Basic XPS Information Section

The Basic XPS Information Section provides fundamental XPS spectra, BE values, FWHM values, BE tables, overlays of key spectra, histograms and a table of XPS parameters.
The Advanced XPS Information Section is a collection of additional spectra, overlays of spectra, peak-fit advice, data collection guidance, material info,
common contaminants, degradation during analysis, auto-oxidation, gas capture study, valence band spectra, Auger spectra, and more.
Published literature references, and website links are summarized at the end of the advanced section.
 Periodic Table – HomePage                     XPS Database of Polymers                   Six (6) BE Tables


 

Terbium (Tb)

 

Terbium Chloride – TbCl3 Terbium Metal – Tbo Terbium Oxide – Tb4O7

 

  Page Index
  • Expert Knowledge & Explanations


Terbium (Tbo) Metal

Peak-fits, BEs, FWHMs, and Peak Labels


Terbium (Tbo) Metal
Tb (3d5/2) and (3d3/2) Spectrum – raw
Terbium (Tbo) Metal
Peak-fit of Tb (3d5/2) Spectrum

 Periodic Table – HomePage  
Terbium (Tbo) Metal
Tb (3d5/2) Spectrum – raw
Terbium (Tbo) Metal
Tb (3d5/2) Spectrum – peak-fit


 
Terbium (Tbo) Metal
 Tb (4d) Spectrum – full range
Terbium (Tbo) Metal
 Tb (4d) Spectrum – full range – peak-fit


   
Terbium (Tbo) Metal
 Tb (4d) Spectrum  – zoomed in
Terbium (Tbo) Metal
 Tb (4d) Spectrum  – zoomed in – peak-fit

   

 

Survey Spectrum of Terbium (Tbo) Metal
with Peaks Integrated, Assigned and Labelled

 


 Periodic Table 

XPS Signals for Terbium, (Tbo) Metal

Spin-Orbit Term,  BE (eV) Value, and Scofield σ for Aluminum Kα X-rays (1486 eV, 8.33 Ang)

Overlaps Spin-Orbit Term BE (eV) Value Scofield σ from 1486 eV X-rays IMFP (TPP-2M) in Å
Tb (3d5/2) 1241 49.42 7.26
N (1s) overlaps Tb (4s) 398 1.54 19.96
Tb (4p1/2) 311 1.84 21.16
C (1s) overlaps Tb (4p3/2) 286 3.99 21.5
Tb (4d3/2) 149 10.87 23.36
Si (2s) overlaps Tb (4d5/2) 149 10.87 23.36
Tb (5s) 40 0.281 24.8
O (2s) overlaps Tb (5p) 22 0.804 24.99

σ:  abbreviation for the term Scofield Photoionization Cross-Section, which is used with IMFP and TF to generate RSFs for quantitation

Plasmon Peaks

Energy Loss Peaks

Auger Peaks

 

Energy Loss    Intrinsic Plasmon Peak:  ~xx eV above peak max
Expected Bandgap for Tb2O3:  ~ 4 eV  (https://materialsproject.org/)
Work Function for Tb:  xx eV
*Scofield Cross-Section (σ) for C (1s) = 1.0

 Periodic Table 


 


Valence Band Spectrum from Terbium, Tbo Metal

 Fresh exposed bulk produced by extensive Ar+ ion etching


 


Plasmon Peaks from Terbium, Tbo Metal

 Fresh exposed bulk produced by extensive Ar+ ion etching

Tb (3d) – Extended Range Spectrum Tb (3d) – Extended Range Spectrum – Vertically Zoomed
 Periodic Table 

 

Tb (LMM) Auger Peaks from Terbium Tbo Metal
 Fresh exposed bulk produced by extensive Ar+ ion etching

Tbo Metal – high BE Auger peaks Tbo Metal – low BE Auger peaks
 

Features Observed

  • xx
  • xx
  • xx

 Periodic Table 


 

Artefacts Caused by Argon Ion Etching

C (1s) from Metal Carbide(s)

can form when ion etched Reactive Metal Surfaces capture
Residual UHV Gases (CO, H2O, CH4 etc)

Argon Trapped in Tbo

can form when Argon Ions are used
to removed surface contamination


 

Side-by-Side Comparison of
Tb Native Oxide & Terbium Oxide (Tb2O3)
Peak-fits, BEs, FWHMs, and Peak Labels

Tb Native Oxide Tb2O3
Tb (4d5/2) from Tb Native Oxide on Terbium Metal
Flood Gun ON, 0.1 eV
As-Measured, C (1s) at 285.4 eV
Tb (4d5/2) from Tb2O3
Flood Gun ON
Charge Referenced to C (1s) at 285.0 eV


 
Tb Native Oxide Tb2O3
C (1s) from Tb Native Oxide
on Terbium
C (1s) at 285.4 eV (Flood Gun ON, 0.1 eV)

C (1s) from Tb2O3– pressed pellet
Flood Gun ON
Charge Referenced to C (1s) at 285.0 eV

 
 Periodic Table 

  .
Tb Native Oxide Tb2O3
O (1s) from Tb Native Oxide
on Terbium
As-Measured, C (1s) at 285.4 eV (Flood Gun ON)

O (1s) from Tb2O3 – pressed pellet
Flood Gun ON
Charge Referenced to C (1s) at 285.0 eV



 

  .
Terbium, Tb Native Oxide Terbium Oxide, Tb2O3
Tb (3d) – raw Tb (3d) – raw
 Periodic Table

 


 


Survey Spectrum of Tb Native Oxide

with Peaks Integrated, Assigned and Labelled

 

 Periodic Table 


 

 

Survey Spectrum of Terbium Oxide, Tb2O3
with Peaks Integrated, Assigned and Labelled

 Periodic Table  



Overlays of Tb (4d
)
Spectra for:
Tb Native Oxide and Terbium Oxid (Tb2O3)

Caution: BEs from Grounded Native Oxides can be Misleading if Flood Gun is ON

 

 Overlay of Tbo metal and Tb Native Oxide – Tb (4d)
Native Oxide C (1s) = 285.4 eV (Flood gun ON, 0.1 eV)

 Overlay of Tbo metal and Tb2O3 – Tb (4d)
Pure Oxide C (1s) = 285.0 eV
 Periodic Table  Copyright ©:  The XPS Library 

 


Overlay of Tb (4d)

Tbo Metal, Tb Native Oxide, & Tb2O3  


 

Overlay of Tb Native Oxide, & Tb2O3:   Tb (4d)


After shifting Tb2O3 spectrum by 1.4 eV to align with native oxide edge
as test of charge correction, the spectra align very nicely.

This need to shift means that charge referencing using C (1s) is not good.
This is the one reason to include native oxides in data analyses & comparisons.

 

Features Observed

  • xx
  • xx
  • xx

 Periodic Table 


 

Valence Band Spectra
Tbo, Tb2O

Tbo
Ion etched clean
Tb2O3 – pressed pellet
Flood gun is ON,  Charge referenced so C (1s) = 285.0 eV



Overlay of Valence Band Spectra for:

Tb metal and Tb2O3

Tb2O3 was shifted by 1.4 eV to study charge shift question
See (4d) spectrum overlay results shown above.

Features Observed

  • xx
  • xx
  • xx

 Periodic Table 



 

Terbium Minerals, Gemstones, and Chemical Compounds

 

Monazite – Rare Earth Phosphate Mineral Terbium Sulfate – Tb2(SO4)3-8H2O Terbium Fluoride – TbF3 Terbium Nitrate – Tb(NO3)3-5H2O

 Periodic Table 



 

Six (6) Chemical State Tables of Tb (4d5/2) BEs

 

  • The XPS Library Spectra-Base
  • PHI Handbook
  • Thermo-Scientific Website
  • XPSfitting Website
  • Techdb Website
  • NIST Website

 Periodic Table 



 

Notes of Caution when using Published BEs and BE Tables from Insulators and Conductors:

  • Accuracy of Published BEs
    • The accuracy depends on the calibration BEs used to calibrate the energy scale of the instrument.  Cu (2p3/2) BE can vary from 932.2 to 932.8 eV for old publications 
    • Different authors use different BEs for the C (1s) BE of the hydrocarbons found in adventitious carbon that appears on all materials and samples.  From 284.2 to 285.3 eV
    • The accuracy depends on when the authors last checked or adjusted their energy scale to produce the expected calibration BEs
  • Worldwide Differences in Energy Scale Calibrations
    • For various reasons authors still use older energy scale calibrations 
    • Some authors still adjust their energy scale so Cu (2p3/2) appears at 932.2 eV or 932.8 eV because this is what the maker taught them
    • This range causes BEs in the higher BE end to be larger than expected 
    • This variation increases significantly above 600 eV BE
  • Charge Compensation
    • Samples that behave as true insulators normally require the use of a charge neutralizer (electron flood gun with or without Ar+ ions) so that the measured chemical state spectra can be produced without peak-shape distortions or sloping tails on the low BE side of the peak envelop. 
    • Floating all samples (conductive, semi-conductive, and non-conductive) and always using the electron flood gun is considered to produce more reliable BEs and is recommended.
  • Charge Referencing Methods for Insulators
    • Charge referencing is a common method, but it can produce results that are less reliable.
    • When an electron flood gun is used, the BE scale will usually shift to lower BE values by 0.01 to 5.0 eV depending on your voltage setting. Normally, to correct for this flood gun induced shift, the BE of the hydrocarbon C (1s) peak maximum from adventitious carbon is used to correct for the charge induced shift.
    • The hydrocarbon peak is normally the largest peak at the lowest BE. 
    • Depending on your preference or training, the C (1s) BE assigned to this hydrocarbon peak varies from 284.8 to 285.0 eV.  Other BEs can be as low as 284.2 eV or as high as 285.3 eV
    • Native oxides that still show the pure metal can suffer differential charging that causes the C (1s) and the O (1s) and the Metal Oxide BE to be larger
    • When using the electron flood gun, the instrument operator should adjust the voltage and the XY position of the electron flood gun to produce peaks from a strong XPS signal (eg O (1s) or C (1s) having the most narrow FWHM and the lowest experimentally measured BE. 

 Periodic Table 


Table #1

Tb (4d5/2) Chemical State BEs from:  “The XPS Library Spectra-Base”

C (1s) BE = 285.0 eV for TXL BEs
and C (1s) BE = 284.8 eV for NIST BEs

Element Atomic # Compound As-Measured by TXL or NIST Average BE Largest BE Hydrocarbon C (1s) BE  Source
Tb 65 Tb – element 145.9 eV tallest peak 285.0 eV The XPS Library
Tb 65 Tb-(OH)3 285.0 eV
Tb 65 Tb-2O3 147.8 eV  tallest peak 285.0 eV The XPS Library
Tb 65 Tb-4O7 149.5 eV 285.0 eV The XPS Library

Charge Referencing Notes

  • (N*number) identifies the number of NIST BEs that were averaged to produce the BE in the middle column.
  • The XPS Library uses Binding Energy Scale Calibration with Cu (2p3/2) BE = 932.62 eV and Au (4f7/2) BE = 83.98 eV.  BE (eV) Uncertainty Range:  +/- 0.2 eV
  • Charge Referencing of insulators is defined such that the Adventitious Hydrocarbon C (1s) BE (eV) = 285.0 eV.  NIST uses C (1s) BE = 284.8 eV 
  • Note:   Ion etching removes adventitious carbon, implants Ar (+), changes conductivity of surface, and degrades chemistry of various chemical states.
  • Note:  Ion Etching changes BE of C (1s) hydrocarbon peak.
  • TXL – abbreviation for: “The XPS Library” (https://xpslibrary.com).  NIST:  National Institute for Science and Technology (in USA)

 Periodic Table 


Table #2

Tb (4d5/2) Chemical State BEs from:  “PHI Handbook”

C (1s) BE = 284.8 eV

 Periodic Table 

Copyright ©:  Ulvac-PHI


Table #3

Tb (4d5/2) Chemical State BEs from:  “Thermo-Scientific” Website

C (1s) BE = 284.8 eV

 

No BE Table available

 Periodic Table 

Copyright ©:  Thermo Scientific 


Table #4

Tb (4d5/2) Chemical State BEs from:  “XPSfitting” Website

Chemical State BE Table derived by Averaging BEs in the NIST XPS database of BEs
C (1s) BE = 284.8 eV

 

No Rare Earth BE Tables available

 Periodic Table 

Copyright ©:  Mark Beisinger


Table #5

Tb (4d5/2) Chemical State BEs from:  “Techdb.podzone.net” Website

 

XPS Spectra – Chemical Shift | Binding Energy
C (1s) BE = 284.6 eV

XPS (X線光電子分光法) スペクトル 化学状態 化学シフト ケミカルシフト

Element Level Compound B.E.(eV) min max
Tb 4d Tb 145.9 ±0.4 145.5 146.3
Tb 4d Tb2O3 146.8 ±0.3 146.5 147.0
Tb 4d TbO2 149.2 ±0.2 149.0 149.4
Tb 3d5/2 Tb2O3 1241.5 ±0.3 1241.2 1241.7
Tb 3d5/2 TbO2 1241.5 ±0.3 1241.2 1241.7
Tb 3d5/2 Tb 1242.0 ±0.3 1241.7 1242.3

 Periodic Table 



 
 

Histograms of NIST BEs for Tb (4d5/2) BEs

Important Note:  NIST Database defines Adventitious Hydrocarbon C (1s) BE = 284.8 eV for all insulators.

 

Histogram indicates:  146.0 eV for Tbo based on 2 literature BEs Histogram indicates:  150.9 eV for Tb4O7 based on 3 literature BEs

Table #6


NIST Database of Tb (4d5/2) Binding
Energies

NIST Standard Reference Database 20, Version 4.1

Data compiled and evaluated
by
Alexander V. Naumkin, Anna Kraut-Vass, Stephen W. Gaarenstroom, and Cedric J. Powell
©2012 copyright by the U.S. Secretary of Commerce on behalf of the United States of America. All rights reserved.

Important Note:  NIST Database defines Adventitious Hydrocarbon C (1s) BE = 284.8 eV for all insulators.

 

Element Spectral Line Formula Energy (eV) Reference
Tb 4d Tb 145.98  Click
Tb 4d5/2 Tb2O3 148.70  Click
Tb 4d5/2 Tb2O3 149.10  Click
Tb 4d5/2 TbO2 149.20  Click
Tb 4d BaTbO3 149.55  Click
Tb 4d Tb4O7 149.80  Click
Tb 4d Lu0.5Tb0.5Ba2Cu3O7-x 149.80  Click
Tb 4d5/2 TbCrO3 149.90  Click
Tb 4d5/2 Tb2(SO4)3 150.50  Click
Tb 4d5/2 Tb2(C2O4)3 150.90  Click
Tb 4d5/2 Tb4O7 151.30  Click
Tb 4d Tb4O7 151.55  Click
Tb 4d BaTbO3 151.55  Click
Tb 3d5/2 Tb 1239.40  Click
Tb 3d5/2 Tb2O3 1241.20  Click
Tb 3d5/2 TbO2 1241.40  Click
Tb 3d5/2 Tb2O3 1241.50  Click
Tb 3d5/2 (Ce0.9Tb0.1)PO4 1242.10  Click
Tb 3d5/2 (Ce0.9Tb0.1)PO4 1242.20  Click
Tb 3d5/2 TbPO4 1242.30  Click

 

 

Statistical Analysis of Binding Energies in NIST XPS Database of BEs

 

 

 Periodic Table 


 


Advanced XPS Information Section

 

Expert Knowledge, Spectra, Features, Guidance and Cautions
for XPS Research Studies on Terbium Materials

 

 


 

Expert Knowledge Explanations

 

 Periodic Table 


 

Terbium Chemical Compounds

 

Peak-fits and Overlays of Chemical State Spectra

Pure Tb Metal:  Tb (4d)
Cu (2p3/2) BE = 932.6 eV
Tb2O3:  Tb (4d5/2)
C (1s) BE = 285.0 eV
Tb4O7:  Tb (4d5/2)
C (1s) BE = 285.0 eV

Features Observed

  • xx
  • xx
  • xx

 Periodic Table 


 

Overlay of Tb (4d5/2) Spectra shown Above

C (1s) BE = 285.0 eV

 

 

Chemical Shift between Tb and Tb2O3:  xxx eV
 Chemical Shift between Tb and Tb4O7:  xxx eV

 

 Periodic Table 


 

Terbium Oxide (Tb4O7)
pressed pellet

Survey Spectrum from Tb4O7
Flood gun is ON, C (1s) BE = 285.0 eV
Tb (4d5/2) Chemical State Spectrum from Tb4O7
Flood gun is ON, C (1s) BE = 285.0 eV

 
O (1s) Chemical State Spectrum from Tb4O7
Flood gun is ON, C (1s) BE = 285.0 eV
C (1s) Chemical State Spectrum from Tb4O7
Flood gun is ON, C (1s) BE = 285.0 eV

 
Valence Band Spectrum from Tb4O7
Flood gun is ON, C (1s) BE = 285.0 eV

Overlay of Valence Band from Tb2O3 and Tb4O7
Flood gun is ON, C (1s) BE = 285.0 eV
Tb4O7 BE shifted to align peaks to those from Tb2O3 as test


Shake-up Features for:
Terbium Hepta-oxide, Tb4O7

 

Tb (4d) Overlay for Tb2O3 and Tb4O7
after shifting to align peak tops

 


Features Observed

  • xx
  • xx
  • xx

 Periodic Table 

 


 

 

Terbium Chemical Compounds

 

TbF3

Survey Spectrum Tb (4d5/2) Spectrum
C (1s) Spectrum F (1s) Spectrum
Valence Band Spectrum

 Periodic Table 


Quantitation Details and Information

 

Quantitation by XPS is often incorrectly done, in many laboratories, by integrating only the main peak, ignoring the Electron Loss peak, and the satellites that appear as much as 30 eV above the main peak.  By ignoring the electron loss peak and the satellites, the accuracy of the atom% quantitation is in error.

When using theoretically calculated Scofield cross-section values, the data must be corrected for the transmission function effect, use the calculated TPP-2M IMFP values, the pass energy effect on the transmission function, and the peak area used for calculation must include the electron loss peak area, shake-up peak area, multiplet-splitting peak area, and satellites that occur within 30 eV of the main peak.

 

Quantitation from Pure, Homogeneous Binary Compound
composed of Terbium – Tb2O3

 

This section is focused on measuring and reporting the atom % quantitation that results by using:

  • Scofield cross-sections,
  • Spectra corrected to be free from Transmission Function effects
  • A Pass Energy that does not saturate the detector system in the low KE range (BE = 1000-1400 eV)
  • A focused beam of X-ray smaller than the field of view of the lens
  • An angle between the lens and the source that is ~55 deg that negates the effects of beta-asymmetry
  • TPP-2M inelastic mean free path values, and
  • Either a linear background or an iterated Shirley (Sherwood-Proctor) background to define peak areas

The results show here are examples of a method being developed that is expected to improve the “accuracy” or “reliability” of the atom % values produced by XPS.

 

 Periodic Table 

Copyright ©:  The XPS Library

 

 

Terbium Alloys

   
XxCu XxCu
 Periodic Table   
XxCu XxCu

 

Copyright ©:  The XPS Library 

 



 


XPS Facts, Guidance & Information

 Periodic Table 

    Element Terbium (Tb)
 
    Primary XPS peak used for Peak-fitting: Tb (4d)  
    Spin-Orbit (S-O) splitting for Primary Peak: Spin-Orbit splitting for “d” Orbital, ΔBE = xxx eV
 
    Binding Energy (BE) of Primary XPS Signal: 146 eV
 
    Scofield Cross-Section (σ) Value: Tb (4d) = 10.87
 
    Conductivity: Tb resistivity =  
Native Oxide suffers Differential Charing
 
    Range of Tb (4d5/2) Chemical State BEs: 145-150 eV range   (Tbo to TbF3)  
Signals from other elements that overlap
Tb (4d5/2) Primary Peak:
  xxx
Bulk Plasmons:   ~xx eV above peak max for pure
Shake-up Peaks: xx
Multiplet Splitting Peaks:   xx

 

 

General Information about
XXX Compounds:
  xx  
Cautions – Chemical Poison Warning

xx 

Copyright ©:  The XPS Library 

 Periodic Table 



 

Information Useful for Peak-fitting Tb (4d5/2)

 

  • FWHM (eV) of Tb (4d5/2) for Pure Tbo ~1.2 eV using 25 eV Pass Energy after ion etching:
  • FWHM (eV) of Tb (4d5/2) for Tb2O3 ~2.4 eV using 50 eV Pass Energy  (before ion etching)
  • Binding Energy (BE) of Primary Signal used for Measuring Chemical State Spectra:  146 eV for Tb (4d5/2) with +/- 0.2 uncertainty
  • List of XPS Peaks that can Overlap Peak-fit results for Tb (4d5/2):  xxx

 Periodic Table 


 

General Guidelines for Peak-fitting XPS Signals

 

  • Typical Energy Resolution for Pass Energy (PE) setting used to measure Chemical State Spectra on Various XPS Instruments
    • Ag (3d5/2) FWHM (eV) = ~0.90 eV for PE 50 on Thermo K-Alpha
    • Ag (3d5/2) FWHM (eV) = ~1.00 eV for PE 80 on Kratos Nova
    • Ag (3d5/2) FWHM (eV) = ~0.95 eV for PE 45 on PHI VersaProbe
    • Ag (3d5/2) FWHM (eV) = ~0.85 eV for PE 50 on SSI S-Probe
  • FWHM (eV) of Pure Elements: Ranges from 0.4 to 1.0 eV across the periodic table
  • FWHM of Chemical State Peaks in any Chemical Compound:  Ranges from 1.1 to 1.6 eV  (in rare cases FWHM can be 1.8 to 2.0 eV)
  • FWHM of Pure Element versus FWHM of Oxide:  Pure element FWHM << Oxide FWHM  (e.g. 0.8 vs 1.5 eV, roughly 2x)
  • If FWHM Greater than 1.6 eV:  When a peak FWHM is larger than 1.6 eV, it is best to add another peak to the peak-fit envelop.
  • BE (eV) Difference in Chemical States: The difference in chemical state BEs is typically 1.0-1.3 eV apart.  In rare cases, <0.8 eV.
  • Number of Peaks to Use:  Use minimum. Do not use peaks with FWHM < 1.0 eV unless it is a or a conductive compound.
  • Typical Peak-Shape:  80% G: 20% L,   or Voigt : 1.4 eV Gaussian and 0.5 eV Lorentzian
  • Spin-Orbit Splitting of Two Peaks (due to Coupling):  The ratio of the two (2) peak areas must be constrained.
  • Constraints used on Peak-fitting: typically constrain the peak area ratios based on the Scofield cross-section values
  • Asymmetry for Conductive materials:  20-30% with increased Lorentzian %
  • Peak-fitting “2s” or “3s” Peaks:  Often need to use 50-60% Lorentzian peak-shape

Notes:

  • Other Oxidation States can appear as small peaks when peak-fitting
  • Pure element signals normally have asymmetric tails that should be included in the peak-fit.
  • Gaseous state materials often display asymmetric tails due to vibrational broadening.
  • Peak-fits of C (1s) in polymers include an asymmetric tail when the energy resolution is very high.
  • Binding energy shifts of some compounds are negative due to unusual electron polarization.

 Periodic Table 


 

 

Contaminants Specific to Terbium

 

  • Terbium develops a thick native oxide due to the reactive nature of clean Terbium .
  • The native oxide of Tb Ox is 5-8 nm thick.
  • Terbium thin films often have a low level of iron (Fe) in the bulk as a contaminant or to strengthen the thin film
  • Terbium forms a low level of Carbide when the surface is ion etched inside the analysis chamber

 

Commonplace Contaminants

 

  • Carbon and Oxygen are common contaminants that appear on nearly all surfaces. The amount of Carbon usually depends on handling.
  • Carbon is usually the major contaminant.  The amount of carbon ranges from 5-50 atom%.
  • Carbon contamination is attributed to air-borne organic gases that become trapped by the surface, oils transferred to the surface from packaging containers, static electricity, or handling of the product in the production environment.
  • Carbon contamination is normally a mixture of different chemical states of carbon (hydrocarbon, alcohol or ether, and ester or acid).
  • Hydrocarbon is the dominant form of carbon contamination. It is normally 2-4x larger than the other chemical states of carbon.
  • Carbonate peaks, if they appear, normally appear ~4.5 eV above the hydrocarbon C (1s) peak max BE.
  • Low levels of carbonate is common on many s that readily oxidize in the air.
  • High levels of carbonate appear on reactive oxides and various hydroxides.  This is due to reaction between the oxide and CO2 in the air.
  • Hydroxide contamination peak is due to the reaction with residual water in the lab air or the vacuum.
  • The O (1s) BE of the hydroxide (water) contamination normally appears 0.5 to 1.0 eV above the oxide peak
  • Sodium (Na), Potassium (K), Sulfur (S) and Chlorine (Cl) are common trace to low level contaminants
  • To find low level contaminants it is very useful to vertically expand the 0-600 eV region of the survey spectrum by 5-10X
  • A tiny peak that has 3 or more adjacent data-points above the average noise of the background is considerate to be a real peak
  • Carbides can appear after ion etching various reactive s.  Carbides form due to the residual CO and CH4 in the vacuum.
  • Ion etching can produce low oxidation states of the material being analyzed.  These are newly formed contaminants.
  • Ion etching polymers by using standard Ar+ ion guns will destroy the polymer, converting it into a graphitic type of carbon

 Periodic Table 


 

Data Collection Guidance

 

  • Chemical state differentiation can be difficult
  • Collect principal Tb (4d) peak as well as Tb (3d).
  • Long time exposures (high dose) to X-rays can degrade various polymers, catalysts, high oxidation state compounds
  • During XPS analysis, water or solvents can be lost due to high vacuum or irradiation with X-rays or Electron flood gun
  • Auger signals can sometimes be used to discern chemical state shifts when XPS shifts are very small

 Periodic Table 


 

Data Collection Settings for Terbium (Tb)

 

  • Conductivity:  Metal readily develops a native oxide that is sensitive to Flood Gun – Differential Charging Possible – float sample recommended
  • Primary Peak (XPS Signal) used to measure Chemical State Spectra:  Tb (4d5/2) at 146 eV
  • Recommended Pass Energy for Measuring Chemical State Spectrum: 40-60 eV    (Produces Ag (3d5/2) FWHM ~0.7 eV)
  • Recommended # of Scans for Measuring Chemical State Spectrum:  4-5 scans normally   (Use 10-25 scans to improve S/N)
  • Dwell Time:  50 msec/point
  • Step Size:  0.1 eV/point   (0.1 eV/step or 0.1 eV/channel)
  • Standard BE Range for Measuring Chemical State Spectrum:  140- 170 eV
  • Recommended Extended BE Range for Measuring Chemical State Spectrum:  120 -220eV
  • Recommended BE Range for Survey Spectrum:  -10 to 1,100 eV   (above 1,100 eV there are no useful XPS signals, except for Ge, As and Ga, above 1100 is waste of time)
  • Typical Time for Survey Spectrum:  3-5 minutes for newer instruments, 5-10 minutes for older instruments
  • Typical Time for a single Chemical State Spectrum with high S/N:  5-10 minutes for newer instruments, 10-15 minutes for older instruments 

 Periodic Table 


 

Effects of Argon Ion Etching

  • Carbides appear after ion etching Tb and various reactive surfaces.  Carbides form due to the presence of residual CO and CH4 in the vacuum.
  • Ion etching can produce low oxidation states of the material being analyzed.  These are newly formed contaminants.
  • Ion etching polymers by using standard Ar+ ion guns will destroy the polymer, converting it into a graphitic type of carbon

 

 Periodic Table 

Copyright ©:  The XPS Library 


Gas Phase XPS or UPS Spectra


 

Chemical State Spectra from Literature
from Thermo website



End of File