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Hitachi X800 Field Emission Gun (FEG) Scanning Electron Microscope (SEM)
Operating Instructions
A. Getting Started
- You should find all the lights on the front panel green, the SC Air Lock Valve and the SEC Air Lock Valve should be flashing green.
- One of the objective apertures should be in the path of the beam.
- Please be careful flipping the toggle switches - you must pull on the toggle switches before you flip them.
- Log into the log book, note any problems during your session.
- Load your sample using tweezers and wearing gloves.
B. Inserting a Sample
- Turn on the Display Power - this turns on the display, as well as a light inside the sample chamber.
- Set the X, Y, Z, TILT and ROTATE to the exchange position. The exchange position of the Z axis is 18. (Note that this is different from the value displayed on the chamber.)
- Check that the manual door (MV1) and the SC Air Lock valve are closed.
- Air the Sample Exchange Chamber (SEC) by pressing AIR.
- When the door becomes ajar, slide out the chamber.
- Using gloves, screw the rod into the sample base.
- Slide the SEC closed.
- Evacuate the SEC by pressing EVAC.
- Turn on the monitor for the chamberscope.
- Depress the white button on the GW type 43 panel, to turn on the chamberscope.
- Important! After the SEC reaches high vacuum (look for green lights on both the sample chamber (SC) and the SEC vacuum indicators), open the manual door.
- Insert the rod into the SC, sliding the sample base into the stage, watching on the monitor.
- Unscrew the rod from the sample base.
- Important! Pull the rod back out until it clicks into its clip, and close the manual door (MV1).
- Release the white button on the GW type 43 panel to turn off the chamberscope.
C. Turning on the Beam and Obtaining an Image
- Set the accelerating voltage, Vo , to the desired voltage, by turning the wheels on the control panel under
the left monitor. If Vo will be 5 kV or less, set the VO knob to A.
- If you are the first user of the day, set the flash intensity to 2. The tip will be flashed when the beam is turned on.
- Check that both the SEC and SC vacuum lights are green, indicating high vacuum.
- Open the SC Air Lock Valve, pulling on the toggle switch before flipping it.
- Turn the beam on by pressing HVON. The emission current should be 10 mA.
- If you have flashed the tip, set the flash intensity back to 0.
- Decrease the magnification to a minimum: 40X.
- Check that the Auto Brightness and Contrast (ABC) switch is on Auto, and press the ABC button.
- Focus using the coarse focus knob, or AFC (Automatic Focus Control)
- Increase the magnification to 7K - 10K X.
- Move the image in and out of focus using the coarse focus knob. If features on your sample shift as you
move in and out of focus, the objective aperture needs to be aligned. You may also use the aperture align (beam wobble) switch to rock in and out of focus automatically. Adjust the X and Y knobs on the
objective aperture until the features do not shift as the image is brought in and out of focus.
- Stigmate the image using the X, Y stigmator knobs. Do this by repeating a circle of adjusting the X, then the Y, and then focusing.
- If the beam current drops too far below 10 mA, boost it back up to 10mA by pressing the HVON button.
D. SEM Image Acquisition/Saving Procedure:
Open iXRF EDS2004 Software
Enter the accelerating voltage (kV) and magnification in the fields on the upper right:
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- Set microscope on scan speed 1, 2, 3 or 4 (not TV mode).
- Acquire image: click on camera button or go to File then New then image.
- Adjust image resolution (if necessary): go to Properties then Acquisition
- Set Resolution to 512. (it may already be set to 512; this is a good size for both resolution and disk space economy.)
- Adjust the micron bar on the image (if necessary): go to Edit then Annotations
- Set Length to whatever value you want to display on the image.
- Check the box next to micron bar to display it on the image.
- Check that the size of a feature in the collected image matches the same feature in the image on the SEM
CRT: choose Annotations, and then the ruler icon; click one end of the feature, drag the mouse to the other end of the feature, and note the size. If the size is the same as on the SEM (10% error is
acceptable), continue to next step. If the sizes differ significantly, see note on Calibration.
- Save image: click on save button or go to File then Save (or SaveAs)
- Select the location to save the image: Use C:\Public\your name. (Where your name is your last name.)
- name the file, click on Save. (This saves the image as a .imx file type; this can only be opened in iXRF.
You must do the following step so that the image can be opened in other software.)
- Export image in a usable format: go to File then Export; if you want the micron bar on your image, check the box next to with Annotations.
- Select Save as type
- Select JPEG to save your image as a .jpg format image (do not use JTIF). (You may use another format if you like, but JPEG
format gives excellent resolution while using minimum disk space. The .tif format is popular but for the same image, its size will be at least 10 times larger than a .jpg
and the resolution is essentially the same.)
- name the file, click Save.
- Send the files across the campus network to your account.
- Close iXRF EDS2004 Software.
E. Removing the Sample
- Turn off the beam by pressing the green READY/OFF button.
- Close the SC Air Lock Valve (pull on the toggle switch first!).
- Set the X, Y, Z, TILT, and ROTATE to the exchange position (the Z axis should be set to 18.)
- Depress the white button (it will light up) on the GW type 43 panel, to turn on the chamberscope. Also turn ON the monitor, if it is not already on.
- Retract the EDS detector if it is visible and near the sample.
- Check that the SEC green light is on. Important! Open the manual door.
- Retrieve the sample base with the insertion rod, watching on the chamberscope monitor for the clearance of the sample.
- Close the manual door.
- Release the white button on the GW type 43 panel to turn off the chamberscope.
- Air the SEC by pressing AIR, the manual door should be closed.
- When the door becomes ajar, slide out the chamber.
- Using gloves, unscrew the rod from the sample base.
- Slide the SEC closed.
- Evacuate the SEC by pressing EVAC.
- Turn off the Display Power, and the chamberscope monitor.
F. Notes
- The chamberscope gives off infrared radiation, therefore always turn it off when operating the KEVEX
EDX detector or the backscatter detector. It interferes with both attachments.
- To change the objective aperture, turn the aperture knob in or out. You will generally use apertures 1 or 2 for EDX on the SEM. Apertures 3 and 4 are generally used for imaging.
- Objective aperture sizes:
- Suitable IP pressures:
- iXRF software Calibration: Adjust the magnification in the software: go to Properties then Magnification Calibration.
- Set the microscope mag to that shown on the microscope.
- Set the Image magnification to that shown on the microscope
- Measure a feature in the image on the SEM CRT, using the dashed micron bar on the bottom of the CRT. Enter that value into Line length
(in microns) in the software. Click the square with the diagonal line running through it, and draw a line over the same feature in thecollected image, this time, and click Update Calibration.
Check that the micron bar in the software now shows the correct size. The iXRF software calibration is complete.
- Taking a Polaroid picture: insert the film into the Polaroid camera and then press the PHOTO button. When
the light under the PHOTO button dims, pull out the film in one quick, smooth motion. Allow to develop for 20 sec, then peel apart.
- Film and f-stops:
G. Backscatter Detector Operation
- Image the sample in the secondary mode as described in the operating instructions.
- Turn ON the chamberscope and turn ON the monitor.
- Insert the BSE detector, watching on the chamberscope that it slides under the polepiece.
- Turn OFF the chamberscope (the BSE detector is sensitive to infrared radiation).
- Turn BSE detector power ON, located on GW BSED bin.
- Select A on Ch2 (next to PHOTO button).
- Select slow scan speed, 2 or slower.
- On the GW BSED bin, adjust the CONTRAST and BRIGHTNESS half way.
- Turn ON chamberscope to watch the BSE detector while...
- ...pulling half way out, so as to block the beam completely.
- Turn OFF the chamberscope.
- Obtain waveforms; put OFFSET ADJUST at Ch A.
- Adjust two BSE waveforms on top of each other with GW BSED panel BRIGHTNESS.
- Turn OFF OFFSET ADJUST.
- Insert the BSE detector all the way.
- Make any adjustments to contrast and brightness from the GW 120 panel.
- To record BSE image: flip RATE switch to RECORD.
- Check that the recording CRT corresponds to the CRT showing the BSE image.
- Load film and push PHOTO button.
- Remove detector when done by pulling gently on the rectangular box until the teflon knob protruding from the top is behind the silver lock mechanism.
- Push Ch 2 SE button.
- Turn GW BSED detector power OFF.
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