X-Ray Photoelectron Spectroscopy (XPS) Prof. Paul K. Chu

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1 X-Ray Photoelectron Spectroscopy (XPS) Prof. Paul K. Chu

2 X-ray Photoelectron Spectroscopy Introduction Qualitative analysis Quantitative analysis Charging compensation Small area analysis and XPS imaging Instrumentation Depth profiling Application examples

3 Photoelectric Effect Einstein, Nobel Prize 1921 Photoemission as an analytical tool Kai Siegbahn, Nobel Prize 1981

4

5 XPS is a widely used surface analysis technique because of its relative simplicity in use and data interpretation.

6 KE = hn - BE - F SPECT BE = hn - KE - F SPECT hu: Al K a (1486.6eV) P 2s P 2p 1/2-3/2 Kinetic Energy

7 Peak Notations L-S Coupling ( j = l s ) e - s= 1 2 s= 1 2 j = l j = l 1 2

8 For p, d and f peaks, two peaks are observed. The separation between the two peaks are named spin orbital splitting. The values of spin orbital splitting of a core level of an element in different compounds are nearly the same. Au The peak area ratios of a core level of an element in different compounds are also nearly the same. Spin orbital splitting and peak area ratios assist in elemental identification

9 General methods in assisting peak identification (1) Check peak positions and relative peak intensities of 2 or more peaks (photoemission lines and Auger lines) of an element (1) Check spin orbital splitting and area ratios for p, d, f peaks A marine sediment sample from Victoria Harbor Si 2s Si 2p Al 2s Al 2p The following elements are found: O, C, Cl, Si, F, N, S, Al, Na, Fe, K, Cu, Mn, Ca, Cr, Ni, Sn, Zn, Ti, Pb, V

10 Analysis Depth Inelastic mean free path ( ) is the mean distance that an electron travels without energy loss For XPS, is in the range of 0.5 to 3.5 nm 3 0 x - Only the photoelectrons in the near surface region can escape the sample surface with identifiable energy Measures top 3 or 5-10 nm 0 e e x - 1- e 1 dx dx

11 B.E. = Energy of Final state - Energy of initial state (one additional +ve charge) B A + B Redistribution of electron density B A B B.E. provides information on chemical environment

12 Example of Chemical Shift

13 Example of Chemical Shift

14 Chemical Shifts

15 Chemical Shifts

16 Factors Affecting Photoelectron Intensities For a homogenous sample, the measured photoelectron intensity is given by I i, c f N i i, c cos F T D A I i,c : Photoelectron intensity for core level c of element i f: X-ray flux in photons per unit area per unit time N i : Number of atoms of element i per unit volume d i,c : Photoelectric cross-section for core level c of element i : Inelastic mean free path of the photoelectron in the sample matrix : Angle between the direction of photoelectron electron and the sample normal F: Analyzer solid angle of acceptance T: Analyzer transmission function D: Detector efficiency A: Area of sample from which photoelectrons are detected Detector

17 Quantitative Analysis Peak Area of element A Atomic I A SA % 100% I i i S i Sensitivity factor of element A Peak Areas / Sensitivity factors of all other elements Peak Area measurement Need background subtraction Au 4f

18 Empirical Approach k = constant S = sensitivity factor of a core level of element A M = No. of A in the empirical formula A A A A A M I k S A F F A A F F A A F A M M I I S M S M S I I For example, Teflon (-CF 2 -) 1 2 F C C I I S Usually assume S F =1

19 Examples of Sensitivity Factors 1s Li 2 CO 3 C 1s Li 2 SO 4 S 2p KBF 4 K 2p NH 4 BF 4 N 1s Na 2 SO 3 S 2p 2.95 CuSO 4 S 2p 3.25 K 2 SO 4 S 2p Ag(COCF 3 ) 3 F 1s Na 5 P 3 O 10 Na 2s 3.40 C 6 H 2 NS 2 K 3 O 9 K 2p S 1 N A S Ai N i 1 N = number of compounds tested

20 X-ray damage Some samples can be damaged by x-rays For sensitive samples, repeat the measurement to check for x-ray damage.

21 Charging Compensation Electron loss and compensation For metal or other conducting samples that grounded to the spectrometer e- e - X-ray e- e - e - sample Electrons move to the surface continuously to compensate the electron loss at the surface region.

22 For resistive samples "current" net loss of electrons from the surface e - V R I Potential developed at the surface Resistance between the surface and the ground I 10nA 10nA 10nA R 1k 1M 1000M V 10-5 V 0.01V 10V Not important Important for accurate B.E. measurements Note: for conducting samples, charging may also occur if there is a high resistance at the back contact.

23 Differential (non-uniform) surface charging Broadeningofpeak Sample

24 Charge Compensation Techniques Low Energy Electron Flood Gun filament ~2eV-20eV Electrons optics e -

25 Electron source with magnetic field Low energy electrons and Ar + filament e analyser -ve X-ray electrons + Low energy Ar beam Low energy electron beam Sample Sample Magnet A single setting for all types of samples

26 Shift in B.E. of a polymer surface

27 Effects of Surface Charging

28 Small area analysis and XPS Imaging Photoelectrons Aperture of Analyzer lens Photoelectrons Aperture of Analyzer lens X-ray Sample X-ray Sample Spot size determined by the analyser Both monochromated and dual anode x-ray sources can be used Spot size determined by the x-ray beam

29 Instrumentation Electron energy analyzer X-ray source Ar ion gun Neutralizer Vacuum system Electronic controls Computer system Ultrahigh vacuum < 10-9 Torr (< 10-7 Pa) Detection of electrons Avoid surface reactions/ contamination

30 XPS system suitable for industrial samples

31 Vacuum Chamber Control Electronics Turbopump Ion pump Sample Introduction Chamber

32 Dual Anode X-ray Source

33 Commonly used

34 X-ray monochromator n =2dsin For Al K 8.3Å Advantages of using x-ray monochromator Narrow peak width Reduced background No satellite & ghost peaks use (1010) planes of quartz crystal d = 4.25Å o = 78.5 a

35 Cylindrical Mirror Analyzer CMA: Relatively high signal and good resolution ~ 1 ev

36 Concentric Hemispherical Analyzer (CHA) Resolution < 0.4 ev

37 X-ray induced secondary electron imaging for precise location of the analysis area x-ray secondary electrons x 500mm

38 Peak Area Depth Profiling Ar + Sputtered materials Sputtering Time

39 Peak Area Concentration Depth Scale Calibration 1. Sputtering rate determined from the time required to sputter through a layer of the same material of known thickness 2. After the sputtering analysis, the crater depth is measured using depth profilometry and a constant sputtering rate is assumed Sputtering Time Depth

40 Angle Resolved XPS

41 Plasma Treated Polystyrene Angle-Resolved XPS Analysis High-resolution C 1s spectra

42 Plasma Treated Polystyrene O concentration is higher near the surface (10 degrees take off angle) C is bonded to oxygen in many forms near the surface (10 degrees take off angle) Plasma reactions are confined to the surface

43 Angle-resolved XPS analysis Oxide on silicon nitride surface

44 Typical Applications

45 Silicon Wafer Discoloration

46 Depth Profiling Architectural Glass Coating Architectural glass coating ~100nm thick coating Sputtered crater Sample platen 75 X 75mm

47 Depth profile of Architectural Glass Coating O 1s O 1s O 1s 60 Ti 2p 40 Si 2p Nb 3d Ti 2p N 1s Si 2p 20 N 1s Al 2p 0 0 Surface 200 Sputter Depth (nm)

48 Depth profiling of a multilayer structure Nickel (30.3 nm) Chromium (31.7 nm) Chromium Oxide (31.6 nm) Nickel (29.9 nm) Chromium (30.1 nm) Silicon (substrate) Ni 2p Cr 2p metal Cr 2p oxide Ni 2p Cr 2p metal Si 2p 40 O 1s Sputter Depth (nm) 185

49 Depth Profiling with Sample Rotation Atomic concentration (%) Ni 2p Ni 2p Cr 2p Ni 2p Cr 2p Cr 2p O 1s O 1s Ni 2p Cr 2p Ni 2p Cr 2p Ni 2p Cr 2p Si 2p Si 2p Si 2p Ions: 4 kev Sample still Cr/Si interface width (80/20%) = 23.5nm Ions: 4 kev With Zalar rotation Cr/Si interface width (80/20%) = 11.5nm Ions: 500 ev With Zalar rotation Sample High energy ions Sample rotates High energy ions Low energy ions 40 O 1s Sputtering depth (nm) 185 Sample rotates Cr/Si interface width (80/20%) = 8.5nm

50 Multi-layered Drug Package Optical photograph of encapsulated drug tablets SPS Photograph Cross-section of Drug Package Al foil Polymer Coating A Polymer Coating B Adhesion layer at interface? 100 X 100mm 1072 X 812µm

51 -Si 2p -Si 2s Polymer coating A Photograph of cross-section 10µm x-ray beam 30 minutes Al foil Binding Energy (ev) Polymer A / Al foil Interface 10µm x-ray beam 30 minutes 0 10µm x-ray beam 30 minutes 1072 X 812µm Polymer coating B 1000 Binding Energy (ev) Binding Energy (ev) 0

52 10µm x-ray beam 11.7eV pass energy 30 minutes Polymer coating A C 1s Photograph (1072 X 812um) Al foil C H O=C-O CCl Interface Binding Energy (ev) 278 Polymer coating B Atomic Concentration (%) Area C O N Si A Interface B A silicon (Si) rich layer is present at the interface µm x-ray beam 11.7eV pass energy 30 minutes O=C-O CH CNO 288 Binding Energy (ev) C 1s 278

53 XPS study of paint Paint Cross Section Polyethylene Substrate Mapping Area Adhesion Layer Base Coat Clear Coat 695 x 320µm 1072 x 812mm

54 Elemental ESCA Maps using C 1s, O 1s, Cl 2p, and Si 2p signals C O Cl Si 695 x 320mm

55 C 1s Chemical State Maps C 1s CH CHCl O=C-O 695 x 320mm

56 Small Area Spectroscopy High resolution C 1s spectra from each layer Polyethylene Substrate CH n Polyethylene Substrate Base Coat CH n Adhesion Layer CN C-O O-C=O Adhesion Layer CH n Base Coat Clear Coat CH n CHCl Clear Coat O-C=O C-O CN 300 Binding Energy (ev) x 500µm 300 Binding Energy (ev) 280

57 Atomic Concentration* (%) Analysis Area C O N Cl Si Al Substrate Adhesion Layer Base Coat Clear Coat *excluding H Quantitative Analysis

58 Summary of XPS Capabilities Elemental analysis Chemical state information Quantification (sensitivity about 0.1 atomic %) Small area analysis (5 mm spatial resolution) Chemical mapping Depth profiling Ultrathin layer thickness Suitable for insulating samples

59 Sample Tutorial Questions What is the mechanism of XPS? What are chemical shifts? How is depth profiling performed? What is angle-resolved XPS? Is XPS a small-area or large-area analytical technique compared to AES? Is XPS suitable for insulators? What kind of applications are most suitable for XPS?

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