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_SEM-InstructionManual
- 1. Hitachi SU-70 UserManual Last updated: 04/09/2015 R. Basantkumar Log In to the SEM computer User name: Password: Sample Preparation 1. If conductive, place a carbon tape strip on the sample holder, and then place the sample on the tape, or place your sample, and then place carbon strip on the top and bottom of the sample for a conductive path 2. If not conductive, sputter a thin film of Iridium on the sample, and then follow step 1 Starting Conditions 1. Read the gauge to ensure that the microscope is at appropriate vacuum (10-3 -- 10-5 Pa). SpecimenLoading 1. Press the “AIR” button to vent the exchange chamber 2. Swing back the door when the chamber vents. 3. Mount the sample holder so that the bottom holes connects into the grooves on the door and then rotate to lock position 4. Close door 5. Press the “OPEN” button. Wait until “EVAC” button stops flashing and the chamber door opens 6. Gently slide the sample exchange rod in completely. (Watch the chamber camera as you do this to ensure a secure connection.) 7. Rotate the rod to unlock position and withdraw rod, pull out completely 8. Press the “CLOSE” button, and wait for the vacuum to be ready SpecimenUnloading 1. Set stage to “EXC” exchange position 2. Press “OFF” to turn the beam off 3. Press the “OPEN” button. Wait until “EVAC” buttons stops flashing and the chamber door opens 4. Gently slide the sample exchange rod in completely, and then rotate to lock position. 5. Withdraw rod, pull out completely 6. Press the “CLOSE” button 7. Press the “AIR” button to vent the exchange chamber
- 2. Hitachi SU-70 UserManual Last updated: 04/09/2015 R. Basantkumar 8. Swing back the door when the chamber vents. 9. Dismount the sample holder by rotating the rod to unlock position 10. Close door 11. Press the “EVAC” button Software Setup / Obtaining an Image 1. Once the vacuum has reached, click the “HOME” and “ON” to move the stage and turn on the beam Note: Make sure the working distance is set at 15mm, 2. Select low magnification “LM” and reduce the magnification to a minimum 3. Adjust the auto brightness and contrast (“ABC”) so you can see something and focus using the knob on console. (If you have little signal: do the beam alignment) 4. Use the joystick to move the stage to an area of interest on the sample 5. Now turn on the high magnification “HM” Note: Bring the specimen to a desired working distance by typing in the corresponding value into the “Z” box then press the “Enter” key. DO NOT bump into the end of column 6. Go up in magnification and focus to the best of your ability Alignment 1. Beam Alignment a. Make sure “Align Beam” is selected. Adjust X and Y knobs on control panel to maximize signal (brightness) 2. Aperture Alignment a. Find feature at about 3,000X or more (more is better). b. Make sure “Aperture Align” is selected c. Adjust X and Y knobs to minimize motion of image. (Keep feature in field of view by moving stage.) d. Work up to higher mags (15,000X or more) as needed. e. When done, press “Align” and focus 3. Stigmate X & Stigmate Y a. Find feature at higher magnification (8,000X or more—again, more is better). b. Roll focus and look for stretching of image. It will switch from one direction to another. Set focus where stretching switches. (If you can’t see the stretch just get the best focus you can.) c. Adjust X and Y to get sharpest image d. Work up to higher magnifications as needed e. Adjust focus if necessary Aperture alignment and astigmatism correction should be done well above the magnification at which the images are acquired.
- 3. Hitachi SU-70 UserManual Last updated: 04/09/2015 R. Basantkumar Acquiring an Image 1. Click “Slow 3” then “ABC” and 2. Press 1280 (add capture). It will take about a few seconds to scan and the frame will be frozen 3. Click Fast 1, then Run to unfreeze image once the image has been captured Exporting Images 1. Open the PCI program (start menu) 2. Select Database a. Select Sample b. New and type a sample name (copy the title name) 3. Select File and Series name a. Paste the copied title name and place a – (dash & space) 4. Go back to the Hitachi program a. Highlight all the images you want and click export 5. The images will be exported to the PCI program a. Back in the PCI program, click file, save as and click OK for each image b. Then click file, data manager move to the sample tab and select all c. Now click file, export all and browse and place your sample in new folder 6. From here, you can transfer your images using an approved USB flash drive (Images are saved twice)
- 4. Hitachi SU-70 UserManual Last updated: 04/09/2015 R. Basantkumar EDX 1. Switch to the EDX monitor NOTE: To switch between the two monitors it is either Ctrl+Alt+1 (SEM) or Ctrl+Alt+2 (EDX) 2. Open “INCA” software a. Username: INCA b. Password: INCA 3. Remember to adjust your working distance on the image to be at 15mm, refocus, re-stigma align and aperture align a. Do not change it once the chamber camera is turned off 4. Turn off the chamber camera by pressing the red flip button switch in front of the camera monitor 5. Open Inca and use “Point and ID” 6. Select a sample name 7. Now go down the list on your EDX monitor a. Press Green Light in “Site of Interest” to take image b. Go to “Acquire Spectra” use point or box to select areas of interest c. Go to “Confirm Elements” Note: Check peaks to make sure elements make sense and line up to programmed peaks d. Go to “Quant” and put on “All Spectra Click on quant e. Go to “Compare” and set-up Spectrum (Choose Spectrum 1 then put in other Spectrums for comparison, if needed) f. Go to “Report” 8. Then export to MS Word a. In MS Word go to Change Styles → Style Set → Word 2003 b. Clean up Report, and Delete Extra Blank Pages that occur c. Use/Add Excel Phase Template if needed d. Add Comments as necessary 9. Then click on report in word format 10. Once in word, change the style to 2003 format 11. Repeat Steps 7-8 for each Spectra 12. Save Report on D: Drive and on Flash Drive (save twice)