Philips CM200 User 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.
Emergency Contact Information:
•David Mui –Staff Scientist: Cell 438.938.6886; Email: [email protected]
•S. Kelly Sears –Facility Manager: Cell 514.576.1926; Email: [email protected]
•Joaquin Ortega –Director: Office 514.398.6348; [email protected]
Philips CM200 200kV TEM
Simplified Operating Manual
(Prepared by David Liu, S Kelly Sears and Joaquin Ortega)
Safety
•Do not wander behind the microscope or step on cables.
•There is one computer for the CM200 TEM.
1. The support PC (SPC) is for taking digital images with the AMT XR41B CCD camera and
collecting spectra with the EDAX Genesis Energy Dispersive Spectrometer (EDS) and
Genesis software. Note: Ensure you copy your data at the end of each TEM session.
Data older than three months may be deleted without notice.
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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•ROTATE the Panel Dim knob to illuminate
the console panel lighting and emission
gauge. Clockwise rotation of the Data Dim
knob increases the brightness of the CRT
screen.
•VERIFY the UHV and HIVAC indicator lights
on the console are lit (Green). If they are
NOT lit, PRESS the Vacuum System On
button and wait (20 to 30 minutes) until
the two lights come on.
•VERIFY the black rubber mat is covering the viewing
window and carefully FILL the anti-contaminator cold
finger dewar (cold trap) with liquid nitrogen. The first
dewar flask of the day should last ~30 to 40 minutes.
Later dewars will each last 2 to 3 hours. Do NOT allow the
cold finger to fall below 50% or to warm up as the column
vacuum will deteriorate significantly. REPLACE the
styrofoam cap on the top of the dewar.
•The CRT screen will display the CM200 status startup
page or, more likely, one of the Modes or Mode
Selection pages. If the Ready light (on the pushbutton
directly below the CRT screen, to the right) is lit,
pressing it will move the screen selection back in the
hierarchy of the pages. PRESS the Modes key to obtain
the Mode Selection page.

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•PRESS the Vacuum key on the CRT Screen to
check the vacuum status of the instrument. It
should read Ready at the top center of the CRT
screen. VERIFY the Ion Getter Pump (IGP) value
is lower than 20 Log.
•If it READS Start-Up, contact FEMR staff for
assistance and wait for the vacuum to improve
before the microscope can be used. Note: Do
NOT use the microscope (i.e., do NOT turn on the
filament) if the IGP value is 20 Log or higher.
•PRESS the Ready button to RETURN to the TEM
Brightfield page (black arrow).
•VERIFY the Apertures: Condenser Aperture (C2) is
at 4; Objective Aperture is 3 and the Selected
Area Electron Diffraction (SAED) Aperture is out
(position of the lever is to the right) except when
performing electron diffraction.
2. Specimen Loading and Holder Insertion/Removal
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.
A. Removing the Sample Holder from the CompuStage (Column)
Condenser Aperture
Objective Aperture
Selected Area Aperture

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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
6. Camera Control and Imaging
a. CREATING a new Background Image. Note: The background image compensates for
phosphor inhomogeneity and optical imperfection.
i. VIEW the electron beam on the TEM viewing screen.
ii. CENTRE the beam.
iii. REMOVE specimen from column or locate a hole on TEM grid
iv. SET the magnification to roughly the magnification you will take the images.
v. SPREAD the beam with C2 control clockwise so that the current is about 1.0
second on the exposure meter.
vi. LIFT the viewing screen and cover the viewing glass window with the black rubber
mat.
vii. On the AMT software, SELECT the menu item Corrections --> Acquire Background.
viii. ADJUST the intensity knob (C2) so the histogram on the AMT software is
approximately centred in the box. When this is correct, PRESS the orange
command button.
ix. It will take ~60 seconds for the background correction to be completed. WAIT until
the Click Live Imaging button is re-enabled.
b. On the AMTv600 program, PRESS Live Image.

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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.
7. Eucentric Height Adjustment
a. Using the Magnification knob, SET the
Magnification to 5,800x and the use the
Joystick to locate and centre a small
feature on the TEM grid, i.e. small hole or
particle
b. FOCUS the feature using the Step Size
knobs. The Outer Knob changes the Focus,
and the Inner Knob (i.e. the step size
adjustment) modifies the amount of focus
change per click of the Outer Knob.
c. FOCUS the feature using the knobs marked
Step Size. The Outer Knob changes the
Focus, and the Inner Knob (i.e. the step size
adjustment) modifies the degree of focus
change per click of the Outer Knob.