1. This document provides recipes and step-by-step instructions for preparing TEM lamella and atom probe tomography (APT) samples using a focused ion beam (FIB). 2. The TEM lamella preparation involves patterning and trenching the area of interest, liftout of the sample using an omniprobe needle, mounting on a TEM grid, and thinning to electron transparency. 3. The APT sample preparation similarly uses the FIB to pattern platinum deposition, mill trenches, lift out a sample chunk, weld it to mounting posts, and shape it into a fine needle for analysis.

1. FIB manual
TEM lamella recipe for ASS
APT needle recipe*
Niels Cautaerts
Last updated 15/05/18
*mostly valid for FEI FIB instruments, slight variations between models

2. Geometry inside the FIB
E - beam
Ga - beam
52 °
Stage
Eucentric height
7 or 10 mm (depends on FIB model)

3. Preliminary steps
1. Install the specimen
• Vent the chamber.
• Follow the loading procedure. Make sure grids and/or Si needle pads are also installed.
• Pump the chamber.
2. Starting the session & E-beam alignment
• Wait for good vacuum (Threshold?).
• Beam control > WAKE UP on both the E and I beams.
• Warm up the Pt-Gas heater (in patterning). This can take 10 min or more.
• Select the right acceleration voltage and current for the E-beam.
• Start viewing with the E-beam.
• Move to the specimen where you will perform FIB work.
• Go to 2k magnification or above. Focus the image. Click the “Link working distance with Z”
button. Then move the specimen to eucentric height with Z movement. The specimen should
remain in focus.
• Go to 10k magnification or above and adjust beam astigmatism.

4. Preliminary steps
3. Eucentric height adjustment
• Make sure beam tilts are zero’d
• Focus the AOI at 3500x or above
• Make sure that Z-Y linking is checked off and Eucentric is checked on.
• Tilt the sample 5-10°. Adjust the stage with Z so that what was initially in the center of the
viewing screen is again centered
• Work your way up to 52°. If the area in the center of the screen remains in the center
between 0 and 52° tilt, the AOI is at eucentric height.
• Watch out when you tilt to 52° that you don’t touch the pole pieces with the stage. This is especially
dangerous when working with tall samples. A 180° stage rotation may make your desired tilt possible.
!!!Every time you make a major movement, the eucentric height alignment should
be redone!!!
In a well aligned FIB, eucentric height should coincide with the crossover point of
the E and I beams.

5. Preliminary steps
4. Ion beam set-up
• Switch your control to the ion beam by selecting that view window
• Reset beam shift (Stage > Zero beam shift)
• Select 10-30 pA current for viewing
• Focus the Ion beam image - this should not have to be done often!
!!!Every time you switch voltage or current on the ion beam, the image
will shift and focus will be different. Correct this with beam shift and
focus respectively. Don’t move the stage based on the ion beam
image!!!

6. TEM lamella preparation
recipe
This recipe has been shown to work reasonably well for making TEM
samples from ion irradiated austenitic steel. Milling steps may need to
be adjusted depending on your material.

7. Patterning and trenching
• Choose an AOI and go to
eucentric height (see earlier)
• Go to 52° tilt. Make the
pattern on the right in the
indicated order.
• Insert the GIS for the first
step. Retract for continuing
to the trenching step!
• Do the cleaning cross
sections at 53.5 and 50.5° for
front (lower) and back
(higher) respectively.
1) Pt-dep, 15x2x2 µm, 30 kv, 0.3 nA
2) RCS, 20x10x15 µm, 30 kv, 15 nA
2) RCS, 20x10x15 µm, 30 kv, 15 nA
3) CCS, variable, 30 kv, 3 nA
3) CCS, variable, 30 kv, 3 nA

8. Liftout
• Tilt to 0°. Make a J-cut on the
lamella. Getting the pattern is
easiest if you click in the help file.
• Bring the easylift needle to park
position. Insert GIS. Manouvre
needle down and attach to the
side of the specimen.
• Cut the lamella loose. Currents are
given on the right.
• Lift the specimen out slowly.
Retract the GIS. Then retract the
easylift needle.
1) CCS, variable, 30 kv, 3 nA
2) Pt-dep
1.5x1.5x? µm, 30 kv, 50 pA
3) CCS, variable, 30 kv, 3 nA

9. Preparation of the grid and mounting
• Go to the TEM grids. Bring one of the
posts to eucentric height. Best is the tip
where the sample will be mounted.
Prepare the tip as seen on the right.
• If the grid is not pre-tilted, do the milling
at 0°.
• If the grid is pre-tilted, also do the milling
at 0° but rotate the stage 180°.
• Insert the easilift to park. Insert the
GIS. Bring the sample to the post and
weld it on. Then cut the easylift loose.
• If the grid is not pre-tilted, do all this at 0 °
tilt.
• If the grid is pre-tilted, rotate the stage 180
° and tilt 52°
1) Regular, 10x15x20 µm, 30 kv, 30 nA
2) Regular, variable,
30 kv, 30 nA
1) Regular, variable, 30 kv, 1 nA
2) Pt-dep variablex? µm,
30 kv, 0.1-0.3 nA

10. Thinning and cleaning
• Tilt the stage such that the sample is
aligned with the ion beam
• For non-pre-tilted this is 52 °. The stage
can be rotated 180 °.
• For pre-tilted this is only 0 °. Only one
configuration works.
• Tilt a bit back and forth to thin the
specimen on both sides. Higher angles
are for doing the front. Smaller angles
are for doing the back.
• For the cleaning at low voltage, use a
regular rectangle to mill for ~1 min over
the whole specimen. 5 kV can still be
used to thin the specimen further, but it
should already be quite thin after the 30
kV, 50 pA step.
kV Current Angle (°) Thickness
30 1 nA ±2.5 800 nm
30 0.5 nA ±2.5 400 nm
30 0.1 nA ±2 150 nm
30 50 pA ±1 <100 nm
5 48 pA ±3.5
2 27 pA ±5

11. APT sample preparation
recipe
This recipe has been shown to work reasonably well for making APT tips
out of ion irradiated austenitic steel. Milling steps may need to be
adjusted depending on your material.

12. 1. Pt patterning
Instructions
• Tilt stage to 52°
• Draw a Pt-dep box (15 µm wide, 2 µm high,
0.3 µm thick)
• Set ion voltage to 30 kV, current to 0.1 nA.
Take a snapshot and make necessary focus
and shift adjustments.
• Insert Pt GIS needle
• Start patterning (“Play” button)
• When done, retract the GIS. Set I-beam
current to 30 pA and take an image to check
the deposit.
• Delete the Pt-dep pattern.
Stage configuration
I-beam
52 °
15
2
View diagram

13. 2. Milling
Instructions
• Tilt the stage to 22 °
• Draw a cross-section pattern (22 µm wide,
3.5 µm high, 3-5 µm deep). Change type to
“Si”.
• Set scan direction so the thick line is at the
bottom. Move it so it is just slightly above
the Pt deposit (the image is rotated 180 °,
you will actually mill below the deposit).
• Set beam current to 7-15 nA. Take snapshot
and adjust the pattern location or beam
shift/focus.
• Start patterning.
• Delete the pattern
Stage configuration View diagram
I-beam
22 °
30 °
Pt
22
3.5

14. 3. Cleaning
Instructions
• Draw a cleaning cross section over the milled
area. Change type to “Si”.
• Adjust the scan direction so the thick line is
at the bottom.
• Set the beam current to 3 nA. Take snapshot
and adjust pattern location.
• Start patterning. Check occasionally on
progress with snapshot.
• Delete the pattern.
Stage configuration View diagram
I-beam
22 °
30 °
Pt
22
2-3

15. 3. Final preparation of lift-out bar
Instructions
• Tilt the stage back to 0°. Rotate the stage by
180°. Use eucentric rotation. Find the AOI
back and check eucentric height.
• Repeat steps 2-3 (milling and cleaning) using
this configuration. You should now have an
equilateral triangle prism supported on two
sides by the bulk.
• Make a small cut on the left hand side. Use 3
nA beam current, “Si”, 3 micron depth. The
bar will then be ready to weld to the
omniprobe.
• Tilt the stage back to 0°. For all omniprobe
work the stage should not be tilted.
Stage configuration View diagram
I-beam
22 °
30 ° Pt
Sample
180 °
Sample

16. 4. Sample lift out
Instructions
• Make double sure you are at eucentric height. The
omniprobe can crash into the sample if you deviate 100
micron.
• Set ion beam current to 30 pA for viewing.
• Insert Pt-GIS and then insert the omniprobe.
• Move tip to park position. Then move it with X, Y and Z
until the needle (almost) touches the bar near the left
hand side. Use both the E and I-beams alternatingly. You
can spot near-contact when a “shadow” appears below
the needle.
• Weld the bar onto the needle using 50 pA I-current.
Pattern thickness of 0.5-1 µm thick should suffice. Don’t
pattern too much on the needle – it is wasted.
• Cut the bar loose on the other side (3 nA, “Si”, 3 µm
deep).
• Lift out the specimen with Z, then move to park position,
then retract omniprobe.
• Retract the Pt-GIS.
View diagrams
Pt
Electron beam view
Pt
Ion beam view
Welding
Pt
Ion beam view
Cuting
Pt
Ion beam view
Lift-out

17. 5. Welding to Si coupon
Instructions
• Move to the Si coupon and to the first tip where you
want to place a needle. Bring this tip to eucentric height.
• Insert the GIS and Omniprobe again. Move to park
position. Maneuver with the Omniprobe so that the bar
is directly over the coupon tip. Use both the I and E
beam to adjust.
• Weld the bar to the needle (50 pA I-current,1 µm thick )
• Cut the welded part loose (3 nA, “Si”, 3 µm deep). Don’t
make cut too wide.
• Move the Omniprobe up to a safe distance. Move the
stage to the next needle. Repeat welding, cutting and
moving to a new tip until the bar is finished. You should
be able to create 5-6 welded chunks.
• Retract Omniprobe and GIS.
• Rotate the stage 180°. Check Eucentric height. Re-insert
GIS.
• Weld all the chuncks on the other side as well using the
same settings. You can check the quality of your welds
by rotating the stage to 90 °.
View diagrams
Pt
Ion beam view
- Welding
Pt
Ion beam view
-Cutting
@ 90° stage rotation
Ion beam view

18. 6. Shaping the needles
Instructions
View diagrams
• Make sure GIS and Omniprobe are retracted. Make sure
you have one of the chuncks on eucentric height.
• Rotate the stage to 90°. Tilt stage to 52°
• Draw an annular milling (“Si”) pattern and center it over
the chunk. Make the scan direction so that the thick line
is in the center. Use the settings in the table. In each
step make the pattern smaller and lower current and
voltage to obtain a very fine needle.
• Make sure you center your pattern each time you change current or
voltage – the image in the ion view will shift. At low voltages it will
be hard to focus the ion image.
• Check the progress of your needle in the E-beam image. For ion
irradiated specimens it is important not to mill too much away from
the top of the specimen
• After all the steps in the table are complete, take a good
image of the needle with the E-beam. You will need this
for the APT reconstruction (measuring tip radius)
• Repeat this for all the chunks on the coupon.
• Store your needles in vacuum as much as possible.
Voltage
(kV)
Current Outer diameter
(micron)
Inner diameter
(micron)
Depth/Z
(micron)
30 3 nA 6 4 0.3
30 1 nA 4.5 2 0.3
30 0.3 nA 4 1.5 0.2
30 0.3 nA 3.5 1 0.2
30 0.1 nA 3 0.75 0.2
30 0.1 nA 2.5 0.5 0.1
30 30 pA 2 0.25 0.1
5 48 pA 2 0 Watch shape on E-beam
2 27 pA 2 0 Such that it lasts about 2 min
Stage configuration
Sample
90 °
I-beam
52 °
E-beam I-beam