Difference between revisions of "EBSD using JEOL 7100F FEG-SEM"
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| − | All samples for EBSD must be polished using the procedure outlined here or to a similar quality before EBSD. | + | All samples for EBSD must be polished using the procedure outlined [[AM Sample Preparation for SRAS and EBSD| here]] or to a similar quality before EBSD. |
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| − | They also need to be thoroughly cleaned using the procedure outlined here or similar. | + | They also need to be thoroughly cleaned using the procedure outlined [[How to clean a sample prior to lithography | here]] or similar. |
| − | |||
Finally, you could use the plasma cleaner (upstairs in the sample prep room of the NMRC), but the ion cleaning head does a similar job. | Finally, you could use the plasma cleaner (upstairs in the sample prep room of the NMRC), but the ion cleaning head does a similar job. | ||
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==Installing the sample== | ==Installing the sample== | ||
| − | Check if sample is in “Specimen Exchange” position | + | Check if the sample is in the “Specimen Exchange” position |
VENT the specimen exchange chamber | VENT the specimen exchange chamber | ||
| − | Wear latex gloves. Open door, place sample in chamber, close the door | + | '''Wear latex gloves'''. Open door, place sample in chamber, close the door |
(Place the area you want to EBSD closest to the outer edge of the door/closest to you when the door is shut) | (Place the area you want to EBSD closest to the outer edge of the door/closest to you when the door is shut) | ||
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Move ion cleaning head out | Move ion cleaning head out | ||
| − | =SEM= | + | ==SEM== |
Fill the reservoir with liquid nitrogen | Fill the reservoir with liquid nitrogen | ||
| − | '''Wear latex | + | '''Wear latex gloves'''. Move sample into chamber using the stick |
Wait for chamber vacuum to go down to 10-4 | Wait for chamber vacuum to go down to 10-4 | ||
| − | Switch beam ON | + | Switch beam '''ON''' |
==Mechanical Alignment (Beam)== | ==Mechanical Alignment (Beam)== | ||
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Check dynamic focus is off | Check dynamic focus is off | ||
| − | Apature 3 (or 2) 50μm (or70) Spot size 8 Filter 3 | + | Apature '''3''' (or 2) 50μm (or70) Spot size 8 Filter 3 |
| − | Set working distance to | + | Set working distance to '''10m'''m |
| − | Go to about 30,000 mag | + | Go to about '''30,000''' mag |
Hit ALIGN | Hit ALIGN | ||
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==Alignment (Sample)== | ==Alignment (Sample)== | ||
| − | Change working distance to 20mm and Spot size 11 | + | Change working distance to '''20mm''' and Spot size '''11''' |
Hit ALIGN | Hit ALIGN | ||
| − | Go to about 2000 mag | + | Go to about '''2000''' mag |
Align using the X and Y nobs on the control panel | Align using the X and Y nobs on the control panel | ||
| − | Set tilt to 70deg | + | Set tilt to '''70deg''' |
| − | Switch on Dynamic Focus | + | '''Switch on Dynamic Focus''' |
Focus the centre then the top | Focus the centre then the top | ||
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=EBSD= | =EBSD= | ||
| − | Move detector into 180-188 max – 195 absolute MAX | + | Move detector into 180-188 max – '''195 absolute MAX''' |
Find your region of interest and close the camera | Find your region of interest and close the camera | ||
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Select the area you want to map | Select the area you want to map | ||
| − | Once area is selected (based on grain size) pick a suitable step size and time | + | Once the area is selected (based on grain size) pick a suitable step size and time |
''Settings'' | ''Settings'' | ||
| − | Pick resolution you want | + | Pick the resolution you want |
✔ Store Patterns | ✔ Store Patterns | ||
| Line 151: | Line 149: | ||
✔ Acquire post-acquisition image | ✔ Acquire post-acquisition image | ||
| − | = | + | =Removing the sample= |
Retract EBSD detector | Retract EBSD detector | ||
| Line 159: | Line 157: | ||
Switch Dynamic focus off | Switch Dynamic focus off | ||
| − | Wear latex gloves. Once the sample has stopped moving used the stick and pull the sample out | + | '''Wear latex gloves'''. Once the sample has stopped moving used the stick and pull the sample out |
VENT the specimen exchange chamber | VENT the specimen exchange chamber | ||
| − | Open door, remove the sample from the chamber, close the door | + | Open the door, remove the sample from the chamber, close the door |
EVAC the chamber | EVAC the chamber | ||
Latest revision as of 09:20, 20 August 2021
All samples for EBSD must be polished using the procedure outlined here or to a similar quality before EBSD.
They also need to be thoroughly cleaned using the procedure outlined here or similar.
Finally, you could use the plasma cleaner (upstairs in the sample prep room of the NMRC), but the ion cleaning head does a similar job.
Contact Elisabeth Steer <pczeds@exmail.nottingham.ac.uk> if you want to use the plasma cleaner.
Contact Martin Roe <epzmjr@exmail.nottingham.ac.uk> for SEM training.
Contact Nigel Neate <epzncn@exmail.nottingham.ac.uk> for EBSD training.
Contents
Installing the sample
Check if the sample is in the “Specimen Exchange” position
VENT the specimen exchange chamber
Wear latex gloves. Open door, place sample in chamber, close the door
(Place the area you want to EBSD closest to the outer edge of the door/closest to you when the door is shut)
EVAC the chamber
Using the plasma cleaner
Move ion cleaning head in
Open valve on top of the argon bottle (2-3 turns) to open it, wait 5 seconds and close it
Set voltage, time and hit START
Move ion cleaning head out
SEM
Fill the reservoir with liquid nitrogen
Wear latex gloves. Move sample into chamber using the stick
Wait for chamber vacuum to go down to 10-4
Switch beam ON
Mechanical Alignment (Beam)
Check dynamic focus is off
Apature 3 (or 2) 50μm (or70) Spot size 8 Filter 3
Set working distance to 10mm
Go to about 30,000 mag
Hit ALIGN
Align using the mechanical X and Y nobs on the SEM
Alignment (Sample)
Change working distance to 20mm and Spot size 11
Hit ALIGN
Go to about 2000 mag
Align using the X and Y nobs on the control panel
Set tilt to 70deg
Switch on Dynamic Focus
Focus the centre then the top
EBSD
Move detector into 180-188 max – 195 absolute MAX
Find your region of interest and close the camera
Recheck focus and dynamic focus
Scan image
Settings
Image scan size 1024 ( or greater for a better resolution of the background IMAGE ONLY)
Dwell time 35
✔ SE
☐ BSE
✔ FSE
✔ Auto
✔ Tilt centre
Optimise pattern
Binning 4x4
Gain 15
Hit Auto exposure
90% signal strength
✔ Auto background
✔ Static background
Frame average
Check static background (300)
Optimise Solver
Settings
No of bands 6 MIN
Hough resolution 40-60
MAD as low as possible
Acquire Map
Select the area you want to map
Once the area is selected (based on grain size) pick a suitable step size and time
Settings
Pick the resolution you want
✔ Store Patterns
✔ Beam off after scan
✔ Acquire post-acquisition image
Removing the sample
Retract EBSD detector
Click Specimen Exchange position on the SEM window
Switch Dynamic focus off
Wear latex gloves. Once the sample has stopped moving used the stick and pull the sample out
VENT the specimen exchange chamber
Open the door, remove the sample from the chamber, close the door
EVAC the chamber
