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An Introduction to Surface Analysis by XPS and AES, 2nd Edition

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An Introduction to Surface Analysis by XPS and AES, 2nd Edition

John F. Watts, John Wolstenholme

ISBN: 978-1-119-41758-3 November 2019 280 Pages

Description

Provides a concise yet comprehensive introduction to XPS and AES techniques in surface analysis

This accessible second edition of the bestselling book, An Introduction to Surface Analysis by XPS and AES, 2nd Edition explores the basic principles and applications of X-ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES) techniques. It starts with an examination of the basic concepts of electron spectroscopy and electron spectrometer design, followed by a qualitative and quantitative interpretation of the electron spectrum. 

Chapters examine recent innovations in instrument design and key applications in metallurgy, biomaterials, and electronics. Practical and concise, it includes compositional depth profiling; multi-technique analysis; and everything about samples—including their handling, preparation, stability, and more. Topics discussed in more depth include peak fitting, energy loss background analysis, multi-technique analysis, and multi-technique profiling. The book finishes with chapters on applications of electron spectroscopy in materials science and the comparison of XPS and AES with other analytical techniques.

  • Extensively revised and updated with new material on NAPXPS, twin anode monochromators, gas cluster ion sources, valence band spectra, hydrogen detection, and quantification
  • Explores key spectroscopic techniques in surface analysis
  • Provides descriptions of latest instruments and techniques
  • Includes a detailed glossary of key surface analysis terms
  • Features an extensive bibliography of key references and additional reading
  • Uses a non-theoretical style to appeal to industrial surface analysis sectors

An Introduction to Surface Analysis by XPS and AES, 2nd Edition is an excellent introductory text for undergraduates, first-year postgraduates, and industrial users of XPS and AES.

Preface to First Edition 4

Preface to Second Edition 5

Acknowledgements 7

1 Electron Spectroscopy: Some Basic Concepts 8

1.1 Analysis of Surfaces 8

1.2 Notation 9

1.2.1 Spectroscopists’ Notation 9

1.2.2 X-Ray Notation 10

1.3 X-Ray Photoelectron Spectroscopy (XPS) 11

1.4 Auger Electron Spectroscopy 14

1.5 Scanning Auger Microscopy (Sam) 17

1.6 The Depth of Analysis in Electron Spectroscopy 18

1.7 Comparison of XPS and AES/SAM 21

1.8 The Availability of Surface Analytical Equipment 22

2 Electron Spectrometer Design 24

2.1 The Vacuum System 24

2.2 X-Ray Sources for XPS 26

2.2.1 Choice of X-Ray Anode 27

2.2.2 X-Ray Monochromators 31

2.2.3 Synchrotron Sources 34

2.3 The Electron Gun for AES 34

2.3.1 Electron Sources 35

2.3.2 The Electron Column 38

2.3.3 Spot Size 39

2.4 Analysers for Electron Spectroscopy 40

2.4.1 The Cylindrical Mirror Analyser 41

2.4.2 The Hemispherical Sector Analyser 43

2.4.3 Calibration of the Electron Spectrometer Energy Scale 49

2.5 Near Ambient Pressure XPS 50

2.6 Detectors 52

2.6.1 Channel Electron Multipliers 52

2.6.2 Microchannel Plates 54

2.6.3 Two-Dimensional Detectors 54

2.7 Small Area XPS 55

2.7.1 Lens-Defined Small Area XPS 56

2.7.2 Source Defined Small Area Analysis 56

2.8 XPS Imaging and Mapping 57

2.8.1 Serial Acquisition 57

2.8.2 Parallel Acquisition 58

2.9 Angle Resolved XPS 62

2.10 Automation 64

3 The Electron Spectrum: Qualitative and Quantitative interpretation 66

3.1 Qualitative Analysis 66

3.1.1 Unwanted Features in Electron Spectra 68

3.1.2 Data Acquisition 68

3.2 Chemical State information 70

3.2.1 X-Ray Photoelectron Spectroscopy 70

3.2.2 Peak Fitting of XPS Spectra 73

3.2.3 Auger Electron Spectroscopy 77

3.2.4 X-AES 77

3.2.5 Chemical State Plots 79

3.2.6 Shakeup Satellites 80

3.2.7 Multiplet Splitting 81

3.2.8 Plasmons 82

3.3 Quantitative Analysis 82

3.3.1 Quantification in XPS 83

3.3.2 Quantification in AES 87

4 Compositional Depth Profiling 90

4.1 Non-Destructive Depth Methods 90

4.1.1 Measurements at a Single Emission Angle 90

4.1.2 Angle Resolved XPS Measurements 91

4.1.3 Measurement of Overlayer Thickness Using ARXPS 94

4.1.4 Elastic Scattering 96

4.1.5 Multilayer Thickness Calculations Using ARXPS 96

4.1.6 Compositional Depth Profiles from ARXPS Measurements 99

4.1.7 Variation of Analysis Depth with Electron Kinetic Energy 102

4.1.8 Background Analysis 103

4.2 Depth Profiling By Sputtering with Energetic Ions 106

4.2.1 The Sputtering Process 106

4.2.2 Experimental Method 106

4.2.3 The Nature of the Ion Beam 108

4.2.4 Sputter Yield and Etch Rate 111

4.2.5 Factors Affecting the Etch Rate 112

4.2.6 Factors Affecting the Depth Resolution 113

4.2.7 Calibration 116

4.2.8 Ion Gun Design 116

4.3 Sectioning 118

4.3.1 Fib Sectioning 118

4.3.2 Angle Lapping 119

4.3.3 Ball Cratering 120

5 Multi-Technique Analysis 121

5.1 UV Photoelectron Spectroscopy (Ups) 121

5.2 Low Energy Ion Scattering Spectroscopy (LEISS) 122

5.3 Reflection Electron Energy Loss Spectroscopy (REELS) 124

5.3.1 Elastic Scattering 124

5.3.2 Inelastic Scattering 126

5.4 Work Function Measurements 127

5.5 Energy Dispersive X-Ray Analysis 128

6 The Sample 130

6.1 Sample Handling 130

6.2 Sample Preparation 132

6.3 Sample Mounting 134

6.4 Sample Stability 134

6.5 Contamination and Damage During Analysis 135

6.6 Controlling Sample Charging 136

6.6.1 Sample Charging in XPS 137

6.6.2 Sample Charging in AES 138

7 Applications of Electron Spectroscopy in Materials Science 140

7.1 Introduction 140

7.2 Metallurgy 140

7.2.1 Grain Boundary Segregation 140

7.2.2 Electronic Structure of Metallic Alloys 143

7.2.3 Surface Engineering 145

7.3 Corrosion Science 150

7.4 Ceramics 157

7.5 Microelectronics and Semiconductor Materials 162

7.5.1 Mapping Semiconductor Devices Using AES 163

7.5.2 XPS Failure Analysis of Microelectronic Devices 166

7.5.3 Depth Profiling of Semiconductor Materials 168

7.6 Polymeric Materials 172

7.7 Adhesion Science 179

7.8 Nano-Technology 186

7.9 Biology 190

7.10 Energy 193

8 Comparison of XPS and AES with Other Analytical Techniques 197

Glossary 201

Bibliography 210

Documentary Standards in Surface Analysis 217

The Scope of TC201 217

The Purpose of TC201 217

International Standards Relevant To Electron Spectroscopies 217

Appendix 1 220

Auger Electron Energies 220

Appendix 2 221

Table of Binding Energies Accessible with Alka Radiation. 221

Index 225