Electron Microscope Imaging Service—Philips 420 Transmission Microscope

2.1 Specimen holders
The microscope is supplied with the Single Tilt specimen holder as standard. A range of holders supplying additional movements to the basic X, Y, Z and tilt of the goniometer stage, or special treatments, are available as options.
The following general instructions apply to all holders for the EM420 (holders for EM420 and CM10 are interchangeable):
i. When handling parts of specimen holders that enter the vacuum (beyond the sealing 'O'- ring), always use nylon or similar gloves. NO GREASE
ii. The specimen, spacing rings, and clamping devices should only be manipulated using pointed tweezers and special tools provided. These should be maintained in a clean condition.
iii. Before use check the holder tip with a magnifying glass to ensure that it is clean and dry. The critical bearing surface is made of sapphire. Check also that the seating of the specimen carrier is clean and does not contain residues. Clean with compressed air cans.
iv. The O-ring on the rod should be checked for possible dirt and excessive quantities of grease, although it must not be completely dry.
v. When a specimen holder is not in use, store it in its box. Keep the specimen support clean and also store it in the box when not in use. O -Ring
2.2 Mounting a specimen in the single tilt holder
i. Check that the tip of the holder and the clamping device are clean and dry
ii. Rest the holder on its support with the spring clamp horizontal, ensuring that the tip is properly supported by the recess in the block.
iii. Lift the clamp to its fullest extent using the tool, which fits into a hole into the front of the clamp.
iv. Carefully place the specimen (if a grid, with the specimen uppermost) in the carrier (14) . View with a magnifying glass to make sure that it is correctly loaded.
v. Carefully lower the clamp onto the specimen (or grid) making sure that the specimen remains correctly in position.
CAUTION: This procedure must be carefully controlled, otherwise the clamp can be damaged, resulting in specimen instability.
2.3 Removing a specimen from the single tilt holder
i. Rest the specimen holder on its support (as described in section 2.2 above).
ii. Lift the clamping device (as described in section 2.2) .
iii. Remove the specimen by inverting the holder over a Petri dish or filter paper.
2.4 Beam astigmatism correction Everything acting upon the beam in the illuminating system can contribute to its astigmatism. Thus, whenever the condition of any component in the system is charged (e.g. spot size, or aperture sizes) the beam astigmatism may change and therefore need to be corrected. The alignment of the condenser stigmator is carried out during installation and does not need subsequent realigning.
Beam astigmatism correction is carried out as follows:
i. Insert a specimen (see section 2.2) .
ii. Set Magnification control (9) to position 25, or higher > 23000×.
iii. Adjust specimen height (see section 3. 10.3 in instruction manual, pg. # 151) .
iv. Focus the image (control 15a, 15b).
v. Remove the specimen from the beam.
vi. Select maximum beam intensity (intensity control 5a close to fully counter-clockwise).
vii. Undersaturate the filament (control 2a) until a filament image is obtained. If necessary, adjust Gun tilt controls (16) until a symmetrical filament image is obtained.
viii. If necessary, readjust the intensity until the structure of the filament is visible in the central area of the image. This will usually be sharp in two perpendicular directions for different settings of the intensity controls (5a, b).
ix. Adjust the Condenser stigmator controls (17) until filament structure is sharply focused in all directions for one setting of the intensity control.
x. Saturate the filament (control 2a).
*Once filament saturated for one emission current, through coupling it is saturated at all emission current settings.
2.5 EDAX Operations on the Philips
i. Use the low-background single-tilt specimen holder
ii. Find an area of interest on your sample.
iii. Remove the objective aperture.
iv. Lower spot size in necessary
v. Insert the detector via the computer control.
vi. The microscope is now ready for EDAX acquisition.
vii. Adjust the TEM Spot Size to a smaller spot if dead-time is over 40%, use a larger spot size if it is less than 10%. The detector will automatically withdrawal if the counts are too high.
viii. When you wish to observe the sample remove the detector and insert the objective aperture.