Hitachi HF2000 TEM User manual

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HITACHI HF2000 TEM
Operation Manual
- Alignment and Operation -
Dear users,
To help you have a smooth and successful TEM observation, I wrote up this basic operation manual.
Systematic theoretical training plus hands-on practical training may be the best way to understand the
details of this operation instruction for HF2000 TEM.
There are some notes in this instruction. Please read and follow them carefully, and please make sure you
follow what I told you ask before you touch the TEM if you do not know the consequence of your action.
Takamichi MIYAZAKI / June 2009
Contents
1. Startup
2. Set the sample (loading)
3. Applying High Voltage
4. Prepare for beam alignment
5. Correct condenser astigmatism
6. Z-height adjustment
7. Voltage center
8. Image focus and Objective lens astigmatism correction
9. Selected area electron diffraction
10. Bright field imaging
11. Photographing
12. CCD camera
13. Sample tilt
14. Astigmatism correction of beam tilt
15. High resolution imaging
16. Microbeam diffraction
17. Sample exchange (unloading)
18. Shutdown
19. Film exchange

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1. TEM startup
•Check the comments in the TEM log book. Enter your name,
laboratory and contact information on the log book before any
action on the TEM.
•Make sure that TEM vacuum is good. At the vacuum state
(right panel), SPEC, COL, and CAM indicators should be
VAC position (all green), and GUN indicator is at EVAC
position (green flashing).
•Make sure that TEM is set at standby positions:
a) OBJ. TEMP. MONITOR: 210C and below
b) Objective, selected area and condenser apertures are out (position 0).
c) GV (Gun Valve) is Closed
d) ACC. VOLTAGE: off; HV: on at 200kV
e) Sample position: X = 0, Y = 0; Sample tilts: 0
f) Bright/Dark field selector set at Bright field.
g) Microscope is at [ANA1] mode.
h) Magnification: 1000K – 1500K
i) Normally, the sample holder stays TEM. It is situated at position A
j) Lens Current (C1, C2, OBJ) : not 0
k) Unexposed film number: 50 FULL
Film number: 1 0
•After confirmation of the standby positions, enter chiller temperature and pressure, COMPR pressure,
HV tank pressure, and vacuum state on the log book.
Position A
EVAC
Selected Area
diffraction aperture
Objective aperture
Correct condenser
a
p
erture
X-ray detector
a
p
erture
Right main panel
Vacuum state

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2. Set the sample (loading)
Normally, the sample holder stays in TEM. It is situated at position A (see in the following diagram).
Note: Objective aperture must be out during sample holder loading / unloading.
•Turn the switch on goniometer to Air. Wait till SPEC is at Air position (red light on vacuum state) and
pull the holder out.
•The sample is securely seated in the holder
•Loading sample holder into TEM
Follow the route indicated in the diagram below to load
your sample holder into the TEM.
1) Insert the sample holder horizontally along and
press it, then turn the switch to EVAC.
2) When electron sound rings, turn the holder clockwise till it stops.
3) Let the sample holder go into the TEM horizontally along and smoothly. The sample
holder must be under control.
4) Turn the sample holder counter-clockwise till it stops
5) Let the holder go into the TEM fully.
B位置
C位置
A位置
（EVAC⇔
A
IR）
Ｂ
位置
A位置
Ｂ位
置
Bposition
Aposition
Cposition
Aposition
Bposition
EVAC / AIR

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3. Applying HV
•Apply HV when vacuum is good
•Make sure that the applying HV conditions are set at following state:
V0 VOLTAGE 200kV
RRATIO 5.5
I1 CURRENT 30µA
•Press the [FE] bottom once (left panel) and press [FLASH] when it’s flashing. IF current rise up, if the
IF current is lower than 0.30 mA, repeatedly press [FLASH] bottom till IF current is > 0.30mA.
•After IF current exceeds 0.30mA, wait till V0 VOLTAGE rises up to 200kV. Then V1 and V2 Voltage
rises gradually up to the setting value (watch the ACC VOLT on the CRT monitor).
•Enter the V1 Voltage and IF current on the log book (Yellow book).
********************************************************************************
When the emission current drops below 10µA, press [I1C] and recalibrate extraction voltage to raise the
emission current to 30µA. The beam wander off during the process but return by the end of the I1C state.
Repeat alignment procedure because the changed extraction voltage affects the caustic.
********************************************************************************
4. Prepare for beam alignment
•Press [ANA1] to change selected mode: Analysis →TEM mode.
•Reset switch (Red square button)
[I1C]
[FLASH]
Left main panel

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5. Correct condenser astigmatism（Magnification : 100K ~ 200K）
Be sure to use the correct condenser astigmatism for TEM mode:
•Open the GV and make sure you hear it click open.
•Turn the Brightness control (left panel) to crossover, and center the beam with the Brightness
Centering knobs (right panel).
•Using the condenser stigmator (right sub panel) make the caustic as round or axial symmetry. And
using the 3rd order stigmator (left sub panel) makes the caustic as symmetry. The 3rd order correction
will be slight and the controls should be close to the center positions.
•The correctly aligned caustic will appear as a circle with Star in TEM mode. The image is shown
below.
•Insert condenser aperture (First aperture) and
minimize the swinging beam using the condenser
X/Y adjustment screws when passing through
crossover.
3rd Cond Stig
2nd Cond Stig
3rd Cond stigmator
2nd Cond stigmator

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6. Z-height adjustment
•Move edge of sample and set the objective lens current to 5.72 using focus control. Focus the sample
using the Z-height adjustment screw on the specimen holder entry port.
Note: An objective lens current of 5.72 is the optimal setting for minimum spherical aberration.
You may also focus sample using wobblers method or minimum contrast method for the image
focus.
7. Voltage center
•Move edge of sample.
•Turn on [HVM] (HV MODULATION, right panel). The image feature may oscillate.
•Adjust BEAM TILT (right sub panel) to minimize the vibration of the feature.
•Turn off [HVM] (right panel).
•Repeat the alignment procedure a few times because the beam tilt and objective stigmatism correction
have disturbed the condenser stigmatism corrections. In general, completing the alignment procedure
twice will be sufficient.
Z-height adjustment

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左サブパネル
左サブパネル
8. Astigmatism correction of objective lens
•Reset the OBJ STIGM-X and Y control knobs (stigmator)
on the left sub panel.
＊This returns setting to the stigmator to preset level.
•Set a magnification 2 or 3 times higher than used for
photographing.
•Turn the focus control knob clockwise so as to obtain
slightly over-focused image, and a fringe appears outside
the collodion hole.
•Adjust the OBJ STIGM-X and Y control knobs so that the width of the fringe outside the collodion
hole becomes uniform.
•Manipulate the focus control knob so as to approach just focus from over-focus in order to narrow the
fringe width.
•Find a as granularity a amorphous as possible and adjust the OBJ STIGM-X and Y control knobs so
that granularity a amorphous becomes finer granularity as shown in the figure below.
9. Image focus and Objective lens astigmatism correction
(Including Selected area electron diffraction (SAED))
This is to tell you how to correct objective lens astigmatism using amorphous film which is useful in
recording a high resolution image.
•Center a small hole / particle / the sharp edge of sample.
•Insert and center a suitable Selected Area (SA) aperture.
•Press [DIFF] (left panel) and set the camera length to 0.80m using Magnification knob. If the central
spot (transmitted wave) is still disk, focus the pattern by adjusting Diffraction Spot (left panel).
Note: Open the beam to form a parallel illumination on the sample by turning Brightness
clockwise. Diffraction spots will become weaker and smaller. If the central spot is disk instead of
a spot, adjusting Diffraction Spot is needed.
Left sub panel

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•Insert objective aperture into the central spot that should be centered by using the objective X/Y
adjustment screws.
•Press [ZOOM] to seen a bright field image.
•Pull out SA aperture
•Correct the astigmatism by adjusting fine focus and OBJ STIG X and Y controls if necessary.
(Using minimum contrast method and amorphous contrast)
10. Bright fielding imaging
•Find an interesting sample area.
•Focus the beam and sample to the crossover.
•Press [DIFF]. (see Sec.9, SAED)
Note: If the central spot is not at the viewing center, center it using the INTER ALIGN X and Y knobs
(left sub panel). If the spot is not round, make it round using INTER STIG X and Y knobs (left sub
panel).
•Insert the objective aperture into the beam by turning the aperture handle clockwise.
•Press [ZOOM] to see a bright field image.
•Adjust fine focus and OBJ STIG if necessary.
•Adjust Brightness so that Auto exposure time is between 2-5 seconds.
•Cover the viewing window
•Press [Photo] to expose the film and record a bright field image.
電子回折図形
明視野像
格子（多波干渉）像
Bright fielding imaging
Electron diffraction pattern
Electron diffraction pattern
Lattice imaging

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11. Photographing for film
Usage of auto exposure time set mode
Time mode provides a function for automatically setting the exposure time so as to obtain optimum
photographic density on a film in response to a determined brightness.
•Set the exposure time setting knob at AUTO.
•Press the PHOTO key to start film exposure.
Manual mode
•Set a desired exposure time by turning the EXPOSURE TIME control knob. The set exposure time is
displayed at the bottom right on the CRT.
•Optimum exposure time lines for
Bright field image: 1 to 4 seconds
Dark field image: 12 to 30 seconds
Selected area diffraction pattern: 0.5 to 1 seconds
Nano beam diffraction pattern: 8 to 16 seconds
•Press the PHOTO key to start recording
12. CCD camera
•Turn on the power to TV monitor and control.
•Open the beam by turning Brightness clockwise. Brightness will become weaker.
Note: Do not use CCD camera for diffraction pattern, low-magnification image and direct beam.
•Cover the viewing window.
•Press [STOP] and [PHOTO].

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13. Sample tilt
•Press [DIFF]. (see Sec.9, SAED)
•Adjust the sample tilt with electron beam direction along the zone axis.
14. Astigmatism correction of beam tilt
•Turn the WOBBLER ANGELE control on the right main panel fully clockwise.
•Press the WOBBLER ON/OFF switch.
•When astigmatism is not corrected, rotating motion in a specific direction is observed. Adjust the
[BTX] and [BTVX] controls on the left sub panel so that non-directional image rotation is observed as
shown below.
•Turn the WOBBLER ANGELE control counterclockwise by 3 steps. When astigmatism is not
corrected, adjust the [BTY] and [BTVY] controls on the left sub panel so that non-directional image
rotation is observed as shown below.
FOOT
RIGHT
FOOT
LEFT
HAND
LEFT
HAND
RIGHT
FOOT
RIGHT
HAND
LEFT