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Scanning Electron Microscope

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					                  SEM Standard Operating Procedure

Loading the Sample and Analysis
   1. Sign in the logbook.
   2. Wear gloves and screw your sample to the fixture (for details refer to Guide for
       New Users). Make sure that the sample is secured.
   3. Flip display power switch up. You need to pull the switch before you can flip it
       up.
   4. Turn on the (a) monitor and (b) camera.
   5. Press “red” air button to open the exchange chamber.
   6. Screw fixture with sample to the metal rod. Turn the metal rod clockwise to
       tighten.
   7. Press the exchange chamber door close and hold, then press the “green” evac
       button. You may remove your gloves at this point.
   8. Wait for the chamber pressure to go down to 1. This will take at least 5 mins.
   9. Lift the handle to open the specimen chamber.
   10. Push the rod into the specimen chamber. Make sure sample and fixture are
       securely placed on the specimen chamber.
   11. Unscrew the metal rod by turning it counterclockwise.
   12. Pull the rod completely out of the specimen chamber.
   13. Close the specimen chamber.
   14. Set the timer to 2 mins.
   15. After 1 min, click switch to open the SC air lock valve.
   16. After the 2nd min, press the “on‟ button to activate the electron beam.
   17. Press PF1 and enter a value to choose the voltage level. Usually, 15 KV is used.
   18. Press PF2 and choose the working distance.
   19. Press PF2 and choose the lower or upper detector. For the lower detector, a
       working distance of 15 mm is used while for the upper detector it is 5 mm.
   20. Press PF7 and select choice “number” to label your sample.
   21. If you will be using the lower detector, tilt the sample to 40 degrees.
   22. If you will be using the upper detector, lift the “z” knob to 5mm.
   23. Look into the monitor and find your sample by pressing the lower magnification
       button and by adjusting the magnification knob to the lowest level. Locate
       sample by controlling the knobs attached to the specimen chamber. For more
       information with diagrams, refer to Guide for New Users or the Manual.
   24. After locating your sample, remove lower magnification by pressing the lower
       magnification button again.
   25. Adjust the magnification knob to the lowest magnification possible.
   26. Focus the image by rotating the focus control knobs (coarse or fine knobs).
   27. Increase magnification slowly.
   28. Repeat steps 26 and 27 until you find your target image at desired magnification.
   29. If image is poor, adjust brightness and contrast.
   30. Also, adjust through astigmatism (stigma) alignment.
   31. If the picture is shaking, minimize shaking by pressing PF3, then:
            (a) Select beam adjustment by hitting return button. Try to center the view
                by controlling the stigma/align knobs.
            (b) Select Aperture Align by hitting return button. Minimize shaking by
                controlling the stigma/align knobs.
           (c) Select Stigma Align X by hitting the return button. Minimize shaking by
               controlling the stigma/align knobs.
           (d) Select Stigma Align Y by hitting the return button. Minimize shaking by
               controlling the stigma/align knobs. Press PF16 to exit.
   32. Improve picture quality by pressing TV 1, 2, 3, or 4.
   33. Place printing paper and hit button to print image on screen.
   34. If you plan NOT to use the EDS, skip to step 59.
   35. If you plan to use the EDS, continue to step 36.

EDS Standard Operating Procedure
(Please refer to the Reference Manual located beside the instrument for detailed
information)
    36. Turn off the camera.
    37. Insert the liquid nitrogen container (EDS Nitrogen Trap) to up to 3.5.
    38. Turn on the PC monitor.
    39. Give the password (User Name: semuser Password: 4F7m7y).
    40. In the SEM monitor, find something that you want to analyze by pushing the
              button. You can move this box using the cursor buttons. Press        to lock
       the area on the screen to be scanned.
   41. In the EDS PC, press acquisition button „ACQ.‟
   42. Once the result is constant or the lifetime is approximately 100, press „ACQ.‟
   43. Press IDENT to label elements.
   44. Press KLM to remove labeled elements.
   45. For quantification, choose Quant_periodic_table. Choose the desired elements.
   46. Click Run.
   47. To print spectrum press PLOT. Follow procedure (see Appendix A) in
       transferring spectral file to the server if you want an electronic file of this
       spectrum.
   48. To get a digital image, right click on the desktop.
   49. Choose <Voyager>, and then click on <Image Processing & Analysis>.
   50. A blue-bordered window will pop up. Hit ACQ to acquire the digital image.
   51. You may have to wait for several frames to get a very good image.
   52. Stop acquiring by hitting ACQ.
   53. Follow procedure (Appendix B) in transferring image file to the server to get an
       electronic file of this image.
   54. Right click to exit and choose exit Sunview. DO NOT CHOOSE SHUT DOWN.

   55. Go back to normal mode by pressing          button.
   56. Click the TV mode.
   57. Return the liquid nitrogen container to 12.
   58. Turn on the camera.
Sample Removal
   59. Turn off the electron beam.
   60. Close the SC air lock valve.
   61. Tilt back all knobs to their normal position. If you used the lower detector, tilt
       back 40 degrees.
   62. Open the specimen chamber by lifting the handle.
   63. Push metal rod into the specimen chamber and screw the fixture.
   64. Completely pull out the metal rod.
   65. Close the specimen chamber.
   66. Wear your gloves.
   67. Press the “red” air button to open the exchange chamber.
   68. Unscrew the fixture.
   69. Close and hold the exchange chamber door then press “evac” button.
   70. Turn off the display power switch.
   71. Turn off camera.
   72. Turn off monitor.
   73. Take out your printing paper.
   74. Turn off printer.
   75. Sign out in the logbook.

APPENDIX
A. Transferring Spectral Data to the CEC Server

   1. Go to the <Main Menu>
   2. Select <Input/Output>
   3. Save spectrum as <Spectrum 1>. You may save up to 8 spectra.
   4. Hit <Accept>.
   5. Enter the filename (i.e. sample) for this spectrum and hit <Accept>.
   6. Go back to <Input/Output> and select <Convert>.
   7. Choose <To_EMSA> and hit <Accept>.
   8. Spectrum 1 will show up. Hit <Accept>.
   9. Enter a new filename for the converted data (i.e. sampleconv) and hit <Accept>.
   10. Right click on the desktop and go to <Shells>.
   11. Click on <Shell Tool>.
   12. A Voyager prompt will show up. Type in “ls” for list. This will show the
       different file folders.
   13. Choose the folder “spectra” by typing “cd spectra”.
   14. Type in “ls” to list the files in the “spectra” folder. You should be able to find
       your converted file (i.e. sampleconv.emsa).
   15. Now log on to the CEC server by typing “ftp hilton.cec.wustl.edu” at the Voyager
       prompt.
   16. It will ask for your log in name and password. This should be the same name and
       password when using your CEC account.
   17. At the ftp prompt, transfer your converted file to the cec server by typing “put
       sampleconv.emsa”
   18. You may check if this converted file successfully transferred to the cec server by
       typing “ls”.
   19. Exit ftp by typing “bye”.
   20. To exit the Voyager software, right click on the desktop and hit <Exit>.
Opening Converted File from the CEC Server

  1. Open the FTP software (SSH Client) in your PC.
  2. Transfer the converted file (sampleconv.emsa) from the CEC server to your PC.
  3. Open file using Microsoft Excel.
  4. The <Text Import Wizard> dialog box will appear. Make sure that the
     “delimiters” option is chosen. Click <Next>.
  5. Check the box next to <comma>. This will remove the commas on the converted
     file and will put individual data points into individual cells. Click <Next>.
  6. Make sure the <General> type is chosen. Click <Finish>.


B. Transferring Image File to the CEC Server

  1. Go to the <Main Menu>
  2. Select <Input/Output>
  3. Save image as <Grey 1>. You may save up to 8 images.
  4. Hit <Accept>.
  5. Enter the filename (i.e. sample) for this image and hit <Accept>.
  6. Go back to <Input/Output> and select <Convert>.
  7. Choose <To_TIFF> and hit <Accept>.
  8. Grey 1 will show up. Hit <Accept>.
  9. Enter a new filename for the converted data (i.e. sampleconv) and hit <Accept>.
  10. Right click on the desktop and go to <Shells>.
  11. Click on <Shell Tool>.
  12. A Voyager prompt will show up. Type in “ls” for list. This will show the
      different file folders.
  13. Choose the folder “images” by typing “cd images”.
  14. Type in “ls” to list the files in the “spectra” folder. You should be able to find
      your converted file (i.e. sampleconv.tif).
  15. Now log on to the CEC server by typing “ftp hilton.cec.wustl.edu” at the Voyager
      prompt.
  16. It will ask for your log in name and password. This should be the same name and
      password when using your CEC account.
  17. At the ftp prompt, transfer your converted file to the cec server by typing “put
      sampleconv.tif”
  18. You may check if this converted file successfully transferred to the cec server by
      typing “ls”.
  19. Exit ftp by typing “bye”.
  20. To exit the Voyager software, right click on the desktop and hit <Exit>.
  21. Open the FTP software (SSH Client) in your PC.
  22. Transfer the converted file (sampleconv.tif) from the CEC server to your PC.
  23. You can view this file by using picture viewer.

				
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