X-Ray Photoelectron Spectroscopy - An Introduction to Principles and Practices

Informationen zum Autor Dr. van der Heide currently serves as the Group Lead of the Surface Analysis department at Samsung Austin, Texas which houses state-of-the-art XPS, AES, SIMS and AFM instrumentation. Former Assistant Professor, Chemistry Department, University of Houston, TX. Klappentext 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. Zusammenfassung 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. Inhaltsverzeichnis Foreword xi Preface xiii Acknowledgments xv List of Constants xvii 1 Introduction 1 1.1 Surface Analysis 1 1.2 XPSESCA for Surface Analysis 5 1.3 Historical Perspective 6 1.4 Physical Basis of XPS 7 1.5 Sensitivity and Specificity 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-Resolv...

List of contents

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
&n

Report

"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)

Product details

• Authors: van der Heide, P van der Heide, Paul Van der Heide, Paul (University of Houston Van Der Heide, van der Heide Paul
• Publisher: Wiley, John and Sons Ltd
• Languages: English
• Product format: Hardback
• Released: 27.01.2012
• EAN: 9781118062531
• ISBN: 978-1-118-06253-1
• No. of pages: 272
• Subjects: Natural sciences, medicine, IT, technology > Chemistry > Theoretical chemistry; Chemie, Physikalische Chemie, Analytische Chemie, chemistry, Materialwissenschaften, Materials science, Physical Chemistry, Analytical Chemistry, Allg. Materialwissenschaften