The KNI Lab at Caltech - User contributions [en]

Nova 200 NanoLab: SEM & EDS

2021-02-09T00:42:46Z

Mcaban: /* Video Tutorials */

{{InstrumentInfoboxOneImage|
|InstrumentName = Nova 200
|HeaderColor = #F5A81C
|ImageOne = Nova-200-NanoLab.jpg
|ImageTwo = Nova-200-NanoLab.jpg
|InstrumentType = [[Equipment_List#Microscopy|Microscopy]]
|RoomLocation = B203 Steele
|LabPhone = 626-395-1542
|PrimaryStaff = [[Miguel Caban-Acevedo, PhD]]
|StaffEmail = mcaban@caltech.edu
|StaffPhone = 626-395-5994
|Manufacturer = FEI (now Thermo Fisher)
|Model = Nova 200 NanoLab
|Techniques = SEM, EDS Immersion Lens Imaging
|RequestTraining = mcaban@caltech.edu
|EmailList = kni-sem-fib
|EmailListName = SEM-FIB
}}
== Description ==
The Nova 200 is the KNI's highest-resolution field-emission gun (FEG) analytical scanning electron microscope (SEM), equipped with an immersion lens for imaging sub-10 nm features and energy dispersive spectroscopy (EDS) for compositional analysis. It is also outfitted with a gallium focused ion beam (Ga-FIB) column, which is currently not operational because the [[Nova_600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe | Nova 600 NanoLab]] and [[ORION NanoFab: Helium, Neon & Gallium FIB | ORION NanoFab]] together meet the KNI's Ga-FIB demand; Ga-FIB could be reactivated on the Nova 200 in the future. See a full list of training and educational resources for this instrument below.
===== SEM Applications =====
* Ultra-High-Resolution Imaging (Immersion Mode aka UHR Mode)
* High-Resolution Imaging (Field-Free Mode aka Normal Mode)
* Secondary Electron (SE) imaging with an Everhart-Thornley Detector (ETD) & Through-the-Lens Detector (TLD)
* Backscattered Electron (BSE) imaging with a TLD
* Tungsten deposition via Gas Injection System (GIS)
* Automated imaging with RunScript program & AutoScript language
===== EDS Applications =====
* Spectrum acquisition for quantitative compositional analysis
* Linescan acquisition for 1D spatial compositional analysis
* Map acquisition for 2D spatial compositional analysis

== Resources ==
===== Equipment Data =====
* [https://caltech.box.com/s/xlvbr7cfwiqzcpc9hpq4jxed8mhl6c4j Microscopy Pass-down equipment information]
===== SOPs & Troubleshooting =====
* SEM SOPs ([https://caltech.box.com/s/4yv8f5att77k3zq1rm6p0mqhkd8quslh Short Version] | [https://caltech.box.com/s/xwjdudqdl793gkc5kl71zez5nnc5y2xb Long Version])
* EDS SOPs ([https://caltech.box.com/s/52uckmx1silq90vq918gziohjtbqzyh5 Short Version] | [https://caltech.box.com/s/kukccwu1m8ekfjo6jds4jupvzwsjs3z1 Long Version])
* [https://caltech.box.com/s/sz9pai0icsntnef6me23veiwtwdui0gm 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]
* EDS ESPRIT 2 Software ([https://caltech.app.box.com/file/766742876889 Overview] | [https://caltech.app.box.com/file/766741003217 Basic Spectrum Collection and ID] | [https://caltech.app.box.com/file/766741864978?s=l77v3pct05r6q856sq53az5t0bugc6n4 Spectrum Acquisiton] | [https://caltech.app.box.com/file/766739703125 AutoID Verification] | [https://caltech.app.box.com/file/766742375532 Object Mode (Multi-Point Analysis)] | [https://caltech.app.box.com/file/766738174372 Line Profile Analysis])

===== Graphical Handouts =====
* [https://caltech.box.com/s/pxl99bbc1jm1tbjshfaotm91xm0mqs1i SEM & EDS/WDS Concepts]
* [https://caltech.box.com/s/k2iy75hxiwkehv0ogqelz2sux9e1cs5k SEM Alignments]
* [https://caltech.box.com/s/ijd8gprg9gcavb6of5uegu7osinzsdet Guide to Optimizing SEM Imaging]
===== Presentations =====
* Scanning Electron Microscopy: Principles, Techniques & Applications
** [https://caltech.box.com/s/lulkj0pwm053akyya1shazg8wzgudq9f Pptx Slides] | [https://youtu.be/Zh21tp3aPEw YouTube Lecture]
* Gallium Focused Ion Beam Microscopy: Principles, Techniques & Applications
** [https://caltech.box.com/s/f4k8jan85n5lf6f2tutjx4rkfzjq7y68 PPtx Slides] | [https://youtu.be/3eSzisbNcGo YouTube Lecture]

===== Manufacturer Manuals =====
* [https://caltech.box.com/s/og4309108q4k2jwhkaxqtpiujg2al5iu Nova NanoLab Operation Manual]
* [https://caltech.box.com/s/fime6qbew8bj2zac9a0vc4gx4qaivssd Bruker Quantax EDS Operation Manual]
* [https://caltech.box.com/s/zb5m72tc5c61pegangjjwj3wc8rbj1vr Gas Injection Systems – Deposition of Tungsten (Technical Note)]
* [https://caltech.box.com/s/th6cpko7opc9pccn2ukmdc88oh8oa6zw Gas Injection Systems – Delineation Etch for SiO2 (Technical Note)]
* [https://caltech.box.com/s/u56ho1hve4pf9713aw09iolukfc8wsb1 Gas Injection Systems – Selective Carbon Etching (Technical Note)]
* [https://caltech.box.com/s/b95pg59k003i9vn8y9elzem0tnxqg3fb Gas Injection Systems – Beam Chemistries Presentation]
* [https://caltech.box.com/s/110tb0o8avjziwa1y4d017dbbcpkxfop Scripting – AutoScript Language Manual (year 2000 Technical Note: most complete)]
* [https://caltech.box.com/s/n0abqy5z1e9a8hbyf38qybxu86sqz3vb Scripting – AutoScript Language Manual (year 2005 Technical Note: less complete, still useful)]
* [https://caltech.box.com/s/tlqgvtkkiahi261megm087i61gqlfzrc Scripting – RunScript Manual]
* [https://caltech.box.com/s/36j0n01ig7f757kvkiebvqjqj0el2yvp EDAX Genesis EDS & WDS Operation Manual (replaced - historic reference)]

===== Simulation Software =====
* [http://www.gel.usherbrooke.ca/casino/What.html CASINO Electron Beam Simulation Software] – simulate e-beam/specimen interactions (very useful for EDS & WDS)
* [http://www.srim.org/ The Stopping & Range of Ions in Matter (SRIM)] – simulate i-beam/specimen interactions
===== Calibrate Measurements with NIST Standard =====
* 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.
===== Sample Preparation =====
* Use the [[Carbon Evaporator]] to make non-conductive samples conductive by applying 2-10 nm of evaporated carbon.
* Use the [[Tergeo Plus ICP- & CCP-RIE: Oxygen & Argon Plasma Cleaner |
O2/Ar Plasma Cleaner]] to remove hydrocarbons from the sample surface to avoid creating dark contamination spots on your features while imaging them.
===== 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)
===== Guide to Choosing KNI SEMs & FIBs =====
*[[Guide to Choosing KNI SEMs & FIBs | Consult this guide for help in choosing the best SEMs and FIBs for your work]]

== Specifications ==
===== Manufacturer Specifications =====
* [https://caltech.box.com/s/nmws6w7643ne8mraljjar6c4epw0anpp Nova 200 NanoLab Data Sheet] (not all parameters apply to our instrument, see below for details specific to the KNI's Nova 200)
===== SEM Specifications =====
* Minimum Feature Size Resolved in Immersion Mode: ~5 nm
* Voltage Range: 0.2 to 30.0 kV
* Current Range: ~10 pA to 20 nA
* Apertures: 30 μm, 40 μm, 50 μm, 100 μm
* Eucentric Height: ~4.8 mm working distance (WD)
* Stage Range: ±25 mm X & Y travel, 50 mm Z travel, -12 to 58° tilt, 360° rotation
* ETD Grid Bias Range: -150 to 300 V
* TLD Bias Range: -100 to 150 V
* Ultimate Vacuum: 5e-6 mbar
 
 
== Related Instrumentation in the KNI ==
===== Scanning Electron Microscopes (SEMs) =====
* [[Nova 600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe|Nova 600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe]]
* [[Nova 200 NanoLab: SEM, EDS & WDS | Nova 200 NanoLab: SEM & EDS]]
* [[Sirion: SEM & EDS | Sirion: SEM & EDS]]
* [[Quanta 200F: SEM, ESEM, Lithography & Probe Station | Quanta 200F: SEM, ESEM, Lithography & Probe Station]]

===== Focused Ion Beam (FIB) Systems =====
* [[Nova 600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe|Nova 600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe]]
* [[ORION NanoFab: Helium, Neon & Gallium FIB | ORION NanoFab: Helium, Neon & Gallium FIB]]
===== Sample Preparation for Microscopy =====
* [[Carbon Evaporator | Carbon Evaporator (Leica EM ACE600) to make samples conductive]]
* [[Tergeo Plus ICP- & CCP-RIE: Oxygen & Argon Plasma Cleaner | Oxygen & Argon Plasma Cleaner (Tergeo Plus ICP- & CCP-RIE) to remove hydrocarbons from surface]]
===== Transmission Electron Microscopes =====
* [[Tecnai TF-30: 300 kV TEM, STEM, EDS & HAADF | Tecnai TF-30: TEM, STEM, EDS & HAADF (50-300 kV)]]
* [[Tecnai TF-20: 200 kV TEM, STEM, EDS, EELS, EFTEM & Lithography | Tecnai TF-20: TEM, STEM, EDS, EELS, EFTEM & Lithography (40-200 kV)]]
===== Scanning Probe Microscopes =====
* [[Dimension Icon: Atomic Force Microscope (AFM) | Dimension Icon: Atomic Force Microscope (AFM)]]
* [[Dektak 3ST: Profilometer | Dektak 3ST: Profilometer]]

Nova 200 NanoLab: SEM & EDS

2021-02-09T00:25:18Z

Mcaban: /* Video Tutorials */

{{InstrumentInfoboxOneImage|
|InstrumentName = Nova 200
|HeaderColor = #F5A81C
|ImageOne = Nova-200-NanoLab.jpg
|ImageTwo = Nova-200-NanoLab.jpg
|InstrumentType = [[Equipment_List#Microscopy|Microscopy]]
|RoomLocation = B203 Steele
|LabPhone = 626-395-1542
|PrimaryStaff = [[Miguel Caban-Acevedo, PhD]]
|StaffEmail = mcaban@caltech.edu
|StaffPhone = 626-395-5994
|Manufacturer = FEI (now Thermo Fisher)
|Model = Nova 200 NanoLab
|Techniques = SEM, EDS Immersion Lens Imaging
|RequestTraining = mcaban@caltech.edu
|EmailList = kni-sem-fib
|EmailListName = SEM-FIB
}}
== Description ==
The Nova 200 is the KNI's highest-resolution field-emission gun (FEG) analytical scanning electron microscope (SEM), equipped with an immersion lens for imaging sub-10 nm features and energy dispersive spectroscopy (EDS) for compositional analysis. It is also outfitted with a gallium focused ion beam (Ga-FIB) column, which is currently not operational because the [[Nova_600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe | Nova 600 NanoLab]] and [[ORION NanoFab: Helium, Neon & Gallium FIB | ORION NanoFab]] together meet the KNI's Ga-FIB demand; Ga-FIB could be reactivated on the Nova 200 in the future. See a full list of training and educational resources for this instrument below.
===== SEM Applications =====
* Ultra-High-Resolution Imaging (Immersion Mode aka UHR Mode)
* High-Resolution Imaging (Field-Free Mode aka Normal Mode)
* Secondary Electron (SE) imaging with an Everhart-Thornley Detector (ETD) & Through-the-Lens Detector (TLD)
* Backscattered Electron (BSE) imaging with a TLD
* Tungsten deposition via Gas Injection System (GIS)
* Automated imaging with RunScript program & AutoScript language
===== EDS Applications =====
* Spectrum acquisition for quantitative compositional analysis
* Linescan acquisition for 1D spatial compositional analysis
* Map acquisition for 2D spatial compositional analysis

== Resources ==
===== Equipment Data =====
* [https://caltech.box.com/s/xlvbr7cfwiqzcpc9hpq4jxed8mhl6c4j Microscopy Pass-down equipment information]
===== SOPs & Troubleshooting =====
* SEM SOPs ([https://caltech.box.com/s/4yv8f5att77k3zq1rm6p0mqhkd8quslh Short Version] | [https://caltech.box.com/s/xwjdudqdl793gkc5kl71zez5nnc5y2xb Long Version])
* EDS SOPs ([https://caltech.box.com/s/52uckmx1silq90vq918gziohjtbqzyh5 Short Version] | [https://caltech.box.com/s/kukccwu1m8ekfjo6jds4jupvzwsjs3z1 Long Version])
* [https://caltech.box.com/s/sz9pai0icsntnef6me23veiwtwdui0gm 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]
* EDS ESPRIT 2 Software

===== Graphical Handouts =====
* [https://caltech.box.com/s/pxl99bbc1jm1tbjshfaotm91xm0mqs1i SEM & EDS/WDS Concepts]
* [https://caltech.box.com/s/k2iy75hxiwkehv0ogqelz2sux9e1cs5k SEM Alignments]
* [https://caltech.box.com/s/ijd8gprg9gcavb6of5uegu7osinzsdet Guide to Optimizing SEM Imaging]
===== Presentations =====
* Scanning Electron Microscopy: Principles, Techniques & Applications
** [https://caltech.box.com/s/lulkj0pwm053akyya1shazg8wzgudq9f Pptx Slides] | [https://youtu.be/Zh21tp3aPEw YouTube Lecture]
* Gallium Focused Ion Beam Microscopy: Principles, Techniques & Applications
** [https://caltech.box.com/s/f4k8jan85n5lf6f2tutjx4rkfzjq7y68 PPtx Slides] | [https://youtu.be/3eSzisbNcGo YouTube Lecture]

===== Manufacturer Manuals =====
* [https://caltech.box.com/s/og4309108q4k2jwhkaxqtpiujg2al5iu Nova NanoLab Operation Manual]
* [https://caltech.box.com/s/fime6qbew8bj2zac9a0vc4gx4qaivssd Bruker Quantax EDS Operation Manual]
* [https://caltech.box.com/s/zb5m72tc5c61pegangjjwj3wc8rbj1vr Gas Injection Systems – Deposition of Tungsten (Technical Note)]
* [https://caltech.box.com/s/th6cpko7opc9pccn2ukmdc88oh8oa6zw Gas Injection Systems – Delineation Etch for SiO2 (Technical Note)]
* [https://caltech.box.com/s/u56ho1hve4pf9713aw09iolukfc8wsb1 Gas Injection Systems – Selective Carbon Etching (Technical Note)]
* [https://caltech.box.com/s/b95pg59k003i9vn8y9elzem0tnxqg3fb Gas Injection Systems – Beam Chemistries Presentation]
* [https://caltech.box.com/s/110tb0o8avjziwa1y4d017dbbcpkxfop Scripting – AutoScript Language Manual (year 2000 Technical Note: most complete)]
* [https://caltech.box.com/s/n0abqy5z1e9a8hbyf38qybxu86sqz3vb Scripting – AutoScript Language Manual (year 2005 Technical Note: less complete, still useful)]
* [https://caltech.box.com/s/tlqgvtkkiahi261megm087i61gqlfzrc Scripting – RunScript Manual]
* [https://caltech.box.com/s/36j0n01ig7f757kvkiebvqjqj0el2yvp EDAX Genesis EDS & WDS Operation Manual (replaced - historic reference)]

===== Simulation Software =====
* [http://www.gel.usherbrooke.ca/casino/What.html CASINO Electron Beam Simulation Software] – simulate e-beam/specimen interactions (very useful for EDS & WDS)
* [http://www.srim.org/ The Stopping & Range of Ions in Matter (SRIM)] – simulate i-beam/specimen interactions
===== Calibrate Measurements with NIST Standard =====
* 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.
===== Sample Preparation =====
* Use the [[Carbon Evaporator]] to make non-conductive samples conductive by applying 2-10 nm of evaporated carbon.
* Use the [[Tergeo Plus ICP- & CCP-RIE: Oxygen & Argon Plasma Cleaner |
O2/Ar Plasma Cleaner]] to remove hydrocarbons from the sample surface to avoid creating dark contamination spots on your features while imaging them.
===== 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)
===== Guide to Choosing KNI SEMs & FIBs =====
*[[Guide to Choosing KNI SEMs & FIBs | Consult this guide for help in choosing the best SEMs and FIBs for your work]]

== Specifications ==
===== Manufacturer Specifications =====
* [https://caltech.box.com/s/nmws6w7643ne8mraljjar6c4epw0anpp Nova 200 NanoLab Data Sheet] (not all parameters apply to our instrument, see below for details specific to the KNI's Nova 200)
===== SEM Specifications =====
* Minimum Feature Size Resolved in Immersion Mode: ~5 nm
* Voltage Range: 0.2 to 30.0 kV
* Current Range: ~10 pA to 20 nA
* Apertures: 30 μm, 40 μm, 50 μm, 100 μm
* Eucentric Height: ~4.8 mm working distance (WD)
* Stage Range: ±25 mm X & Y travel, 50 mm Z travel, -12 to 58° tilt, 360° rotation
* ETD Grid Bias Range: -150 to 300 V
* TLD Bias Range: -100 to 150 V
* Ultimate Vacuum: 5e-6 mbar
 
 
== Related Instrumentation in the KNI ==
===== Scanning Electron Microscopes (SEMs) =====
* [[Nova 600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe|Nova 600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe]]
* [[Nova 200 NanoLab: SEM, EDS & WDS | Nova 200 NanoLab: SEM & EDS]]
* [[Sirion: SEM & EDS | Sirion: SEM & EDS]]
* [[Quanta 200F: SEM, ESEM, Lithography & Probe Station | Quanta 200F: SEM, ESEM, Lithography & Probe Station]]

===== Focused Ion Beam (FIB) Systems =====
* [[Nova 600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe|Nova 600 NanoLab: SEM, Ga-FIB, GIS & Omniprobe]]
* [[ORION NanoFab: Helium, Neon & Gallium FIB | ORION NanoFab: Helium, Neon & Gallium FIB]]
===== Sample Preparation for Microscopy =====
* [[Carbon Evaporator | Carbon Evaporator (Leica EM ACE600) to make samples conductive]]
* [[Tergeo Plus ICP- & CCP-RIE: Oxygen & Argon Plasma Cleaner | Oxygen & Argon Plasma Cleaner (Tergeo Plus ICP- & CCP-RIE) to remove hydrocarbons from surface]]
===== Transmission Electron Microscopes =====
* [[Tecnai TF-30: 300 kV TEM, STEM, EDS & HAADF | Tecnai TF-30: TEM, STEM, EDS & HAADF (50-300 kV)]]
* [[Tecnai TF-20: 200 kV TEM, STEM, EDS, EELS, EFTEM & Lithography | Tecnai TF-20: TEM, STEM, EDS, EELS, EFTEM & Lithography (40-200 kV)]]
===== Scanning Probe Microscopes =====
* [[Dimension Icon: Atomic Force Microscope (AFM) | Dimension Icon: Atomic Force Microscope (AFM)]]
* [[Dektak 3ST: Profilometer | Dektak 3ST: Profilometer]]