FEI Sirion XL30 SEM

Standard Operating Procedure

v.0119

1

XL30 Operating Procedure

Table of Contents

1. Imaging Parameters2. Imaging Modes3. Enable SEM4. Load Sample5. Sample Touch6. Stage Movement7. Start E-Beam8. Calibrate Stage Clearance9. Raise Stage10. Correct Astigmatism11. Lens Alignment12. Acquire Micrograph13. Acquire Extra-High Definition

14. Filters15. Export Micrographs16. Shutdown17. Default Settings

2

Imaging ParametersZ Position

Imaging is generally done between +5 and +15mm of clearance.

Beam Accelerating VoltageControls beam penetration into the sample.

5 kV is the default and works for the widest variety of samples.

Lower voltage gives more surface sensitivity to images.

Higher voltages can generate materials contrast.

Spot SizeCorresponds to e-beam current (1-7, lowest to highest).

Spot 3 gives good signal/noise ratio at TV scanrate.

Nonconductive samples, beam-sensitive samples, and very high magnification (>50kX) may need lower current to control charging.

Signal/Noise improves with higher currents but overall resolution is lower.

Beam Tab

3

Imaging ModesDetectors

The default SE mode uses an Everhart-Thornley detector to collect secondary electrons.

The through-lens detector (TLD) can be used alone to improve SE contrast or together with Ultra-High Resolution (UHR) mode.

There is a solid-state Backscatter detector available, which is more sensitive to Z-contrast than the TLD Backscatter mode.

Ultra-High Resolution Mode (UHR)UHR mode is not safe for ferromagnetic samples or with the EDS detector inserted.• Minimum magnification ~1000X• Requires Working Distance between 4.5 and 7mm.• 4 modes are available on the TLD, access them

through the Detector Tab -> Change.

4

Detector Tab

UHR On/Off

Enable SEM

1. Login to the UW Coral webpage and “Enable” the SEM.

• Confirm XL Microscope Control program is running on the right monitor and the Scandium database is open on the left.

• The system on/off panel (SOOP) on the front of the microscope table is for Staff use.

• Do not close programs on the SEM PC, please leave them running.

5

If software is closed launch XL first and let it fully load before starting Scandium.

System On/Off Panel (SOOP)

Load SampleSample Requirements

• Maximum mounted size is 50 x 50 x 20mm (L x W x H).• Everything should be clean and dry.• Remove any lose debris with compressed N2.

1. Select “Vent” in the Vacuum Flap.

2. When chamber reaches 1 atm, open the door.

3. Insert mounted sample and tighten set screw (finger tight).

4. Check the clearance with the Height Marker. If the sample is above the 5mm mark do not close the door.

5. Watch the sample on the CCD monitor as you close the chamber.

6. Click “Pump” in the Vacuum menu.

6

Sample TouchIf ‘Microscope Problem: Sample Touch Alarm’ appears while loading:

1. Look at the CCD monitor to verify there is no contact with the roof of the chamber.

2. If it is clear that there is no contact, click “OK” and continue.

3. If there might be contact, do not attempt to move the stage or unload your sample – get staff assistance.

7

Stage Movement1. Maximize the “Stage” Flap to see the

Stage Reference Table.

2. Double click the table to move your sample to the center. The beam location is marked with an “X”.

• You can also move the stage with the “Get” tool by double left double-clicking on the electron image.

• Or you can use the Stage Tracking tool.

8

Stage Flap Max/Min

Stage Reference Table

Start E-Beam1. Wait for vacuum status to read “Vacuum OK.”

2. Start the E-Beam from “Beam” Flap by clicking the high-tension button (kV).

3. Auto adjust brightness and contrast as needed.

9

“Microscope Confirm Focus” will appear

DO NOT CLOSE THIS BOX

High-Tension (kV)

1. Move to the tallest part of the sample (+/- 1mm).

2. Use ‘+’ and ‘ –’ buttons on number pad to increase/decrease magnification.

3. Focus the image with the right mouse button.

4. With magnification ≥ 2000X and sample in focus click “OK.”

Calibrate Stage Clearance (Z)

10

• Working Distance (WD) value will update the Stage Clearance.

• Always calibrate stage clearance before moving closer to the roof of the chamber.

Focus

Stage Clearance Calibration Box

Raise StageWhen the stage is moving up or down cover the Cancel

button in the Stage Movement window.

1. Check that stage coordinates are in “Absolute.”

2. In the “Stage” menu select Z = +15 mm and click “Goto.”

11

3. Cover the “Cancel” button and watch the CCD monitor.

4. Refocus the image at ≥ 2000X.

5. Click Z<=>FWD in the “Stage” Flap to reopen the Stage Calibration Box.

6. Click “OK” to update the stage clearance.

7. Select the final Z ( 5 mm) and click “Goto,” cover the “Cancel” button.

Stage Flap

Final Z (Absolute coordinates)Low kV: Z < 5 mm [flat samples]X-ray Microanalysis: Z = 5.0 mmUHR Mode: 5 < Z < 7 mmEucentric Height: Z = 5 mmLow Magnification: Z ~ 15 mm

Correct Astigmatism

1. Do your best to focus the image. (See examples below)

• Focused image should not have streaks or distortion.

2. Hold down “Shift” key and right mouse button to start the correction.

3. Drag green cross in X & Y until image is clear.

4. Refocus image and repeat if you still see astigmatism.

12

Incorrect focus with astigmatism Correct focus with astigmatism

Lens Alignment (optional)

1. In Scan Tab select TV.

2. Increase magnification to 20,000X and focus image.

3. From “Beam” Flap click the “Lens Modulator” box.

4. In the “Lens Align.” window, left-click and hold to start lens alignment.

5. Move the green cross on the image.

6. Find location where the image oscillates in/out of focus but doesn’t move in XY.

6. Uncheck Lens Modulator when done.

13

Acquire Micrograph

14

Standard Definition F2 Capture(single frame: 720 x 968 pixels ~ 300 kb)

1. Push “F2” key to grab an image.

2. Select your folder in the Scandium database.

3. Wait for ‘snowflake’ button to turn yellow.

4. Click camera icon to transfer image to Database ‘Scandium.’

5. Unfreeze image with ‘snowflake’ button to return to live imaging.

Snowflake button

Acquire Extra-High Definition

Extra-High Definition F5 Capture

(single frame: 968 x 1404 pixels ~ 1.2 Mb)

1. From “Image” Tab in Scandium, select “Configure Input.”

2. Select “Input” Tab and chose:

Standard High Definition = F2

Extra High Definition = F5

3. In Microscope Control XL push the “F5” key to grab an image.

4. The file is saved as LAST.TIF on the C: drive.

5. Drag-and-drop to M: and rename OR move to Scandium to add a scale bar.

6. Reset Input to Standard/High Def when you are done.

15

FiltersIf the F2 scan shows signs of charging, you may be able to reduce or eliminate these artifacts by Integrating TV scans.

1. From the Filter Tab choose “Integrate 128” frames.

• The image will start black and build as frames are added.

2. Wait for the Snowflake icon to turn yellow.

3. Click camera icon to transfer image to Scandium database.

4. Unfreeze image with ‘snowflake’ button to return to live imaging.

• You can change the number of frames integrated in Filter Tab > Setup > Integrate TV

16

Export Micrographs

1. Highlight the thumbnails to transfer in Scandium.

2. Click to export images as TIFs.

3. Browse “My Computer” and select Coral drive (M:) or (Q:) as the destination.

4. Click “OK” to transfer images.

• Files will be saved for 2 weeks on the M: drive and then automatically deleted.

• File export to JPG is does not function.

17

Remember to download images:

Files are automatically deleted from M-drive

after 2 weeks.

Browse

1. Verify Stage Tilt = 0 degrees.

2. Reset detector(s) to SE.

3. Turn off e-beam high tension.

Shutdown

18

4. In Absolute Coordinates type Z = 30 mm and click “Goto.”

5. Message ‘Exceeds stage limit.’ Click “Yes” to move stage down.

6. Watch stage lower on CCD.

7. Select “Vent” in Vacuum Flap.

8. Reset E-Beam to 5kV, spot 2.

9. Reset any changes you made to scan speed, averaging, or scan rotation.

10. Export micrographs to Coral.

11. Open the chamber, loosen set screw and remove samples.

12. Close the chamber door and click “Pump” in Vacuum Flap.

13. Disable Sirion-SEM in Coral.

Default SettingsScandium

Setup > Image > Configure Input >

Standard/High Def.

HARDWARE

• Stage Switch: “A” (Alarm)

• A/B Switch Box: A (EDS)

• Belkin KVM Switch: EDS

• CCD Camera Toggle: On

• External (CCD) Monitor: On

• EDS detector: Retracted

19

SOFTWARE

Microscope Control

• Magn > Reference (Videoprint)

• Beam > 5kV

Spot Size 2

• Scan > Full frame

• Scan Presets > Slow 1: 1.7ms, 484 lines

Slow 2: 6.7ms, 484 lines

Slow 3: 16.5 ms, 484 lines

Slow 4: 33.2ms, 484 lines

Single: 33.2ms, 968 lines

XHD: 66.4ms, 1420 lines

• Filter (TV) > Average 4 frames Standard def.

• Filter (Slow Scans) > Live, Standard def.

• Stage > Stage Current

Auto beam shift zero