other way
round. Click the Stop button to freeze the current energy loss and the Cancel
button to terminate the test run.
Additional blacklevel The Additional blacklevel correction check box is only available for video
correction cameras. Select the check box to correct a camera offset while acquiring an
ESI series.
To perform an additional blacklevel correction, the first and the last image of

related topics
Online-Shading correction 12
EFTEM • ESI

the series will then be recorded with an unexposed camera. After the
acquisition is finished, the average will be taken from these two offset
images and subtracted from the ESI images.
Warning You should usually use the online shading correction that is included in the
logical input channel. In this case an additional blacklevel correction is not
neccessary.
Check Blacklevel... Click the Check Blacklevel... button to adjust the offset intensity of your
camera. The button is only available for video cameras.
How to... How to adjust the blacklevel intensity:
It is assumed that
• you are working with a video camera.
• the system has switched into the live mode, i. e., the Align with live
mode check box has been selected in the EFTEM options, ESI dialog
box.
1) Switch on the online histogram in the active input channel, i. e., select
the Configure Input > Display > Online histogram check box.
2) Click the Check Blacklevel... button in the ESI Acquisition dialog box.
" The beam blanker and camera shutter will be automatically
activated by clicking on this button.
" A message box appears, prompting you to adjust the blacklevel
intensity.
3) Change the camera offset until the whole image appears black with
some brighter pixels so that no negative camera offset will be
superimposed on the ESI images.
" Check the settings in the online histogram. The histogram should
look similar to the one displayed.
4) Confirm the message with OK.
" The beam blanker and camera shutter will be turned off
automatically.
" The system returns to the ESI acquisition dialog box.
5) Select the energy loss with the highest image intensity after correcting
the offset to obtain the optimum camera adjustment.
58

6) Adjust the gain on the camera in such a way that the brightest image
pixels are displayed in white to use the full dynamic range of the
camera.
" Check the settings in the online histogram. The histogram should
look similar to the one displayed.
" In case the live image is quite noisy due to low intensity and high
amplification, you should use the Image > Set Input... command to
select a logical input channel with a higher number of averaging
cycles.

ESI, Define series...


Use this command to assign single energy-filtered images to an ESI series.

Definition A valid ESI series consists of several energy-filtered images. Each image
of the series is linked with a special parameter set including the meaning of
the energy windows, the energy loss and the element under investigation.
The Image Information dialog box of all ESI images contains an additional
tab, the EFTEM Data tab.
ESI, Define series...

Application It is not necessary to define an ESI series explicitly:


• if you load an existing ESI series using the ESI > Load series...
command, or
• if you acquire a new ESI series using the ESI > Acquisition... command.
In these cases, all necessary information is available. In particular, the
energy losses, the meaning of the image, the position of the images in the
image buffer box is known.
Note If you want to extract an element distribution image from an existing image
EELS series, do not use the ESI > Define series... command. Use the EELS
> Image EELS > ESI Mapping... command instead.
What will happen... After defining an ESI series
• the EFTEM Data tab is added to all images of the series.
• all ESI commands requiring a valid ESI series will be available.
Note The newly defined ESI series will not be saved automatically. Use the
EFTEM > ESI > Save Series... command to save the series in a special
series directory.

59

Method The Method list offers all possible methods to analyze an ESI series.
EsiVision will automatically check the number of images loaded and skip all
methods that cannot be applied.
Select the desired method from the list to activate all required images in the
Windows group.
Example If two images are loaded, only the 2 window method is offered.

related topics
Background approximation methods 5
EFTEM • ESI

HCI image included Select the HCI image included check box to add a high contrast image to the
ESI series. The HCI row in the Windows group will be enabled.
Windows Depending on the selected background-fitting method, the Windows groups
offers only images necessary for the ESI series. For each image you have
to specify the number of the image buffer and the energy-loss value.
Example For the 3 window method, there are three images required: the W2 and W1
images are necessary to extrapolate the background intensity beyond the
ionization edge by a power law, the MAX image contains the element-
specific information. The other ESI images are disabled.
Image To apply the ESI commands, the system has to know where to find the
individual images of the ESI series. Enter the number of the image buffer of
the corresponding image into the Image field.
Energy loss Enter the energy loss of the corresponding image into the Energy loss field.
Use the Select Element... button to load predefined energy-loss values for a
specific element.
Predefined settings When opening the dialog box, EsiVision will try to read the energy-loss value
of the image in the active image buffer. The energy loss can only be read if
the image was acquired using an EFTEM function. Otherwise the energy
loss is set to 0 eV.
When changing the number of the image buffer in the Image field, EsiVision
automatically updates the energy loss if an energy loss is linked with the
image.
Set EFTEM Data... Click the Set EFTEM Data... button to enter all data to be added to the image
information. You will find these data on the EELS Data tab.
Select Element... EsiVision offers a set of default energy-loss values for each element and
method. Use the Select Element... button to load predefined energy loss
values for a specific element.
OK Click OK to confirm the settings.
Plausibility check EsiVision will check whether the assigned energy windows and energy loss
values are possible. You will get a warning message if entries are
contradictory. Correct the entries and close the ESI Define Series dialog box
again. For example: the energy loss of the W2 energy window must be
smaller than the energy loss of the MAX energy window. You cannot assign
60

one image buffer twice, i. e., the image buffers for two energy windows must
be different.

ESI, Quality Check...


Use this command to detect a possible specimen drift within an ESI image series. The quality check is
also suitable for visually determining whether the element of interest is present.

Available This command is only available if a valid ESI image series is loaded.

What will happen... After calling the command, all the images of the active ESI series including
the HCI image are successively displayed onscreen. When the displaying
loop has reached the first or the last image of the series, the sequence will
start anew with the first image. The end of one complete run through the
series is indicated by an acoustic signal.

related topics
Background approximation methods 5
ESI, R-Map

Note Please note that due to the 16-bit display LUT the absolute mean intensity
of an image cannot be judged on the monitor. Although the mean brightness
of two images may appear the same, the absolute may be different.
However, the existence of element specific information should be clearly
visible.
Quality check delay You can set the time a single image of the series is displayed onscreen. Use
the EFTEM > Options... command to open the ESI tab. Enter the desired
time in ms in the Quality check delay field.
A message box contains the
meaning of the currently-
displayed ESI image and its
energy loss.

Click the Cancel button to terminate the quality-check loop.

ESI, R-Map
Use this command to check the acquisition conditions of an ESI series.

Available This command is only available


• if a valid ESI image series is loaded and
• the ESI series contains two images at energy losses below the
ionization edge, i. e., the 3 windows or all possible windows method
was chosen for ESI image acquisition.
What will happen... Calculating the R-Map
The images at ∆EW2 and ∆EW1 are used to compute the exponent 'r' pixel
by pixel. 'r' determines the decrease of the background intensity in cases
where a power law (A 'E-r) is assumed. If the result is much smaller or larger
than expected, the corresponding pixels will be colored blue (too small,
r < 2) or red (too large, r >6). When mapping an appropriate ESI series, the
resulting image should contain few red or blue image points only.

61

related topics
Meaning of the different energy windows 7
Background approximation methods 5
EFTEM • ESI

The image document is


divided into four viewports
containing the ESI images
for calculating an Fe
element-distribution image.
The R-Map is shown in the
upper-left viewport. The
homogeneous
R-Map proves that the ESI
series has been acquired
properly. Non-reliable R-
values are obtained only
inside specimen holes (they
appear black in the energy-
filtered images).

To display the Z values and


the color palette of the R-
Map, use the Image > Scale
Bar > Properties...
command. On the Display
tab, select the Palette bar
check box. Use the
[Shit+F4]-keystroke to show
and hide the palette bar in
the image.

Destination Image The ESI > R-Map command overwrites the image in the image buffer after
Buffer the last image of the ESI series. The currently set destination image buffer
in the operands block is ignored. Make sure that the image buffer does not
contain an important image before calling the command.
62

Image Properties of the The resulting image has some special properties:
R-Map • The image is automatically named ’R-Map’.
• The bit depth of the resulting image is always 8 bits, even if the images
of the ESI series are 16-bit images.
• The image type is changed to a false-color image. The applied false-
color LUT can be displayed in the viewport. To do so, use the Image >
Scale Bar > Properties... command. On the Display tab select the
Palette bar check box. Use the [Shit+F4]-keystroke to show and hide
the palette bar in the image.
• The resulting image is Z calibrated, i. e., use the Measure > Pixel value
command to measure the resulting r value for any image pixel.
• The following comment is added to the image information of the
resulting image:
ESI: R-Map
3 window (all possible windows)
ESI, Drift Correction...

Possible reasons for a If mapping produces many red or blue pixels, you should check for the
bad R-Map following:
• There are other ionization edges at energy losses below the edge
under investigation. In this case, the background cannot be fitted
properly by applying a power law.
• The specimen is considerably thicker than the mean free path length
for inelastic scattering (~ 100 nm for organic specimens are 10 µg/
cm²). In this case, the exponent 'r' will not lie within the typical interval
the computation is based on.
• If whole areas of the image are colored, there may be a hole inside the
imaged specimen region.

ESI, Drift Correction...


Use this command to have a specimen drift corrected automatically. If necessary, you may correct the
automatic shift values interactively.

Available This command is only available if a valid ESI image series is loaded.

Specimen drift during In cases where a lengthy acquisition time was necessary, it is possible that
ESI acquisition the specimen was drifting during the acquisition of that ESI series. A
specimen drift can be caused by thermal drift or narrow tears near the
irradiated specimen area which progress by electron irradiation. If you
nevertheless consider the ESI series suitable for analysis, you will have to
correct the specimen drift before using the ESI > Analyze... command.
Before you use this • Load or create a valid ESI series.
command • Activate the image buffer containing the image of the ESI series you
want to use as reference image. As reference image, an image
containing a clearly visible structure should be used, e. g. the image at
the ionization edge (i.e. ∆EMAX or ∆EIO1).
Note Do not use the HCI image as reference image because the contrast of the
HCI image may be completely different than the contrast of the remaining
images of the ESI-series.

63
What will happen... 1) The system will automatically compare the reference image with the
remaining images of the ESI series. EsiVision applies a pattern-
recognition routine and calculates a shift according to the reference
image.
If a contrast inversion occurs during the series, a more sophisticated
drift detection algorithm may be necessary. All images of the series are
filtered by an edge enhancement filter and the drift is calculated on the
filtered images series. Select the EFTEM > Options > ESI > Edge
enhancement on drift correction check box to activate this calculation
method. Note that edge enhancement will slow down the drift
correction. Therefore you should only select the check box if the usual
drift correction does not lead to satisfying results.
2) When the calculation is finished, the difference image between the
compared images is displayed in the active viewport. Every shift of the
two images should be visible as a pseudo-topographical structure. Use
the arrow buttons in the ESI Drift Correction dialog box to correct the

related topics
ESI, Analyze... 67
Meaning of the different energy windows 7
EFTEM • ESI

remaining image shift interactively.


An interactive drift correction may be necessary if the ESI series
contains a contrast inversion due to a very pronounced element
concentration.
3) You can subsequently perform the drift correction to every image of the
ESI series that is shifted compared to the reference image.
4) After clicking OK, the corrected images substitute the original images
of the ESI series, i. e., they overwrite the image buffers containing the
original image.
5) In a final step, the system reduces the image size of the ESI images by
cutting the margins produced by an image shift.
The two schematic images
are shifted. The shift image
has to be shifted one pixel to
the right and two pixels
upwards. To correct the Y
shift, the first two lines are
cut from the reference
image and the last two lines
from the shift image. The X
shift is corrected by cutting
the first and last rows.

Description of the dialog box


64

Reference image The Reference image field shows the currently used reference image. You
may use any image of the ESI series as reference image. Just activate the
image buffer containing the reference image before using the ESI > ESI Drift
Correction... command.
ESI, Save Series...

Shift image The Shift image list offers the remaining images of the ESI series. Choose
one of the images from the list to check and correct the calculated shift
values with respect to the reference image. The system remembers the
modified shift values until you actually perform the drift correction by clicking
OK.
Note You should always check and correct each image of an ESI series because
the drift of the individual images may be different.

X shift The X and Y shift fields display the calculated shift values of the shift image
Y shift according to the reference image. These shift values are applied to the
image after clicking OK.
Arrow buttons Click the arrow buttons to move the shift image in the direction indicated.
The image is shifted one pixel per click. The resulting difference image is
immediately displayed on screen. The shift values are updated accordingly.
Click the central button to reset the shift values to the calculated drift value.
Reset Click the Reset button to set both shift values to zero.
OK Click OK to confirm the current shift values. All images of the ESI series are
shifted by the calculated values. The image sizes are reduced accordingly.

ESI, Save Series...


Use this command to save an acquired ESI series as a whole.

Available This command is only available if the image buffer box contains a valid ESI
image series.
What will happen... Each ESI series has the following properties:
• ESI images
The ESI series comprises all images acquired using the EFTEM > ESI
> Acquisition... command. An ESI series does not include the element-
distribution image produced by the Analyze... command or the
overview image created by the Presentation... command.
• Directory of the ESI series
Each ESI series is situated in its own directory. The directory is

65
automatically created when saving the series.
• Folder name extension
The directory name is characterized by the extension ESI. This suffix is
added automatically by the system when saving the series.
• Series description
A description is automatically saved with the series. The description
consists of the keyword ’ESI series’, the energy-loss range and the
selected analyzing method. It is saved in a separate file in the ESI
series directory.
• File names
The file names of the ESI images are standardized. The file name is
composed of the name of the element, the ionization edge and a
consecutive number, e. g., ’Crl21.tif’ (element: Cr, ionization edge L2,
first image of the series).

related topics
ESI, Acquisition... 52
EFTEM • ESI

Warning You have to use the EFTEM > ESI > Load series... command (in the EFTEM
menu) to load an existing ESI series. You cannot use the usual image series
commands Image > Image Series > Load... command because this
command would not recognize the ESI image series as an image series. If
you use the File > Open... command to load the ESI images separately,
EsiVision will not recognize the ESI series.

Folder name The Folder name field shows the current path name. Add the name of the
series you want to save. Choose a content relevant name to make it easier
to locate the series later on. There is no need to type in the expected folder
name extension (ESI); the system will append it automatically. You can
choose the directory using the Look in list.
New Click the New button to save the new ESI series in the specified folder. The
66

system will automatically append the extension ESI to the directory name so
you can recognize a directory containing an ESI series at a glance.
OK Click the OK button to overwrite an existing ESI series. If the selected
directory does not contain a valid ESI series you will get an error message.
Description In case you have selected a directory which already contains an ESI series,
a short description of the ESI series is displayed in the Description group.

ESI, Load Series...


Use this command to load an already existing ESI series from disk - as a whole. Afterwards you may
apply all ESI analysis commands, e. g., you may perform a drift correction or calculate an element
distribution image.

Warning The ESI series will overwrite the first image buffers. The number of image
buffers needed depends on the selected background approximation
method, the maximum number is 10.
If one of the first image buffers is write protected, you can either remove the
write protection before loading the ESI series or terminate the command.
ESI, Analyze...

Folder name Specify the drive and the directory containing the ESI series you would like
to load in the Folder name field. When opening the dialog box, the system
automatically selects the ESI series which had been loaded last.
Description The Description group contains the most important information on the
selected ESI series. If the selected directory does not contain a valid ESI
series, the Description group disappears.

ESI, Analyze...
Use this command to calculate a qualitative element-distribution image by analyzing the energy-filtered
images of an ESI series.

Available This command is only available if a valid ESI image series is loaded.

67
Warning The Analyze... command will overwrite the two image buffers that follow the
last image of the current ESI series.
If these image buffers are write protected, you can either remove the write
protection or stop the analysis of the ESI series.
Definition An element distribution image contains information about the spatial
distribution of a special element.

What will happen... The analyzing routine will run automatically after selecting the background
approximation method in the ESI Analysis dialog box. Confirm the selected
method with OK to have the element-distribution image computed.
Preview When you select a background fitting method in the ESI Analysis dialog box,
the resulting element distribution image is calculated immediately. A preview
is displayed in the active viewport.

related topics
How to acquire an ESI-image series 9
EFTEM • ESI

Destination image buffer The resulting element-distribution image is put into the image buffer that
follows the last image of the ESI series. This is the unprocessed net element
distribution.
Display LUT of the The display LUT of the element-distribution image is automatically optimized
element-distribution for all 16-bit ESI images. Note that the gray value of the element distribution
image differs greatly from the gray-value range of the individual ESI images.
Image information The element-distribution image is named after the method used, e. g., ’3
window power law difference’. The image information of the element-
distribution image also contains the additional EFTEM Data tab. The
EFTEM data includes, e. g., the element under investigation. The Energy
window field indicates that the image is an element-distribution image.
Presentation Image It is possible to create an additional presentation image immediately after
analyzing the ESI series. To do so, select the EFTEM > EFTEM Options >
ESI > Always calculate presentation check box. In this case, the ESI >
Presentation... command is called automatically.
Note The element-distribution image does not belong to an ESI series, i. e., you
cannot use the ESI > Save Series... command to save the presentation
image along with the ESI images.

Background The Background Approximation list offers several methods for extrapolating
approximation and subtracting the background intensity. Select the desired one from the
68

list.
The list contains only those methods using the energy windows of the
current ESI series. For example: the WL-image with an energy loss beyond
the white line is needed for the 3 window white line method. If the current
ESI series does not contain the WL image, the method will not be listed.
Processing Background intensity at the ionization edge is calculated for each image
pixel. You determine how the background-intensity image is used in the
Processing group.
Difference Select the Difference option to subtract the background-intensity image from
the image at the ionization edge. This is the standard option for calculating
an element distribution image.
Ratio Select the Ratio option to divide the image at the ionization edge by the
background-intensity image. Use this processing method for calculating the
jump ratio. It is usually not used to calculate an element distribution image.

related topics
ESI, Presentation... 69
Background approximation methods 5
ESI, Presentation...

2 window difference If you select the 2 window difference method, the ESI Element Distribution
dialog box is opened.
OK Click OK to write the element-distribution image into the image buffer
following the last image of the ESI series.

The ESI Element Distribution dialog box


This dialog box opens when you calculate an element-distribution image using the 2 window difference
method.

Calculating the It is assumed that the background intensity of all image pixels decreases by
element distribution the same factor k. k is usually less than or equal to one (0 ≤ k ≤ 1). The
image image at ∆EW1 is multiplied by k and subsequently subtracted from the
∆EMAX image. The result is displayed onscreen after maximizing contrast
and the ESI Element Distribution dialog box opens.

Factor Use the Factor scroll bar to change k in percentage terms. Provided the
offset is zero, a factor of 0 would underestimate the background intensity
because the pure intensity at the ionization edge is taken as an element
distribution image. A factor of 100 would overestimate the background
intensity because no decrease of the background intensity for higher energy
losses is considered.
The proposed k factor is calculated for each ESI series.
Offset Use the Offset scroll bar to superimpose an offset onto the resulting image.
i. e., the function
SN = S(∆EMAX) - (S(∆EW1) · Factor/100) + Offset

69
is applied to every image pixel. Furthermore, the result is displayed at
maximized contrast.

ESI, Presentation...
Use this command to optimize the presentation of the net elemental distribution. You can apply a false-
color LUT to display the element-specific information in a particular color and remove shot noise.

Available This command is only available if


• the image buffer box contains a valid ESI image series and
• the net element-distribution image has already been calculated. To do
so, use the ESI > Analyze... command first.
Warning The Presentation... command will overwrite the image buffer after the
element distribution image.
If this image buffer is write protected, you can either remove the write
protection or stop presentation function.
EFTEM • ESI

Destination Image The resulting presentation image is put into the image buffer that follows the
Buffer element distribution image.
Image information The presentation image is named ’Presentation’. The image information of
the element-distribution image contains the additional EFTEM Data tab. The
EFTEM data includes, e. g., the element under investigation. The Energy
window field indicates that the image is a presentation image.
Image type The presentation image is an 8-bit false-color image, i. e., the element
concentration is coded into 256 different colors. If the ESI images are 16-bit
images, information depth is reduced. On the other hand, the human eye
can differentiate better between colors than gray values, therefore small
variations in element concentration can be better recognized due to color
coding.
Displaying Color bars Use the Image > Scale Bar > Properties... command to add a palette bar in
the image showing the active display LUT. Activate the Display tab and
select the Palette bar check box.
Note The presentation image does not belong to an ESI series, i. e., you cannot
use the ESI, Save Series... command to save the presentation image along
with the ESI images.
70

Histogram The histogram of the element-distribution image is displayed in the dialog


diagram (above). Most of the image points are black in a typical element-
distribution image. This results in a dominating peak in the lower gray-value
range of the histogram. Use the slider at the left side to change the Y scaling
so that the peak corresponding to the element-specific information becomes
visible.
Limits for presentation You can exclude image areas (which contribute to the elemental map only
mask due to a slight fluctuation) in the background intensity in the Limits for
presentation mask group.
Low Use the slider to define the Low and High threshold values. The line cursors
High in the histogram diagram are updated accordingly. Use a local minimum for
the lower limit to separate the background from the element-distribution
ESI, Overview

information. The presentation image will only contain the image points with
gray values located between the lower and the higher background. The gray
values of all other image points are set to 0 (black).
Preview Upon opening the dialog box, all image points located between the current
thresholds are displayed in green. Use the preview to monitor the effect the
thresholds you select have on the presentation image. Note that the false-
color LUT used for the preview does not equal the color scheme used for the
resulting presentation image.
Color scheme You can choose among three different false color LUTs to be applied to the
presentation image in the Color scheme group.
Red In general, the higher the element concentration, the brighter the color.
Green Image areas with no element concentration are displayed in black. There
Blue are three different false color LUT’s available, each of which provides a
different color impression. For example, select the Red option to map image
areas with low element concentration to red, and areas with high
concentration to yellow.
Linear Check the Linear check box to use a false color LUT with a fixed hue value.
You will have a uniform colored presentation image as a result. All gray
values inside the limits for the presentation mask are colored either in red,
green or blue.
Sigma filtering Select the Sigma filtering check box to apply a sigma filter to the net
element-distribution image. Statistical noise is filtered out by the sigma filter.

ESI, Overview
Use this command to display an overview of the most important images of the ESI series and the
corresponding element distribution.

Available This command is only available if


• the image buffer box contains a valid ESI image series and
• the net element-distribution and presentation image have already been
calculated. To do so, select the EFTEM > Options > ESI > Always calc-
ulate presentation check box and use the ESI > Analyze... command

71
after the acquisition of the ESI series.
Warning The Overview command will overwrite the image buffer following the
presentation image.
If this image buffer is write protected, you can either remove the write
protection or stop the overview function.
What will happen... After calling the Overview command, the images are mounted in a 2 x 2 grid
and put in the image buffer following the presentation using the image name
'Overview'. Size and the calibration of the images are preserved.

related topics
ESI, Analyze... 67
EFTEM • ESI

Composition of overview The images for a three windows method are mounted as follows:
image
1 2 The HCI image is optional. If
∆EW1 ∆EMAX no HCI image was recorded,
the image segment remains
energy loss just maximum of the
below the ionization edge
empty.
ionization edge Instead of the W1 image, the
3 4 WL image is displayed for a
series analyzed by the white
(HCI) Presentation
line method.
High Contrast image
Image
Overlay information The corresponding energy losses and the acceleration voltage used when
acquiring the ESI series are displayed in the image overlay. The element
distribution is entitled (e. g., 'Fe-distribution').
The overlay information is written to the data layer of the overlay. To edit the
overlay information, unlock the data layer first. To do so, click the Overlay
Button Bar button in the Standard button bar. Click the Layer button in the
Overlay button bar and use the Lock Data Layer command if a check is
shown in front of the command.
Destination image buffer The resulting overview image is put into the image buffer that follows the
presentation image.
Image information The overview image is named ’Overview’. The image information of the
overview image also contains the additional EFTEM Data tab. The EFTEM
data includes, e. g., the element under investigation. The comment ’ESI:
Overview’ is automatically added.
Image type The overview image is a 24-bit true-color image.
Note The overview image does not belong to an ESI series, i. e., you cannot use
the ESI, Save Series... command to save the overview image along with the
ESI images.
Resulting overview of an
ESI series when using the
ESI, Overview command.
72

Iron was detected in this


example.
ESI, Combine Images...

ESI, Combine Images...


Use this command to superimpose one, two or three element-distribution images onto the HCI image.
The resulting image enables you to link specimen structures and element distribution.

Available This command does not expect an ESI image series. You may also apply
this command to color a specified image area for other purposes.
Before you use this • Load the High Contrast Image or another image of the ESI series with
command a high contrast. In order to recognize the specimen structures as
clearly as possible, it may be useful to maximize the contrast of the HCI
image.
• Load the element-distribution images you want to superimpose onto
the HCI-image. Up to three images are possible.
• It is assumed that the images correspond to the same specimen area.
A specimen drift between the acquisition of the different ESI-series can
be correct when combining the images.
This is an example of the
Combine Images...
command. The element
distribution images for
chromium and titanium
show image areas with high
element concentration. The
combined image (lower
right) enables you to locate
the element in the
specimen.

73

What will happen... When opening the dialog box, EsiVision automatically reads out the image
information of all images loaded currently loaded in the image manager. The
meaning of an image for an ESI-series is added to the EFTEM Data tab of
the Image Information dialog box. EsiVision is automatically detecting HCI-
and presentation images.
EFTEM • ESI

Use the Images tab of the


Combine Images dialog box
to determine which images
you would like to combine.

Background (HCI) The Background (HCI) field contains the image buffer number of the first
HCI image loaded. The name of the image in the selected image buffer is
also given.
If you want to use another image as reference image, enter the
corresponding number of the image buffer into the Background (HCI) field.
Red The Red, Green and Blue fields contain the image buffer numbers of the
Green currently loaded presentation images. The image names of the selected
Blue image buffers are also given.
Select the Red, Green or Blue check box to overlap the corresponding
images with the high contrast image. If the system does not propose the
correct images, you can change the image buffer number. If you enter an
empty image buffer, the check box is disabled.
In case there are less than three element-distribution images, clear one or
two color check boxes.
Destination Enter the number of the destination image buffer into the Destination field.
The resulting combination image will overwrite the image in the specified
image buffer.
Use the Thresholds tab of
the Combine Images dialog
box to weight the different
element distribution images.
74

Low Use the scroll bars or the Low and High fields to enter the thresholds. The
High thresholds define the gray-value range of the element-distribution image
that is displayed in color. The other gray values are set to black. The
thresholds are defined for each color separately. You will automatically see
a preview of the resulting combined image in the current image buffer. When
you change the threshold settings, the image is immediately updated.
Image EELS

Use the Drift tab of the


Combine Images dialog box
to correct a drift between the
different element
distribution images and the
HCI image.

Adjust Click the Adjust button to shift the corresponding color image with respect to
the high contrast image.
How to... How to adjust an element distribution image to the high contrast image:
1) Click the first Adjust button to shift the red element distribution image.
" A rectangle appears in the image.
2) Define the preview area by moving the rectangle to an image area
where the specimen drift is clearly visible. Confirm the setting with the
left mouse button.
" A message box appears.
3) Start the drift correction by clicking OK.
" The selected rectangular image is zoomed to the size of the image
document.
4) Use the keyboard’s arrow keys to move the element distribution image.
" The preview image is automatically updated.
5) Press [Enter] to apply the changes and return to the Combine Images
dialog box.
" The shift values are displayed in the dialog. The X- and Y-values
correspond to pixels, not to absolute X- or Y-distances.

75
Image EELS
Use this command to open a submenu for the acquisition, analysis and file
management of image EELS series.

Available Most of the image EELS commands are only available if a valid Image EELS
series is loaded.
Creating valid image • Use the Image EELS > Acquisition... command to acquire a new image
EELS series EELS series and apply image EELS operations, e. g., checking the
quality of the series or calculating an electron energy loss spectrum
from a special specimen region.
EFTEM • Image EELS

• Use the Image EELS > Load series... command to load an existing
image EELS series. When using this command, the series will
automatically be detected as a valid series - by all image EELS
commands.
Do not load the series using the File > Open... command. The system
will not recognize it as an image EELS series, even if you load the
images in the correct sequence.
• Use the Image EELS > Define series... command to assign single
energy-filtered images to an image EELS series. This is necessary
when EFTEM images were not saved using the Image EELS > Save
series... command.

Image EELS Options


Use the EFTEM > Options... command to open the EFTEM Options dialog box. Use the Image EELS tab
to define some general options for the image EELS method.
76

Camera Specify options that are considered by the Image EELS > Acquisition...
command in the Camera group. The parameters for image acquisition are
set by the active logical input. For example, you can reduce image size by
binning.

related topics
Image EELS, Acquisition... 78
Image EELS, Load Series... 90
ESI, Define series... 58
How to define an input channel for image EELS acquisition 13
Image EELS

Preferred Choose the name of the input channel that is to be used for the acquisition
of image EELS series from the Preferred list. As soon as you call the Image
EELS > Acquisition... command, the active input channel is replaced by the
input channel specified in this list.
(none) Choose the (none) entry to not automatically change the active input
channel before using the Image EELS > Acquisition... command.
Note Automated Image EELS acquisition requires the remote control of the
microscope to set the energy loss (and to switch the beam blanker on or off).
When the remote control is not enabled, the Image EELS > Acquisition...
command is not available. Defining a preferred input channel only makes
sense if the usual inputs are also capable of remote control. Otherwise, you
have to choose a valid input channel (via [F6]) before image EELS
acquisition anyway.
Align with live mode Select the Align with live mode check box to switch on the live mode as soon
as the Image EELS Acquisition dialog box opens. Use the live image to find
the optimum energy windows and camera settings, e. g., the exposure time.
It is strongly recommended to use the live mode for optimizing the
acquisition parameters.
Preprocessing A series of macro steps can be defined in an input. The macro is performed
Postprocessing before or after image acquisition. Use the Preprocessing or Postprocessing
list to specify at which points of the acquisition process these steps are to be
performed.
For example, you can use the pre- and postprocessing feature to raise the
final fluorescent screen automatically before acquiring an image and to
lower the screen again afterwards. These steps need not be performed for
every single image of the series.
Always Using the Preprocessing or Postprocessing list, you determine whether the
Never pre- or postprocessing steps are to be performed for every image of the
series (Always) or for no image of the series (Never).
Only first image Preprocessing steps are often useful only for the first image (Only first
Only last image image), e. g., initializing hardware components. On the other hand,
postprocessing steps are often only necessary for the last image (Only last
image), e. g., reset camera settings.

77
Quality check delay The Image EELS, Quality Check command toggles through all images of an
existing image EELS series. Enter the time in [ms] each image should be
displayed onscreen into the Quality check delay field. The default setting is
500 ms. The maximum possible delay time is 10000 ms (= 10 s), the
minimum is 0.
Acquisition delay The Image EELS > Acquisition... command acquires a lot of images at
different energy-loss positions. Enter the time in [ms] the system should wait
between two successive snapshots into the Acquisition delay field. The
default setting is 500 ms. The minimum acquisition delay time is 100 ms, the
maximum 10 s (= 10000 ms).
Drift correction It is possible that the specimen has drifted during the acquisition of an image
EELS series - in particular when the acquisition time was lengthy. Before
creating a spectrum of certain specimen structures, the specimen drift has
to be corrected.
Decide which images of the image EELS series are considered when
performing a drift correction in the Drift correction group.

related topics
Image EELS, Quality Check 86
Image EELS, Drift Correction... 86
EFTEM • Image EELS

Linear, using high Choose the Linear, using high contrast images (faster) option to have only
contrast images two images compared for calculating a total object drift. These images are
(faster) two high contrast images and have been acquired before and after the
whole image EELS series. A uniform movement of the specimen is assumed
in order to calculate the displacement of every single image simply by
executing the following:
total object drift
drift between image n and image n + 1 = ------------------------------------------------------------------------------------
number of image EELS images – 1

This option speeds up the calculation of specimen drift because a time-


consuming pattern-recognition routine has to be applied only once.
Nevertheless, the calculated drift values are only a proposal; you may
interactively modify the drift values for each individual image afterwards.
Individual, using every Choose the Individual, using every image (slower) option to have a drift with
image (slower) respect to a reference image calculated for every single image of the series.
This drift-correction method may take some time because an image EELS
series may consist of more than 100 images.
Edge enhancement If a contrast inversion occurs during the series, a more sophisticated drift
detection algorithm may be necessary. All images of the series are filtered
by an edge enhancement filter and the drift is calculated on the filtered
images series.
Select the Edge enhancement check box to activate this calculation method.
Note that edge enhancement will slow down the drift correction. Therefore
you should only select the check box if the usual drift correction does not
lead to satisfying results.

Image EELS, Acquisition...


Use this command to record a new image EELS series to generate spectra of certain image structures.

Available The Image EELS > Acquisition... command is only available if the remote
control is activated.

Warning The acquisition of an image EELS-series will overwrite the contents of the
78

image buffers.
If one of the required image buffers is write protected, you can either remove
the write protection during the image EELS acquisition or stop the
acquisition process.
You may also The Image EELS > Acquisition... command is also available on the EFTEM
button bar.

Image EELS Options There are some general settings for all image EELS acquisitions. They are
summarized on the Image EELS tab in the EFTEM Options dialog box.

related topics
How to define an input channel for ESI acquisition 7
Image EELS, Acquisition...

Preset settings Upon opening the Image EELS Acquisition dialog box, the system
automatically loads the parameters which were used for recording the last
image EELS series. The energy loss on the microscope is automatically set
to the energy loss ∆EMAX, the maximum intensity of the currently selected
ionization edge.

79
Element Enter the element you want to investigate into the Element field. Only
internationally-standardized abbreviations are accepted.
Periodic table... Use the Periodic table... button to open a dialog box showing the periodic
table of elements. To select an element, simply click on the desired element
button and confirm your choice with OK.
The quick info displays the full element name and the ionization edges
below 2000 eV.

Edge The Edge field specifies the ionization edge of the selected element. As far
as predefined parameter sets are concerned, this field is only for your
information. When working with user-defined parameter sets, you can enter
the edge type.
Slit width Enter the present slit width of the microscope into the Slit width field. The
smaller the slit width, the better is the energy resolution of the resulting
spectrum.

related topics
Image EELS Options 76
EFTEM • Image EELS

Scheme The Scheme list offers all available parameter sets for the active element.
This parameter set includes all settings in the dialog box except the display
mode of the spectrum diagram, i. e. - specifically, the element, the START
and END positions, and the energy increment.
Predefined schemes EsiVision offers at least one predefined parameter set for each element. The
name of a predefined scheme consists of the element symbol (e. g., Ca), the
symbol of the ionization edge (e. g., L2) and the word ‘Atlas’. A particular set
of energy values is linked to this predefined scheme. To load a predefined
scheme for a special element, click the Periodic Table... button.
Energy values defining A particular set of energy values is linked to a predefined scheme. These
the image EELS series energy values are defined as follows:
∆EION threshold ionization energy ∆EION and ∆EMAX only determine the
indicating the beginning of the shape and the energy range of the
ionization edge displayed schematic spectrum and do
∆EMAX position of maximum intensity not influence the acquisition procedure
of the ionization edge with
energy window width
dE = 15 eV
START = 2∆EMAX - ∆EION
proposed energy loss value of the first image of the image EELS series
STOP = 2∆EION - ∆EMAX
proposed energy loss value of the last image of the image EELS series

User-defined schemes To define your own parameter set for an element, type a new name in the
Scheme field. The Edge field will then become an edit field which you can
use to specify the type of the ionization edge. The Delete and Save buttons
will be enabled. After loading a previously saved parameter set, the
spectrum diagram is updated immediately.
Save Click the Save button to save the present parameter set for a specific
element. To load an existing user-defined parameter set, insert the
corresponding element in the Element field. Then, all available parameter
sets associated with this element are listed in the Scheme list.
The Save button is only available if a new name is entered into the Scheme
field.
Delete Click the Delete button to delete a previously saved parameter set for a
80

specific element. To do so, enter the element into the Element field and
select the corresponding parameter set from the Scheme list.
The Delete button is only available if a user-defined parameter set exists for
the active element.
Diagram The diagram in the dialog box displays a spectrum of the required energy-
loss range. You can either display the whole energy range from 0-2000 eV
or only the energy range around the ionization edge. The Y values auto-
matically range from 0 to the maximum intensity of the displayed energy
range.
Show Spectrum Decide which spectrum should be displayed in the diagram in the Show
Spectrum group. You may display all three types of spectra simultaneously
and overlapping, but you cannot switch off all spectra at the same time. If
only one spectrum is left, the check box is not available anymore. In this
case, you have to display a second one before you are allowed to switch the
spectrum off.
Symbolic Select the Symbolic check box to display only a schematic energy-loss
spectrum. The schematic spectrum does not represent the real shape of the
selected ionization edge. Without exception, the ionization edges in the
schematic spectrum show a saw tooth shape with the ionization threshold
Image EELS, Acquisition...

energy at ∆EION and the maximum intensity at ∆EMAX. The schematic


spectrum of, e. g., a white line will thus not differ from the schematic
spectrum of, e. g., a delayed edge.
EELS atlas Select the EELS atlas check box to display the spectrum of the EELS atlas
belonging to the selected element and ionization edge. There is exactly one
spectrum available for each element and ionization edge.
If you use the Full range option to display the spectra in the diagram, the
EELS atlas spectra are not displayed with a linear Y scale. This is because
the ionization edges would not be visible due to the tremendous intensity of
the zeroloss peak.
Spectrum Select the Spectrum check box to work with your own reference spectra.
The contents of a specific spectrum buffer is displayed in the diagram. The
number of the spectrum buffer has to be specified in the field below the
Spectrum check box. The default spectrum buffer is the active one.
The Spectrum check box is only available if the specified spectrum buffer
contains a valid EELS spectrum. If the specified spectrum does not cover
the whole energy range, only a part of the spectrum will be displayed.
The following information is
indicated in the diagram of
the Image EELS Acquisition
dialog box:
z the energy-loss spectrum
z the energy range covered
by the image EELS series
(green rectangle)
z the current energy loss on
the microscope (blue
triangle at the top of the
diagram)
z the position of the
ionization edges, here for Fe
and Co.

81
Restrict the energy range Restrict the energy region being investigated to the range of an ionization
edge in order to decrease the acquisition time of an image EELS series.
Setting the energy range Use the mouse to change the given START and STOP energy loss values
for the image EELS for the image EELS series directly in the spectrum diagram. Before setting
series the energies, choose the element and the ionization edge.
To change the START energy, you first click at the left side of the green area
indicating the energy-loss range.
" A blue line cursor appears, the exact energy value is displayed
below the diagram and at the same time updated on the
microscope.
To change the energy value, drag the blue line cursor with the depressed
left mouse button to the desired energy position.
" The green-colored energy range will be extended by the diagram
cursor. Increasing the energy range will also increase the number
of images in the image EELS series. The current number is
continuously updated and displayed in the Frames required field.
" The associated energy value displayed will be continuously
updated on the microscope and displayed below the diagram.
EFTEM • Image EELS

For the precise positioning of the energy window, use the left and right
keyboard arrows.
" The energy range is shifted step by step in the corresponding
direction. The minimal energy increment depends on the current
microscope settings.
" It is not possible to move the energy loss beyond the energy range
displayed. To expand the energy range, change the energy scale
to Full range.
Note The START energy loss must always be less than the STOP energy loss.

Setting the energy loss You may also set the energy loss on the microscope via the remote control
on the microscope without changing the energy window position. Use this feature if you are
working in the live mode to find, e. g., the optimum position for the high
contrast image. To do so, activate the blue arrow at the upper side of the
diagram. Drag the arrow to the desired energy position.
" The energy loss on the microscope changes. The START and
STOP positions remain unchanged.
Element Label... Click the Element Label... button to indicate certain ionization edges in the
spectrum diagram. A periodic table will be displayed on screen where you
can select the desired elements simply by clicking on the corresponding
element symbols. Use this option to get an overview of the positions of
ionization edges occurring in the selected energy range.
Energy scale Change the displayed energy range of the spectrum diagram in the Energy
scale group.
Element region Select the Element region option to display the default energy range only
(including the selected ionization edge).
Full range Select the Full range option to see the entire energy range covered by the
spectrometer. If Full scale has been selected and the green-colored energy
interval has been shifted out of the energy region, the Element region option
will be disabled. You cannot choose this option until the two regions overlap
again.
You may use the Full range option to check the conditions for acquiring the
HCI images with an energy loss beyond the energy loss range of the image
82

EELS series.
Camera Control... The Camera Control dialog box is usually not available when a dialog box is
opened. Click the Camera Control... button to activate the Camera Control
dialog box in order to adjust the exposure time. To go back to the Image
EELS Acquisition dialog box, just click somewhere on the dialog box.
Energy increment Enter the energy interval between two adjacent images of the image EELS
series into the Energy increment field. The maximum-possible energy
interval is 100 eV.
Frame required The Frames required field displays the number of images the series consists
of. This number depends on the energy increment and the energy range and
is automatically updated when changing a relevant parameter.
Time required The Time required field displays the time needed for acquiring the whole
image EELS series. The time needed depends on the energy increment and
the energy range and is automatically updated when changing a relevant
parameter.

related topics
Camera Control... 56
Image EELS, Acquisition...

HCI at Enter the energy value for acquiring a high contrast image into the HCI at
field. As opposed to ESI series acquisition, HCI images are mandatory for
image EELS series. The system automatically acquires two HCI images,
one before the first image of the image EELS series, and one after the last
image of the image EELS series.
Why acquire HCI The High Contrast Image should enable you to select the image structures
images? for generating the image EELS spectra or to correct a possible specimen
drift.
Optimum energy-loss for The position of the maximum intensity of the ionization edge ∆EMAX is
HCI images proposed as default energy loss for the HCI image. You should choose an
energy loss where the structure-sensitive image contrast is high, but make
sure that the intensity range of the HCI image does not exceed the adjusted
dynamic range of the camera (to avoid saturation of the signal). This means,
the energy loss for the HCI image should not be much smaller than the
energy range of the image EELS series.
Acquire test spectrum Select the Acquire test spectrum check box to calculate a spectrum from a
specific specimen area during the acquisition of the image EELS series.
How to... How to acquire a test spectrum
1) Before using the Image EELS > Acquisition... command, choose an
empty spectrum buffer.
2) Use the Image EELS > Acquisition... command and set the
parameters.
3) Activate the blue rectangle in the diagram of the Image EELS
Acquisition dialog box.
4) Set an energy loss where the specimen structure is clearly visible.
5) Check the Acquire test spectrum check box.
" A circle is drawn into the image.
6) Resize and position the circle to select the image area for the test
spectrum. Choose a specimen area where a high element
concentration is presumed.
7) Click the right mouse button to return to the Image EELS Acquisition
dialog box.
8) Start the acquisition by clicking OK:

83
" After each image acquisition, the mean intensity value of the
selected circular area is calculated and displayed in the graph
document. The Y-Range of the spectrum is continuously updated.
OK Click OK to start a fully-automatic acquisition of the image EELS series.
Message boxes inform you on the ongoing procedure. You may terminate
the acquisition procedure at any time by clicking the Cancel button in one of
the message boxes.

Using an SIT camera


If you use an SIT-camera, the Image EELS Acquisition dialog box looks
slightly different. The features described below are only relevant for video
cameras.
Note All images of an image EELS series are to be recorded with the same gain
of the camera, i. e., you are not allowed to have the brightness and contrast
of the images automatically adjusted by the camera. Do not set the DAGE
SIT-camera to ’manual’ for example.
EFTEM • Image EELS

Before acquiring an Before recording a new image EELS series, check the offset of the camera
image EELS series and maximize the dynamic range. This is only necessary when using a video
camera.
Test... Click the Test... button in the Image EELS Acquisition dialog box to check
the energy range of the image EELS series and the image intensities. Click
the Test... button to start the test loop.
Energy The starting energy value will be the current
Start/Stop START value. Clicking on the Start button begins
Cancel the test run and as a result, the button changes its
functionality to Stop. All energy values of the
image EELS series will be sent to the microscope
in turn. When the test loop has reached the lowest
or highest energy value, the sequence of the test
loop will run in the reverse direction. Click the Stop
button to freeze the current energy loss and Cancel to terminate the test run.
Additional blacklevel Select the Additional blacklevel correction check box to correct a camera
correction offset while acquiring an image EELS series.
To perform an additional blacklevel correction, the first and the last image of
the series will be recorded using an unexposed camera. After acquisition
has been completed, the average will be taken from these two offset images
and subtracted from the ESI images.
Note Additional blacklevel correction should generally not be necessary. Use the
shading correction of the input channel to correct shading effects directly at
acquisition.
Check Blacklevel... Click the Check Blacklevel... button to adjust the offset intensity of your
camera.

Image EELS, Define Series


Use this command to assign single energy-filtered images to an image EELS series.

Definition A valid image EELS series consists of several energy-filtered images.


Each image of the series is linked with a special parameter set including the
meaning of the energy windows, the energy loss and the element under
84

investigation. The Image Information dialog box of all ESI images contains
an additional tab, the EFTEM Data tab.
Application It is not necessary to define an image EELS series explicitly:
• if you load an existing image EELS series using the Image EELS, Load
series... command, or
• if you acquire a new image EELS series using the Image EELS >
Acquisition... command.
In these cases, all necessary information is available. In particular, the
energy losses, the meaning of the image, the position of the images in the
image buffer box is known.
What will happen... After defining an image EELS series
• the EFTEM Data tab is added to all images of the series.
• all commands requiring a valid image EELS series will be available.

related topics
How to define an input channel for image EELS acquisition 13
How to adjust the blacklevel intensity: 58
Background approximation methods 5
Image EELS, Define Series

Note The newly defined image EELS series will not be saved automatically. Use
the EFTEM > Image EELS > Save Series... command to save the series in
a special series directory.
Before you use this Save and delete all images from the image manager. Load all images of the
command images EELS series into the image manager. Load the image with the
lowest energy loss first.

Preset Values If you load images that already have an EFTEM Data tab in the image
information, EsiVision will read out the relevant data. In this case the Image
EELS Define Series dialog box is already filled out.
First HCI image A valid image EELS series requires two high contrast images, one that is
Second HIC image acquired before the first image of the series, and one after the last image of
the series. In the HCI images the important image structures should be
clearly visible. They are used for correcting the specimen drift and selecting
image areas for spectrum calculation.
Use the arrow buttons next to the First / Second HCI image field to enter the
number of the image buffer that contains the first or the second HCI image.
HCI energy loss In the HCI energy loss field enter the energy loss of the two HCI images.
First series image Use the arrow buttons next to the First series image field to enter the number
of the image buffer of the image with the lowest energy loss.
Image number Use the arrow buttons next to the Image number field to enter the entire
number of images in the series. An image EELS series must at least

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comprise 5 images.
EsiVision automatically detects how many image buffers contain an image
and propose this value minus two high contrast images.
Start energy loss In the Start or End energy loss field enter the lowest and the highest energy
End energy loss loss. The energy loss of all in-between images are calculated assuming that
the images were acquired using equidistant energy steps.
Set EFTEM Data... Click the Set EFTEM Data... button to enter all data to be added to the image
information. You will find these data on the EELS Data tab.
Select Element... EsiVision offers a set of default energy-loss values for each element and
method. Use the Select Element... button to load predefined energy loss
values for a specific element.
OK Click OK to confirm the settings.
Plausibility check EsiVision will check whether the assigned values are possible. You will get
a warning message if entries are contradictory. Correct the entries and close
the Image EELS Define Series dialog box again. For example: the energy
loss of the W2 energy window must be smaller than the energy loss of the
MAX energy window. You cannot assign one image buffer twice, i. e., the
image buffers for two energy windows must be different.
EFTEM • Image EELS

Image EELS, Quality Check


Use this command to view all the images of an image EELS series.

Available This command is only available if a valid image EELS series is loaded.

What will happen... After calling the command, all the images of the active image EELS series -
including the HCI-images - are successively displayed onscreen. When the
display loop has reached the first or the last image of the series, the
sequence will start anew by displaying the first image.
Application When looking at the images, pay attention to a possible specimen drift. The
quality check is also suitable to determine visually whether the element of
interest is present.
Quality-check delay You can manually determine how long a single image of the series is
displayed onscreen. Use the EFTEM > Options... command to open the
Image EELS tab. Enter the desired time in ms in the Quality check delay
field. The preset value is 500 ms.
A message box displays the
current energy loss.

Start / Stop Click the Stop button to interrupt the quality-check loop with the current
energy loss. You may use the slider to display an image with another energy
loss.
Click the Start button to continue the quality-check loop.
Close Click the Close button to terminate the quality-check loop.

Image EELS, Drift Correction...


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Use this command to have a specimen drift corrected automatically in the whole image EELS series. If
necessary, you may correct the automatic shift values interactively.

Available This command is only available if a valid image EELS series is loaded.

Specimen drift during The acquisition of an image EELS series takes a long time. It is possible that
image EELS the specimen drifts during the acquisition. A specimen drift can be caused,
acquisition e. g., by thermal drift or narrow tears near the irradiated specimen area
which progress due to electron irradiation. Before creating a spectrum of
certain specimen structures, specimen drift has to be corrected (artifacts
decrease local resolution).
Image EELS, Drift There are two different methods available for the drift correction of image
Options EELS series on the Image EELS tab of the EFTEM Options dialog box.

related topics
Image EELS Options 76
Image EELS, Drift Correction...

• Choose the Linear, using high contrast images (faster) option to have
just the two high contrast images compared - for calculating a total
object drift.
• Choose the Individual, using every image (slower) option to have a drift
with respect to a reference image calculated for every single image of
the series. The reference image can be any image of the series
What will happen... • Linear Option
The system calculates how much the HCI image, recorded before
acquisition of the image EELS series, has shifted with respect to the
HCI image recorded after acquisition was completed. Because both
high contrast images are taken at the same energy loss, the contents
of the first HCI image should not differ considerably from the contents
of the second one, except for the object drift. After performing a pattern-
recognition routine via cross correlation, a uniform movement of the
specimen is assumed in order to calculate the displacement of every
single image of the series on the basis of the total object drift.
• Individual Option
The system will automatically compare the first high contrast image
with all the other images of the image EELS series. EsiVision applies a
pattern-recognition routine and calculates a shift according to the
reference image.
• When the calculation is complete, the difference image between the
compared images is displayed in the active viewport. Every shift of the
two images should be visible as a pseudo-topographical structure. Use
the arrow buttons in the Image EELS Drift Correction dialog box to
correct the remaining image shift interactively.
• You can subsequently perform the drift correction to every image of the
image EELS series that is shifted toward the reference image.
• After clicking on OK, the corrected images are substituted for the
original images of the image EELS series, i. e., they overwrite the
image buffers containing the original image.
• Lastly, the system reduces the image size of the image EELS images
by cutting the margins produced by an image shift.
After performing the Use the Image EELS, Save Series... command after performing a drift

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drift correction correction to store the corrected images on disk. When loading this image
EELS series later on you need not apply the Drift Correction... command
again.

related topics
Image EELS, Save Series... 88
EFTEM • Image EELS

Description of the dialog box

Reference image The Reference image field shows the currently used reference image.
EsiVision always uses the first high contrast image as reference image.
Shift image Use the Shift image scroll bar to scroll through all images of the image EELS
series. Choose one of the images, e. g., by clicking on the arrow buttons to
check and correct the calculated shift values with respect to the first high
contrast image. The system remembers the modified shift values until you
actually perform the drift correction by clicking on OK.
X shift The X and Y shift fields display the present shift values of the shift image
Y shift according to the first high contrast image. These shift values are used after
clicking on OK.
Arrow buttons Click the arrow buttons to shift the shift image in the indicated direction. The
image is shifted one pixel per click. The resulting difference image is
immediately displayed on screen. The shift values are updated accordingly.
Click the central button to reset the shift values to the calculated drift value.
Reset Click the Reset button to set both shift values to zero.
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OK Click OK to confirm the current shift values. All images of the image EELS
series are then shifted by the calculated values. The image sizes are
reduced accordingly.

Image EELS, Save Series...


Use this command to store an acquired image EELS series as a whole.

Available This command is only available if the image buffer box contains a valid
image EELS series.
What will happen... Each image EELS series has the following properties:
• Energy filtered images
The image EELS series comprises all images acquired using the
Image EELS > Acquisition... command.
• Directory of the image EELS series
Each image EELS series is situated in its own directory. The directory
is automatically created when saving the series.
Image EELS, Save Series...

• Folder name extension


The directory name is characterized by the extension IMG. This suffix
is added automatically by the system when saving the series.
• Series description
A description is automatically saved with the series. The description
consists of the ’image EELS series’ keyword, and the energy-loss
range. It is saved in a separate file in the image EELS series directory.
• File names
The saved image files are named automatically so that the image title
(e. g., VSOKA005) consists of the initials of the operator name (e. g.
VS), the element symbol (e. g., O), the symbol of the ionization edge
(e. g., K) and a consecutive number using an alphanumerical notation.
The operator name is read out from the microscope’s sheet film
camera. The HCI images are indicated by the letter ‘Z’ (e. g.,
VSOKAZ1).
Note Note that the Save Series... command does not save the spectra which
result from applying the Image EELS, Analyze... command.

Warning You have to use the Image EELS, Load series... command to load an
existing image EELS series. You cannot use the usual image series
commands, e. g., Image Series, Load... command (in the Image menu), for
an image EELS series. If you load the images separately, using the File >
Open... command, EsiVision will not recognize the series as a valid image
EELS series.

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Folder name Enter the Folder name, i. e., the name of the series you want to save.
Choose a name indicative of the folder’s contents in order to make it easier
to locate the series later on. There is no need to type in the expected folder
name extension IMG - the system will append it automatically. You can
choose the directory using the Look in list.
EFTEM • Image EELS

New Click the New button to save the new image EELS series under the specified
folder. The system will automatically append the extension IMG to the
directory name so that you can recognize a directory containing an image
EELS series at a glance.
OK Click the OK button to overwrite an existing image EELS series. If the
selected directory does not contain a valid image EELS series, you will get
an error message.
Description If you have selected a directory which already contains an image EELS
series, a short description of the series is displayed in the Description group.

Image EELS, Load Series...


Use this command to load an entire existing image EELS series from the disk. You may afterwards apply
any image EELS analyzing commands, e. g., you may perform a drift correction, calculate spectra of
certain user-defined specimen regions, or extra ESI series.

Warning The image EELS series will overwrite the images buffers.
If one of the required image buffers is write protected, you can either remove
the write protection before loading the image EELS series or terminate the
command.
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Folder name Specify the drive and directory containing the image EELS series you would
like to load in the Folder name field. When opening the dialog box, the
system automatically selects the image EELS series which had been loaded
last.
Description The Description group contains the most important information on the
selected image EELS series. If the selected directory does not contain a
valid image EELS series, the Description group disappears.
Image EELS, Analyze...

Image EELS, Analyze...


Use this command to create spectra of certain specimen areas by analyzing the image EELS series.

Available This command is only available if a valid image EELS series is loaded.

Warning The Image EELS, Analyze... command will overwrite the image buffer
following the last image of the series and a number of spectrum buffers.
If the image or spectrum is write protected, you can either remove the write
protection or terminate the command.
Analyzing an image To extract spectra from an image EELS series, you will have to perform two
EELS series steps.
1) You have to define image regions first. The image regions can be of
arbitrary shape and even overlap. The high contrast image is used for
defining the regions. The regions are then automatically applied to all
images of the image EELS series. You will get an online preview of the
spectrum.
2) The second step is to combine several regions to one spectrum. By this
you are capable of generating spectra of specimen areas which are not
even connected.
What will happen... • For each image of the image EELS series: the mean gray value of
regions assigned to one spectrum is calculated.
• The spectra, as well as their accompanying image regions, are drawn
into the image overlay. The spectra are displayed in the same color as
the corresponding image region.
• The spectra starting with spectrum #1 are subsequently written into the
spectrum buffer box starting with the currently active one.
Spectra properties • Spectrum name
The spectrum buffers are named automatically so that the spectrum
title consists of the term ’Image EELS’, the initials of the operator name
(e. g., CZ), the element symbol (e. g., O), the symbol of the ionization
edge (e. g., K) and the number of the spectrum (e. g., Spectrum 1). The
operator name is read out from the microscope’s sheet film camera.

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• Spectrum Information
The resulting spectrum can be treated like an ordinary energy-loss
spectrum, i. e., the Graph Information dialog box includes additional
tabs with special EFTEM data. All available information from the image
EELS series is used to fill in the EFTEM data fields.
Single-screen version If you are working on a single-screen version, make sure that image and
spectrum document do not overlap.
How to... How to generate spectra from an image EELS series:
You would like to investigate a specimen containing oxygen. It is assumed
that an image EELS series is loaded. This image EELS series consists of 30
images and comprises the energy range 480 eV - 588 eV, i. e., the oxygen
K-edge at 532 eV is included.
EFTEM • Image EELS

1) Use the Special > Preferences... command to select how to define the
circle. On the Measure tab, select the Define circle with 3 points check
box for defining circles via 3 points on their circumference. Clear this
check box for defining circles via center and radius.
2) Activate the dual monitor by clicking on the Dual tab in the Viewport-
Manager.
3) Be sure that all important spectra in the spectrum buffer box have been
saved.
4) Use the EFTEM > Image EELS > Analyze... command.
" The Image EELS Analysis dialog box is opened.
" A copy of the first high contrast image of the series is displayed on
the dual monitor.
The first high contrast image is copied from image buffer #1 to the
image buffer following the last image of the series.
" An empty spectrum document is displayed on the windows monitor.
The energy range is taken from the image series, e. g., in this case
the energy range is 480 eV - 590 eV.
Define the image areas 5) In the Image EELS Analysis dialog box select the Circle option in the
which should Region type group.
contribute to the 6) Click the Add button.
resulting spectra " A mouse cursor appears in the image.
" The Image EELS Analysis dialog box disappears in order not to
overlap the spectrum document.
7) Leftclick to display a circle in the image.
" The system will immediately calculate the resulting spectrum of the
active image area. The spectrum is displayed in the spectrum
document.
8) Move the mouse cursor to the approximate center of the circular image
area.
Keeping the left mouse button depressed, expand or reduce the
circular outline’s size with the mouse.
" The preview spectrum is continuously updated so that you can
interactively find the region with the highest element concentration.
9) Rightclick to confirm the first area.
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" All new areas are automatically assigned to a new spectrum. The
corresponding spectrum number is displayed in the overlay.
10) Repeat the last three steps to define more image areas.
11) Middleclick to return to the Image EELS Analysis dialog box.
12) Click the OK button to create the resulting spectra.
Further processing of 13) Use the Image EELS > ESI Mapping... command to extract an ESI
the image EELS series series from the image EELS series. Use the resulting spectra for
and spectra positioning the energy windows.

related topics
Image EELS, ESI Mapping... 97
Image EELS, Analyze...

Example of an image EELS


series where three different
image regions have been
analyzed. The bright region
contains iron, the
background does not.

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Define regions Define image areas which should contribute to spectra in the Define regions
group. You may add or remove individual image regions until you close the
dialog box with OK.
Region type Select the shape of the image area in the Region type group.
EFTEM • Image EELS

Particle Select the Particle option to use the Append Particles tool for defining the
image areas for the image EELS analysis. Note that the image areas
defined here are not relevant for the particle detection.
Circle Select the Circle option to define circular image areas. You can adjust the
position and the radius of the circular region. Use this option, e. g., to
investigate the element composition of round particles.
Rectangle Select the Rectangle option to define rectangular image areas. You can
adjust the position and the area of the rectangle.
Freehand Select the Freehand option to delineate specimen structures precisely which
are to contribute to the individual spectra. In the freehand mode, you may
either define line segments by leftclicking on the points of the line segments,
or you can draw the contour freehand by simply keeping the left mouse
button depressend while moving the mouse about. Rightclick to auto-
matically close the area.
Add Click the Add button to define the image areas contributing to the individual
spectra. The mouse pointer will appear in the image where you may define
the specified region type. Each image area is automatically assigned to
another spectrum. The number of the spectrum is drawn into the image
overlay.
Online spectrum preview The system calculates the spectrum inside the current region when defining
the image regions. This spectrum is continuously updated when changing
the image area.
When you use the Freehand option, there is no preview spectrum available.
Using the mouse Use the left mouse button to define the image region. Move the mouse to
position the active region.
Rightclick to set the active region.
Use the middle mouse button (middleclick) to return to the Image EELS
Analysis dialog box.
Delete Click the Delete button to definitively remove one of the already set image
regions. The mouse pointer appears in the image. Leftclick on the region
you want to remove.
This button is only available if there is at least one image region.
Define spectra Use the Define spectra group to determine which areas belong together and
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are to contribute to one spectrum. You may at any time add or remove
individual image regions to a spectrum until you close the dialog box via OK.
How to... How to assign the image areas to the spectra:
1) In the Define spectra group, select one of the spectra 1-6. The
spectrum number refers to the number of the spectrum buffer of the
resulting spectrum.
2) Click the Set button.
" A mouse cursor appears in the image.
3) Leftclick on every region that should contribute to the spectrum.
" The regions are colored in the spectrum color. The spectrum
number is also indicated.
4) Rightclick to return to the Image EELS Analysis dialog box.
File... Click the File... button to save or load a set of image regions. Use this feature
to apply standardized image areas to more than one image EELS series.
A previously-defined set of image areas is added to the image, i. e., existing
image areas are not deleted.
related topics
Parallel EELS Options 102
Image EELS, Analyze...

ESI contrast analysis Select the ESI contrast analysis check box to plot the ESI contrast of the
selected specimen areas against the energy loss. The contrast is
determined by the following formula:
standard deviation (of all gray values in the region)
ESI contrast = ----------------------------------------------------------------------------------------------------------------------------
mean value (of all gray values in the region)
Draw spectra into Select the Draw spectra into image overlay check box to add the image
image overlay areas and the resulting spectra to the image overlay after clicking OK. An
existing image overlay is not effected.
Clear the check box to add only the image areas to the image overlay. The
resulting spectra are only written into the spectrum buffer box.
OK Click OK to create the resulting spectra.

The Append Particles Tool

Action buttons Use the action buttons on the right hand side of the dialog box to select the
method for the definition of an image area. Confirm one area by clicking the
right mouse button.
Middle mouse button By using the middle mouse button or the [Esc] key you can end the definition of
[Esc] the area and return to the dialog box.
Methods for the Definition of an image area

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Button Using the mouse
Polygon Mark the end points of the partial sections: leftclick
Delete partial sections step-by-step: shift key + leftclick
Mark the last point, close polygon: rightclick
Interpolating Mark the end points of the partial sections: leftclick
Polygon Delete partial sections step-by-step: shift key + leftclick
End definition: rightclick
(The polygon is an interpolating ’’spline’’ curve. It links the defined image points so
that an continuous outline without angles appears.)
Freehand Mark the end point of the partial sections: leftclick
Polygon To draw freehand: hold left button depressed
Delete partial sections step-by-step: shift + leftclick
Mark last point, close polygon: rightclick
EFTEM • Image EELS

Ellipse Draw circle: depress left button and move mouse horizontally and vertically
Confirm circle: rightclick

Rectangle Draw rectangle with long and short side: depress left button and move mouse
horizontally and vertically
Confirm rectangle: rightclick
Rotated Draw rectangle in any position: depress left button and move mouse
rectangle Position rectangle/rotate: move mouse
To change between position and rotate mode: 1x leftclick
Confirm rectangle: rightclick
Magic Wand Mark starting point and define middle pixel value: 1x leftclick
Increase tolerance: depress left button and move mouse right
Decrease tolerance: depress left button and move left
Delete starting point and set new: 1x leftclick
Confirm particle: rightclick

Undo Use the last action button Undo to delete the last drawn area. Multiple
clicking deletes the last areas successively.
The Undo button lets you delete only areas which were defined during the
current Append Particles session.
Magic Wand Due to the fact that image EELS series are quite noisy, the Magic Wand
option is most probably not suitable. The magic wand assumes that there is
a coherent area with almost the same pixel values.
Color space For Image EELS series, the Color space option is not relevant.
Smoothing You can smooth the image before you use the magic wand. In this way,
image imperfections will be suppressed and the area will be rounder for
example. The rank filter serves as a smoothing filter. In this way, noise and
single bright or dull pixels and ’’shot noise’’ are filtered out. 50% is the fixed
rank value. Enter the size of the neighboring environment of the rank filter
into the Smoothing field. The smoothing filter is deactivated by using the
value 0. The larger the value, the larger the image areas with deviations, but
also with actual separating lines will be suppressed. Look for a smoothing
value with which imperfect pixels will be suppressed and the area rounded,
but which does not affect other areas.
Fill holes Mark the Fill holes check box to add pixels to the area which are spatially
within the area, but which have pixel values outside the threshold values. In
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this way you can fill differently colored inclusions or noise pixels within an
image structure. Undo the marking to produce areas with holes.
Outline The Outline check box is not relevant for image EELS.
OK With OK you close the dialog box. All old and new areas of the image will be
hatched blue-gray. If you have activated a classification scheme within the
framework of an area analysis, the areas will be filled with the color of their
classification. The overlay will be displayed completely.
Image EELS, ESI Mapping...

Image EELS, ESI Mapping...


Use this command to produce an element-distribution image by analyzing the energy-filtered images of
the image EELS series. This method is especially suited for analyzing ELNES structures in materials
science.

Available This command is only available if a valid image EELS series is loaded.

Warning The Image EELS > ESI Mapping... command will overwrite the image
buffers following the last image of the image EELS series.
If one of the required image buffer is write protected, you can either remove
the write protection or terminate the command.
How to create an The image EELS series consists of a tremendous amount of images with
element distribution different energy-loss values and, typically, a small energy width. In order to
create an element-distribution image, you have to choose specific images
from the image EELS series: one image containing element-specific
information, ∆EMAX, and at least one image containing unspecific
background information only (e. g., ∆EW2, ∆EW1). In the Image EELS ESI
Mapping dialog box, you can use the image EELS spectra created by the
Image EELS > Analyze... command to select the suitable images from the
image EELS series. You may also combine adjacent images to reduce the
noise.
Meaning of the different
energy windows ESI image Meaning
∆EW2, ∆EW1 position of the 1st or 2nd window below the edge
(∆EW2 < ∆EW1 < ∆EIO ).
The images are used for extrapolation of the
background intensity.
∆EMAX position of maximum intensity of the ionization edge
∆EWL position of the 2nd window beyond a white line
∆EIOi, i=1-3 positions of three energy windows beyond the
ionization edge used for the multi window method

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What will happen... After calling the Image EELS > ESI Mapping... command, an element-
distribution image is automatically calculated from the active image EELS
series. The element and the edge is taken from the series, the energy
windows from a predefined set of parameters for this special element.
Preview When you change the parameters in the Image EELS ESI Mapping dialog,
e. g., the background-fitting method or the position of the energy windows,
the resulting element-distribution image is calculated immediately. A
preview is displayed in the active viewport.
When an image EELS spectrum is displayed in the dialog box, the back-
ground curve is also shown. The background curve is continuously updated
when changing the background approximation method or the position of the
energy windows.
Results of ESI Mapping After closing the Image EELS ESI Mapping dialog box via OK, a new ESI
series is created. You may use all commands of the ESI submenu to save
or analyze the series.
In addition, an element-distribution image is automatically created. It is
related topics
ESI, Analyze... 67
EFTEM • Image EELS

possible to create a presentation image, too. To do so, select the Always


calculate presentation check box on the ESI tab (in the EFTEM Options
dialog box). In this case, the ESI > Presentation... command is called auto-
matically. Use the ESI > Combine Images... command to superimpose one,
two, or three element-distribution images onto the HCI image. The resulting
image enables you to link specimen structures and element distribution.
Destination image buffer The resulting images are put into the image buffers that follow the last image
of the image EELS series.
Description of the dialog box
The Image EELS ESI Mapping dialog box is organized in the same way as
the acquisition dialog boxes.
Before you use this To optimize the signal to noise ratio for the desired element, use the EFTEM
command > Image EELS > Analyze... command first to calculate a spectrum of an
image region that contains the element. Display this spectrum in the Image
EELS ESI Mapping dialog box. To do so, select the Spectrum check box and
enter the number of the spectrum buffer.
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Preset settings Upon opening the Image EELS ESI Mapping dialog box, the element, edge,
and energy range are automatically loaded from the active image EELS
series.

related topics
ESI, Presentation... 69
ESI, Combine Images... 73
Image EELS, ESI Mapping...

Element The element from the active image EELS series is displayed in the Element
field. The element and its ionization edge were set when acquiring the image
EELS series.
Investigating two You will usually not change the element, but you may enter any other
elements in one image element provided the energy windows of the selected element are within the
EELS series energy range of the image EELS series. Take this into consideration when
acquiring the image EELS series: If you want to extract two ESI series from
one image EELS - in order to create two element-distribution images - the
energy of the image EELS series has to comprise both ionization edges.
Example In order to investigate the elements nickel and iron with one image EELS
series, the energy range should be at least 660 - 860 eV (Fe, L3: 708 eV, Ni,
L3: 850 eV).
Periodic table... Use the Periodic table... button to open a dialog box showing the periodic
table of elements. To select an element, simply click on the desired element
button and confirm your choice with OK.
The quick info displays the full element name and the ionization edges
below 2000 eV.
Edge The Edge field specifies the ionization edge of the element. The element
and its ionization edge were set when acquiring the image EELS series.
Slit width The Slit width field displays the slit width of the microscope when acquiring
the current image EELS series. The width of the energy windows displayed
in the spectrum diagram depend on the slit width.
Scheme The Scheme list offers all available parameter sets for the active element.
The scheme includes only the position of the energy windows, the other
settings of the dialog box, e. g., the window width cannot be saved in a
separate file. The parameter set is connected with the ionization edge and
has been defined when acquiring the image EELS series. You are only able
to choose another scheme if the energy windows of the selected scheme
are within the energy range.
User-defined schemes To define your own scheme for an element, type a new name in the Scheme
field. The Delete and Save buttons will be enabled. After loading a
previously saved scheme, the energy positions in the spectrum diagram are
updated and the window width is reset to the slit width.

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Method The selected Method determines the amount of images and the position of
the energy losses. The images of the image EELS series with suitable
energy losses are assigned to the energy windows required by the selected
method. The energy windows will be immediately displayed in the spectrum
diagram. The proposed energy values are empirical values resulting in an
optimum background stripping for the selected method, e. g., the 3 window
method. However, you may change the position of the energy windows to
adjust the method to the actual spectrum.
Required ESI images for the
different background Method required ESI images
approximation methods
2 window ∆EW1, ∆EMAX
3 window ∆EW2, ∆EW1, ∆EMAX
3 window white line ∆EW1, ∆EMAX, ∆EWL

related topics
Image EELS, Acquisition... 78
How to acquire an ESI-image series 9
Background approximation methods 5
EFTEM • Image EELS

multi window ∆EW2, ∆EW1, ∆EIO1, ∆EIO2, ∆EIOz


all possible windows ∆EW2, ∆EW1, ∆EIO1, ∆EIO2, ∆EIO3,
∆EMAX, ∆EWL

Background The Background approximation list offers several methods for extrapolating
approximation background intensity. Select the one desired from the list.
Preview functions The resulting background spectrum is immediately calculated and displayed
in the spectrum diagram if an image EELS spectrum is shown. The resulting
element-distribution image is displayed onscreen.
Processing Background intensity at the ionization edge is calculated for each image
pixel. You determine how the background intensity image is used in the
Processing group.
Difference Select the Difference option to subtract the background intensity image from
the image at the ionization edge.
Ratio Select the Ratio option to divide the image at the ionization edge by the
background-intensity image.
Diagram The diagram in the dialog box displays a spectrum of the required energy-
loss range. The energy range of the spectrum in the diagram equals the
energy range of the active image EELS series. The Y range is automatically
optimized.
Show Spectrum Decide which spectrum should be displayed in the diagram in the Show
Spectrum group. You may display all three types of spectra (simultaneously)
and overlapping, but you cannot switch off all spectra at the same time. If
only one spectrum is left, the check box is no longer available. In this case,
you must display a second one before you are allowed to switch the
spectrum off.
Symbolic Select the Symbolic check box to display a schematic energy-loss spectrum
only. The schematic spectrum does not represent the real shape of the
selected ionization edge. Without exception, the ionization edges in the
schematic spectrum show a saw tooth shape with the ionization threshold
energy at ∆EIO1 and the maximum intensity at ∆EMAX. So the schematic
spectrum of, e. g., a white line will not differ from the schematic spectrum of,
100

e. g., a delayed edge.


EELS atlas Select the EELS atlas check box to display the spectrum of the EELS atlas
belonging to the selected element and ionization edge. There is exactly one
spectrum available for each element and ionization edge.
Spectrum Select the Spectrum check box to display a spectrum calculated from the
image EELS series. The number of the spectrum buffer has to be specified
in the field below the Spectrum check box. The default spectrum buffer is the
active one.
Checking the It is recommended to use this option to find the optimum position of the
background fitting energy windows. Using an image EELS spectrum you may:
• position the energy window ∆EMAX precisely at the actual maximum of
the element-specific peak.
• check the background correction because the system continuously
computes and calculates the background spectrum. For the three
windows method, vary the position and width of the energy windows
∆EW2 and ∆EW1 until the optimum background fit was found.
Image EELS, ESI Mapping...

The following information is


indicated in the diagram of
the Image EELS ESI
Mapping dialog box:
z an energy-loss spectrum
including the energy range
of the image EELS series
(red, blue or magenta
curve).
z the position and the width
of the various energy
windows (green rectangles).
z the calculated background
spectrum for the current
positions of the energy
windows.

Selecting the images for Use the mouse to select the images for the ESI series from the image EELS
the ESI series series in the spectrum diagram directly.
To assign an image from the image EELS series to a special energy window,
you first activate the energy window, e. g., W2, by simply clicking on the
corresponding green rectangle.
" A blue line cursor appears, the energy-loss value is displayed
below the diagram
To select an image, drag the blue line cursor with the left mouse button
depressed to the desired energy-loss value.
" The green-colored columns will trace the diagram cursor. EsiVision
will assign the image with the selected energy loss to the activated

101
energy window.
Window Width You can combine successive images to one image of the resulting ESI
series in the Window Width group. This can be useful for increasing the
intensity at element-specific peaks, or for reducing the noise for better
background subtraction.
To increase the accuracy of the element-distribution image, the background
is calculated for each MAX window separately. The resulting energy-
distribution images are added to get the final element-distribution image.
Window All energy windows are listed in the Window list that are required for the
selected background approximation method. Select the energy window for
which you wish to increase the energy width.
Meaning of the different
energy windows ESI image Meaning
∆EW2, ∆EW1 position of the 1st or 2nd window below the edge
(∆EW2 < ∆EW1 < ∆EIO ).
The images are used for extrapolation of the
background intensity.
EFTEM • Parallel EELS

∆EMAX position of maximum intensity of the ionization edge


with a width of the energy window dE = 15 eV
∆EWL position of the 2nd window beyond a white line
∆EIOi, i=1-3 positions of three energy windows beyond the
ionization edge used for the multi window method

Images Enter the number of images the system should combine into the Images
field. For example, enter 2 to take the average of two successive images.
OK Click OK to extract the ESI series from the image EELS series.

Parallel EELS
Use this command for recording an EELS by means of a camera or, alternatively, for subsequently
analyzing an existing image of an EELS.

Definition In the following, the term spectrum denotes the graphical plot of the
intensity values versus the energy-loss values. To avoid confusion with the
electron energy-loss spectrum generated in the energy-dispersive plane of
the microscope, the latter will be called EELS. The EELS can be recorded
in the spectrum mode by a camera.

Parallel EELS Options


Use the EFTEM > Options... command to open the EFTEM Options dialog box. Use the Parallel EELS
tab to define some general options for the parallel EELS method.
102
Parallel EELS

Camera Options considered by the parallel EELS acquisition commands are


specified in the Camera group. The acquisition parameters are set by the
active logical input. For example, you should switch off any binning to get
the full spatial resolution of the camera and thus an optimum energy
resolution.
Preferred Select the name of the input channel that is to be used for the acquisition of
parallel EELS from the Preferred list. As soon as you call the Parallel EELS
> Acquisition... > Wide Range Acquisition... or Calibration... command, the
active input channel is replaced by the input channel specified in this list.
(none) Choose the none entry to not automatically change the active input channel.
Align with live mode Select the Align with live mode check box to switch on the live mode as soon
as the acquisition or calibration dialog box opens. Use the live image to
control the spectrum acquisition visually. It is strongly recommended to
enable the live mode.
Preprocessing A series of macro steps can be defined in an input. The macro is performed
Postprocessing before or after image acquisition. Use the Preprocessing or Postprocessing
list to specify at which points of the acquisition process these steps are to be
performed.
For example, you can use the pre- and postprocessing feature to have the
final fluorescent screen automatically be raised before acquiring a spectrum.
Always Using the Preprocessing or Postprocessing list you determine whether the
Never pre- or postprocessing steps should be performed for every image of the
series (Always), or for no image of the series (Never).
Calibration The parameters in the Calibration group are used when calibrating the
spectrum. For determining the energy dispersion and the energy loss
position, the zeroloss peak is used. Usually the intensity of the zeroloss
peak is some orders of magnitude higher than the intensity of the residual
spectrum. Therefore, the exposure time and the illumination aperture have
to be adapted.
Acquisition time Enter the exposure time for acquiring the zeroloss peak into the Acquisition
time field. The system uses the zeroloss to calibrate the energy dispersion
of a given spectrum magnification. When the zeroloss is displayed, the
system automatically takes the exposure time entered into this field. You

103
should enter a short exposure time, e. g., 50 ms, to avoid overexposures or
damaging the camera.
Use lowest illumination Select the Use lowest illumination aperture check box to reduce the
aperture illumination aperture when acquiring the zeroloss peak.
Wide range parallel The parameters in the Calibration group are used when using the EFTEM >
EELS Parallel EELS > Wide Range Acquisition... command.
Acquisition delay For acquiring a wide range parallel EELS spectrum, several images are
taken. Each image comprises a different energy loss region. Into the
Acquisition delay field enter the time in [ms] the system should wait after the
energy loss region is changed and another image is taken. The delay time
guarantees stable microscope conditions. One reason for the delay time is
the afterglow of the fluorescence screen. The delay time makes sure that the
whole intensity of the spectrum region acquired before is decayed before the
next energy region is acquired. If you use a YAG scintillator, you will need a

related topics
How to define an input channel for ESI acquisition 7
Parallel EELS, Calibration... 118
EFTEM • Parallel EELS

longer delay time.


The default setting is 500 ms. The minimum acquisition delay time is
100 ms, the maximum 10 s (= 10000 ms).
Upper intensity limit The lower the energy loss, the higher is the intensity. When acquiring a wide
Lower intensity limit range parallel EELS, EsiVision has to adjust the intensity of two adjacent
spectrum regions. As soon as the intensity is higher than the upper limit,
EsiVision first halves the exposure time. If the intensity is still higher than the
allowed maximum intensity, EsiVision reduces the illumination aperture.
The limits are specified as a percentage of the maximum camera gray value.
The preset value for the Upper intensity limit is 80% of the maximum gray
value of the camera. The preset value for the Lower intensity limit is 5% of
the maximum gray value of the camera.

Parallel EELS, Acquisition...


Use this command for speedy parallel recording of energy-loss spectrum. The energy-loss spectrum is
acquired at high resolution. The image intensity is directly transformed into an energy-loss spectrum.

Available The Parallel EELS > Acquisition... command is only available if the remote
control is activated.

Warning This command will overwrite the active image and spectrum buffer.
If the image or spectrum is write protected, you can either remove the write
protection or terminate the parallel EELS acquisition.
You may also The Parallel EELS > Acquisition... command is also available on the EFTEM
button bar.

Parallel EELS Options There are some general settings for all parallel EELS acquisitions which are
summarized on the Parallel EELS tab in the EFTEM Options dialog box.
Before using this Before using the Parallel EELS > Acquisition... command, make sure to use
command a small filter entrance diaphragm to select the specimen area you want to
investigate or use the spot / Diff. mode.
Online shading EELS images should always be recorded with online shading correction
correction activated. Otherwise, flatfield contributions of the gain image may appear as
104

intensity variations of the EELS.


To switch on the online shading correction, use the Image > Set Input...
command to select a suitable input and use the Image > Configure Input...
command to modify the input. The Shading correction group is located on
the Input tab.
Energy calibration The energy range displayed depends on the acceleration voltage, the
energy-loss value and energy dispersion adjusted on the microscope, i. e.,
on the magnification of the EELS on the camera target. To get properly
calibrated spectra, you have to calibrate the energy axis for each
magnification and acceleration voltage. The calibration data is automatically
stored in a calibration list.
Note Note that the energy calibration also depends on the binning mode of the
camera. A camera using 2x2 binning uses other calibration values than a
camera using no binning. EsiVision will prompt you to calibrate the PEELS
when you change the input channel.
Calculating the The spectrum is calculated from a rectangular image area - a ROI (Region
spectrum Of Interest). The ROI can also be rotated relative to the image sides. The
spectrum is the intensity distribution as a function of energy loss. EsiVision
Parallel EELS, Acquisition...

takes the average of all columns vertical to the energy axis. Every column
of the ROI at a certain energy-position corresponds to a particular energy
channel. The width of the ROI defines how many values are averaged when
calculating the spectrum. The length of the ROI defines the energy range of
the resulting spectrum. The energy scale of the resulting spectrum will be
automatically adjusted to the active energy dispersion.
Resulting spectrum All spectra processing functions provided by the Graph menu can be applied
to the resulting spectrum afterwards.
Spectrum name The spectrum buffers are named automatically so that the spectrum title
consists of the term ’Parallel EELS’, the element abbreviation, and the
ionization edge.
Spectrum Information The resulting spectrum can be treated like an ordinary energy loss
spectrum, i. e., the Graph Information dialog box includes additional tabs
with special EFTEM data.

Description of the dialog box


The Parallel EELS Acquisition dialog box is organized in the same way as
the other acquisition dialog boxes.

105

Preset settings Upon opening the Parallel EELS Acquisition dialog box, the system auto-
matically loads the parameters which were used for recording the last
parallel EELS.
Settings on the Please be aware that the following settings on the microscope are changed
microscope automatically by the remote control as well:
EFTEM • Parallel EELS

• The energy loss is set to the currently active CENTER energy.


• The spectrum magnification is altered corresponding to the
magnification of the last parallel EELS.
Element Enter the element you want to investigate into the Element field. Only
internationally standardized abbreviations are accepted.
Periodic table... Use the Periodic table... button to open a dialog box showing the periodic
table of elements. To select an element, simply click on the desired element
button and confirm your choice via OK.
The quick info displays the full element name and the ionization edges
below 2000 eV.
Edge The Edge field specifies the ionization edge of the selected element. As far
as predefined parameter sets are concerned, this field is only for information
purposes. For user-defined parameter sets, you can enter the edge type.
Scheme The Scheme list offers all available parameter sets for the active element.
This parameter set for parallel EELS acquisition includes the center energy
of the energy range.
Diagram The diagram in the dialog box displays a spectrum of the required energy
loss range. You can either display the whole energy range from 0-2000 eV
or the energy range around the ionization edge only. The Y values auto-
matically range from 0 to the maximum intensity of the displayed energy
range.
Show Spectrum You decide which spectrum should be displayed in the diagram in the Show
Spectrum group. You may display all three types of spectra simultaneously
and overlapping, but you cannot switch off all spectra at the same time. If
only one spectrum is left, the check box is not available anymore.
Symbolic Select the Symbolic check box to display a schematic energy-loss spectrum
only. The schematic spectrum does not represent the real shape of the
selected ionization edge. Without exception, the ionization edges in the
schematic spectrum show a saw tooth shape, with the ionization threshold
energy at ∆EION and the maximum intensity at ∆EMAX. The schematic
spectrum of, e. g., a white line will thus not differ from the schematic
spectrum of, e. g., a delayed edge.
EELS atlas Select the EELS atlas check box to display the spectrum of the EELS atlas
106

belonging to the selected element and ionization edge. There is exactly one
spectrum available for each element and ionization edge.
Spectrum Select the Spectrum check box to work with your own reference spectra.
The contents of a specific spectrum buffer is displayed in the diagram. The
number of the spectrum buffer has to be specified in the field below the
Spectrum check box. The default spectrum buffer is the active one.
The Spectrum check box is only available if the specified spectrum buffer
contains a valid EELS spectrum.
Parallel EELS, Acquisition...

The following information is


indicated in the diagram of
the Parallel EELS
Acquisition dialog box:
z the energy-loss spectrum
z the energy range covered
by the parallel EELS at the
current spectrum
magnification (green
rectangle)
z the current energy loss on
the microscope (blue
triangle at the top of the
diagram)

Significant energy values You can select the following energy values in the spectrum diagram
of a parallel EELS START first energy loss of the parallel EELS
CENTER this energy loss is actually set on the microscope.
The CENTER energy is the energy loss of the active
ionization edge and must not necessarily be the actual
center energy loss.
STOP last energy loss of the parallel EELS
CURRENT an energy loss outside the energy range of the parallel
EELS.
This energy loss is set on the microscope.

Shifting the parallel The energy range of a parallel EELS is fixed by the spectrum magnification,
EELS you may however use the mouse to shift the whole parallel EELS in the
spectrum diagram directly.
To select one of the significant energy-loss values of the parallel EELS, click
at the position of the energy loss, e. g., click at the middle of the green area
to select the CENTER energy.

107
" A blue line cursor appears, the exact energy value is displayed
below the diagram and simultaneously updated on the microscope.
To change the energy value, drag the blue line cursor with the left mouse
button depressed to the desired energy position.
" The whole energy range will move to the new energy loss.
" The CENTER energy loss will be continuously updated on the
microscope and displayed below the diagram.
" You are allowed to move the parallel EELS to any energy loss.
Change the energy scale to Full range to have the full energy range
of the energy filter displayed.
Setting the energy loss You may also set the energy loss on the microscope via the remote control
on the microscope without shifting the parallel EELS. To do so, activate the blue arrow at the
upper side of the diagram. Drag the arrow to the desired energy position.
" The energy loss on the microscope changes. The energy position
of the parallel EELS in the diagram remains unchanged.
EFTEM • Parallel EELS

Element Label... Click the Element Label... button to indicate certain ionization edges in the
spectrum diagram. A periodic table will be displayed onscreen where you
can select the desired elements simply by clicking the corresponding
element symbols. Use this option to get an overview of the positions of
ionization edges occurring in the energy range selected.
Energy scale You change the displayed energy range of the spectrum diagram in the
Energy scale group.
Element region Select the Element region option to display the default energy range only
(including the selected ionization edge).
Full range Select the Full range option to see the entire energy range covered by the
spectrometer. If Full scale has been selected and the parallel spectrum has
been shifted out of the energy region, the Element region option will be
disabled. You cannot choose this option until the two regions overlap once
again.
Camera Control... The Camera Control dialog box is usually not available when a dialog box is
opened. Click the Camera Control... button to activate the Camera Control
dialog box in order to adjust the exposure time. To go back to the Parallel
EELS Acquisition dialog box just click somewhere on the dialog box.
Time integration Select the Time integration check box to combine an averaged linescan with
time integration. Snapshots will be taken successively and all spectra
recorded will be averaged.
Note When the Time integration check box is selected, the energy loss on the
microscope is fixed during the acquisition.

Limit integration to ... Select the Limit integration to check box to give a maximum number of
Cycles frames that are averaged when acquiring the spectrum. Enter the number of
frames into the Cycles field.
Use this option to get comparable spectra from different image regions. The
check box is only available when the Time integration check box is selected.
Spectrum Use the Spectrum magnification slider to enter the desired magnification of
magnification the spectrum. You can only select spectrum magnifications with valid
calibration data.
When changing the spectrum magnification in the dialog, the spectrum
magnification on the microscope is also updated via remote control.
108

Date The date of the last calibration is shown beside the slider.
Calibrate... Click the Calibrate... button to update the energy calibration for the selected
spectrum magnification. You may also use the Parallel EELS > Calibration...
command instead.
Test... Click the Test... button to check the position of the ROI. Use this feature if
the spectrum has been shifted after the last spectrum calibration. You
cannot change the position of the ROI in the image, but you may shift the
whole spectrum with respect to the position of the ROI.
What will happen... After clicking the Test.... button, an acquisition routine is started: A snapshot
is made and the current acquisition ROI is displayed as a red rectangle in
the overlay of the image. Then the next snapshot is taken and the ROI is
displayed and so on. The CENTER energy is indicated. A dialog box is
opened simultaneously.

related topics
Camera Control... 56
Parallel EELS, Calibration... 118
Parallel EELS, Acquisition...

Before starting the parallel


EELS acquisition, you may
check whether the spectrum
still lies inside the current
ROI.

Test, Align Spectrum Click the Align Spectrum button to correct a possible energy shift via remote
control. The energy loss on the microscope will be set to 0 eV and the Align
Spectrum tool is opened. If the Use lowest illumination aperture check box
is selected in the EFTEM Options > Parallel EELS tab, EsiVision will
automatically reduce the exposure time and illumination aperture. This
option avoids overexposure of the camera when the zeroloss peak is
acquired.
The system takes successive snapshots. After each snapshot, the ROI with
the CENTER energy loss is displayed. Use one of the arrow buttons to
position the zeroloss exactly on the center energy. Click the Close button to
return to the Parallel EELS Acquisition dialog box.
Use the Align Spectrum tool
to shift the spectrum into the
current ROI. The arrow
buttons control the
spectrum shift coils on the
microscope. Use the vertical
direction first, and the
horizontal direction
afterwards.

Test, OK Click OK in the message box if the ROI is properly aligned. The system will 109
return to the Parallel EELS Acquisition dialog box and switch back to the live
mode.
OK Click OK to start the parallel EELS acquisition. The resulting spectrum is
displayed in the spectrum document and the following dialog box is opened.
The ionization edge under investigation and the current energy loss is
indicated.
EFTEM • Parallel EELS

Parallel EELS If the Time integration check box is selected and no limit is set, an averaged
Acquisition, Stop linescan is combined with a time integration. Snapshots will be taken
successively and all the spectra recorded will be averaged. Click the Stop
button when you are satisfied with the spectrum.
If the Time integration check box is selected and a limit is set, EsiVision will
automatically stop the acquisition when the number of frames given in the
Cycles field are acquired. The Stop button changes its functionality to Start.
If the Time integration check box is not selected, one spectrum after another
is calculated by an averaged linescan over the ROI. Click the Stop button to
keep the current spectrum and stop the acquisition.
Parallel EELS If the Time integration check box is selected, the number of averaged
Acquisition, Integration snapshots are indicated in the Integration count field.
count
Parallel EELS Click the Next Acquisition button to return to the Parallel EELS Acquisition
Acquisition, Next dialog box. The resulting spectrum will be written into the next spectrum
Acquisition buffer.
Parallel EELS Click OK to finish the acquisition. The resulting parallel spectrum is written
Acquisition, OK into the active image buffer. The active image buffer contains the EELS
image with the analyzed ROI in the image overlay.

Parallel EELS, Wide Range Acquisition...


Use this command for speedy parallel recording of user-defined ranges of the energy-loss spectrum.
The energy-loss spectrum is acquired at high resolution. The image intensity is directly transformed into
an energy-loss spectrum. To cover a wide energy loss range, the resulting spectrum consists of several
individual spectra that are acquired with a small energy loss overlap started with the highest energy loss.
EsiVision automatically adjusts the intensities of the spectra by reducing the exposure time and
illumination aperture.

Available The Parallel EELS > Wide Range Acquisition... command is only available
if the remote control is activated.

Warning This command will overwrite the active image and spectrum buffer.
If the image or spectrum is write protected, you can either remove the write
110

protection or terminate the parallel EELS acquisition.


You may also The Parallel EELS > Wide Range Acquisition... command is also available
on the EFTEM button bar.

Parallel EELS Options There are some general settings for all parallel EELS acquisitions which are
summarized on the Parallel EELS tab in the EFTEM Options dialog box.
Before using this Before using the Parallel EELS > Wide Range Acquisition... command you
command should use a small filter entrance diaphragm to select the specimen area
you want to investigate or use the spot / Diff. mode.
Online shading EELS images should always be recorded with online shading correction
correction activated. Otherwise, flatfield contributions of the gain image may appear as
intensity variations of the EELS.
To switch on the online shading correction, use the Image > Set Input...
command to select a suitable input and use the Image > Configure Input...
command to modify the input. The Shading correction group is located on
the Input tab.

related topics
Parallel EELS Options 102
Parallel EELS, Wide Range Acquisition...

Energy calibration The energy range displayed depends on the acceleration voltage, the
energy-loss value, and energy dispersion adjusted on the microscope, i. e.,
on the magnification of the EELS on the camera target. To get properly-
calibrated spectra, you have to calibrate the energy axis for each
magnification and acceleration voltage. The calibration data is automatically
stored in a calibration list.
Note Note that the energy calibration also depends on the binning mode of the
camera. A camera using 2x2 binning uses other calibration values than a
camera using no binning. EsiVision will prompt you to calibrate the PEELS
when you change the input channel.
Calculating the The spectrum is calculated from a rectangular image area - an ROI (Region
spectrum Of Interest). The ROI can also be rotated relative to the image sides. The
spectrum is the intensity distribution as a function of energy loss. EsiVision
takes the average of all columns vertical to the energy axis. Every column
of the ROI at a certain energy-position corresponds to a particular energy
channel. The width of the ROI defines how many values are averaged when
calculating the spectrum. The length of the ROI defines the energy range of
the resulting spectrum. The energy scale of the resulting spectrum will be
automatically adjusted to the active energy dispersion.
Resulting spectrum All spectra processing functions provided by the Graph menu can be applied
to the resulting spectrum afterwards.
Spectrum name The spectrum buffers are named automatically so that the spectrum title
consists of the term ’Parallel EELS’, the element abbreviation and the
ionization edge.
Spectrum Information The resulting spectrum can be treated like an ordinary energy loss
spectrum, i. e., the Graph Information dialog box includes additional tabs
with special EFTEM data.

111
EFTEM • Parallel EELS

Description of the dialog box


The Wide Range Parallel EELS Acquisition dialog box is organized in the
way same as the other acquisition dialog boxes.

Preset settings Upon opening the Wide Range Parallel EELS Acquisition dialog box, the
112

system automatically loads the parameters which were used for recording
the last parallel EELS.
Settings on the Please be aware that the following settings on the microscope are changed
microscope automatically by the remote control as well:
• The energy loss is set to the currently active CENTER energy.
• The spectrum magnification is altered corresponding to the
magnification of the last parallel EELS.
Element Enter the element you want to investigate into the Element field. Only
internationally standardized abbreviations are accepted. If you want to
calculate an element ratio from the spectrum, choose the element with the
higher ionization energy. For example, if there is oxygen and iron in the
specimen, choose Fe. The resulting spectrum will then comprise the iron L3
ionization edge at 708 eV and the oxygen K ionization edge at 532 eV.
Periodic table... Use the Periodic table... button to open a dialog box showing the periodic
table of elements. To select an element, simply click the desired element
button and confirm your choice via OK.
The quick info displays the full element name and the ionization edges
below 2000 eV.
Parallel EELS, Wide Range Acquisition...

Edge The Edge field specifies the ionization edge of the selected element. As far
as predefined parameter sets are concerned, this field is only for information
purposes. For user-defined parameter sets, you can enter the edge type.
Scheme The Scheme list offers all available parameter sets for the active element.
This parameter set for parallel EELS acquisition includes the center energy
of the energy range.
Diagram The diagram in the dialog box displays a spectrum of the required energy
loss range. You can either display the whole energy range from 0-2000 eV
or the energy range around the ionization edge only. The Y values auto-
matically range from 0 to the maximum intensity of the displayed energy
range.
Show Spectrum You decide which spectrum should be displayed in the diagram in the Show
Spectrum group. You may display all three types of spectra (simultaneously)
and overlapping, but you cannot switch off all spectra at the same time. If
only one spectrum is left, the check box is not available anymore.
Symbolic Select the Symbolic check box to display a schematic energy-loss spectrum
only. The schematic spectrum does not represent the real shape of the
selected ionization edge. Without exception, the ionization edges in the
schematic spectrum show a saw tooth shape, with the ionization threshold
energy at ∆EION and the maximum intensity at ∆EMAX. The schematic
spectrum of, e. g., a white line will thus not differ from the schematic
spectrum of, e. g., a delayed edge.
EELS atlas Select the EELS atlas check box to display the spectrum of the EELS atlas
belonging to the selected element and ionization edge. There is exactly one
spectrum available for each element and ionization edge. Note that a non-
linear Y-range is used if the Element region option is selected from the
Energy scale group. In this case, the spectrum is splitted in such a way that
the low loss region including the zeroloss peak and the energy range of the
ionization edge are both visible.
Spectrum Select the Spectrum check box to work with your own reference spectra.
The contents of a specific spectrum buffer is displayed in the diagram. The
number of the spectrum buffer has to be specified in the field below the
Spectrum check box. The default spectrum buffer is the active one.
The Spectrum check box is only available if the specified spectrum buffer

113
contains a valid EELS spectrum.
EFTEM • Parallel EELS

The following information is indicated in the diagram of the Wide Range


Parallel EELS Acquisition dialog box:
z the energy-loss spectrum
z the energy range covered by the parallel EELS (green rectangle)
z the current energy loss on the microscope (blue triangle at the top of the
diagram)
Significant energy values You can select the following energy values in the spectrum diagram:
of a parallel EELS START first energy loss of the parallel EELS
STOP last energy loss of the parallel EELS
CURRENT an energy loss outside the energy range of the parallel
EELS.
This energy loss is set on the microscope.

Defining the energy The proposed energy loss range includes the zeroloss peak because the
range of the wide range zero is necessary for the spectrum deconvolution. You may of course
parallel EELS interactively decrease or increase the energy loss range in the diagram of
114

the dialog box:


To select one of the significant energy-loss values of the parallel EELS, click
at the position of the energy loss, e. g., click at the beginning of the green
area to select the START energy.
" A blue line cursor appears, the exact energy value is displayed
below the diagram and simultaneously updated on the microscope.
To change the energy value, drag the blue line cursor with the pressed left
mouse button to the desired energy position.
" The energy range will be changed accordingly.
" You are allowed to use the whole energy range of the spectrometer:
Change the energy scale to Full range to have the full energy range
of the energy filter displayed.
Setting the energy loss You may also set the energy loss on the microscope via the remote control
on the microscope without changing the parallel EELS energy range. To do so, activate the
blue arrow at the upper side of the diagram. Drag the arrow to the desired
energy position.
" The energy loss on the microscope changes. The energy position
of the parallel EELS in the diagram remains unchanged.
Parallel EELS, Wide Range Acquisition...

Element Label... Click the Element Label... button to indicate certain ionization edges in the
spectrum diagram. A periodic table will be displayed onscreen where you
can select the desired elements simply by clicking the corresponding
element symbols. Use this option to get an overview of the positions of
ionization edges occurring in the energy range selected.
Energy scale You change the displayed energy range of the spectrum diagram in the
Energy scale group.
Element region Select the Element region option to display the proposed energy range only
(starting with -20 eV and including the selected ionization edge).
Full range Select the Full range option to see the entire energy range covered by the
spectrometer. If Full scale has been selected and the parallel spectrum has
been shifted out of the energy region, the Element region option will be
disabled. You cannot choose this option until the two regions overlap once
again.
Camera Control... The Camera Control dialog box is usually not available when a dialog box is
opened. Click the Camera Control... button to activate the Camera Control
dialog box in order to adjust the exposure time. To go back to the Parallel
EELS Acquisition dialog box, just click somewhere on the dialog box.
Time integration Select the Time integration check box to combine an averaged linescan with
time integration. A user-defined number of snapshots will be taken
successively and all the spectra recorded will be averaged.
Note When the Time integration check box is selected, the energy loss on the
microscope is fixed during the acquisition.

Integration cycles Enter the number of snapshots that are to be averaged into the Cycles field.
Frames required The Frames required field shows the number of images needed to cover the
selected energy range. The higher the spectrum magnification the more
images you need.
Spectrum Use the Spectrum magnification slider to enter the desired magnification of
magnification the spectrum. You can only select spectrum magnifications with valid
calibration data.
When changing the spectrum magnification in the dialog the spectrum
magnification on the microscope is also updated via remote control.

115
Date The date of the last calibration is shown beside the slider.
Calibrate... Click the Calibrate... button to update the energy calibration for the selected
spectrum magnification. You may use the Parallel EELS > Calibration...
command instead.
Test... Click the Test... button to check the position of the ROI. Use this feature if
the spectrum has been shifted after the last spectrum calibration. You
cannot change the position of the ROI in the image, but you may shift the
whole spectrum with respect to the position of the ROI.
What will happen... After clicking the Test.... button, an acquisition routine is started: a snapshot
is made and the current acquisition ROI is displayed as a red rectangle in
the overlay of the image. Then the next snapshot is taken and the ROI is
displayed and so on. The CENTER energy is indicated. A dialog box is
opened simultaneously.

related topics
Camera Control... 56
Parallel EELS, Calibration... 118
EFTEM • Parallel EELS

Before starting the parallel


EELS acquisition you may
check whether the spectrum
lies still inside the current
ROI.

Test, Align Spectrum Click the Align Spectrum button to correct a possible energy shift via remote
control. The energy loss on the microscope will be set to 0 eV and the Align
Spectrum tool is opened. If the Use lowest illumination aperture check box
is selected in the EFTEM Options > Parallel EELS tab, EsiVision will
automatically reduce the exposure time and illumination aperture. This
option avoids overexposure of the camera when the zeroloss peak is
acquired.
The system takes successive snapshots. After each snapshot, the ROI with
the CENTER energy loss is displayed. Use one of the arrow buttons to
position the zeroloss exactly on the center energy. Click the Close button to
return to the Parallel EELS Acquisition dialog box.
Use the Align Spectrum tool
to shift the spectrum into the
current ROI. The arrow
buttons control the
spectrum shift coils on the
microscope. Use the vertical
direction first, and the
horizontal direction
afterwards.
116

Test, OK Click OK in the message box if the ROI is properly aligned. The system will
return to the Wide Range Parallel EELS Acquisition dialog box and switch
back to live mode.
OK Click OK to start a fully-automatic acquisition of the wide range parallel
EELS. The acquisition starts with the highest energy loss. Message boxes
inform you on the ongoing procedure. You may terminate the acquisition
procedure at any time by clicking on the Cancel button in one of the
message boxes.
Parallel EELS, Wide Range Acquisition...

In the sample, there are 9


images needed to cover the
whole energy range. The
current image is the second
on at an energy loss position
of 651,0 eV.

Integration cycle The Wide Range Parallel EELS Acquisition message boxes informs you
Image about the current number of averaged frames at the current energy-loss
Energy loss position (Integration cycle) and the current energy loss position. To cover
the whole energy range, usually more than one spectrum images is needed.
The Image field gives the current number of the spectrum image and the
Energy loss field the current energy loss on the microscope.
EsiVision will automatically
reduce exposure time and
illumination aperture when
the intensity of the currently
acquired part of the
spectrum is too high.

The lower the energy loss the higher is the intensity. EsiVision automatically
adjusts the intensity of two adjacent spectrum regions. As soon as the
intensity is higher than a user-defined limit, EsiVision first halves the
exposure time. If the intensity is still higher than the allowed maximum
intensity EsiVision reduces the illumination aperture.
To define the limits, use the EFTEM > Options... command. Enter the limits
into the Upper or Lower intensity limit fields. The limits are specified as a

117
percentage of the maximum or minimum camera gray value.
Please note that exposure time and illumination apertures are never
automatically increased. If the a user-defined limit is under-run, EsiVision
will prompt you to adjust the intensity manually. Use the Camera Control to
increase the exposure time. The maximum possible exposure time is
10 sec.
EFTEM • Parallel EELS

Parallel EELS, Calibration...


Use this command to determine the position of the spectrum and the energy dispersion. The calibration
data depends on the high voltage, the spectrum magnification, and on the currently used input channel.
Each binning mode requires its own calibration data.

Warning The Parallel EELS > Calibration... command will overwrite the active
spectrum and image buffer.
If spectrum or image is write protected, it is not possible to calibrate the
system.
Why calibrate? Before acquiring a parallel EELS, you have to inform the system where the
energy axis is and how many columns perpendicular to the energy axis
should be averaged to get the intensity belonging to a specific energy loss.
To get a proper calibration of the energy axis, the system has to know at
least two energy-loss values. The energy dispersion, i. e., the energy loss
per pixel, can then be calculated.
When calibrating? When acquiring a parallel EELS spectrum the system checks whether a
valid spectrum calibration is available or not. If no calibration data is found
for the current spectrum magnification and high voltage, you will get a
message box offering to start the calibration routine.
Click the Calibrate... button
to start the calibration
routine.

What will happen... For calibration, a wizard guides you through the multiple calibration steps.
Just follow the instructions given in the dialog box.
How to... How to calibrate the system for parallel EELS acquisition
The energy-filtering microscope in use can be controlled by EsiVision via the
118

remote control.
1) Use the EFTEM > Options... command and select the Parallel EELS
tab.
2) Enter a delay time in the Calibration > Acquisition time field. The
system will wait the set delay time between two acquisitions of the
spectrum
Select the Use lowest illumination aperture check box.
Confirm via OK.
" It is only necessary to set or check these options once and not
before every spectrum calibration.
3) Select empty image and spectrum buffers.
4) Use the EFTEM > Parallel EELS > Calibration... command to open the
first dialog box.
" If calibration data for current spectrum magnification and high
voltage already exist, you will get a message box.
Click Yes to continue the calibration process. The existing

related topics
Parallel EELS Options 102
Parallel EELS, Calibration...

calibration will be substituted with the new one.


Click No to cancel the calibration process.
" The Parallel EELS Calibration dialog box is opened.
" The spectrum document is activated.
" The system switches to the live mode. This does not depend on the
setting in the EFTEM Options > Parallel EELS dialog box.

1st Calibration step: Defining the spectrum position


The Parallel EELS
Calibration dialog box
guides you through the
calibration procedure step
by step.
For defining the spectrum
position, set the energy loss
so that the spectrum is
clearly visible from one
border of the image to the
other.

5) Use the Energy loss slider to set an energy loss at which the spectrum
is visible in full in the live image.
" The energy loss on the microscope is adjusted via remote control.
" The spectrum should be clearly visible. If necessary, click the
Camera Control... button to adjust the exposure time. You return to
the Parallel EELS Calibration dialog box simply by left-clicking
somewhere in the dialog box.
6) Click the Next > button to place a red rectangle within the image. The
area of the rectangle defines the ROI (region of interest) that

119
contributes to the spectrum. Position the red rectangle exactly around
the parallel energy loss spectrum.
Mouse Control " Leftclick on the lowest energy loss in the image to define the
starting point.
" Leftclick on the highest energy loss in the image to define the last
point.
" Keep the left mouse button depressed to increase the width of the
ROI.
7) Rightclick to confirm the present ROI position and size and return to the
Parallel EELS Calibration dialog box. Clicking the middle mouse button
(middleclicking) cancels the procedure.
" The length of the ROI should be as long as possible. However it
must completely fit into the image, otherwise you cannot finish the
ROI definition mode.
" The energy loss on the microscope is automatically set to 0 eV. To
avoid damage to the camera by the zeroloss intensity, EsiVision will
automatically switch to the lowest illumination aperture and
exposure time.
EFTEM • Parallel EELS

" The zeroloss is automatically detected via the maximum of the


spectrum.

2nd Calibration step: Calculating the energy dispersion


The system calculates the
energy dispersion from the
position of the zeroloss at
two known energy losses

8) Use the Energy loss slider to set an energy loss at which the zeroloss
is visible at the (left) border of the ROI.
9) Click the Next > button to calculate the energy dispersion from the two
zeroloss positions.
" The system detects the new position of the zeroloss at this energy-
loss via the maximum of the spectrum.
" The energy dispersion calculated for the current spectrum
magnification is displayed in the Parallel EELS Calibration dialog
box.
" The spectrum ROI and the present position of the zeroloss are
displayed in the image overlay.
120

10) Click the Finish button to close the dialog box and save the new
calibration data.
" The new calibration data is saved in the Parallel EELS Calibration
History list. The calibration data includes the spectrum
Parallel EELS, Show Calibration Data...

magnification, the high voltage, the offset, the dispersion, and the
date. Open the calibration history by clicking on the Info... button in
the Parallel EELS Calibration dialog box.
Use the parallel EELS
calibration history to look up
the current calibration data.

Parallel EELS, Show Calibration Data...


Use the parallel EELS calibration history to display a list of the existing calibration data sets. You may
also delete individual calibration data sets.

121

Parallel EELS, Intensity Profile...


Use this command to create a spectrum from an existing image of an EELS.

Available This command is only available if the active image buffer contains a gray-
value image.

Warning The Parallel EELS > Intensity Profile... command will overwrite the active
spectrum buffer.
If the spectrum is write protected, you can either remove the write protection
or terminate the spectrum import.
EFTEM • Parallel EELS

Online shading EELS images should always be recorded with the online shading correction
correction activated. Otherwise, flatfield contributions of the gain image may appear as
intensity variations of the EELS.
Calculating the spectra The spectrum is calculated from a rectangular image area, ROI (Region Of
Interest). The ROI can also be rotated with respect to the image sides.
EsiVision takes the average of all columns of the ROI. Every column at a
certain energy-position corresponds to a particular energy channel. The
width of the ROI defines how many values are averaged when calculating
the spectrum. The length of the ROI defines the number of channels of the
resulting spectrum. The energy scale of the resulting spectrum will be
automatically adjusted to the active energy dispersion.
Resulting spectrum All spectra-processing functions provided by the Graph menu can be
applied to the resulting spectrum afterwards.
Spectrum name The spectrum buffers are named automatically so that the spectrum title
consists of the term ’Parallel EELS’ and the name of the EELS image.
Spectrum Information The resulting spectrum can be treated just like an ordinary energy-loss
spectrum, i. e., the Graph Information dialog box includes additional tabs
with special EFTEM data.
How to... How to generate a spectrum from an EELS image
The EELS image includes the zeroloss peak.
1) Load the EELS image you want to analyze.
" It is not necessary to align the energy axis of the EELS horizontally.
" The image is usually a 16-bit image because the 256 gray values
of an 8-bit image do not cover the dynamic range of an electron
energy-loss spectrum, especially in the low-loss region.
2) Activate an empty spectrum buffer.
3) Use the Parallel EELS > Intensity Profile... command.
" The spectrum calculated from the current region of interest is
displayed in the spectrum document.
Position the region of
interest so that the parallel
energy-loss spectrum is
122

completely enclosed.

4) Click the Define ROI button to define the region of interest.


" The mouse cursor will appear in the active image document.
" A pink arrow indicates the energy axis. The arrow points in the
direction of increasing energy loss.
Parallel EELS, Intensity Profile...

The spectrum document


displays the spectrum of the
present region of interest.
The arrow points towards
the direction of increasing
energy loss.

5) Position the red rectangle exactly around the parallel energy-loss


spectrum.
Mouse Control " Use the depressed left mouse button to increase or decrease the
width and length of the ROI. The spectrum preview is continuously
updated.
" Leftclick to switch between the rotation mode and the translation
mode.
Translation mode " Change the position of the ROI simply by moving the mouse in the
translation/shift mode.
Rotation mode " Rotate the ROI around the center of the ROI simply by moving the
mouse in the rotation mode.
" Rightclick to confirm the present ROI position and size and return
to the Parallel EELS Import dialog box.
The ROI must completely fit into the image, otherwise you cannot
finish the ROI definition mode.
" Middleclick to cancel the procedure.
6) Enter the energy dispersion of the analyzed image into the Dispersion
field.
" If you do not know the energy dispersion, you may also calibrate the
resulting spectrum using the calibration functions (in the Graph
menu).

123
7) If the acquired spectrum includes the zeroloss, click the Find Zero-Loss
button.
" The maximum intensity of the current spectrum is located and
indicated by a second perpendicular line. The maximum intensity is
assigned to 0 eV.
" The center energy is calculated from the zeroloss position found,
and from the energy dispersion.
8) Click OK.
" The active spectrum buffer contains the resulting spectrum.
" The next time you use the Parallel EELS, Intensity Profile...
command, ROI position and size, and energy values remain
unchanged.

related topics
Zeroloss Calibration... 34
EFTEM • Serial EELS Acquisition...

Description of the dialog box

Preset settings Upon opening the Parallel EELS Intensity Profile dialog box, the system
automatically loads the parameters which were used for importing the last
spectrum from an EELS image. This allows you to analyze a series of EELS
images acquired under the same conditions without setting the parameters
every single time. The parameters include
• the position and size of the ROI,
• the zeroloss position,
• the energy value of the center energy and
• the energy dispersion.
Center energy Enter the energy loss at the center position of the ROI into the Center energy
field. However, you normally will not know the energy loss at this position -
rather the energy dispersion. If the zeroloss is included in the displayed
energy range, then click the Find Zero-Loss button and the system will
calculate the center energy accordingly.
Dispersion Enter the energy dispersion of the microscope into the Dispersion field.
When using a LEO 912, the dispersion depends on the magnification and
the acceleration voltage.
Note If the spectrum contains at least two characteristic peaks, e. g., the zeroloss
and an element-specific plasmon loss, you may also calibrate the resulting
spectrum using the Calibration functions (in the Graph menu):

Define ROI Click the Define ROI button to define the image area (used for spectrum
calculation) via mouse. The ROI should contain the complete spectrum.
Find Zero-Loss Click the Find Zero-Loss button to locate the maximum intensity of the
124

current spectrum. The maximum intensity is indicated by a second


perpendicular line in the ROI and assigned to 0 eV. The center energy is
calculated from the zeroloss position found, and from the energy dispersion.

Serial EELS Acquisition...


Use this command for the serial acquisition of an energy-loss spectrum by means of an electron detector
(usually a scintillator-photomultiplier combination).

Definition In the following, the term spectrum denotes the graphical plotting of
intensity values versus energy-loss values. To avoid confusion with the
electron energy-loss spectrum generated in the energy dispersive plane of
the microscope, the latter will be called EELS.
Available • The Serial EELS Acquisition... command is only available when special
hardware is installed: You need an IEEE interface and a digital
multimeter to read in the photomultiplier signal. The system checks the
status of the EFTEM Options > Serial EELS > Serial EELS hardware
installed check box.
Serial EELS Acquisition...

• The Serial EELS Acquisition... command is only available if the remote


control is activated. The remote control is activated in the logical input
channel. Thus, although no camera is needed for acquiring a serial
EELS, be sure that the active input is capable of remote control.
Warning This command will overwrite the active image and spectrum buffer.
If the image or spectrum is write protected, you can either remove the write
protection or terminate the serial EELS acquisition.

Serial EELS Options


Use the EFTEM > Options... command to open the EFTEM Options dialog box. Use the Serial EELS tab
to define some general options for the serial EELS method.

125
Serial EELS hardware Select the Serial EELS hardware installed check box if you want to acquire
installed serial energy loss spectra. In this case, the system assumes that you have
installed the IEEE interface, a digital multimeter and a photomultiplier-
scintillator combination on the microscope.
Acquisition delay Enter the time between the setting of a new energy loss value and the start
of the recording into the Acquisition delay field. The default value is 300 ms.
Begin acquisition with Select the Begin acquisition with low energy check box to start the serial
low energy EELS acquisition with the START energy value.
Usually, the acquisition routine begins at the STOP energy loss and ends at
the START energy value. The recommended recording sequence from
higher to lower energy loss values is due to the afterglow of the scintillator-
photomultiplier combination because the intensity usually decreases with
increasing energy loss. The higher the incident electron intensity, the longer
the influence of the afterglow on the recorded signal.
Upper intensity limit The photomultiplier output signal must be within a certain range. Enter the
maximum output signal into the Upper intensity limit field. The default value
is 1 V. When intensity exceeds the upper intensity limit, acquisition stops
and you have to reduce intensity on the microscope.
EFTEM • Serial EELS Acquisition...

Lower intensity limit The photomultiplier output signal must be within a certain range. Enter the
minimum output signal into the Lower intensity limit field. The default value
is 1 µV. When intensity drops below the lower intensity limit, acquisition
stops and you have to increase intensity on the microscope.

What is serial EELS?


Definition A serial EELS is recorded by amplifying the intensity impinging on the PMT
(Photomultiplier Tube). The PMT output is digitized and read in by means of
a digital multimeter. The Serial EELS Acquisition... command is the only
acquisition method offered where no image has to be taken.
A serial EELS can be recorded in the spectrum mode as well as in the image
or diffraction mode of the microscope. In cases involving the EELS image or
diffraction mode, the final image plane contains a filtered image or diffraction
pattern. The image structure of interest or solid angle is to be positioned
above the diaphragm in front of the PMT. When the energy loss on the
microscope is continuously being changed, a spectrum of the selected
image structure or solid angle is recorded.
How to... How to acquire a serial EELS:

General image EELS 1) Use the EFTEM > Options... command.


settings " It is only necessary to set or check these options once and not
before every serial EELS acquisition.
2) Activate the EFTEM Options > Serial EELS tab.
3) Select the Serial EELS hardware installed check box.
Before using the 4) You should switch over from the image or diffraction mode of the
command microscope to the spectrum mode.
5) Set energy loss to zero.
6) The zeroloss should then be positioned precisely over the diaphragm
of the PMT to ensure a correct assignment of the energy channels.
7) Adjust the energy-selecting slit with the desired slit width surrounding
the zeroloss peak exactly.
8) If necessary, switch back to the image or diffraction mode afterwards.
9) Activate the spectrum buffer which is to contain the serial EELS.
126

Setting the acquisition 10) Choose the EFTEM > Serial EELS Acquisition....
parameter 11) Expose the scintillator to the electron beam by lifting the final
fluorescence screen.
12) Select the desired element symbol in the Serial EELS Acquisition
dialog box.
13) Select the desired ionization edge from the Scheme list.
14) If necessary, change the proposed START or STOP energy loss
values by clicking on the corresponding energies in the spectrum
diagram and moving the diagram cursor with a pressed mouse button
to the desired energy.
15) Enter the desired energy interval between two successive energy
channels in the Energy increment field.
16) Enter the desired integration time for one energy channel in the
Acquisition Time field.
17) Check the PMT output signal at different energy-loss values by clicking
on the Test... button.
18) If necessary, adjust intensity by changing either the incident electron
current density or the PMT gain.
Serial EELS Acquisition...

19) Click Cancel to terminate the test run in the Test Serial EELS
Acquisition dialog box.
Acquiring the serial 20) Start the acquisition of the serial EELS by clicking on OK.
EELS " You may follow the acquisition of the spectrum in the spectrum
document.
" The Serial EELS Acquisition dialog box contains the following
information:
Energy loss the current energy loss on
the microscope
Intensity the current output signal
of the photomultiplier
Time left the remaining acquisition
time

These values are continuously updated during the acquisition.


21) If the output signal of the photomultiplier exceeds the lower or upper
limit, the acquisition is interrupted to avoid possibly damaging the
scintillator in front of the PMT due to overexposure.
Adjust the intensity on the microscope and click the Continue button in
the Serial EELS Acquisition dialog box.
" The acquisition is continued. The part of the spectrum with the
adjusted intensity is automatically adapted to the intensity of the
existing spectrum.
Note Be aware of the fact that the intensity values of the spectrum do not
represent the actual recorded output signal of the PMT if the PMT gain has
been changed during the acquisition routine.
Resulting spectrum " When the acquisition has been finished, the dialog box is automat-
ically closed and the resulting spectrum overwrites the currently-
active spectrum buffer. The spectrum is named ‘Serial EELS’ +

127
element abbreviation + ionization edge.
EFTEM • Serial EELS Acquisition...

Description of the dialog box

Preset settings Upon opening the Serial EELS Acquisition dialog box, the system auto-
matically loads the parameters which were used for recording the last serial
EELS. The energy range displayed in the diagram may therefore be quite
different from the energy loss currently adjusted on the microscope.
However, the energy loss on the microscope will not be altered until you
select an energy loss in the schematic spectrum via mouse click.
128

Element Enter the element you want to investigate into the Element field. Only inter-
nationally standardized abbreviations are accepted.
Periodic table... Use the Periodic table... button to open a dialog box showing the periodic
table of elements. To select an element, simply click the desired element
button and confirm your choice via OK.
The quick info displays the full element name and the ionization edges
below 2000 eV.

Edge The Edge field specifies the ionization edge of the selected element. For
predefined parameter sets this field is only for information. For user-defined
parameter sets you can enter the edge type.
Slit width Enter the present slit width of the microscope into the Slit width field. The
energy windows displayed in the spectrum diagram are modified
accordingly. The system does not select the slit width; it has to be done by
yourself.
Serial EELS Acquisition...

Scheme The Scheme list offers all available parameter sets for the active element.
These parameter sets includes all settings in the dialog box except the
display mode of the spectrum diagram, i. e. - specifically, the element, the
START and END position and the energy increment.
Predefined schemes For each element, EsiVision offers at least one predefined parameter set.
The name of a predefined scheme consists of the element symbol (e. g., C),
the symbol of the ionization edge (e. g., K) and the word ‘Atlas’. A particular
set of energy values is linked to this predefined scheme. To load a
predefined scheme for a special element, click the Periodic Table... button.
Energy values defining A particular set of energy values is linked to a predefined scheme. These
the image EELS series energy values are defined as follows:
∆EION threshold ionization energy ∆EION and ∆EMAX only determine
indicating the beginning of the the shape and the energy range
ionization edge of the displayed schematic
∆EMAX position of maximum intensity of spectrum and do not influence the
the ionization edge with energy acquisition procedure.
window width dE = 15 eV
START = 2∆EMAX - ∆EION
proposed energy-loss value of the first image of the image EELS series
STOP = 2∆EION - ∆EMAX
proposed energy-loss value of the last image of the image EELS series

User-defined schemes To define your own parameter set for an element, type a new name in the
Scheme field. The Edge field will become an edit field which you can use to
specify the type of ionization edge and the Delete and Save buttons will be
enabled.
What will happen... After loading a previously saved parameter set, the spectrum diagram is
updated immediately.
Save Click the Save button to save the present parameter set for a specific
element. To load an existing user-defined parameter set, insert the
corresponding element in the Element field. Then, all available parameter
sets associated with this element are listed in the Scheme list.
The Save button is only available if a new name is entered in the Scheme
field.
Delete Click the Delete button to delete a previously saved parameter set for a

129
specific element. To do so, enter the element in the Element field and select
the corresponding parameter set from the Scheme list.
The Delete button is only available if a user-defined parameter set exists for
the active element.
Diagram The diagram in the dialog box displays a spectrum of the required energy-
loss range. You can either display the whole energy range from 0-2000 eV
or simply the energy range around the ionization edge. The Y values auto-
matically range from 0 to the maximum intensity of the displayed energy
range.
Show Spectrum Decide which spectrum should be displayed in the diagram in the Show
Spectrum group. You may display all three types of spectra simultaneously
and overlapping, but you cannot switch off all spectra at the same time. If
only one spectrum is left, the check box is no longer available. In this case,
you have to display a second one before you are allowed to switch the
spectrum off.
Symbolic Select the Symbolic check box to display a schematic energy-loss spectrum
only. The schematic spectrum does not represent the real shape of the
selected ionization edge. Without exception, the ionization edges in the
EFTEM • Serial EELS Acquisition...

schematic spectrum show a saw tooth shape with the ionization threshold
energy at ∆EION and the maximum intensity at ∆EMAX. So the schematic
spectrum of, e. g., a white line will not differ from the schematic spectrum of,
e. g., a delayed edge.
EELS atlas Select the EELS atlas check box to display the spectrum of the EELS atlas
belonging to the selected element and ionization edge. There is exactly one
spectrum available for each element and ionization edge.
Spectrum Select the Spectrum check box to work with your own reference spectra.
The contents of a specific spectrum buffer are displayed in the diagram. The
number of the spectrum buffer has to be specified in the field below the
Spectrum check box. The default spectrum buffer is the active one.
The Spectrum check box is only available if the specified spectrum buffer
contains a valid EELS spectrum. If the specified spectrum does not cover
the whole energy range, only a part of the spectrum will be displayed.
The following information is
indicated in the diagram of
the Serial EELS Acquisition
dialog box:
z the energy-loss spectrum
z the energy range covered
by the serial EELS (green
rectangle).

Setting the energy range Use the mouse to change the given START and STOP energy loss values
for the serial EELS for the serial EELS directly in the spectrum diagram. Before setting the
energies, choose the element and the ionization edge.
To change the START energy, first click at the left side of the green area
indicating the energy-loss range.
130

" A blue line cursor appears, the exact energy value is displayed
below the diagram and at the same time updated on the
microscope.
To change the energy value, drag the blue line cursor with the depressed
left mouse button to the desired energy position.
" The green-colored energy range will be extended in the diagram
cursor. Increasing the energy range will also increase the number
of channels in the serial EELS and thus the time required for
acquiring the whole spectrum. The acquisition time is continuously
updated and displayed in the Time required field.
" The associated energy value displayed will be continuously
updated on the microscope and below the diagram.
For the precise positioning of the energy window, use the left and right
keyboard arrows.
" The energy range will be shifted step by step in the corresponding
direction. The minimal energy increment depends on current
microscope settings.
Serial EELS Acquisition...

" You are not permitted to move the energy loss outside the
displayed energy range. Change the energy scale to Full range to
expand the energy range.
Note The START energy loss must always be smaller than the STOP energy loss.

Element Label... Click the Element Label... button to indicate certain ionization edges in the
spectrum diagram. A periodic table will be displayed onscreen where you
can select the desired elements simply by clicking on the corresponding
element symbols. Use this option to obtain an overview of the positions of
ionization edges occurring in the selected energy range.
Energy scale Change the displayed energy range of the spectrum diagram in the Energy
scale group.
Element region Select the Element region option to display only the energy range including
the selected ionization edge.
Full range Select the Full range option to see the entire energy range covered by the
spectrometer. If Full scale has been selected and the green-colored energy
interval has been shifted out of the energy region, the Element region option
will be disabled. You cannot choose this option until the two regions overlap
once again.
Energy increment Enter the energy interval between two adjacent energy channels into the
Energy increment field. The energy increment determines the total number
of channels the serial EELS consists of.
Acquisition Time Enter the integration time for each intensity value into the Acquisition Time
field.
Time required The Time required field displays the total acquisition time. This time
depends on the energy increment and the energy range and is automatically
updated according to the entered parameters.
Test... Click the Test... button to check the output of the PMT at certain energy-loss
values. The Test Serial EELS Acquisition dialog box opens.
OK Click OK to continue the acquisition of a serial EELS by beginning
acquisition.

131
EFTEM • Serial EELS Acquisition...

The Test Serial EELS Acquisition dialog box


Available The Test Serial EELS Acquisition dialog box is opened when you click the
Serial EELS Acquisition > Test... button.

Diagram The diagram serves as a visual check of the photomultiplier signal. The
intensity value is plotted against a time axis using a base 10 logarithmic
scale. Use this facility to observe the effect of changing the incident charge
density, the PMT amplification, or the slit width on the PMT signal. The
intensity values are measured using the shortest possible interval between
two successive registrations. In cases where the signal is very noisy, this
can be compensated by setting an appropriate acquisition time in the Serial
EELS Acquisition dialog box.
Energy loss The Energy loss field displays the currently adjusted energy-loss value on
the microscope. When opening the dialog box, the currently set energy
value is automatically transferred to the microscope, i. e., either the START
or the STOP value. However, you are allowed to enter any energy value that
is within the selected energy range.
132

Intensity The Intensity field corresponds to the currently-measured output of the PMT
in µV.
Cancel Click the Cancel button to return to the Serial EELS Acquisition dialog box.
OK Click OK to start a fully automatic acquisition of the image EELS series.
Message boxes keep you informed on the ongoing procedure. You may
terminate the acquisition procedure at any time by clicking on the Cancel
button in one of the message boxes.

Trouble Shooting
If the recorded PMT signal is zero or very low, you should check the
following possible reasons:
• The PMT has not been switched on. Use the toggle switch CAGE /
PMT on the microscope. For more detailed information, please refer to
the microscope’s instruction manual.
• The PMT signal is saturated. In case the PMT output is higher than a
certain threshold, the PMT is automatically switched off. This is
indicated on the microscope panel by the PMT OVERLOAD pilot light.
Reduce the incident charge density and reset the photomultiplier (for
Quantification

detailed information consult the corresponding section of the


microscope’s instruction manual). Be aware of the fact that this
mechanism protects the photomultiplier but not the scintillator.
• The photomultiplier gain is too low. For changing the PMT gain, please
refer to the corresponding section of the microscope’s instruction
manual.
• The incident electron current density is too high.
• The energy-selecting slit width is too narrow.
• The energy-selecting slit is not aligned precisely above the PMT
diaphragm so that no or only reduced electron intensity impinges on
the scintillator.
• The EELS is shifted perpendicular to the energy-selecting direction and
thus, no intensity hits the detector. Shift the EELS carefully (consult the
microscope instruction manual) and observe the result on the signal
displayed in the dialog diagram.
Quantification

Quantification, Element ratio...


Use this command to determine the ratios of two elements from the energy loss spectrum. Only elements
with known cross sections can be quantified.

Before you use this • Load or acquire an EELS spectrum. The spectrum must contain the
command zeroloss and the characteristic ionization edges of the two elements.
• Use the Graph > Calculation > Fourier-Log Deconvolution command to
remove the effects of plural scattering.
• Change the display of the spectrum so that the interesting region of the
spectrum is completely displayed in the spectrum document.
• Switch to the linear display mode. The element ratio cannot be
calculated for a logarithmic spectrum presentation.
The following formula is used to compute the element ratio:
NA I A ( α 0, ∆ ) ⋅ σ B ( α 0, ∆ )
Element ratio = ------- = -----------------------------------------------------
NB I B ( α 0, ∆ ) ⋅ σ A ( α 0, ∆ )

with 133
NA and NB the number of atoms of the element A or B per unit area of the
specimen
σA and σB the cross-section of element A or B for scattering within a defined
range of angle and energy loss
IA and IB the element specific core-loss intensity over an energy region ∆
α0 acceptance angle of the spectrometer
∆ energy integration width
EFTEM • Quantification

The element specific intensities are calculated as the integral over the
ionization edges. The background underlying each ionization edge is to be
subtracted separately. The acceptance angle of the spectrometer is
calculated from the high voltage, the energy resolution, and the
magnification. Magnification and high voltage are read out during the
spectrum acquisition via remote control. They are automatically imported
from the Graph Information > EELS Data tab. The energy integration width
can be varied. The proposed value is 30 eV, but you may increase it when
there are no overlapping ionization edges.
134
Quantification, Element ratio...

EsiVision will automatically rescale the displayed Y-range to the maximum


Y value.
Element A Use the functions in the Element A group to set the parameters for
calculating the integral of the characteristic ionization edge over a specific
energy window. The width of the energy window is defined by the value in
the Integration width field.
Select Click the Select button to determine the ionization edge in the spectrum.
Select the ionization edge by directly clicking at the beginning of the edge.
EsiVision will automatically try to identify the edge. The Select Element
dialog box offers a few suitable ionization edges. Only elements with known
cross-sections are offered. The ionization edge that fits best is selected.
Confirm the proposal with OK or select another ionization edge.
To select an element, simply
click in the spectrum just
before the ionization edge
starts. EsiVision will
automatically identify the
element. Confirm the setting
with OK.

Background Click the Background button to subtract the unspecific background under
the ionization edge. The background intensity is calculated from the
spectrum progression before the interesting ionization edge.

135
What happens The Background Subtraction dialog box is opened. The energy range of the
spectrum that is used for the background fit is determined by a lower and
upper limit. The proposed lower limit is the lowest energy loss that is
displayed in the graph document. The proposed upper limit is the selected
position of the ionization edge.
The calculated background curve and the lower and upper limits are drawn
into the graph document.
Use the command in the dialog box to adjust the limits and to change the
background fitting method.
EFTEM • Quantification

The background subtraction


is performed for each
element separately.

Use the Background


Subtraction dialog box
to set the upper and lower
limits and to change the
fitting method.
136

Background From the Assumed function list, choose the suitable fitting method. After
Subtraction > choosing a new fitting method, the background is automatically recalculated
Assumed function from the spectrum values and indicated in the spectrum document. The
dialog box shows the fitting formula and the computed fitting parameters for
the current spectrum.
Quantification, Element ratio...

The following table gives an overview of the available fitting methods. IBg is
the background intensity and ∆E the energy loss, A and r are variable
parameters that are calculated during the background fit.
Fitting method Formular Description
Linear I Bg = A ⋅ ∆E + r The background is approximated by a line.

Power I Bg = A ⋅ ( ∆E ) r A power law is used. In case there are no overlapping edges


before the interesting ionization edge, the power law should
provide the best results.
Exponential r ⋅ ∆E An exponential law is used.
I Bg = A ⋅ e
2 point (linear) I Bg = A ⋅ ∆E + r The line is defined by the two intensities at the position of
the lower and upper energy loss. The curve progression is
not considered. Use this option to compute background
below a white line.
Background Use the Reference group to define the energy range that is used for the
Subtraction > background fit. The energy range is defined by the lower and the upper limit.
Reference
Background Click the Set Lower button to change the position of the first limit. Move the
Subtraction > line cursor to the desired energy loss and click the left mouse button to
Set Lower recalculate the background and return to the dialog box. The background
curve is continuously updated.
Background Click on the Set Upper button to change the position of the second limit. The
Subtraction > upper limit should be set directly before the interesting ionization edge.
Set Upper Move the line cursor to the desired energy loss and click the left mouse
button to recalculate the background and return to the dialog box. The
background curve is continuously updated.
Background Click the OK button to confirm the current background curve for the active
Subtraction > OK element. The Background Subtraction dialog box is closed.
Sigma The Sigma field shows the resulting partial cross-section for the specified
element and microscope parameters.
The calculation of the cross-section is based on the dipole oscillator strength
as used in optical theory. Dipole conditions apply, provided the energy loss
is located not too far from the ionization edge and over a restricted angular

137
range. The integrated optical oscillator strength is tabulated for many
elements and ionization edges.
You will get an error message in the Element Ratio dialog box if the set
parameters do not fit to the dipole approximation.
The preset unit of the cross-section is cm², but you may also output the
cross-section in barn (1 barn = 10-24 cm²). Use the EFTEM > Option...
command. On the General tab, select the Show cross section in barn [b] tab.
Integration width In the Integration width field, enter the energy range that is used to calculate
the element specific core-loss intensity. Ideally, the integration width should
be so large that the whole element specific signal is considered in the
calculation.
The energy integration width can be varied. The proposed value is 30 eV,
but you may increase it when there are no overlapping ionization edges.
Please keep in mind that for comparable results the same integration width
must be used.
EFTEM • Quantification

Set Click the Set button to define the integration width interactively. The
integration width for the two elements must be the same. The position of the
lower integration limit is always the ionization energy. The position of the
upper integration limit may be changed for the ionization edge with the lower
energy loss.
Microscope parameter The microscope parameters High voltage and Magnification are
automatically read out from the Graph Information > EELS Data tab. The
acceptance angle is calculated from the TEM-magnification, the high
voltage and the energy resolution of the spectrum.
Energy resolution In the Energy resolution field, you may enter the full width at half maximum
of the zeroloss peak as value. Use the Graph > Calibration > Zero-Loss
Calibration... command to have the FWHM determined by EsiVision.
Element Ratio A/B The Element Ration A/B field shows the resulting element ratio. If the result
cannot be calculated, an error message is displayed. In this case, check the
background subtraction parameters and the microscope parameters.
Copy Graph to Click the Copy Graph to Clipboard button to take a screenshot of the current
Clipboard contents of the spectrum window. This screenshot will include the back-
ground curves and the lines indicating the integration width.
You may save the contents of the clipboard as an image. Close the Element
Ratio dialog box and activate an empty image buffer. Use the [Crtl+V] or the
Edit > Paste command to copy the screenshot into the image buffer. Save
the image as usual by the File > Save as... command.
OK Click the OK button to finish the quantification. EsiVision will automatically
create a new measurement sheet containing the most important parameters
of the quantification.
138

Accumulate measuring It is possible to accumulate measurements in one output sheet. To do so,


results activate the existing measuring sheet first and use the EFTEM >
Quantification > Element ratio... command afterwards. The results are then
appended to the active measurement sheet.

Quantification, Ratio Image...


Use this command to calculate a quantitative element distribution image from two element distribution
images. The resulting image shows the ratios of two elements.

Before you use this • Load two element distribution images showing the same specimen
command area. Use the EFTEM > ESI commands to acquire and analyze the two
element distribution images. To calculate the net element distribution

related topics
ESI 49
Quantification, Ratio Image...

the three window method should be used. The acquisition parameters


(slit width, high voltage and magnification) must not be changed during
the acquisition.
The following formula is used to compute the element ratio for each image
point separately:
NA I A ( α 0, ∆ ) ⋅ σ B ( α 0, ∆ )
Element ratio = ------- = -----------------------------------------------------
NB I B ( α 0, ∆ ) ⋅ σ A ( α 0, ∆ )

with
NA and NB the number of atoms of the element A or B per unit area of the
specimen
σA and σB the cross-section of element A or B for scattering within a defined
range of angle and energy loss. The cross-section is calculated
IA and IB the element specific core-loss intensity over an energy region ∆
α0 acceptance angle of the spectrometer
∆ energy integration width

Visualization tools The gray values of the resulting image are calibrated.
To show a palette bar, use the Image > Scale Bar > Properties... command.
Select the Palette bar check box.
Use the Oper > 3D-Surface > Create command to create a 3D plot of the
ratio image. You may use the high contrast image - if available - as texture
image to get an impression where the highest or lowest element
concentrations are located.
To measure the element ratio of individual image points, use the Measure >
Pixel Value command.

139

Image In the Image field, enter the number of the image buffer where the element
distribution image for the element A is located. EsiVision automatically reads
out the ionization edge and energy loss from the Image Information >
EFTEM Data tab.
EFTEM • Quantification

Select If the image was not acquired using the EFTEM module, there is no EFTEM
Data tab in the image information. In this case, the values from the last
calculation are proposed. Click the Select button to chose the element and
the ionization edge in question from the periodic table.
Sigma The Sigma field shows the resulting partial cross-section for the specified
element and microscope parameters.
The calculation of the cross-section is based on the dipole oscillator strength
as used in optical theory. Dipole conditions apply, provided the energy loss
is not located too far from the ionization edge and over a restricted angular
range. The integrated optical oscillator strength is tabulated for many
elements and ionization edges.
You will get an error message in the Ratio Image dialog box if the set
parameters do not fit to the dipole approximation.
Microscope parameter The microscope parameters High voltage and Magnification are
automatically read out from the Graph Information > EELS Data tab. The
acceptance angle is calculated from the TEM-magnification, the high
voltage and the energy resolution. Typical values for the energy resolution
is 3 eV for Image EELS and 15 eV for ESI series.
OK Click the OK button to finish the quantification. The resulting image
overwrites the destination image buffer.
Drift Correction... Click the Drift Correction... button to correct a possible specimen drift
between the two element distribution images. The drift between the images
is determined automatically. However, you may change the automatically
calculated shift values interactively.
140

X shift The X and Y shift fields display the calculated shift values between the two
Y shift images. These shift values are applied to the second image (Element B)
after clicking OK.
Arrow buttons Click the arrow buttons to move the second image (Element B) in the
direction indicated. The image is shifted one pixel per click. The resulting
difference image is immediately displayed onscreen. If the difference image
shows no structure, the two images are aligned. The shift values are
updated accordingly.
Click this button to reset the shift values to the calculated drift value.
Reset Click the Reset button to set both shift values to zero.
OK Click OK to confirm the current shift values. The second image showing the
element distribution of element B is shifted by the calculated values. The
image sizes of both images are reduced accordingly.
Specimen Thickness

Specimen Thickness
Use the commands in this group to measure the local thickness of an TEM-specimen. The thickness
information is derived from measurement of the probability of inelastic scattering.

The following formula is used to compute the specimen thickness:


I tot
specimen thickness = λln  -----------------
I zeroloss

with
Itot total area beneath the complete spectrum
Izeroloss the area under the zeroloss peak
λ total mean free path for inelastic scattering.
The mean free path length is calculated from the high voltage, the
objective aperture and the mean atomic number.

Specimen Thickness, From Spectrum...


Use this command to measure the local thickness of the specimen from the electron energy loss
spectrum. It is provided that the mean atomic number of the specimen is known.

Available The Specimen Thickness > From Spectrum... command is only available if
the current spectrum was acquired by the EFTEM module.
Before you use this Load or acquire an EELS spectrum. The spectrum must contain the
command zeroloss. Do not deconvolute the spectrum.

141

Relative thickness The relative thickness is directly calculated from the zeroloss integral and
the total integral. The unit of the relative thickness is the mean free path
(MFP). The relative thickness does not depend on the element composition
of the specimen.

specimen thickness I tot


relative thickness = ---------------------------------------------- = ln  --------------------
mean free path λ  I zeroloss
EFTEM • Specimen Thickness

Mean atomic number Enter the mean atomic number of the area contributing to the spectrum. If
you do not know the atomic number of your specimen, click the Periodic
Table... button to select an element from the periodic table of elements. The
atomic number of the selected element will then be used.
High voltage The mean atomic number, high voltage, and the objective aperture are
Objective aperture needed to calculate the mean free path length. High Voltage and the
diameter of the objective diaphragm are automatically imported from the
Graph Information > EELS Data and Microscope tab. However, you may
correct the values interactively in the Specimen Thickness from Spectrum
dialog box.
Mean free path The resulting mean free path and absolute specimen thickness is shown in
Specimen thickness the dialog box.
Density If the density of the specimen is known, the value of the absolute thickness
Mass thickness can be converted into the mass thickness of the specimen. Typical density
values for each element are included in the EELS atlas. Just click the
Periodic table... button to import the value into the dialog box.
OK Click the OK button to finish the thickness calculation. EsiVision will
automatically create a new measurement sheet containing all parameters of
the computation. If you need the values for advanced calculations, you may
export the EsiVision sheet to Excel. Select the whole sheet by [Crtl+a] or
click on a header to select a single column. [Crtl+c] copies the selected
values into the clipboard. [Crtl+v] pastes the sheet for example into
Microsoft-Excel.

Specimen Thickness, From Image...


Use this command to create a thickness map from two acquired images, the elastic and the global bright-
142

field image. The thickness is calculated for each image point. The resulting image is Z-calibrated.

Useful commands for The resulting image is Z-calibrated. EsiVision provides several useful
Z-calibrated images functions you may use with Z-calibrated images:
• To display a palette bar in the image:
Use the Image > Scale Bar > Properties... command to open the Scale
Bar Properties dialog box. Select the Palette bar check box on the
Display tab. Clear the false color palettes only check box. Confirm the
settings with OK. Now, you may use the [Shift +F4]-keystroke to show
or hide the palette bar in image viewports.
The palette bar shows the unit of the Z-calibration, e.g. [nm] when
calculating the absolute specimen thickness.
• To create a 3D-surface:
The resulting image is thickness map of the specimen. Activate the
resulting image and use the Oper > 3D-Surface > Create command. A
3D-model of the thickness map is created. Keep the [Crtl] key
depressed and use the arrow buttons on the keyboard to rotate and tilt
the 3D-model.
Specimen Thickness, From Image...

• To measure the thickness of special specimen areas:


Use the Measure > Pixel Value command to measure the thickness of
individual image points. Use the Measure > Intensity Profile commands
to create one-dimensional thickness profiles.
To measure the mean thickness of special specimen areas, you have
to use the automatic particle detection. Use the Analysis > Append
Particles... command to define the image areas you are interested in.
Use the particle parameter Intensity Gray Value Mean for calculating
the mean thickness in the selected images areas.

Thickness calculation The Thickness calculation group offers three formulas for the thickness
computation. The thickness is computed for each image point.
Relative thickness map The relative thickness is directly calculated from the relation between the
elastic (0 eV) and global brightfield image (without energy filtering).

global brightfield intensity


relative thickness = ln  ----------------------------------------------------------------
elastic brightfield intensity

143
The unit of the relative thickness is the mean free path (MFP). The relative
thickness does not depend on the elemental specimen composition, thus
the element specific fields in the dialog box are not necessary.
Consequently, the fields are grayed.
For a specimen area with homogeneous absolute thickness, the relative
thickness map represents the distribution of the mean atomic number. The
higher the atomic number the higher is the relative thickness of specimen
areas.
Specimen thickness The absolute specimen thickness is calculated for each image point. The
map resulting image is Z-calibrated. For example, use the Measure > Value
command to measure the thickness of individual image points. You will get
measuring results in units of length.

global brightfield intensity


specimen thickness = mean free path λ ln  ----------------------------------------------------------------
 elastic brightfield intensity
EFTEM • Specimen Thickness

For calculating the absolute specimen thickness, the mean free path length
must be known. Enter the mean atomic number, the high voltage, and the
diameter of the objective aperture.
Mass thickness map If the density of the specimen is known, the value of the absolute thickness
can be converted into the mass thickness of the specimen. Typical density
values for each element are included in the EELS atlas. Just click the
Periodic table... button to import the value into the dialog box. The unit of the
mass thickness is µg/cm².
mass thickness = density ⋅ specimen thickness
Image buffer If you have already acquired the images, load the images into the image
manager. In the Image buffer group, you have to specify where the two
images needed are located. Enter the number of the image for the elastic
filtered image and the global brightfield image.
If you want to acquire now, use the Image buffer group to specify two empty
image buffers for the two images.
Acquire... 1) Before you use the EFTEM > Specimen Thickness > From Image...
command: Click the Camera Control... button to activate the Camera
Control dialog box in order to adjust the exposure time.
2) Click the Acquire... button to start the image acquisition:
" EsiVision will automatically switch to the live mode. The system
prompts you to adjust the intensity.
3) Set the energy loss to zero on the microscope or use the EFTEM > Set
Energy-Loss... command.
4) Remove the energy slit and adjust the intensity for the global brightfield
image.
5) Insert the energy slit for acquiring the zeroloss image.
6) In EsiVision, continue the acquisition by clicking OK in the Specimen
Thickness from Images message box.
" The elastic brightfield image is acquired and written into the
selected image buffer.
" A second message box appears.
7) Remove the energy slit on the microscope and click OK to return to the
144

Specimen Thickness from Images dialog box.


Do NOT change the illumination aperture or the exposure time.
" The global brightfield image is acquired and written into the
selected image buffer.
8) Click OK.
OK Click the OK button to finish the thickness calculation. EsiVision will write the
resulting image into the destination image buffer. If the destination image
buffer contains one of the two required images, the next empty image buffer
is chosen.
Specimen Thickness, From Image...

Note that the mean


brightness of the global
brightfield image (GBF) is
much higher than the mean
brightness of the elastic
brightness image (EBF).
The brightness of the
images appear quite similar
because of the automatic
16-bit display.
The resulting image (right) is
a thickness map of the
specimen.

Drift Correction... Click the Drift Correction... button to correct a possible specimen drift
between the two images. The drift between the images is determined
automatically. However, you may change the automatically calculated shift
values interactively.

X shift The X and Y shift fields display the calculated shift values between the two
Y shift images. These shift values are applied to the second image (global bright
field) after clicking OK.
Arrow buttons Click the arrow buttons to move the second image (global bright field) in the
direction indicated. The image is shifted one pixel per click. The resulting
difference image is immediately displayed on screen. If the difference image
shows no structure, the two images are aligned. The shift values are

145
updated accordingly.
Click central button to reset the shift values to the calculated drift value.
Reset Click the Reset button to set both shift values to zero.
OK Click OK to confirm the current shift values. The global bright field image is
shifted by the calculated values. The image sizes of both images are
reduced accordingly.
EFTEM • Specimen Thickness

Specimen Thickness, Interactive...


Use this command to measure the local thickness of the specimen by measuring the electron current
impinging on either the small fluorescence screen or on the camera collector. The current is measured
first for the zeroloss and afterwards for the global bright field.

Relative thickness The relative thickness is directly calculated from the zeroloss intensity and
the global brightfield intensity. The unit of the relative thickness is the mean
free path (MFP).

specimen thickness I tot


relative thickness = ---------------------------------------------- = ln  -----------------
mean free path λ I zeroloss

Measure... 1) Click the Measure... button to start the measurement. The system will
guide you through the measurement.
2) Select the measuring mode Small screen or Camera collector and
confirm with OK.
146

3) Adjust slit for zeroloss measurement and confirm with OK.


4) Remove slit and confirm with OK.
" The resulting mean free path and absolute specimen thickness is
shown in the dialog box.
Mean atomic number Enter the mean atomic number of the specimen. If you do not know the
atomic number of your specimen, click the Periodic Table... button to select
an element from the periodic table of elements. The atomic number of the
selected element will then be used.
Microscope Parameter...

High voltage The mean atomic number, high voltage and the objective aperture are
Objective aperture needed to calculate the mean free path length. High Voltage and the
diameter of the objective diaphragm are automatically imported from the
Graph Information > EELS Data and Microscope tabs. However, you may
correct the values interactively in the Specimen Thickness Interactive dialog
box.
Density If the density of the specimen is known, the value of the absolute thickness
Mass thickness can be converted into the mass thickness of the specimen. Typical density
values for each element are included in the EELS atlas. Just click the
Periodic table... button to import the value into the dialog box.

Microscope Parameter...
Use this command as a pocket calculator that computes the acceptance angle of the energy loss
spectrometer. Check the microscope parameter, for example, before you acquire an ESI series.

The following formula is used to compute the acceptance angle α. The


constant is depending on the microscope type.
α = ( constant ⋅ M ⋅ ∆ ) ⁄ U
with
M magnification
∆ energy resolution
U high voltage

147

High voltage The High voltage and the Magnification are automatically read in via remote
Magnification control. If you change one of the settings while the dialog is open, just click
the Update button.
Objective aperture in Enter the diameter of the current objective diaphragm in µm. The objective
mrad aperture in mrad is automatically calculated.
Energy resolution In the Energy resolution field, enter the current slit width of the spectrometer
diaphragm. A typical value for Image EELS is 3 eV, for ESI 15 eV.
Acceptance angle The Acceptance angle field shows the resulting value. You will get an error
message if the objective aperture exceeds the acceptance angle. In this
case insert a greater objective diaphragm.
EFTEM • Set Energy-Loss...

Set Energy-Loss...
Use this command to set a certain energy loss on the microscope using the remote control.

Available The Set Energy-Loss... command can only be used if the remote control is
activated.

Current energy loss Enter the desired energy loss value in the Current energy loss field. The
energy loss on the microscope will be updated immediately.
If you change the settings from a high energy loss to a low one - e. g., from
100 eV to 0 eV - a warning message appears before changing the energy
loss. Reduce the intensity on the microscope and confirm the message box
by clicking on OK.
Stepwidth An energy increment of 1 eV is used when scrolling the current energy loss
up or down by means of the arrow buttons.

Options...
Use this command for setting preferences within the EFTEM module.

Where do you find the The EFTEM Options dialog box is divided into five tabs. There are general
options described? options (General tab) related to all EFTEM methods and several options for
each method, ESI, Image EELS, Parallel EELS and Serial EELS. The
specialized options are described in the introduction of the relevant method.
148

related topics
Remote Control 3
ESI Options 50
Image EELS Options 76
Parallel EELS Options 102
Serial EELS Options 125
The General tab

The General tab


Use this command for setting several general options for all EFTEM methods, especially for the
acquisition functions.

Definition The general settings affect all kind of EFTEM images, i. e., ESI-image
series, Image EELS series and PEELS images showing an electron energy
loss spectrum.

Monitor selection Choose the monitor for the EFTEM image display in the Monitor selection
group. The EsiVision dual-screen system offers an additional second

149
monitor. This ’dual screen’ is especially meant for displaying images without
disturbing overlapping dialog boxes, messages, or other document
windows.
Which functions are For all methods, the selected monitor is considered during acquisition and
affected? for analysis. The other EFTEM functions, e. g., the drift correction, will not
change the active monitor.
Examples For example, if you select the dual monitor the system will always activate
the dual monitor for the ESI image acquisition. This means that the live
image during image acquisition is displayed on the dual screen.
When using the ESI > Analyze... command, the selected monitor will display
the preview of the element-distribution image. After confirming the
background-fitting method, the selected monitor displays the destination
image buffer.
Available This group is only available for a dual screen system.
Use current monitor Select the Use current monitor option not to change the active monitor
before acquisition and analysis.
EFTEM • Options...

Use windows monitor Select the Use windows monitor option to activate the windows monitor
before acquisition and analysis. The windows monitor shows the EsiVision
graphical user interface (and the operating system and other application
programs).
Use dual monitor Select the Use dual monitor option to activate the dual monitor before
acquisition and analysis. The dual monitor is exclusively for displaying
images. Because the acquisition dialog boxes are relatively large, you
should usually use this option to avoid overlapping dialog boxes or
document windows.
Use MDF option of Select the Use MDF option of microscope check box if you want to use the
microscope MDF (Micro Dose Focusing) mode of your microscope with the EFTEM
acquisition functions. If the check box is selected, you will find an additional
check box in all EFTEM acquisition dialog boxes. The MDF mode is not used
until you select the Micro Dose Focusing check box in the acquisition dialog
boxes.
What will happen... As soon as you switch on the MDF mode, an off-axis region of the specimen
will be irradiated. The original specimen region will not be imaged until the
actual EFTEM acquisition starts. So you can make and check all the settings
without irradiating the later specimen area. Using the MDF mode, you may
acquire EFTEM images with minimal specimen damage due to electron
irradiation.
For further information on the MDF mode, refer to the corresponding section
of the microscope instruction manual.
Warning The MDF (Micro Dose Focusing) option can only be used with special
microscopes, e. g., with a LEO 912. If your microscope does not provide an
MDF mode, ensure that the MDF check box in the EFTEM Options dialog
box is cleared. Otherwise you may encounter difficulties when acquiring
EFTEM series.
Optimized microscope Select the Optimized microscope control check box to avoid unnecessary
control movements of the camera shutter and screen. EsiVision will then check the
status of the camera shutter via remote control before it is used. Optimizing
the microscope control results in quicker EFTEM image acquisition because
moving the camera shutter takes a few seconds.
150

Warning This option can only be used with special microscopes, e. g., with a
LEO 912 equipped with an up-to-date remote control. If there is no remote
control available for your microscope, make sure that the Optimized
microscope control check box in the EFTEM Options dialog box is cleared.
Otherwise, you encounter difficulties when acquiring EFTEM series.
CCD reference current Enter the current measured by the microscope exposure meter - that
corresponds to a CCD camera (the one in use) exposure time of 1 second -
into the CCD reference current field. The default value is 660 pA.
Align the CCD reference The CCD reference current for your system may differ from the default
current value. In this case, change the illumination on the microscope in such a way
that an exposure time of 1 second yields a high-quality image. Take a look
at the exposure meter on the microscope and enter the measured current
into the CCD reference current field.
When is the CCD This CCD reference current is only relevant in cases where
reference current used? z you are working with a high-resolution CCD camera and
z you do not use the live image for acquisition alignment (Clear the Align
with live mode check box on the ESI tab in the EFTEM Options dialog box.)
In this case, it may be difficult to estimate the exposure time for the HCI
The General tab

image during the acquisition of an EFTEM series. Therefore, the system


uses the currently-measured CCD current of the microscope exposure
meter to compute the suitable exposure time and displays a message box
with the proposed exposure time.
Quantification Select the Show cross section in barn [b] check box to use barn instead of
Show cross section in cm² as unit for the cross section in the EFTEM > Quantification > Element
barn [b] Ratio... command.
– 24
1barn = 10 cm 2

151
EFTEM • Options...
152
Index

Numerics E
2 window method 5 EELS
3 window power law 6 background subtraction 36
3 window white line 6 fourier-log deconvolution 40
integration 35
modify split gain 33
A set labels 31
set split gain 32
acquisition zeroloss calibration 34
ESI, acquisition dialog box 52 EELS atlas
how to acquire a parallel EELS 17 auto scaling 45
how to acquire a serial EELS 126 display zeroloss 48
how to acquire an ESI series 9 load reference spectra 41
how to acquire an image EELS series 14 peak identification 47
image EELS, acquisition dialog box 78 set element labels 44
parallel EELS, acquisition dialog box 104 EELS data 27
serial EELS, acquisition dialog box 124 EFTEM button bar 41
analyze EFTEM data 30
ESI 67 EFTEM menu 41
image EELS 91 electron energy loss spectra 19
append particles 95 print 22
auto scaling 45 element ratio 133
energy windows 7
ESI
B acquisition dialog box 52
background approximation methods 5 analyze 67
background subtraction 36 combine images 73
binning 9 define series 58
button bar, EFTEM 41 drift correction 63
high contrast image 54
how to acquire a series 9

153
how to define an input channel 7
C how to position the slit 7
calibration, parallel EELS 118 load series 66
camera control 56 method 5
combine images, ESI 73 options 50
overview image 71
presentation 69
D qualtiy check 60
R-map 61
define series
save series 65
ESI 58
ESI element distribution 69
image EELS 84
ESI mapping, image EELS 97
display spectra 20
display zeroloss, EELS atlas 48
drift correction
ESI 63 F
image EELS 86 fourier-log deconvolution 40
Index

Options 76
G save series 88
graph information 25 SIT camera 83
microscope 28 image information 30
stage 29 integration, EELS 35
graph menu 31 intensity profile, parallel EELS 121

H L
how to load reference spectra 41
acquire a parallel EELS 17 load series
acquire a serial EELS 126 ESI 66
acquire an ESI-image series 9 image EELS 90
acquire an image EELS series 14
acquire an test spectrum, image EELS 83
calibrate the system for parallel EELS 118 M
define an input channel for ESI acquisition 7 microscope information 28
define an input channel for image EELS 13 microscope parameter 147
define an input channel for parallel EELS 16 modify split gain 33
display the EFTEM button bar 41
generate a spectrum from an EELS image
122
generate spectra from an image EELS series
O
91 online histogram 8
load a spectrum of the EELS-atlas 43 online shading correction 8
optimize the spectrum display for a specific options
ionization edge 45 ESI 50
position the energy slit before recording an genera 148
ESI-series 7 image EELS 76
print images and spectra simultaneously 22 parallel EELS 102
print spectra via the report generator 25 serial EELS 125
154

switch on the remote control 3 overview image, ESI 71

I P
image EELS parallel EELS
acquisition dialog box 78 acquisition dialog box 104
analyze 91 calibration 118
define series 84 how to acquire a parallel EELS 17
drift correction 86 how to calibrate the system 118
ESI mapping 97 how to define an input channel 16
How to acquire a series 14 intensity profile 121
how to acquire a series 14 options 102
how to acquire a test spectrum 83 show calibration data 121
how to define an input channel 13 wide range acquisition 110
how to generate spectra 91 peak identification 47
load series 90 print spectra 22
method 11
Index

Q W
quality check wide range parallel EELS
ESI 60 acquisition 110
image EELS 86
quantification
element ratio 133 Z
ratio image 138
specimen thickness 141 zeroloss calibration 34

R
ratio image 138
remote control 3
R-map 61

S
save series
ES 65
image EELS 88
serial EELS 125
acquisition dialog box 124, 128
how to acquire a serial EELS 126
method 126
options 125
test serial EELS acquisition 132
set element labels 44
set energy-loss 148
set labels 31
set split gain 32

155
show calibration data, parallel EELS 121
SIT camera 57
specimen thickness 141
from image 142
from spectrum 141
interactive 146
spectrum buffer box 19
spectrum document 19
spectrum information 25
microscope 28
stage 29
stage information 29

U
Use 50
Index
156

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