CM200 Opertional Manual
CM200 Opertional Manual
CM200 Opertional Manual
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Emergency Information:
1. Medical Emergencies: Contact 911 and McGill Security 514.398.3000
2. Leave TEM as is. Do NOT shut down the vacuum system.
3. If possible, turn off High Tension and Close Column Valve.
4. Exit the Room/Building.
Protective Equipment
• Nitrile gloves for handling sample holder and safety glasses for filling liquid nitrogen
dewar.
1. Initial Set-up
• When the CM200 is operational, the White Standby and
Red Microscope Off buttons will be illuminated and the
White On button will be dark on the front console. Lit
buttons indicate their availability as emergency
functions while the microscope is running.
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Note: the specimen holder, airlock, and CompuStage are delicate, precisely machined
components. Never exert significant force during any step of this procedure. Doing so
may result in serious damage to the instrument or holder.
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a. RESET the sample stage.
b. Always keep light pressure on the purple goniometer surface when removing the
sample holder. PULL the holder straight back without rotating until it stops moving.
c. ROTATE the holder clockwise until it stops. This rotation moves the guide pin
approximately from the 12 o’clock to 5 o’clock position.
d. Gently, while keeping pressure on the goniometer, PULL the sample holder back to
break the airlock vacuum. This will require a small amount of force.
e. REMOVE the holder straight back out of the goniometer while being careful not to
scrape it along the inside of the airlock. Do NOT to touch the holder O-ring or any part
to the tip with bare hands.
B. Specimen Loading
Note: NEVER mount magnetic samples or discs in the clamp holder of the Single Tilt
Sample Holder. The clamp spring is not strong enough to prevent the specimen from
attaching to the objective lens polepiece. Use the Double Tilt Sample Holder for
magnetic samples. NEVER touch the O-ring to the tip of the holder without wearing
nitrile gloves.
a. PLACE the sample holder in the protective stand.
b. REMOVE the sample loading tool from the base of the stand.
c. Using one hand to prevent the holder from slipping out of the stand, INSERT the tool
into the hole in the specimen clamp and GENTLY RAISE the clamp straight up until it
stops.
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d. TRANSFER the TEM grid into the recess
at the end of the holder using the
tweezers.
e. Use the pin tool to gently LOWER the
clamp straight down to hold the grid
securely. RETURN the tool to the base of
the holder stand. To make scanning the
grid easier, you may wish to orient one
set of grid bars parallel to the long axis of
the specimen holder.
f. RETRACT the holder slightly and turn it
upside down. TAP the back end several
times, then turn the holder upright and check that the grid has not moved (movement
suggests the grid is not properly secured).
g. Use the microscope to inspect the holder O-ring for debris. Gently remove any debris
using a sheet of Kimwipe.
C. Inserting the Sample Holder into the CompuStage
a. Carefully ORIENT the Airlock (Sample Holder) Pin on the sample holder with the 5
o’clock position on the CompuStage and gently INSERT the holder into the Airlock
Entryway until it stops. Be careful NOT to scrape the tip on the inner mechanism of
the goniometer. You should feel some resistance as the sample holder O-ring seats
in the Airlock Chamber.
b. Before inserting the holder into the column, the holder needs to be pre-pumped until
the indicator is off.
c. The data monitor screen will automatically open to the Holder Selection Page. PRESS
the appropriate key and then PRESS the Ready button (below the data monitor
screen).
d. The Airlock will begin pumping and the Red LED on the CompuStage will illuminate.
Do NOT move the Sample Holder when the Red LED is illuminated.
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e. After the pumping countdown reaches zero
and the Red LED goes out, SUPPORT the
purple goniometer surface with one hand
and GRIP the holder securely with the
other. Slowly ROTATE the holder
counterclockwise from 5 o’clock to 12
o’clock position.
f. Gently SLIDE the holder to into column of
the microscope until it stops. TAP the end
of the holder to make sure it is securely
seated.
g. After INSERTING the Sample Holder, WAIT
until the IGP value is lower than 20 Log.
h. VERIFY the apertures inserted are correctly
inserted. Condenser (Upper) and Objective
(Middle) apertures are inserted (lever to the left) and the dial at number 3. The
Selected Area Electron Diffraction (SAED) aperture (lower) should be retracted (lever
to the right).
3. High Tension (Accelerating Voltage) and Filament Saturation
a. To select the accelerating
voltage (High Tension), PRESS
the Parameters key to open the
Parameters pages. On the first
of these pages, the kV may be
modified by pressing the left
(lower the HT) or right (increase
the HT) key adjacent to the
High Tension kV notation on
the screen. VERIFY the High
Tension is 200 kV.
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b. Also on the first Parameters
page is the Emission setting.
Increase the filament current
to the saturation value by
TURNING the Filament knob on
the control panel which should
ordinarily be left at 1. A higher
value will produce a brighter
beam image but will also
shorten the lanthanum
hexaboride (LaB6) filament life.
4. TEM Observation
a. VERIFY the Vacuum
(both UHV and HIVAC
lights are illuminated
and the IGP is <20 Log).
b. Log in to the PC with the
Username and
Password: femr.
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c. On the PC screen, OPEN the CCD camera program by CLICKING the AMTV600 icon.
d. On the CRT, PRESS Ready, Mode, choose configuration page. Turn the filament
knob slowly until the Ext voltage reads 3.8. As a rule of thumb, rotate the knob
until you hear two clicks; wait; rotate again for two clicks; wait; repeat until
reaching 3.8.
e. OPEN the valve (from Close to Open,
counterclockwise) to the right of the
microscope. You should see the
electron beam on the fluorescent
screen. Move the region of interest of
your sample to the middle of the
viewing area with the Joystick.
f. On the TEM control panel, PRESS the
Auto Focus button.
g. On the AMTV600 window, CHANGE the
setting from Speedlive (button in red)
to Qualitylive by pressing the button
once.
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5. Focusing the Image and Diffraction Pattern
a. Focusing the image with the image wobbler
i. Set the Focus Step size (inner Step Size knob) to 5 and PRESS the D button to place
the microscope in Diffraction mode.
ii. ADJUST the Camera Length to 620 mm (NOT 6.2 m) using the Mag knob.
iii. ADJUST the Beam Intensity.
iv. Center the Objective Aperture and ACTIVATE the Focus Wobbler.
v. USING the Multifunction X/Y, ENUSRE the two spots are centered in the Objective
Aperture area.
vi. SELECT D, FOCUS (minimum blur), DEACTIVATE the Wobbler
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c. LOCATE a region of
interest on the sample
using the stage
joystick.
d. To accurately focus,
PRESS Focus. The
image will magnify
four times and enable
the imaging of the
carbon grain and fine
tune your focus.
e. Go to higher
magnification. Find
the correct defocus
and image your
sample
f. To save your image, SELECT File tab and Save As. In the Caption Line 1, enter the
filename.
g. PRESS Save with Caption.
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d. From the TEM Brightfield page, PRESS
CompuStage; the CompuStage Register
Control page will appear.
e. PRESS the Alpha Wobbler key and the stage
will automatically rock through a tilt range
of +/- 15°.
8. Beam Alignment
a. USING the Magnification knob, select a magnification of 17,500x.
b. PRESS the Modes key on the CRT screen to access the Mode Selection page, and then
PRESS Configuration. The Configuration page displays the Filament Heating status and
provides a schematic of the available apertures (Aperture Memo) for the condenser
2 (C2), objective, and selected area lenses. Under Cathode, at the top of the page,
LaB6 should be highlighted, indicating that a LaB6 filament is in use. Fil Limit should
be highlighted next to the number (usually between 22 and 30) indicating the
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saturation limit of the filament. With the limit set (highlighted), the operator can turn
the Filament knob clockwise indefinitely without fear of oversaturating the filament.
Turn the filament up to a number that is 4 or 5 less than the indicated filament limit.
c. DEFOCUS the electron beam by TURNING the Intensity knob clockwise to strongly
OVERFOCUS the C2 lens. BRING the beam back to crossover (the smallest image of
the beam) and CENTRE it with the Shift X/Y knobs.
d. CHOOSE a C2 aperture (Position 3 which is a 100-µm aperture) by ROTATING the
largest knurled knob on the topmost aperture control on the column to the desired
position.
e. USING the Intensity knob, slowly OVERFOCUS (TURN clockwise from crossover) the
beam to coincide with the diameter of the intermediate-sized black circle on the
phosphorescent viewing screen. If the defocused beam is not coincident with the
circle, adjust it using the C2 aperture centering controls. These are both the
intermediate-sized knurled knob on the aperture rod and the knurled knob on the
side of the assembly (to the right). DO NOT TWIST THE SMALLEST, INNERMOST KNOB
(WHICH IS NOT KNURLED) BECAUSE IT UNSCREWS THE APERTURE ROD. Repeat these
steps (c and e) until the beam spreads uniformly around the reference circle while
being overfocused (Intensity knob).
f. USING the Intensity knob, adjust the beam to crossover. PRESS the Fine button (to the
left of the Intensity knob; the indicator light turns green when it is on) and use the
Intensity knob to sharpen the desaturated filament image. CENTRE the image using
the Shift X/Y knobs.
g. PRESS the Stig button on the right-hand instrument panel to open the Stigmator
Control page.
h. PRESS the Cond key on the data monitor screen to SELECT the C2 lens for astigmatism
correction. USE the Multifunction X/Y knobs, while rotating the beam through
crossover using the Intensity knob, to obtain the cleanest, roundest desaturated
filament image possible.
i. PRESS the Stig button to return to the Configuration page.
j. TURN the Filament knob clockwise to fully saturate the filament. When the saturation
point (as defined by the FIL LIMIT) has been reached, the microscope will emit a
'beep.'
k. PRESS the Ready button and then the TEM key to return to the TEM BRIGHTFIELD
page.
l. USING the lever to the left of the viewing chamber, lower the small phosphorescent
screen into place. Insert the beam stop (at the right-hand side top of the viewing
chamber) so that it will be visible across the small screen. Use the binoculars to
observe the beam stop. To adjust the binoculars for your eyes, first adjust the
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interpupillary distance so that you can see through them with both eyes; then adjust
each eyepiece so that the rough edges of the beam stop are in focus for each eye.
When you are done, retract the beam stop and lift the small screen back out of view.
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b. PRESS the Align button on the front
console to access the Alignment
Selection page. On the upper right-
hand side of the page, press Rot
Center so that it becomes
highlighted. Now either voltage
or current centering may be
performed; it is not necessary to do
both.
A. Voltage Centering
a. On the lower right-hand side of the page,
select Volt (under Rot Center Volt Curr)
so that it becomes highlighted. This will
cause the high tension to modulate (the
inner Step Size knob adjusts the
amplitude of modulation). If the chosen
feature shifts off center laterally, the
beam is not aligned along the optical axis
of the microscope and must be
corrected.
b. USE the Multifunction X/Y knobs to
stabilize the feature at the centre of the
screen, eliminating all lateral movement.
The feature should appear to be
pulsating.
c. PRESS the Algn button to return to the
TEM Brightfield page.
B. Current Centering
a. On the lower right-hand side of the page, select Curr (under rot center Volt Curr)
so that it becomes highlighted. This will cause the objective lens current to
modulate (the inner Step Size knob adjusts the amplitude of modulation). If the
chosen feature shifts off centre laterally, the beam is not aligned along the optical
axis of the microscope and must be corrected.
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b. Use the Multifunction X/Y knobs to stabilize the feature at the centre of the
screen, eliminating all lateral movement. The feature should appear to be
pulsating.
c. PRESS the ALGN button to return to the TEM Brightfield page.
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f. UNDERFOCUS the image with the Focus knob (turn counter clockwise from the
crossover) to obtain a few Thon
rings.
g. PRESS the Stg button to OPEN
the Stigmator Control page. If it
is not already highlighted, PRESS
the Obj key on this page.
h. With a live image on the CCD
camera, adjust the shape of the
Thon rings until round using the
objective stigmator with the
Multifunction X and Y knobs.
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and forth through focus, from underfocus to overfocus) and observe if a "streaking"
pattern emerges and changes direction between under- and overfocus. If the astigmatism
has been corrected, the specimen will vary only in focus, with no streaking pattern
evident. Repeat steps 4 and 5 until this state is achieved.
f. PRESS the Stig button again to return to the TEM Brightfield page.
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j. For a fixed collection time, SELECT the Preset dropdown menu on the right-hand side
of the Toolbar. Select a spectrum collection time in seconds either from the presets
or by typing in a value.
k. In the adjacent dropdown menu, SELECT a Time Option: Clock
Time, Live Time or ROI Counts. Clock time refers to actual time
passed; live time refers to the actual time the detector is active.
To use ROI Counts, ROIs must first be created. Refer to the EDAX
manual for more detail. The live time setting is preferable for
repeated measurements.
B. Peak identification
a. To adjust the view of the spectrum, USE the expand (<> or ◊),
contract (>< or ∨) and home keys from the toolbar. The toolbar and these controls are
shown in the figure below. The spectrum display may also be adjusted by clicking and
dragging with the mouse.
b. PRESS Clear All in the spectrum collection panel to remove any old peak labels.
c. PRESS the Peak ID button in the Spectrum Panel for automatic peak identification. The
primary peaks identified by the program will be labeled on the spectrum.
d. PRESS HPD to display a theoretical spectrum, based on the identified peaks and the
collection parameters, on top of the collected spectrum. HPD is used to confirm if the
correct elements have been identified.
e. For manual peak ID, PRESS the ◊ symbol to expand the panel. There are several ways
to manually identify peaks.
f. With the mouse, CLICK ON a peak of interest. A list of possible elements will be
displayed. The most likely peaks are at the top of the list. Scroll through the list and
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select an element to display the spectrum peaks on top of the collected spectrum.
CLICK Add to add the element to the Elements list.
g. To remove an element from the Elements list, HIHLIGHT it and CLICK Delete.
h. The Z+ and Z- buttons can be used to scroll through the elements.
i. Check or uncheck the Alpha lines only, elem, shell, and trans boxes to change how
peak labels are displayed.
j. CLICK on the ◊ symbols to hide the panel.
k. To view the original spectrum without overlays, right CLICK with the mouse cursor in
the spectrum window.
l. Known elements can be entered in the text box. PRESS enter to display the spectrum
peaks for that element on top of the collected spectrum. CLICK Add to add the
element to the Elements list.
C. Saving Spectra
a. The spectrum is saved by CLICKING the Save button at the bottom of the Spectrum
Panel. If you use the .spc as the extension, all the spectrum information will be saved
and can be reanalyzed at a later time. It is recommended that you save all your work
with this format.
b. To save an image of the spectrum, Save As using the .tif extension.
c. When completed, close the program.
A. Leave the microscope in the standard condition for the next user.
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i. REMOVE the sample holder. RETRIEVE your TEM grid. REINSERT the holder into the
CompuStage/column of the microscope.
j. CHECK the Scheduler to determine if there is another user after you.
k. If you are NOT the last user of the day, refill the LN2 dewar.
a. REMOVE the LN2 anti-contaminator dewar, pour the remaining LN2 into the large
dewar, and PLACE the microscope dewar on the counter. PLACE a towel below the
dewar platform to collect condensing moisture.
b. On the CRT, GO to the Vacuum page, PRESS the Cryo key, SET the time for six hours
and PRESS the Start key.
C. Retrieving Images from the Support PC (SPC). Note: Files are deleted on the SPC every
three months.
a. COPY your images to a USB drive, LOG OFF the SPC and TURN OFF monitors.
b. CLOSE the AMTv600 program and LOG OUT of the PC.
c. TURN OFF the Panel light with the Panel Dim knob and CRT Screen with the Data Dim
knob.
D. Last Steps
a. SIGN the logbook and LEAVE any relevant comments. If you START the cryo cycle,
please INDICATE in the comments.
b. TURN OFF any lights.
c. EXIT the room and CLOSE the door.
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Notes:
Camera Constant Lλ for SAED
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