Difference between revisions of "EBSD using JEOL 7100F FEG-SEM"

From Applied Optics Wiki
Jump to: navigation, search
(SEM)
(Removign the sample)
 
(5 intermediate revisions by the same user not shown)
Line 20: Line 20:
 
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)
Line 40: Line 40:
 
Fill the reservoir with liquid nitrogen
 
Fill the reservoir with liquid nitrogen
  
'''Wear latex glove'''s. Move sample into chamber using the stick
+
'''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)==
Line 50: Line 50:
 
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 10mm
+
Set working distance to '''10m'''m
  
Go to about 30,000 mag
+
Go to about '''30,000''' mag
  
 
Hit ALIGN
 
Hit ALIGN
Line 62: Line 62:
 
==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
Line 78: Line 78:
 
=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
Line 159: Line 159:
 
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

Latest revision as of 12:28, 19 January 2018

All samples for EBSD must be polished using the procedure outlined here or to a similar quality before EBSD. http://optics.eee.nottingham.ac.uk/wiki/AM_Sample_Preparation_for_SRAS_and_EBSD

They also need to be thoroughly cleaned using the procedure outlined here or similar. http://optics.eee.nottingham.ac.uk/wiki/How_to_clean_a_sample_prior_to_lithography

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.


Installing the sample

Check if sample is in “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 area is selected (based on grain size) pick a suitable step size and time

Settings

Pick resolution you want

✔ Store Patterns

✔ Beam off after scan

✔ Acquire post-acquisition image

Removign 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 door, remove the sample from the chamber, close the door

EVAC the chamber