Sbo Sb2O3 Sb2O5 Sb2S3 Sb2(SO4)3 Sb2Te3 SbF3 InSb GaSb Sb2Te3 (as recd)   Basic 

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


Antimony (Sb)

Stibium

Valentinite – Sb2O3 Metal – Sbo Stibnite – Sb2S3

 

  Page Index
  • Expert Knowledge & Explanations


Antimony (Sbo) Metal

Peak-fits, BEs, FWHMs, and Peak Labels

 

Antimony (Sbo) Metal
Sb (3d) Spectrum – raw spectrum		 Antimony (Sbo) Metal
Peak-fit of Sb (3d) Spectrum (w/o asymm)
→  Periodic Table 
Antimony (Sbo) Metal
Sb (3d) Spectrum – extended range 
 Antimony (Sbo) Metal
Peak-fit of Sb (3) Spectrum (w asymm)
   

 

Survey Spectrum of Antimony (Sbo) Metal
with Peaks Integrated, Assigned and Labelled

→  Periodic Table 

XPS Signals for Antimony, (Sbo) 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
  Sb (3s) 944 3.36 14.3
  Sb (3p1/2) 813 4.76 17.5
  Sb (3p3/2) 766 9.77 17.5
  Sb (3d3/2) 537.41 11.35 21.6
O (1s) overlaps Sb (3d5/2) 528.13 16.39 21.6
Si (2s) overlaps Sb (4s) 153 0.848 27.9
Si (2p) & Hg (4f) overlaps Sb (4p) 99 2.88 28.8
F (2s) overlaps Sb (4d) 32 3.14  

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

Plasmon Peaks

Energy Loss Peaks

Auger Peaks

Energy Loss    Intrinsic Plasmon Peak:  ~xx eV above peak max
Expected Bandgap for Sb2O3: 3.2 – 3.7 eV   (https://www.2dsemiconductors.com/Sb2O3-a/)
Work Function for Sb:  xx eV

*Scofield Cross-Section (σ) for C (1s) = 1.0

→  Periodic Table 

 

Valence Band Spectrum from Antimony, Sbo Metal
 Fresh exposed bulk produced by extensive Ar+ ion etching

 

 

Plasmon Peaks from Sbo Metal
 Fresh exposed bulk produced by extensive Ar+ ion etching

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

 

Sb (LMM) Auger Peaks from Sbo Metal
 Fresh exposed bulk produced by extensive Ar+ ion etching
Sbo Metal – main Auger peak Sbo Metal – full Auger range
 

Features Observed

  • xx
  • xx
  • xx

→  Periodic Table 

 

Evidence for Breakdown in One-Electron Orbital Concept
in Elements Z=46 (Palladium) to Z= 59 (Praseodymium)

Rhodium (4s) and (4p) Peakshapes Antimony (4s) and (4p) Peakshapes Praseodymium (4s) and (4p) Peakshapes

Reference:
G. Wendin, Breakdown of One-Electron Pictures in Photoelectron Spectra, Structure and Bonding Series #45, Springer-Verlag, New York, 1981

 

 

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 Sbo

can form when Argon Ions are used
to removed surface contamination
   

 

Side-by-Side Comparison of
Sb Native Oxide & Antimony Pentoxide (Sb2O5)
Peak-fits, BEs, FWHMs, and Peak Labels

Sb (3d) from Sb Native Oxide
Flood Gun OFF
As-Measured, C (1s) at 285.0 eV
Sb (3d) from Sb2O5 – pressed pellet
Flood Gun ON
Charge Referenced to C (1s) at 285.0 eV

→  Periodic Table 
C (1s) from Sb Native Oxide
on Metal
As-Measured, C (1s) at 285.0 eV (Flood Gun OFF)

C (1s) from Sb2O5 – pressed pellet
Flood Gun ON
Charge Referenced to C (1s) at 285.0 eV

→  Periodic Table 
O (1s) from Sb Native Oxide
As-Measured, C (1s) at 285.0 eV
Flood Gun OFF

O (1s) from Sb2O5 – pressed pellet
Flood Gun ON
Charge Referenced to C (1s) at 285.0 eV
→  Periodic Table

 
 

 

Survey Spectrum of Antimony (Sb) Native Oxide
with Peaks Integrated, Assigned and Labelled

 

→  Periodic Table 

 

 

Survey Spectrum of Antimony Pentoxide, Sb2O5
with Peaks Integrated, Assigned and Labelled

→  Periodic Table  

 

Overlays of Sb (3d) Spectra for
Sbo metal, Sb Native Oxide and Sb2O5

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

 Overlay of Sbo metal and Sb Native Oxide – Sb (3d)
Native Oxide C (1s) = 285.0 eV (Flood gun OFF)

  Overlay of Sbo metal and Sb2O5 – Sb (3d)
Pure Oxide C (1s) = 285.0 eV
Chemical Shift: 3.1 eV
→  Periodic Table  Copyright ©:  The XPS Library 

 

Overlay of Sb (3d)
Sbo Metal, Sb Native Oxide, & Sb2O5

Features Observed

  • xx
  • xx
  • xx

→  Periodic Table 

 

Valence Band Spectra
Sbo, Sb2O5 

Sbo
Ion etched clean		 Sb2O5 – pressed pellet
Flood gun is ON,  Charge referenced so C (1s) = 285.0 eV

Overlay of Valence Band Spectra
for Sbo metal and Sb2O5

Features Observed

  • xx
  • xx
  • xx

→  Periodic Table 

 

Antimony Minerals, Gemstones, and Chemical Compounds

 
Willyamite – CoSbS Kermesite – Sb2S2O Getchellite – AsSbS3 Chalcostibite – CuSbS2

→  Periodic Table 

 

 

Six (6) Chemical State Tables of Sb (3d5/2) 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

Sb (3d5/2) 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
Sb 51 GaSb 527.8 eV 528.2 eV 285.0 eV The XPS Library
Sb 51 InSb 527.9 eV 528.0 eV 285.0 eV The XPS Library
Sb 51 InSb (N*1) 528.0 eV   284.8 eV Avg BE – NIST
Sb 51 Sb (N*8) 528.0 eV 528.3 eV 284.8 eV Avg BE – NIST
Sb 51 Sb – element 528.2 eV   285.0 eV The XPS Library
Sb 51 SbTe 528.8 eV 529.0 eV 285.0 eV The XPS Library
Sb 51 Sb-2S3 (N*6) 529.5 eV 530.0 eV 284.8 eV Avg BE – NIST
Sb 51 Sb2O3 (N*2) 529.9 eV 530.0 eV 284.8 eV Avg BE – NIST
Sb 51 Sb-2O3 530.3 eV 530.6 eV 285.0 eV The XPS Library
Sb 51 Sb-I3 (N*1) 530.4 eV   285.0 eV The XPS Library
Sb 51 CsSbF4 (N*1) 530.8 eV   284.8 eV Avg BE – NIST
Sb 51 Sb-2O5 (N*1) 530.8 eV   284.8 eV Avg BE – NIST
Sb 51 Sb-Cl5 (N*1) 530.9 eV   284.8 eV Avg BE – NIST
Sb 51 Sb-F3 (N*1) 531.7 eV   284.8 eV Avg BE – NIST
Sb 51 KSbF6 (N*2) 532.3 eV 532.9 eV 284.8 eV Avg BE – NIST
Sb 51 Sb-(OH)3     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

Sb (3d5/2) Chemical State BEs from:  “PHI Handbook”

C (1s) BE = 284.8 eV

→  Periodic Table 

Copyright ©:  Ulvac-PHI

Table #3

Sb (3d5/2) Chemical State BEs from:  “Thermo-Scientific” Website

C (1s) BE = 284.8 eV

Chemical state Binding energy (eV), Sb (3d5/2)
Sb metal 528.3
Sb2O3 529.9 eV
Sb2O5 530.9
SbF3 531.7

→  Periodic Table 

Copyright ©:  Thermo Scientific 

Table #4

Sb (3d5/2) 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

→  Periodic Table 

Copyright ©:  Mark Beisinger

Table #5

Sb (3d5/2) 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
Sb 3d5/2 Sb 528.1 ±0.3 527.8 ～ 528.3
Sb 3d5/2 Bu3Sb 528.1 ±0.3 527.8 ～ 528.3
Sb 3d5/2 AlSb 528.7 ±0.2 528.5 ～ 528.9
Sb 3d5/2 Ph3Sb 529.0 ±0.3 528.7 ～ 529.2
Sb 3d5/2 Sulfides 529.3 ±0.2 529.1 ～ 529.5
Sb 3d5/2 Sb2O3 530.0 ±0.3 529.7 ～ 530.3
Sb 3d5/2 CsSbF4 530.6 ±0.3 530.3 ～ 530.8
Sb 3d5/2 Sb2O5 530.8 ±0.3 530.5 ～ 531.0
Sb 3d5/2 Halides 531.1 ±0.7 530.4 ～ 531.7
Sb 3d5/2 NaSbF6 532.1 ±0.3 531.8 ～ 532.3
Sb 3d5/2 KSbF6 532.6 ±0.3 532.3 ～ 532.9

 

→  Periodic Table 

 

Histograms of NIST BEs for Sb (3d5/2) BEs

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

Histogram indicates:  528.0 eV for Sbo based on 9 literature BEs Histogram indicates:  529.5 eV for Sb2S3 based on 6 literature BEs
Sulfur is an Oxygen analog and shows similar BE shifts to Oxygen

Table #6


NIST Database of Sb (3d5/2) 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
Sb 3d5/2 Sb 526.30  Click
Sb 3d5/2 LaSb 527.10  Click
Sb 3d5/2 CeSb 527.20  Click
Sb 3d5/2 InSb 527.97  Click
Sb 3d5/2 InSb 528.00  Click
Sb 3d5/2 Sb 528.00  Click
Sb 3d5/2 Sb95Sn5 528.00  Click
Sb 3d5/2 Sb 528.02  Click
Sb 3d5/2 [Sb(C4H9)3] 528.10  Click
Sb 3d5/2 Sb 528.17  Click
Sb 3d5/2 Sb 528.20  Click
Sb 3d5/2 Sb 528.20  Click
Sb 3d5/2 Sb 528.20  Click
Sb 3d5/2 InSb 528.20  Click
Sb 3d5/2 Sb 528.21  Click
Sb 3d5/2 Sb 528.25  Click
Sb 3d5/2 Sb 528.30  Click
Sb 3d5/2 As15In54Sb31 528.30  Click
Sb 3d5/2 Sb2S3 528.50  Click
Sb 3d5/2 AlSb 528.60  Click
Sb 3d5/2 Sb 528.60  Click
Sb 3d5/2 [SbS(C6H5)3] 528.70  Click
Sb 3d5/2 [Sb(C6H5)3] 528.90  Click
Sb 3d5/2 Sb2S5 529.20  Click
Sb 3d5/2 Cs3Sb2I9 529.20  Click
Sb 3d5/2 Cs3Sb2Cl9 529.30  Click
Sb 3d5/2 Sb2S5 529.30  Click
Sb 3d5/2 Sb2S3 529.50  Click
Sb 3d5/2 Sb2S3 529.50  Click
Sb 3d5/2 [NH3(C4H9)][SbI4] 529.60  Click
Sb 3d5/2 InSbOx 529.60  Click
Sb 3d5/2 Sb2S3 529.70  Click
Sb 3d5/2 [SbBr2(C6H5)3] 529.80  Click
Sb 3d5/2 [Sb(SC12H25)3] 529.80  Click
Sb 3d5/2 Sb2S3 529.80  Click
Sb 3d5/2 Rb3Sb2Br9 529.90  Click
Sb 3d5/2 [NH3(C4H9)][Sb2Cl9] 529.90  Click
Sb 3d5/2 Sb2O3 529.90  Click
Sb 3d5/2 Rb3Sb2I9 529.90  Click
Sb 3d5/2 [MnBr(CO)4(Sb(C6H5)3)] 530.00  Click
Sb 3d5/2 Cs3Sb2Br9 530.00  Click
Sb 3d5/2 [Sb(S2CN(C5H11)2)3] 530.00  Click
Sb 3d5/2 Sb2O3 530.00  Click
Sb 3d5/2 Sb2S3 530.00  Click
Sb 3d5/2 Cs3Sb2Br9 530.10  Click
Sb 3d5/2 Co(NH3)6SbBr6 530.10  Click
Sb 3d5/2 [SbBr2(CH3)3] 530.30  Click
Sb 3d5/2 BiSbO4 530.40  Click
Sb 3d5/2 SbI3 530.40  Click
Sb 3d5/2 [Sb(S2P(OC4H9)2)3] 530.50  Click
Sb 3d5/2 Cs3Sb2Cl9 530.50  Click
Sb 3d5/2 Sb2O3 530.50  Click
Sb 3d5/2 CsSbF4 530.80  Click
Sb 3d5/2 [Co(NH3)6]SbCl6 530.80  Click
Sb 3d5/2 Sb2O5 530.80  Click
Sb 3d5/2 SbCl5 530.90  Click
Sb 3d5/2 Cs[SbCl6] 530.90  Click
Sb 3d5/2 K2SbF5 531.00  Click
Sb 3d5/2 K3Sb3As2O14.5H2O 531.10  Click
Sb 3d5/2 KSb2F7 531.20  Click
Sb 3d5/2 Na2SbF5 531.30  Click
Sb 3d5/2 K3Sb3P2O14.5H2O 531.40  Click
Sb 3d5/2 SbF3 531.70  Click
Sb 3d5/2 [SbCl6(P(C6H5)4)] 531.70  Click
Sb 3d5/2 NaSbF6 532.10  Click
Sb 3d5/2 Sb2O5 532.10  Click
Sb 3d5/2 [SbCl5(OP(C6H5)3)] 532.20  Click
Sb 3d5/2 KSbF6 532.30  Click
Sb 3d5/2 [N(C2H5)4][SbF6] 532.40  Click
Sb 3d5/2 KSbF6 532.90  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 Antimony Materials

 

 

Expert Knowledge Explanations

→  Periodic Table 

 

 

Antimony Chemical Compounds


Peak-fits and Overlays of Chemical State Spectra

Pure Antimony, Sbo:  Sb (3d)
Cu (2p3/2) BE = 932.6 eV		 Sb2O5:  Sb (3d)
C (1s) BE = 285.0 eV		 SbF3:  Sb (3d)
C (1s) BE = 285.0 eV

Features Observed

  • xx
  • xx
  • xx

→  Periodic Table 

 

Overlay of Sb (3d) Spectra shown Above

C (1s) BE = 285.0 eV

 

Chemical Shift between Sb and Sb2O5:  2.9 eV
 Chemical Shift between Sb and SbF3:  4.6 eV

 

→  Periodic Table 

 

Antimony Pentoxide, Sb2O5
pressed pellet

Survey Spectrum from Sb2O5
Flood gun is ON, C (1s) BE = 285.0 eV
 Sb (3d) Chemical State Spectrum from Sb2O5
Flood gun is ON, C (1s) BE = 285.0 eV
  . 
O (1s) Chemical State Spectrum from Sb2O5
Flood gun is ON, C (1s) BE = 285.0 eV
 C (1s) Chemical State Spectrum from Sb2O5
Flood gun is ON, C (1s) BE = 285.0 eV
  . 

Valence Band Spectrum from Sb2O5
Flood gun is ON, C (1s) BE = 285.0 eV
  
 


Shake-up Features for Sb2O5

   
   

 

 

Multiplet Splitting Features for Metal Compounds

Sb metal – NO Splitting for Sb (4s) SbO  – Multiplet Splitting Peaks for Sb (4s)
   

 

 

Features Observed

  • xx
  • xx
  • xx

→  Periodic Table 

 

 

Antimony Chemical Compounds

 

Antimony Fluoride, SbF3

Survey Spectrum Sb (3d) Spectrum
  . 
F (1s) Spectrum C (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 Antimony – Sb2O5

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

 

 

XPS Study of UHV Gas Captured by Freshly Ion Etched Antimony
 
Reveals Chemical Shifts and Chemical States that Develop from Highly Reactive Pure Sbo

Surface was strongly Ar+ ion etched to remove all contaminants, and
then allowed to react overnight with the UHV Gases – CO, H2, H2O, O2 & CH4
that normally reside inside on the walls of the chamber, on the sample stage,
and on the nearby un-etched surface a total of 10-14 hours.  UHV pump was a Cryopump.
Initial spectra are at the front.  Final spectra are at the rear. Flood gun is OFF.
 
 
 
 
Sb (3d) Signal
  O (1s) Signal C (1s) Signal

     
Copyright ©:  The XPS Library
 

 

Antimony Alloys

 

Copyright ©:  The XPS Library 

 

 

XPS Facts, Guidance & Information

→  Periodic Table 

    Element   Antimony (Sb)
  
    Primary XPS peak used for Peak-fitting:   Sb (3d5/2)  
    Spin-Orbit (S-O) splitting for Primary Peak:   Spin-Orbit splitting for “d” Orbital, ΔBE = 9.2 eV
  
    Binding Energy (BE) of Primary XPS Signal:   531 eV
  
    Scofield Cross-Section (σ) Value:   Sb (3d5/2) = 16.39.     Sb (3d3/2) = 11.35
  
    Conductivity:   Sb resistivity =  
Native Oxide suffers Differential Charing		  
    Range of Sb (3d5/2) Chemical State BEs:   530 – 534 eV range   (Sbo to SbF3)  
    Signals from other elements that overlap
Sb (3d5/2) Primary Peak:		   O (1s)  
    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 Sb (3d5/2)

  • FWHM (eV) of Sb (3d5/2) for Pure Sbo :  ~0.8 eV using 25 eV Pass Energy after ion etching:
  • FWHM (eV) of Sb (3d5/2) for Sb2O5:  ~1.6 eV using 50 eV Pass Energy  (before ion etching)
  • Binding Energy (BE) of Primary Signal used for Measuring Chemical State Spectra:  530 eV for Sb (3d5/2) with +/- 0.2 uncertainty
  • List of XPS Peaks that can Overlap Peak-fit results for Sb (3d5/2):  O (1s)

→  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 Antimony

  • Antimony develops a thick native oxide due to the reactive nature of clean Antimony .
  • The native oxide of Sb Ox is 8-9 nm thick.
  • Antimony thin films often have a low level of iron (Fe) in the bulk as a contaminant or to strengthen the thin film
  • Antimony 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 Sb (3d) peak.
  • 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 Metal (Sb)

  • 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:  Sb (3d5/2) at 530 eV
  • Recommended Pass Energy for Measuring Chemical State Spectrum:  40-50 eV    (Produces Ag (4f7/2) 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:  520 – 550 eV
  • Recommended Extended BE Range for Measuring Chemical State Spectrum:  510 – 610 eV
  • Recommended BE Range for Survey Spectrum:  -10 to 1,100 eV   (above 1,100 eV there are no useful XPS signals, except for Ge and Ga)
  • 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 Sb 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
 
 
 

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