FEI Quanta 650 ESEM Procedure

NTS, 06/06/2014, updated NTS 2014MMDD

[Note: This tool is located at TMI in FNT 3.110 on Main Campus.]

[Note: This tool has a lot of free time. The reservation horizon for this tool is ~one week.]

Prep

1. Fill in Log when you enter.

2. Right computer & screen is SEM –do not touch tower.

   1. Left computer & screen saves images and does EDS. Can use USB and internet.

   2. If mouse gets janky, press button on medium whitish box that says 1 or 2 to switch mouse control

3. Start at Vacuum and Beam control tab on right of screen, Sun icon, left tab (status tab)

   1. Check Pressures and current

   2. Mouse over green vase icon at bottom

      1. IG1: gun chamber?

      2. IGP: ion pump

      3. Emission current

Load/Unload Sample

1. Press Vent on Vacuum frame of tab

   1. Vase turns grey when done (2-3 min)

2. Mount sample/s on stub/s.

   1. No sample size restriction as long as it can be mounted on stub (and stage)

   2. They provide DS carbon tape and gloves

   3. They provide stubs, maybe

3. When vented, gently pull out door using aluminum bar

   1. Put stubs with samples into stage

   2. Insert stub/s fully into stage

   3. Stage stub holes have numbers, remember where you mount samples

4. Close door fully

   1. Click Pump button and press door closed for a few seconds

   2. Vase is orange, wait til it’s green, P < 2e-4 T (2-3 min)

5. On Vacuum frame of status tab, we will want high vacuum

   1. Low vacuum is for non-conductive samples and uses water vapor to see. E.g. samples that can’t be coated because of EDX

   2. E-SEM is environmental SEM for wet samples

6. When on high vac ignore chamber pressure in vacuum frame near top. Look at chamber pressure at bottom.

Software Prep

1. Adjust Spot size and High voltage (in Column frame)

   1. Spot size depends on sample size, ranges from 1 to 7.

      1. Smaller spot size is less current and v.v.

      2. Usually 1 is not good enough, 7 is too much.

   2. 3 or 4 is recommended

   3. High voltage is 1-30 kV

   4. Depends on sample resistance to damage, sensitivity

2. These things can be changed after turning beam on.

   1. 10. There are multiple detectors. Default is to have Imaging detector and Chamber camera on

3. Move sample into position

   1. Vertical working distance is 10 mm, is marked

   2. Stage tab at top right, Stage/gear icon, second tab

   3. Go to Coordinates tab

   4. Double click Position 1 for stage to go to stub spot 1 (or Position X for spot X)

4. Now manually raise stage

5. Click Chamber detector screen

   1. Click and hold mouse wheel, a yellow bar appears

   2. Drag up and stage will move up and v.v.

   3. Get sample into position.

6. Turn on Beam

7. First tab, click Beam On

8. Click first detector window and unpause

9. Pause/unpause button at top middle

10. Joystick has X, Y, rotation control

11. Can also use mouse by pressing and holding mouse wheel again

    1. Make sure you have correct detector selected!

12. Can also double left click to move-to

13. Hard panel control of Mag and Focus, Brightness and Contrast

    1. Autobrightness and contrast are OK. Don’t use autofocus or autostigmation.

Note: If no image when Beam is turned on, adjust brightness and contrast first. Next, check detector selection is correct. Go to Detectors dropdown at top left. We want ETD (SE) selected.

1. Press F5 to go from small screen to full screen (and back)

2. Adjust scanning dwell time

   1. Ranges from 300 ns (default) to 1 ms

   2. 300 ns is easiest for focus and alignment.

   3. Tortoise and hare buttons: slower and faster

3. Focus and alignment (minor)

   1. Shouliang calibrates it weekly, we just have to do focus and stigmation adjustment on each sample like normal

   2. Zoom in, focus decently, adjust stigmation, repeat as needed.

      1. Streaking means stigmation is off.

      2. Try to focus to a non-streaking position before adjusting stigmation

4. Can use Reduced area to do focus and get faster response

   1. Helpful at higher mag too

   2. Click Reduced area button at top left. Click again to go back.

5. Can reduce/adjust scan speed for higher quality pictures.

Use

1. Camera button at top center pauses image, save as pops up

   1. Create own folder your first time

   2. Files are saved on left computer

2. Unpause to continue

3. Ruler button at top right to measure features

4. Press delete to delete (FILO deletion order)

   1. Different filter modes: Live, Average, Integrate

   2. Live is normal

   3. A filter mode from previous user could confuse you

Finish Use

1. Pause image for imaging detector.

   1. Make sure Chamber detector is unpaused, to watch stage move

   2. Click Vent, auto-lowers stage for you

2. Unload sample

   1. Close door

   2. Pump down

   3. Finish log info

EDX

1. Open Esprit software on left computer and login

   1. Runs very similar to 2nd floor one (Steps 38, 39, 41-44)

2. Get sample into position

3. Use spot size of 4 maybe 5 for EDX

   1. 27b2. Image quality will go down but EDX results might be better

4. Want spectrometer input counts to be > 1 kcps

   1. Gun kV needs to be large enough, might need to change/increase

5. Go to Spectra mode and acquire spectrum

   1. Select elements as usual, or can click auto button and deselect wrong elements.

      1. Higher energy peaks have lower detection efficiency.

   2. Save spectrum as normal if desired, spreadsheet or graphic

6. Click Objects to do mapping > Mapping Mode

   1. Software chooses which peaks to use

   2. For mapping, you can adjust this by adjusting peaks on elements tab

   3. Use as normal

7. Point scans: scans/acquires spectrum at crosshair (no dimensions just counts vs. energy)

   1. Line scan: scans/acquires along a line you draw and can adjust (one dimension, is composite of elements, looks like a Dektak overlap)

   2. Mapping: acquires a false color map in 2D

   3. Hypermap: makes a spectrum at all points (very slow, select small area)

   4. Turn off/close when done!