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IF IN DOUBT ASKMick: 255-0650Mick: 255-0650 IF IN DOUBT, ASK
FEI FIB
Focused Ion Beam
Operating Manual
Part 1
IF IN DOUBT ASKMick: 255-0650
Chemical Safety
Users are required to have passed Cornell’s on-line laboratory safety training courses before they can use the FIB.
Do not bring chemicals into the laboratory.
Do not bring hazardous samples or materials into the lab. Contact Mick Thomas or John Grazul with any questions.
This is not a storage facility - do not leave or store samples here. You must take specimens, stubs, and raw material with you when you leave.
Lab-supplied chemicals are limited to a squirt bottle of isopropanol, methanol, and a can of Aero-duster. Wear safety glasses and read the MSDS’s before using them.
A First-Aid kit is provided but this is not a substitute for professional medical help.
Fire escape routes are documented on the following page.
Users failing to follow safety rules will be denied access to the lab.
IF IN DOUBT, ASK
IF ANYTHING UNUSUAL HAPPENS, OR IF THERE ISANYTHING YOU ARE UNSURE ABOUT, STOP ANDCONTACT ME! DO NOT PROCEED OR ATTEMPT TO FIXTHE PROBLEM YOURSELF!
IF IN DOUBT, ASKIF IN DOUBT, ASKMick: 255-0650
1.00
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Emergency Shower and Eyewash
Fire Pull Station
In Case of Fire:
Close the door behind youLeave the building
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Fire Extinguisher
First Aid Kit
1.00
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Gas Safety
Nitrogen gas cylinders are to be changed by CCMR staff members only
Lab Telephone
If you don’t have a cell phone, there is a land-line phone for your use in the corner of the NION room
• Campus Police: 5-1111
• Emergency: 911
• Mick: 255-0650
• John: 255-4130
Illness
If you feel sick, please stay at home. This will require re-scheduling your session, but other people will stay healthy.
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1.00
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Rules
If ANYTHING does not even SEEMright, leave everything as is and getMick or John
DO NOT attempt to repair ANY part of themicroscope.
DO NOT remove panels, cables, or any part ofthe FIB.
DO NOT add any software or hardware to anycomputer
Flash Drives (Memory Sticks) are forbiddenData MUST be removed by burning a CD
DO NOT bring food or drink into 150.
Wear gloves when handling samples orshuttles.
Individuals failing to follow the rules will bedenied access to the instrument.
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2.00
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Penalties
Failure to follow these guidelines, unprofessional behavior orcareless use of the equipment will result in loss of permission touse the FIB, in addition to repair charges, if required.
Training requirements
No one is permitted to use the FIB until trained by Mick Thomas.
Room Access
No user is permitted to unlock the door into 150 for the purposeof allowing someone else in to use the FIB.
User Status Signup Room Entry Access
Novice (<2 sessions)
Email ManagerM-F 8am –
5pm
Trained(>2 sessions)
Coral Card SwipeM-F 8am –
5pm
Experienced(>4 sessions)
Coral Card Swipe 24/7
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2.00
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Cancellation
If you sign up and then cannot use your time, cancel your time via Coral or contact Mick at least one weekday before your scheduled time.
Failing to show up
Failure to show up without canceling, unless due to illness or other emergency, can result in use charges
If you fail to show up within 30 minutes of your scheduled starting time the FIB becomes available to other users.
Publication Acknowledgements
When research is published using data from the FIB, the facility and the grant number must be acknowledged, such as:
Data Storage
Data storage and safety is NOT guaranteed!
Users are responsible for their data, and must copy their data to a CD in a timely fashion.
Data will be periodically erased, leaving only one years’ data there.
This work made use of the electron microscopy facilityof the Cornell Center for Materials Research (CCMR)with support from the National Science FoundationMaterials Research Science and Engineering Centers(MRSEC) program (DMR 1120296).
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About this manual (Version 1.0)
This is a limited use manual intended to helpnew users get started on the FEI Focused IonBeam (FIB). It provides information on basicimaging, milling, and TEM sample preparation.It is not intended to be exhaustive, and thereare many principles about focused ion beampractices as well as features of this microscopethat are not covered by this manual. Thismanual will be updated and expanded asneeded.
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Confirm the four circles in the server window turn solid green
If all the circles do not turn solid green then do not proceed – contact Mick
Click on Start
Log on to the xTm Server
Click on Determine
How to start your FIB session
Log into Coral
Log on to Windows on the microscope PC
Click on the FEI System Control icon.
3.00
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Understanding the GUI setup:
Activate an image quadrant by clicking in it. The bottom bar will turnblue, indicating that window is now active.
Electron Image Ion image
TV image Status window
Main Toolbar
Controltoolbars
3.00
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How to Load a Sample
Click on Navigation Button
Click on Unload in the software
When both lights are green lift the lid
and push Unload/Release
The arm should move away from the
shuttle, allowing you to remove it.
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How to Load a Sample
Note that the two clamping arms must be retracted BEFOREremoving the shuttle
Samples must not exceed the allowable height - check heightusing the height gauge.
They must also fit inside the volume of space as shown at left.
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How to Load a Sample
The shuttle is loaded onto the arm with the three locating balls (rubies) are in the appropriate slots on the arm (inside white circles in picture below).
Gently close the lid and push Clamp/Load.
When loaded the rotation should be -62.4 degrees; if not enter that valueas shown below.
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‐62.4
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-10, -10
+10, -10
+10, +10
-10, +10
0, +22
0, 0
How to Find Your Sample in the FIB
Standard stage (at right)
Enter the coordinatesin the boxes for X and Yas shown at right
For TEM stage only:
Front position:X = 0Y = 17
Back position:X = 0Y = -17
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How to Turn On theBeam
Select the upper left handquadrant - this activatesthe electron beam option
Select the voltage and currentfrom the drop -downmenus
Select the Beam Control icon.
Click on Beam On
Un-pause the beam
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?
Electroncolumn
Sample
How to Link Your Sample
The FIB does not know where the sample is in reference to the polepiece(vertical position). The Z value displayed in the Navigation windowwill be wrong. Therefore it is critical to tell the FIB where yoursample is – a process called Linking.
Do not adjust specimen height (Z) until you have Linked at low mag.
Set the magnification to about 50X and focus the beam on the surface ofyour sample
Increase the magnification to about 1000X and refocus
Now STOP – Go no further until you have clicked on the Link icon
4.20
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Using the Z control, raise thestage to 9mm, then 7mm,then 5mm, checking aftereach motion that theimage refocuses and theStage motion looksnormal.
If you see a red circle aroundthe Link icon when youreach 5mm then refocusand click on the Link iconagain.
How to Link Your Sample (con’t)
Coarse alignment
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How to Link Your Sample (con’t)
Fine alignment
Find a distinct feature near the area of interest around 1000X magnification.
Tilt the stage by clicking on the drop-down menu and clicking on 15 degrees.
Electroncolumn
15 degrees
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How to Link Your Sample (con’t)
If the feature has moved (down, for example) then move the mouse over the TV image, click on the middle button (the wheel) and a yellow line will appear.
Move the mouse in the direction necessary to move the feature to the middle of the yellow “+” sign on the electron image. As you do this a yellow arrow will appear showing you the direction you are going.
Repeat at 45 degrees (skip 30 degrees), then finally at 52 degrees.
Reset to 0 degrees tilt
Electroncolumn
45 degrees
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How to Select Imaging Conditions
Field-Free: Use for milling and general imaging
Immersion: Use for higher resolution imaging.
EDX: For use while collecting EDX spectra.
How to Select Acquisition Type
Live: Continuous imaging
Average: Uses N number of frames to form an image
Integrate: Takes N frames and then stops
5.00
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How to Select Detector Type
ETD: Side mounted detector
TTL: Through the Lens detector
STEM: Transmission detector
CDEM: Channeltron Dynamic Electron Multiplier
CCD: TV image
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7.00 How to Check Beam Alignment
Click on Lens Align to wobble the aperture and reduce wobble, if needed.
Click on Crossover to check the beam centering and improve, if needed.
Correct stigmatism with hardware controls.
You are now ready for electron imaging.
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Corrected
Uncorrected
Adjust stigmators
8.00 How to Correct Astigmatism
Adjust the X-stigmator and Y-stigmator so that when you go in and out of focus there is no stretching of the features
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Principles of Ion Milling9.00
In the simplest of examples, start with a bulk material with a film on top
Add platinum to protect the sample during milling
Mill away a volume of space to reveal hidden, sub-surface features
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9.20 How to set the ion beam conditions
Ion milling can occur at any angle up to about 58 degrees. However it is tyically performed at 52 degrees, when the ion beam is at normal incidence to the sample.
Click in the upper right hand quadrant – the bottom bar should change from gray to blue.
Set the beam current to an appropriate value for your sample, keeping it mind that it is milling your sample all the time you are focusing and stigmating.
Note that there is a very large range of beam currents, with the highest over 10,000 times that of the lowest, so be careful to choose the correct value for your purpose.
The higher the voltage:• The sharper the image• The faster the milling• The more the milling surface will
be amorphized
The higher the current:• The better the S/N• The faster the milling• The bigger the tails on the beam
In the Application drop-down menu select Si
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9.20 How to turn on the ion beam
For general milling, make sure the stage is linked and you can tilt to 52 degrees without the feature moving more than 5 um’s
Electroncolumn
52 degrees
If the bar below the Source is gray, click on Wake Up. It will first turn red, then yellow, then green.
When the source is green, click on Beam On.
Remember that imaging with the ion beam is inherently destructive.
Un-pause the beam
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How to mill our sample
Select the desired geometric pattern
Draw the desired size or enter it in digitally
Set the depth (Z value)
Click on the Play icon
To stop the milling click on the Stop icon
9.30
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How to Deposit Platinum
Choose the Patterning tab
Draw a box where you want to deposit platinum.
Under Gas Injection ‐> Overview right click on “Cold” and a “Heater” optionwill appear.. Left click on “Heater”
Click on white box to the left of Pt Dep to insert needle
9.50