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X-ray Photoelectron Spectroscopy: An introduction to Principles and Practices

ISBN: 978-1-118-06253-1
264 pages
December 2011
X-ray Photoelectron Spectroscopy: An introduction to Principles and Practices (1118062531) cover image
This book introduces readers interested in the field of X-ray Photoelectron Spectroscopy (XPS) to the practical concepts in this field. The book first introduces the reader to the language and concepts used in this field and then demonstrates how these concepts are applied. Including how the spectra are produced, factors that can influence the spectra (all initial and final state effects are discussed), how to derive speciation, volume analysed and how one controls this (includes depth profiling), and quantification along with background substraction and curve fitting methodologies.

 

This is presented in a concise yet comprehensive manner and each section is prepared such that they can be read independently of each other, and all equations are presented using the most commonly used units. Greater emphasis has been placed on spectral understanding/interpretation. For completeness sake, a description of commonly used instrumentation is also presented. Finally, some complementary surface analytical techniques and associated concepts are reviewed for comparative purposes in stand-alone appendix sections.

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FOREWORD xi

PREFACE xiii

ACKNOWLEDGMENTS xv

LIST OF CONSTANTS xvii

1 INTRODUCTION 1

1.1 Surface Analysis / 1

1.2 XPS/ESCA for Surface Analysis / 5

1.3 Historical Perspective / 6

1.4 Physical Basis of XPS / 7

1.5 Sensitivity and Specifi city of XPS / 10

1.6 Summary / 11

2 ATOMS, IONS, AND THEIR ELECTRONIC STRUCTURE 13

2.1 Atoms, Ions, and Matter / 13

2.1.1 Atomic Structure / 14

2.1.2 Electronic Structure / 15

2.1.2.1 Quantum Numbers / 16

2.1.2.2 Stationary-State Notation / 18

2.1.2.3 Stationary-State Transition Notation / 20

2.1.2.4 Stationary States / 21

2.1.2.5 Spin Orbit Splitting / 23

2.2 Summary / 25

3 XPS INSTRUMENTATION 27

3.1 Prerequisites of X-ray Photoelectron Spectroscopy (XPS) / 27

3.1.1 Vacuum / 28

3.1.1.1 Vacuum Systems / 32

3.1.2 X-ray Sources / 35

3.1.2.1 Standard Sources / 37

3.1.2.2 Monochromated Sources / 39

3.1.2.3 Gas Discharge Lamps / 41

3.1.2.4 Synchrotron Sources / 41

3.1.3 Electron Sources / 42

3.1.3.1 Thermionic Sources / 42

3.1.4 Ion Sources / 43

3.1.4.1 EI Sources / 43

3.1.5 Energy Analyzers / 44

3.1.5.1 CMA / 46

3.1.5.2 CHA / 46

3.1.5.3 Modes of Operation / 47

3.1.5.4 Energy Resolution / 48

3.1.6 Detectors / 49

3.1.6.1 EMs / 50

3.1.7 Imaging / 52

3.1.7.1 Serial Imaging / 52

3.1.7.2 Parallel Imaging / 54

3.1.7.3 Spatial Resolution / 56

3.2 Summary / 59

4 DATA COLLECTION AND QUANTIFICATION 61

4.1 Analysis Procedures / 61

4.1.1 Sample Handling / 62

4.1.2 Data Collection / 64

4.1.3 Energy Referencing / 65

4.1.4 Charge Compensation / 69

4.1.5 X-ray and Electron-Induced Damage / 71

4.2 Photoelectron Intensities / 72

4.2.1 Photoelectron Cross Sections / 74

4.2.2 The Analyzed Volume / 75

4.2.2.1 Electron Path Lengths / 76

4.2.2.2 Takeoff Angle / 79

4.2.3 The Background Signal / 80

4.2.4 Quantification / 81

4.3 Information as a Function of Depth / 83

4.3.1 Opening up the Third Dimension / 84

4.3.1.1 AR-XPS and Energy-Resolved XPS / 84

4.3.1.2 Sputter Depth Profi ling / 87

4.4 Summary / 97

5 SPECTRAL INTERPRETATION 101

5.1 Speciation / 101

5.1.1 Photoelectron Binding Energies / 102

5.1.1.1 The Z + 1 Approximation / 106

5.1.1.2 Initial State Effects / 107

5.1.1.3 Final State Effects / 118

5.1.1.4 The Auger Parameter / 133

5.1.1.5 Curve Fitting / 135

5.2 Summary / 138

6 SOME CASE STUDIES 141

6.1 Overview / 141

6.1.1 Iodine Impregnation of Single-Walled Carbon Nanotube (SWNT) / 142

6.1.2 Analysis of Group IIA–IV Metal Oxides / 145

6.1.3 Analysis of Mixed Metal Oxides of Interest as SOFC Cathodes / 151

6.1.4 Analysis of YBCO and Related Oxides/Carbonates / 156

6.2 Summary / 163

APPENDICES 167

APPENDIX A PERIODIC TABLE OF THE ELEMENTS 169

APPENDIX B BINDING ENERGIES (B.E.XPS OR B.E.XRF) OF THE ELEMENTS 171

B.1 1s-3s, 2p-3p, and 3d Values / 171

B.2 4s-5s, 4p-5p, and 4d Values / 175

APPENDIX C SOME QUANTUM MECHANICS CALCULATIONS OF INTEREST 177

APPENDIX D SOME STATISTICAL DISTRIBUTIONS OF INTEREST 181

D.1 Gaussian Distribution / 182

D.2 Poisson Distribution / 182

D.3 Lorentzian Distributions / 183

APPENDIX E SOME OPTICAL PROPERTIES OF INTEREST 185

E.1 Chromatic Aberrations / 186

E.2 Spherical Aberrations / 186

E.3 Diffraction Limit / 186

APPENDIX F SOME OTHER SPECTROSCOPIC/SPECTROMETRIC TECHNIQUES OF INTEREST 189

F.1 Photon Spectroscopies / 191

F.1.1 IR, RAIRS, ATR, and DRIFTS / 191

F.1.2 Raman, SERS, and TERS / 192

F.1.3 EDX and WDX / 193

F.1.4 XRF and TXRF / 194

F.2 Electron Spectroscopies / 195

F.2.1 UPS / 195

F.2.2 AES / 195

F.2.3 EELS, REELS, and HREELS / 196

F.3 Ion Spectroscopies/Spectrometries / 196

F.3.1 SIMS / 196

F.3.2 TAP / 197

F.3.3 Ion Scattering Methods / 197

APPENDIX G SOME MICROSCOPIES OF INTEREST 199

G.1 SEM / 200

G.2 HIM / 201

G.3 TEM / 201

G.4 SPM (AFM and STM)-Based Techniques / 202

APPENDIX H SOME REFLECTION/DIFFRACTION TECHNIQUES OF INTEREST 205

H.1 XRD / 206

H.2 GID / 206

H.3 XRR / 207

H.4 LEED / 207

H.5 RHEED / 207

TECHNIQUE ABBREVIATIONS LIST 209

INSTRUMENT-BASED ABBREVIATIONS 213

GLOSSARY OF TERMS 215

QUESTIONS AND ANSWERS 221

XPS VENDORS 229

REFERENCES 233

INDEX 237

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“The book is a useful resource for those interested in the field, and will probably be found to be of particular value by instrumentation support professionals and nonspecialists.”  (Analytical and
Bioanalytical Chemistry
, 14 February 2013)



 


“It is an excellent text and although a competent physicist might already have grasped the principles explained in this book, the multitude of XPS users I come across (PhD chemists, engineers and pharmacists) will find this a breath of fresh air.”  (Chemistry World,  1 September 2012)
 
 
 
 
 
 
 
 
 
 
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