Difference between revisions of "TEM Sample Preparation Equipment"

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|InstrumentName = TEM Sample Prep Tools
|InstrumentName = TEM Sample Prep Tools
|HeaderColor = #F5A81C
|HeaderColor = #F5A81C
|ImageOne =  
|ImageOne = Argon-Mill-Fischione-Model-1010.jpg
|ImageTwo =  
|ImageTwo =  
|InstrumentType = [[Equipment_List#Microscopy|Microscopy]]
|InstrumentType = [[Equipment_List#Support_Tools|Support Tools]],<br>[[Equipment_List#Sample_Preparation_for_Microscopy|Sample Prep for Microscopy]]
|RoomLocation = B242A Keck
|RoomLocation = B242A Keck
|LabPhone = 626-395-8908
|LabPhone = 626-395-8908
|PrimaryStaff = [[Matthew S. Hunt, PhD]]
|PrimaryStaff = [[Guy A. DeRose, PhD]]
|StaffEmail = matthew.hunt@caltech.edu
|StaffEmail = derose@caltech.edu
|StaffPhone = 626-395-5994
|StaffPhone = 626-395-3423
|Manufacturer =  
|Manufacturer = Assorted (see list on page)
|Model = Assorted (see list on page)
|Techniques = Cross-Section Sample Prep,<br>Sample Polishing,<br>3 mm Core Drilling,<br>Dimpling, Argon Milling
|Techniques = Cross-Section Sample Prep,<br>Sample Polishing,<br>3 mm Core Drilling,<br>Dimpling, Argon Milling
|RequestTraining = matthew.hunt@caltech.edu
|RequestTraining = derose@caltech.edu
|EmailList = kni-tf30
|EmailList = kni-tf30
|EmailListName = TF-30
|EmailListName = TF-30
}}
}}
== Description ==
== Description ==
The Sirion is a field emission gun (FEG) scanning electron microscope (SEM) equipped with an immersion lens for imaging sub-10 nm features (so-called "ultra high resolution mode," UHR) and an energy dispersive spectroscopy (EDS) detector for compositional analysis. While it is the KNI's oldest SEM, it is also a very steady instrument, offering a lower-cost alternative to similar high-resolution imaging that is available on the newer [[Nova_600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe | Nova 600]] & [[Nova_200 NanoLab: SEM, EDS & WDS | Nova 200 NanoLab]] platforms. The smaller Sirion chamber also allows for fast pump and vent times, which makes this SEM very useful for quick inspection. See a full list of training and educational resources for this instrument below.
The KNI offers a lab in the Keck sub-basement for preparing TEM samples by traditional means, often to produce cross-section specimens from a bulk sample. This typically involves the following steps:
===== SEM Applications =====
# Glue together a stack of materials, e.g. with the surface of two samples facing each other<br>(if the surface is what you want to observe in the TEM)
* Ultra-High-Resolution Imaging (Immersion Mode aka UHR Mode)
# Cut the stack into thin slices of material, in the appropriate orientation<br>(the thin dimension here will be the same thin dimension in the TEM)
* High-Resolution Imaging (Field-Free Mode aka Normal Mode)
# Cut out a 3 mm circle from this thin slice using a Disk Cutter
* EDX Mode Imaging (reduces background signal on EDS spectra)
# Polish that thin disk down to a thickness of ~100 &mu;m
* Secondary Electron (SE) & Backscattered Electron (BSE) Imaging
# Use a Dimpler to polish a hemispherical dimple into the middle of the disk,<br>such that only a few microns of material remain at the thinnest portion
* Everhart-Thornley Detector (ETD) & Through-the-Lens Detector (TLD)
# Use an Argon Mill to perform the final polish of the thinnest portion,<br>until a hole has been bored through the middle and<br>the edges of that hole are thin enough to be electron-transparent in the TEM
===== EDS Applications =====
 
* Spectrum acquisition for quantitative compositional analysis
== List of Equipment Available ==
* Linescan acquisition for 1D spatial compositional analysis
[[Image:Dimpler-and-Disk-Cuttter.jpg|thumb|top|upright=1.0|The Dimpler (left) and 3 mm Disk Cutter (right)]]  
* Map acquisition for 2D spatial compositional analysis
[[Image:Polishing-Station-Allied-TechPrep.jpg|thumb|top|upright=1.0|The polishing station with automated handling of the polishing jig and control of its sweeping motion]]
* Low-Angle Argon Milling & Polishing Station: Fischione Model 1010 (shown in infobox image)
* Dimpler: Fischione Model 2000
* Ultrasonic Disk Cutter: Model 170
* Polishing Station: Allied TechPrep
* Polishing Station: Buehler Ecomet 3
* Low Speed Saw: Isomet
* Roll Grinder: Buehler Handimet 2
* Various polishing media & accessories:
** Media: grit paper, lapping films, polishing cloths, diamond suspensions, alumina poweders
** Accessories: tripod polisher (South Bay Technology), endpoint polisher (Fischione Model 160)


== Resources ==
== Resources ==
===== SOPs & Troubleshooting =====
===== SOPs =====
* SEM SOPs ([https://caltech.box.com/s/rontehfysbmcyia4448wi31g8gbhepz9 Short Version] | [https://caltech.box.com/s/llpi6ct5wvw6c2tnh81zu32autbi2doy Long Version])
* Paper copies of SOPs are available in the lab for the Argon Ion Mill & Dimpler
* EDS SOPs ([https://caltech.box.com/s/ltcra2dk47k5s8r5mqotbad3i2e6r3lk Short Version] | [https://caltech.box.com/s/kukccwu1m8ekfjo6jds4jupvzwsjs3z1 Long Version])
* [https://caltech.box.com/s/u4c7ep9wyxb3tvcp0o38tczf0o8vpffi Troubleshooting Guide]
===== Video Tutorials =====
* [https://youtu.be/UfF_ljwvepQ Getting Started] | [https://youtu.be/luC-5TgNPsQ Basic SEM Alignment]
* Astigmatism Correction ([https://youtu.be/YeukVt1Fyi0 Details] | [https://youtu.be/WFfOi-rwlbA On Right-Angle Features] | [https://youtu.be/1syySgnTEqU Stigmator Alignment])
* [https://youtu.be/4V-bE6uqHY4 Eucentric Height: What it means, When to use it & How to get there]
* [https://youtu.be/R_RYbtumU20 Adjusting TLD Voltage to Capture SE vs. BSE Signal]
===== Graphical Handouts =====
* [https://caltech.box.com/s/14ffgscc39vhrvlyva0jbucsep7j6dvv SEM & EDS Concepts]
* [https://caltech.box.com/s/k2iy75hxiwkehv0ogqelz2sux9e1cs5k SEM Alignments]
* [https://caltech.box.com/s/ijd8gprg9gcavb6of5uegu7osinzsdet Guide to Optimizing SEM Imaging]
===== Presentations =====
* [https://caltech.box.com/s/lulkj0pwm053akyya1shazg8wzgudq9f Scanning Electron Microscopy: Principles, Techniques & Applications] (includes slides on EDS)
===== Manufacturer Manuals =====
===== Manufacturer Manuals =====
* [https://caltech.box.com/s/BROKEN Sirion SEM Operation Manual (BROKEN)]
* [http://www.labmet.cl/Documentos/Manuales/Manual%20-%20ION%20MILL%20MODEL%201010.pdf Fischione Model 1010 Argon Ion Mill]
* [https://caltech.box.com/s/36j0n01ig7f757kvkiebvqjqj0el2yvp EDAX Genesis EDS Operation Manual]
===== Videos =====
===== Calibrate Measurements with NIST Standard =====
* [https://www.youtube.com/watch?v=NyxfiC13kQ8 Ultrasonic Disk Cutter Model 170 Operation]
* The KNI has a NIST-traceable standard against which SEM measurements can be compared. See Slides 54-55 of the [https://caltech.box.com/s/lulkj0pwm053akyya1shazg8wzgudq9f SEM Presentation] for details. Ask staff for help finding and using the standard in the lab.
<br>
===== Simulation Software =====
<br>
* [http://www.gel.usherbrooke.ca/casino/What.html CASINO Electron Beam Simulation Software] – simulate e-beam/specimen interactions (very useful for EDS)
== Related Instrumentation in the KNI ==
===== Sample Preparation =====
===== Transmission Electron Microscopes =====
* Use the [[Leica EM ACE600: Carbon Evaporator | Carbon Evaporator]] to make non-conductive samples conductive by applying 2-10 nm of evaporated carbon.
* [[Tecnai TF-30: 300 kV TEM, STEM, EDS & HAADF | Tecnai TF-30: TEM, STEM, EDS & HAADF (50-300 kV)]]
* Use the [[Tergeo Plus ICP- & CCP-RIE: Oxygen & Argon Plasma Cleaner |
<!---  
O<sub>2</sub>/Ar Plasma Cleaner]] to remove hydrocarbons from the sample surface to avoid creating dark contamination spots on your features while imaging them.
* [[Tecnai TF-20: 200 kV TEM, STEM, EDS, EELS, EFTEM & Lithography | Tecnai TF-20: TEM, STEM, EDS, EELS, EFTEM & Lithography (40-200 kV)]]
===== Order Your Own Stubs =====
--->
* Stubs used for mounting specimens are considered a personal, consumable item in the KNI. There are some old stubs at each SEM, yet you should buy your own so that you can keep them clean and available to you. There are many stub geometries and configurations, some of which will be right for you to purchase and keep with your other cleanroom items.
** [https://www.tedpella.com/SEM_html/SEMclip.htm.aspx Buy stubs with copper clips] (recommended for most devices, especially those with non-conductive substrates)  
** [https://www.tedpella.com/sem_html/SEMpinmount.htm Buy stubs without copper clips] (OK for devices with conductive substrates)


== Specifications ==
===== Sample Preparation for TEM =====
===== Manufacturer Specifications =====
* [[Nova 600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe|Nova 600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe]]
* [https://caltech.box.com/s/s70o8bkorrygdmmyxmwazr6jyhzb11ma Sirion SEM Product Guide & Data Sheet]
* [[TEM Sample Preparation Equipment | TEM Sample Preparation Equipment: Polishing Stations, 3 mm Disk Cutter, Dimpler, Argon Ion Mill]]
===== SEM Specifications =====
===== Sample Preparation for Microscopy =====
* Minimum Feature Size Resolved: ~7 nm
* [[Carbon Evaporator | Carbon Evaporator (Leica EM ACE600) to make samples conductive]]
* Voltage Range: 0.2 to 30.0 kV
* [[Tergeo Plus ICP- & CCP-RIE: Oxygen & Argon Plasma Cleaner | Oxygen & Argon Plasma Cleaner (Tergeo Plus ICP- & CCP-RIE) to remove hydrocarbons from surface]]
* Current Range: "Spotsize" 1 to 7 (approximately 30 pA to 20 nA), with increments of 1
* Apertures: 30 &mu;m, 40 &mu;m, 50 &mu;m, 100 &mu;m
* Eucentric Height: 5 mm working distance (WD)
* Stage Range: +/- 25 mm X & Y travel, 50 mm Z travel, 0-45&deg; tilt, 360&deg; rotation
* ETD Grid Bias Range: -150 to 300 V
* TLD Bias Range: -100 to 150 V
* Ultimate Vacuum: 3e-6 mbar

Latest revision as of 20:52, 8 February 2022

TEM Sample Prep Tools
Argon-Mill-Fischione-Model-1010.jpg
Instrument Type Support Tools,
Sample Prep for Microscopy
Techniques Cross-Section Sample Prep,
Sample Polishing,
3 mm Core Drilling,
Dimpling, Argon Milling
Staff Manager Guy A. DeRose, PhD
Staff Email derose@caltech.edu
Staff Phone 626-395-3423
Reserve time on LabRunr
Request training by email
Sign up for TF-30 email list
Lab Location B242A Keck
Lab Phone 626-395-8908
Manufacturer Assorted (see list on page)
Model Assorted (see list on page)
[[image:|320px|center|]]

Description

The KNI offers a lab in the Keck sub-basement for preparing TEM samples by traditional means, often to produce cross-section specimens from a bulk sample. This typically involves the following steps:

  1. Glue together a stack of materials, e.g. with the surface of two samples facing each other
    (if the surface is what you want to observe in the TEM)
  2. Cut the stack into thin slices of material, in the appropriate orientation
    (the thin dimension here will be the same thin dimension in the TEM)
  3. Cut out a 3 mm circle from this thin slice using a Disk Cutter
  4. Polish that thin disk down to a thickness of ~100 μm
  5. Use a Dimpler to polish a hemispherical dimple into the middle of the disk,
    such that only a few microns of material remain at the thinnest portion
  6. Use an Argon Mill to perform the final polish of the thinnest portion,
    until a hole has been bored through the middle and
    the edges of that hole are thin enough to be electron-transparent in the TEM

List of Equipment Available

The Dimpler (left) and 3 mm Disk Cutter (right)
The polishing station with automated handling of the polishing jig and control of its sweeping motion
  • Low-Angle Argon Milling & Polishing Station: Fischione Model 1010 (shown in infobox image)
  • Dimpler: Fischione Model 2000
  • Ultrasonic Disk Cutter: Model 170
  • Polishing Station: Allied TechPrep
  • Polishing Station: Buehler Ecomet 3
  • Low Speed Saw: Isomet
  • Roll Grinder: Buehler Handimet 2
  • Various polishing media & accessories:
    • Media: grit paper, lapping films, polishing cloths, diamond suspensions, alumina poweders
    • Accessories: tripod polisher (South Bay Technology), endpoint polisher (Fischione Model 160)

Resources

SOPs
  • Paper copies of SOPs are available in the lab for the Argon Ion Mill & Dimpler
Manufacturer Manuals
Videos



Related Instrumentation in the KNI

Transmission Electron Microscopes
Sample Preparation for TEM
Sample Preparation for Microscopy