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Cheat-SheetB Vincent Crist2019-10-27T18:17:46-07:00
Cheat-Sheet Check List (Do List)
Producing & Publishing XPS Data from Simple Materials
This list assumes that you are allowed to operate the XPS instrument, the Argon Ion (Ar+) etching gun, and know how to exchange sample mounts safely.
X-ray Type:Â Monochromatic Aluminum X-raysÂ
- Check “Instrument Status” before trying to use the XPS instrument
- Is a sample still inside the analysis chamber?
- If true, then remove sample
- If there are no samples inside, then continue
- Is the sample-viewing camera or microscope working?
- Is vacuum in analysis chamber <1 x 10 (-7) mTorr?
- If true, then you are ready to check instrument Calibration BEs, flood gun alignment, and X-ray beam position
- Cut each Calibration Metal to ~5 x 10 mm size. Trap metals using screws or clips. Do NOT use double-sided conductive tape.
- Using a clean single edged razor blade, scrape a 4×4 mm area on the Copper (Cu) sample used to check the Calibration BEs
- Cut a piece of polypropylene to be ~5 x 5 mm size. Scrape the surface with a clean single edged razor blade or a knife. Use double sided tape (3×3 mm) to hold polypropylene.
- Load sample mount that has all 3 Calibration Metals (Cu, Ag, Au), polypropylene (or Teflon), and X-ray Phosphor (P-31, ZnS) into Prep-Lock (Load-lock)
- Wait until pressure is <1 x 10 (-7) mTorr
- Pressure should be <5 x 10 (-8) if you want to collect data to be published
- If pressure is >1 x 10 (-6) mTorr, absolutely do NOT turn on any filaments. Immediately Contact Service.
- NOTE:Â If vacuum pressure is >1 x 10 (-6) mTorr, then all collected data will be bad and filaments oxidized or broken.
- Is cooling water used to cool Aluminum X-ray source running?
- Is water flow rate high enough? (>3 L/min). If true, then continue
- Is water line cool, not cold, to touch? (If too cold, then condensation can cause corrosion.)
- Record “Calibration BEs” and check X-ray Beam position using ZnS phosphor
- If X-rays are ON, then turn X-rays OFF
- If Flood Gun (FG) is ON, then turn FG OFF
- Transfer “Calibration Metals” (Cu, Ag, Au), polymer (polypropylene or Teflon) and X-ray Phosphor (P-31) from Load-Lock into “Analysis Chamber”
- Was Copper (Cu) Calibration Metal sample scraped? If not, then you will need longer ion etching to remove oxide.
- Move “X-ray Phosphor” (ZnS, type P-31) to standard “Sample Analysis Position”
- When pressure is <1 x 10 (-7) mTorr, continue
- Turn ON X-rays
- Maximum power settings
- Largest spot size
- Turn ON Argon Ion (Ar+) Gun to standby condition
- Make sure that ion gun has Argon gas – Do not flood the ion gun with too much Argon (if too much Argon, then filament may break)
- Select maximum acceleration voltage conditions (2-5 keV)
- Select maximum current
- Select 4 x 2 mm (or 4 x 4 mm) raster area
- (We assume that Argon ion gun is already optimized for routine use.)
- Adjust stage height to bring ZnS phosphor into good optical focus (Can you see grains?)
- NOTE:Â Good Optical Focus can be different from Good Electronic Focus by as much as 200 microns up or down
- When sample is not at good electronic focus, then count-rate drops by 10-15% of maximum countrate
- When sample is not at good electronic focus, then the BEs can shift by 0.1-0.2 eV from true value
- Verify that X-ray Beam center is nearly same as Green X-ray Spot on ZnS phosphor (Never ion etch ZnS)
- If not, then adjust optical microscope (or camera) to match
- Record Z-Height, and save as “Home Position” (record XYZ position)
- Move Copper (Cu) to “Home Position”
- Set analysis conditions to measure Cu (2p3) BE at 932.6 eV (KE = 554 eV) using a 10 eV narrow scan mode, or a SnapShot mode (~20 eV window)
- Using fast scan conditions with a large Pass Energy, adjust Z-Height until you find Z-Height position that gives maximum count-rate for Cu (2p3) signal
- Record XYZ position
- Change argon ion gun from standby to operate (unblank) for a minimum of 60 seconds to remove carbon or oxygen from the freshly scraped Copper surface
- Using fast scan conditions, adjust Z-Height to find Z-Height position that gives maximum count-rate for Cu (2p3) signal
- If best count-rate position has changed, then record new XYZ position, and teach new position as new HOME position
- Change fast scan conditions to measure Oxygen (1s) signal at 530 eV
- Measure Oxygen (1s) signal for 1-2 scans or use SnapShot mode (10 sec or continuous).
- If the Oxygen (1s) signal is very noisy, then the Copper surface is clean
- If the Oxygen (1s) signal is large, then ion etch Copper again, for 2-3 minutes
- NOTE: If ion gun is not properly aligned to overlap X-ray Spot, then argon ion etch rate is very small. Stop and adjust ion gun.
- Now we are ready to record the Calibration BE of Cu (2p3), Cu (3p) and Valence Band region
- Select Pass Energy that you normally use to measure high energy resolution (chemical state) spectra
- Use a 10 eV window to record Cu (2p3)Â (2 scans)Â [928 – 938 eV]
- Use a 30 eV window to record Cu (3p)Â Â (2-3 scans)Â [60-90 eV]
- Use a 30 eV window to record Cu Valence Band and Fermi Edge (3-4 scans)Â [ -10 to + 20 eV]
- To check for cleanliness, and to check the “Transmission Function” of the instrument, collect two survey spectra from the copper sample
- Energy range:Â -10 to 1100 eV
- Pass Energies:Â Largest pass energy and pass energy used to measure high energy resolution (chemical state) spectra
- Number of Scans: one (1) scan
- Step Size:Â 0.7-1.0 eV/step
- Move Gold (Au) to “Home Position”
- Set analysis conditions to measure Au (4f) BE at 85 eV (KE = 1401 eV) using a 10 eV narrow scan mode, or a SnapShot mode (~20 eV window)
- Using fast scan conditions with a large Pass Energy, adjust Z-Height until you find Z-Height position that gives maximum count-rate for Au (4f) signal
- Record XYZ position
- Change argon ion gun from standby to operate (unblank) for a minimum of 60 seconds to remove carbon from the Gold (Au) surface
- Now record the Calibration BE of Au (4f) signal
- Select Pass Energy that you normally use to measure high energy resolution (chemical state) spectra
- Use a 10 eV window to record Au (4f)Â (2 scans)Â [79-89 eV]
- Thank You. You have completed the essential recording of Calibration BEs from freshly cleaned Calibration Metals (Cu and Au)
- If you prefer to include Ag (3d) signal, then repeat the Gold cleaning and analysis procedure using Ag (3d) BE at 368.2 eV
- For Insulating Sample – check if Electron Flood Gun is properly aligned
- Turn ON the electron Flood Gun (charge neutralizer)
- Set FG voltage = ~4 eV (10 mA) for older instruments, or
- For very modern instruments, set FG voltage = 0.1 eV
- Move the polypropylene or Teflon sample to “Home Position”
- Move sample 2-3 mm in X and Y to spray electrons over the entire surface which produces a uniform electrical charge over the sample
- Move to the center of the polypropylene (or Teflon) sample
- Set analysis conditions to measure C (1s) BE at 284 eV for polypropylene (or 292 eV for Teflon) using a 20 eV narrow scan mode, or a SnapShot mode (~20 eV window)
- Using fast scan conditions with a large Pass Energy, adjust Z-Height until you find Z-Height position that gives maximum count-rate for C (1s) signal
- Record XYZ position
- If the electron Flood Gun is properly aligned, then the C (1s) signal will be symmetrical and have a FWHM <1.4 eV after peak-fitting
- If you see a small shoulder or a slope on the low BE side, then the Flood Gun needs to be aligned (the shoulder is due to differential charging)
- If you look at this webpage (https://xpslibrary.com/charge-compensation) then you will see examples of differential charging and FWHM for polypropylene and Teflon
- Place a transparent ruler or straight edge on your computer screen. Line the edge to the center of the C (1s) peak maximum
- Adjust the X and Y voltage settings (or the physical position) of the flood gun
- The C (1s) peak will shift to the right to lower BE if you are improving charge control
- The C (1s) peak will shift to the left to higher BE if you are making the charge control worse
- Adjust X and Y several times until the C (1s) BE for polypropylene is below 285.0 eV. For Teflon, the C (1s) BE is ~292 eV.
- If the X and Y voltage positions are optimized, then the FWHM will be <1.3 eV.
- If the C (1s) BE and FWHM are not improving enough, then increase the current and the voltage of the electron flood gun by 10%
- NOTE: electrons from the flood gun can and do cause degradation of a few materials. Avoid very high voltage and high current settings
- NOTE:Â if you place a 90% transparent metal mesh-screen ~1 mm above the surface of the sample, then the electric field will decrease and you will get better results (https://xpslibrary.com/charge-compensation)
- Now, you are ready to collect useful and reliable BEs from both conductors and non-conductors (insulators)
- Remove the Calibration Metals samples and load your samples.
- If you have a large sample mount (e.g. >50 x 50 mm, then you should load your samples, the Calibration Metals, the polypropylene, and X-ray phosphor, all together to save time)
- Prepare Sample
- NOTES:
- Do NOT wear latex gloves (cheap latex gloves have Silicone Oil on outside that contaminate your UHV chamber)
- Do NOT rinse or wipe surface with acetone or IPA, unless you know that someone has touched the surface to be analyzed.
- We use Scotch-brand double-sided adhesive tape – very small pieces
- Smaller sample size minimizes waiting time for sample to finish outgassing, especially porous materials (paper, powder, soft plastic…)
- Smaller sample size gives better charge control – near edge usually
- Decide if sample will degrade by exposure to monochromatic X-rays
- If you suspect that the sample will definitely degrade, then after collecting each spectrum, move sample by 2 mm before collecting next spectrum, and also collect fast 1 scan survey spectrum at start, and also at finish – compare – look for changes in peak heights
- Solid sample – non-conductive (ceramic, plastic, glass, non-porous, insulator)
- Avoid screws, masks, and clips to hold samples – they can cause differential charging near the metal piece
- Place a 10 x 10 mm piece of Scotch brand non-conductive double sided tape on sample stage/mount (must be slightly bigger than sample size)
- Use fine sandpaper to clean both edges of a single-edged razor blade or knife, then wipe edge with IPA or acetone
- Cut or break sample until it is slightly smaller than ~9 x 9 mm (or ~9 x 20 mm). (This style stops outgas from still exposed tape.)
- Scribe a line down the middle of the sample, or use Sharpie marker to make a line (Sharpie pens have silicone, but very little)
- On one side of the scribe line, scrape a 3×3 mm region of surface at 90 deg angle with the freshly cleaned razor blade or knife
- Use 2 pairs of tweezers – press corners of sample onto double-sided tape
- Or, place clean Aluminum foil (kitchen) on top of sample, press to make flat, and discard Al foil
- (Fresh exposed bulk of sample can also give useful results)
- Small grain or powder sample (normal laboratory air)
- NOTES:Â
- Old powders collect moisture from air or CO2 and may change surface chemistry over time. Drying in a vacuum oven may help.
- Brand new bottles of powders from chemical maker may be dirty with adventitious carbon, stabilizers, or contaminants
- Brand new bottles of powders from cheap manufacturing companies will very likely be dirty, have water of hydration – not reported, and have contaminants
- Clean mortar, pestle, and spatula with acetone and IPA 5 minutes before using. Blow dry with clean air or nitrogen. Do not use canned gases.
- Using a clean mortar and pestle, grind grains or powder gently for ~5 minutes
- Use freshly cleaned spatula to transfer and press powder onto non-conductive double sided tape (tape size: 5 x 5 mm)
- Use swab or Q-tip to gently brush off excess powder – trap excess powder in empty glove. Tie glove closed. Dispose safely.
- Solid sample – conductive (pure element, film, steel, alloy, wire, fiber, ball-bearing)
- Use electrical ohm-meter to measure conductivity at surface. Metals often have thick insulating oxides or machine oils due to production
- Clean edges of metal cutting shears with acetone and sandpaper before cutting sample
- Cut sample to be 10 x 10 mm or 20 mm x 20 mm.
- Scrape a small region where you put the screw or clip that traps sample
- Scribe a line down the middle of the sample (or use Sharpie pen)
- Scrape a 4 x 4 mm region with a clean single edged razor blade or knife
- Solid wafer – semiconductor
- Cleave wafer to be 10 x 10 mm. Gently scribe a line down the middle or use a Sharpie pen
- Use a clip or a screw to trap the sample onto the sample mount, or use graphite paint to trap the sample
- If you need true bulk information, then cleave the wafer in a glove box or cleave the wafer in air and very quickly load it into the load-lock
- NOTE: Do NOT use the electron flood gun on semiconductors. BE sure the FG is turned OFF unless you truly need it to control charging.
- Choose Instrument Settings for Data Collection
- X-ray Power:Â Maximum power
- X-ray Beam Size:Â Maximum beam size
- Flood Gun Setting:Â ~4 eV with 10 mA current, or 0.1 eV for dual beam source (Ar+/e-) for truly insulating samples (NOT semiconductors)
- Usual electron take-off-angle
- Choose Data Collection Variables and Collection Settings for Each Position (Sample)
- Always analyze as received first – before any ion etching
- Survey Spectrum #1:Â -10 eV to 1,100 eV, 1 eV/step (1 eV/channel), 50 msec/step, 3-5 scans
- C (1s) spectrum:Â 275 – 305 eV, PE =50 eV, 0.1 eV/step, 50 msec/step, 5-10 scans
- O (1s) spectrum:Â 515 – 575Â eV, PE =50 eV, 0.1 eV/step, 50 msec/step, 5-10 scans
- Element signal #1 spectrum:Â xxx-xxx eV (60 eV window), PE =50 eV, 0.1 eV/step, 50 msec/step, 5-10 scans
- Element signal #2 spectrum:Â xxx-xxx eV (60 eV window), PE =50 eV, 0.1 eV/step, 50 msec/step, 5-10 scans
- Valence Band spectrum:Â -10 – 40 eV, PE =100 eV, 0.2 eV/step, 50 msec/step, 10-20 scans
- Auger Signal Spectrum: xxx-xxx eV (100 eV window), PE =100 eV, 0.2 eV/step, 50 msec/step, 5-10 scans
- Survey Spectrum #2:Â -10 eV to 1,100 eV, 1 eV/step (1 eV/channel), 50 msec/step, 3-5 scans
- NOTE:Â The repeat 2nd survey spectrum checks for sample degradation due to analysis
- Collect the second survey spectrum after very soft ion etching that removes only 1-2 nm of adventitious carbon
- Define and Record each position to be analyzed. Take photo of sample inside instrument if possible.
- Move stage to locate center of each sample position to be analyzed
- Select O (1s) signal at 530 eV (NOTE:Â Oxygen and carbon exist on all as-received samples)
- Select “snapshot” or “fast scan conditions” to measure the O (1s) signal intensity
- Adjust Z-Height to get the strongest intensity for the O (1s) signal
- Define/Record each sample position to be analyzed
- NOTE: Optical focus is often wrong by 100-200 microns. Better to use electronic focus
- Collect Data
- Define sample analysis position #1 using Snapshot mode or fast scan mode to find maximum (best) count rate from O (1s) or C (1s) signals
- Continue collecting data from each sample or sample position
- If degradation is suspected, then move to fresh position ~2 mm away, to define a new fresh position to collect the next spectrum
- Do not use slits or apertures
- Do not tilt sample
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- Native Oxides FG ON-OFF, 5 MB (*.sdp)
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- Natural FWHM
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- Nb – Basic Spectra
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- Ni – Basic Spectra
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- O – Basic Spectra
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- Original S-Probe, 90 MB (*.mrs)
- Os – Basic Spectra
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- Overlaid Chemical State Spectra – Examples
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- Oxidation Treatments
- P – Basic Spectra
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- Pb – Basic Spectra
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- Pt – Basic Spectra
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- Rh – Basic Spectra
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- Sb – Basic Spectra
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- FWHM = Peak-width
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- Pure Element – Survey Spectra + L
- Pure Element Spectra – Main Signals
- Pure Element Spectra – Survey Scans
- Pure Elements
- Pure Single Crystal – CaCO3 (Calcite)
- Quantification – Atom%s
- Quantification – Atom%s
- Quantification – Atom%s
- Quantification – Atom%s
- Quantum Mechanics of XPS
- Quases
- Rare Earth Materials…, 36 MB (*.vgd)
- Rare Earth Metals – Principle
- Rare Earth Suppliers
- Rb – Basic Spectra
- Re – Basic Spectra
- Reference Materials
- Refund Policy
- Registration Form – IXIR System
- Reliable BEs ?
- Reliable Peak-fits ?
- Repeatability
- Reproducibility
- Research Members
- Rh – Basic Spectra
- Ru – Basic Spectra
- S – Basic Spectra
- s, p, d, f Peak-widths
- S-Probe, 200 MB (*.mrs, ASCII)
- Sample (Specimen)
- Sample (specimen) Handling
- Sample (specimen) History
- Sample (specimen) Storage
- Sample Degradation
- Sample Mount Charge-up
- Sample Mounts
- Sample Prep Equipment
- Sample Preparation Bench
- Sample Preparation Methods
- Sample Size, Shape & Form
- Satellite Peaks?
- Sb – Basic Spectra
- Sb overlaps O – ratios
- Sc – Basic Spectra
- Scattering Effects
- SCE Values
- Scofield SFs – Al X-rays – Crist Modified for Thermo K-Alpha
- Scofield SFs – Al X-rays – Theoretically Calculated – Central Field Potential – SCF
- Scofield SFs – Al X-rays – Thermo Modified
- SDP_v8 software
- Se – Basic Spectra
- Selenides
- SEM-EDS Information Depth
- Semiconductor Suppliers
- Sessa
- SF Table #6
- Shake-up – Cu (2+) vs Cu (1+)
- Shake-up – pi to pi*
- Shake-up peaks
- Shake-up Structures
- Sherwood & Proctor Background
- Shirley Background
- Shirley Background
- Shop
- Si – Basic Spectra
- Signal-to-Noise (S/N)
- Silicates
- Silicides
- Simple Peak-fit Examples
- Simple Peak-fit Examples 2
- Single Crystal Suppliers
- Single Crystal Suppliers
- Single Crystals, 240 MB (*.vgd)
- Single Xtals, 2D, Graphene, Nano, Perovskite
- SiS Standards
- Sm – Basic Spectra
- Smoothing – Bad vs OK
- Sn – Basic Spectra
- Software
- Software Operation
- Source of Spectra in The XPS Library
- SpecMaster Pro, 1.8 GB (*.sdp)
- SpecMaster, 527 MB (*.sdp)
- Spectra Data Processor (SDP) – 1 yr Free Use
- Spectra Data Processor v7 – Training Videos
- Spectra Examples
- Spectra Handbooks
- Spectra-Bases #1
- Spectra-Bases #2
- Spin-Orbit Coupling
- Spin-Orbit Coupling
- Spin-Orbit Coupling
- Sr – Basic Spectra
- SRD 64 Electron Elastic Scattering Cross-Sections
- SRD 71 Electron IMFP Database
- SRD 82 Electron EAL Database
- Standards
- Statistics
- Sticking Coefficients
- Store
- Strategic Partners
- Sub-Structure
- Subscriptions
- Sulfates
- Sulfides
- Sulfides from H2S (air)
- Summaries of BE Tables – NIST
- Summaries of BE Tables – NIST
- Super Coster-Kronig Effect – Ti (2p1) in TiO2
- Surface Charging
- Surface Chemical Reaction
- Surface Chemistry
- Surface Contaminants
- Surface Photo-Chemistry
- Surface Reactivity
- Surface Science Western (UWO) Application Notes
- SurfaceSpectra – XPS Handbook of Polymer Spectra
- Survey Spectra Examples
- Sven Tougaard
- Synchrotron Labs
- Synchrotrons
- Synchrotrons for XPS
- Synthetic Peaks
- Ta – Basic Spectra
- Tables & Guides
- Tb – Basic Spectra
- Tc – Basic Spectra
- Te – Basic Spectra
- Teaching Members
- Team
- Technical Support
- Tellurides
- Temp
- Terms & Phrases for XPS
- Terms of Use
- Tesla Coil Irradiation
- Tesla Coil Irradiation Effects
- TEST
- Test Page
- Tests of RSFs
- Th – Basic Spectra
- The History of XPS
- Thermo Application Notes
- Thermo K-Alpha XPS
- Thermo’s Modified Scofield SFs Al X-rays
- Thickness Estimates
- Ti – Basic Spectra
- Titanates
- Tl – Basic Spectra
- Tm – Basic Spectra
- ToF-SIMS Information Depth
- Too Many Peaks – O (1s) – native SiOx
- Tougaard Backgound
- Tougaard Background
- Tougaard Background
- TPP-2M and IMFPs
- TPP-2M IMFP Calculator
- Trace level signals
- Training & Videos
- Translate TXL Website to Your Language
- Translate TXL Website to Your Language
- Transmission Function
- Transmission Function
- Trouble-Shooter Pro
- Troubleshooting
- Tungstates
- TXL #2, 2.0 GB (*.vgd)
- TXL HQ IP-eSF, 340 MB (*.vgd)
- TXL Members
- TXL Misc, 60 MB, (*.vgd)
- TXL Store
- TXL Ultimate, 3 GB (*.txt, *.sdp, *.vgd)
- U – Basic Spectra
- UHV Gas Capture, 1 MB (3d plots)
- UKSAF Links
- Ulvac-PHI Application Notes
- Ulvac-PHI ASFs
- Ulvac-PHI ASFs – March 2002
- Ulvac-PHI SFs as Plots
- Unifit
- University Labs
- Useful Websites
- V – Basic Spectra
- Valence Band Examples
- Valence Band Spectra – Elements
- Valence Band, 3 MB (*.txt, *.sdp)
- Vanadates
- Vegh Background
- VG Eclipse Database, 9 MB (*.dts)
- Vibrational Bands – Gases & Polymers
- Video of Website Menus
- Videos of TXL Website
- Vincent Fernandez
- Vincent S. Smentkowski (USA)
- Vocabulary
- Voigt Peak-shape
- W – Basic Spectra
- Wagner Book of XPS BEs (NIST)
- Wagner SFs – Al X-rays – PHI Modified for 5800 Omni-5
- Wagner SFs – Al X-rays – PHI Modified for MultiPak v8
- Wagner SFs – Al X-rays – Empirically Defined : F (1s)=1.0 vs C (1s)=1.0
- Wagner’s Original ASFs
- Wall Charts & Wall Posters
- Website Menus Display
- Wikipedia – XPS
- Work Functions of Elements
- X-pedia for Elements
- X-ray Beam Alignment
- X-ray Beam Size
- X-ray Data Booklet – LBL
- X-ray Degradation of Polymers, 1 MB (*.sdp)
- X-ray Energies
- X-ray Energies
- X-ray Sources
- XI – Application Notes
- XI Sample Spectra
- XML Site-Map of The XPS Library
- XPS
- XPS (.SDP format) 7304 data-sets
- XPS (.SDP format) 7304 data-sets
- XPS (.VMS, .ISO, .TXT) 3177 data-sets
- XPS (.VMS, .ISO, .TXT) 3177 data-sets
- XPS (.VMS, .ISO, .TXT) 3177 data-sets
- XPS Basics
- XPS Basics
- XPS BE On-line Database – NIST
- XPS by Element
- XPS Detection Limit
- XPS Detection Limits
- XPS Detection Limits
- XPS Instruments, Components & Parts Makers
- XPS International Application Notes
- XPS International Database Websites
- XPS Job Openings
- XPS Jobs at XPS Makers
- XPS Jobs at XPS Makers
- XPS Journals
- XPS Labs
- XPS Labs around the World
- XPS Library – SEO TERMS
- XPS Manufacturers who Donated
- XPS Opportunities at Contract Analysis Labs
- XPS Papers – NIST
- XPS Peak-fitting MOVIES
- XPS Service by TXL
- XPS Simplified, 14 MB (*.vgd)
- XPS Spectra & AES Spectra Libraries
- XPS Theory
- XPS Training Videos
- Y – Basic Spectra
- Yb – Basic Spectra
- Your Suggestions – Your Ideas to improve TXL
- Zn – Basic Spectra
- Zr – Basic Spectra
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