• Preface to First Edition xi Preface to Second Edition xiii Acknowledgements xvii
• 1 Electron Spectroscopy: Some Basic Concepts 1 1.1 Analysis of Surfaces 1 1.2 Notation 3 1.2.1 Spectroscopists' Notation 3 1.2.2 X-ray Notation 4 1.3 X-ray Photoelectron Spectroscopy 4 1.4 Auger Electron Spectroscopy (AES) 8 1.5 Scanning Auger Microscopy 12 1.6 The Depth of Analysis in Electron Spectroscopy 13 1.7 Comparison of XPS and AES/SAM 16 1.8 The Availability of Surface Analytical Equipment 17
• 2 Electron Spectrometer Design 19 2.1 Introduction 19 2.2 The Vacuum System 19 2.3 X-ray Sources for XPS 22 2.3.1 Choice of X-ray Anode 23 2.3.2 X-ray Monochromators 27 2.3.3 Synchrotron Sources 30 2.4 The Electron Gun for AES 31 2.4.1 Electron Sources 31 2.4.1.1 Thermionic Emitter 32 2.4.1.2 Lanthanum Hexaboride Emitter 32 2.4.1.3 Cold Field Emitter 32 2.4.1.4 Hot Field Emitter 33 2.4.1.5 Comparison of Electron Emitters for AES 34 2.4.2 The Electron Column 35 2.4.3 Spot Size 35 2.5 Analysers for Electron Spectroscopy 37 2.5.1 The Cylindrical Mirror Analyser 38 2.5.2 The Hemispherical Sector Analyser 41 2.5.2.1 CAE Mode of Operation 42 2.5.2.2 CRR Mode of Operation 44 2.5.2.3 Comparison of CAE and CRR Modes 46 2.5.2.4 The Transfer Lens 47 2.5.3 Calibration of the Electron Spectrometer Energy Scale 48 2.6 Near Ambient Pressure XPS 49 2.7 Detectors 52 2.7.1 Channel Electron Multipliers 52 2.7.2 Microchannel Plates 54 2.7.3 Two-Dimensional Detectors 54 2.7.3.1 The Resistive-Anode Detector 55 2.7.3.2 The Delay-Line Detector 55 2.8 Small Area XPS 56 2.8.1 Lens-Defined Small Area XPS 56 2.8.2 Source-defined Small Area Analysis 57 2.9 XPS Imaging and Mapping 57 2.9.1 Serial Acquisition 58 2.9.2 Parallel Acquisition 59 2.9.2.1 Parallel Imaging Using a Hemispherical Spectrometer 59 2.9.2.2 Parallel Imaging Using a Spherical Mirror Analyser 60 2.9.2.3 Spatial Resolution and Chemical Imaging 61 2.10 Angle Resolved XPS 64 2.11 Automation 66
• 3 The Electron Spectrum: Qualitative and Quantitative Interpretation 69 3.1 Introduction 69 3.2 Qualitative Analysis 69 3.2.1 Unwanted Features in Electron Spectra 72 3.2.2 Data Acquisition 72 3.2.2.1 Core Level Spectra 72 3.2.2.2 Valence Band Spectra 73 3.3 Chemical State Information 74 3.3.1 X-ray Photoelectron Spectroscopy 74 3.3.2 Peak Fitting of XPS Spectra 78 3.3.3 Auger Electron Spectroscopy 81 3.3.4 X-AES 82 3.3.5 Chemical State Plots 84 3.3.6 Shakeup Satellites 86 3.3.7 Multiplet Splitting 87 3.3.8 Plasmons 87 3.4 Quantitative Analysis 88 3.4.1 Quantification in XPS 89 3.4.1.1 Calculating Atomic Concentration 89 3.4.1.2 Measuring Peak Intensity 92 3.4.2 Quantification in AES 94
• 4 Compositional Depth Profiling 97 4.1 Introduction 97 4.2 Non-destructive Depth Methods 98 4.2.1 Measurements at a Single Emission Angle 98 4.2.2 Angle Resolved XPS Measurements 99 4.2.3 Measurement of Overlayer Thickness Using ARXPS 101 4.2.4 Elastic Scattering 103 4.2.5 Multilayer Thickness Calculations Using ARXPS 104 4.2.6 Compositional Depth Profiles from ARXPS Measurements 107 4.2.7 Variation of Analysis Depth with Electron Kinetic Energy 110 4.2.8 Background Analysis 112 4.3 Depth Profiling by Sputtering with Energetic Ions 115 4.3.1 The Sputtering Process 115 4.3.2 Experimental Method 116 4.3.3 The Nature of the Ion Beam 118 4.3.3.1 Noble Gas Ions 118 4.3.3.2 Cluster Ions 119 4.3.3.3 Metal Ions 121 4.3.4 Sputter Yield and Etch Rate 122 4.3.5 Factors Affecting the Etch Rate 123 4.3.5.1 Material 123 4.3.5.2 Ion Current 123 4.3.5.3 Ion Energy 123 4.3.5.4 Nature of the Ion Beam 124 4.3.5.5 Angle of Incidence 124 4.3.6 Factors Affecting the Depth Resolution 124 4.3.6.1 Ion Beam Characteristics 124 4.3.6.2 Crater Quality 125 4.3.6.3 Beam Impurities 125 4.3.6.4 Information Depth 126 4.3.6.5 Original Surface Roughness 127 4.3.6.6 Induced Roughness 127 4.3.6.7 Preferential Sputtering 127 4.3.6.8 Redeposition of Sputtered Material 128 4.3.7 Calibration 128 4.3.8 Ion Gun Design 128 4.3.8.1 Electron Impact Ion Guns 128 4.3.8.2 Argon-Cluster Ion Guns 129 4.3.8.3 Liquid Metal Ion Guns 131 4.4 Sectioning 131 4.4.1 FIB Sectioning 131 4.4.2 Angle Lapping 132 4.4.3 Ball Cratering 133
• 5 Multi-technique Analysis 135 5.1 Introduction 135 5.2 Ultraviolet Photoelectron Spectroscopy (UPS) 135 5.3 Low Energy Ion Scattering Spectroscopy (LEISS) 137 5.4 Reflection Electron Energy Loss Spectroscopy (REELS) 139 5.4.1 Elastic Scattering 140 5.4.2 Inelastic Scattering 141 5.5 Work Function Measurements 142 5.6 Energy Dispersive X-ray Analysis (EDX) 143
• 6 The Sample 145 6.1 Sample Handling 145 6.2 Sample Preparation 147 6.3 Sample Mounting 149 6.4 Sample Stability 149 6.5 Contamination and Damage During Analysis 151 6.6 Controlling Sample Charging 152 6.6.1 Sample Charging in XPS 152 6.6.2 Sample Charging in AES 154
• 7 Applications of Electron Spectroscopy in Materials Science 157 7.1 Introduction 157 7.2 Metallurgy 157 7.2.1 Grain Boundary Segregation 158 7.2.2 Electronic Structure of Metallic Alloys 160 7.2.3 Surface Engineering 163 7.3 Corrosion Science 168 7.4 Ceramics 176 7.5 Microelectronics and Semiconductor Materials 181 7.5.1 Mapping Semiconductor Devices Using AES 182 7.5.2 XPS Failure Analysis of Microelectronic Devices 186 7.5.3 Depth Profiling of Semiconductor Materials 188 7.5.3.1 Transistor Gate Dielectrics 188 7.5.3.2 Inorganic Chemical State Profiling 189 7.5.3.3 Organic Semiconductor Profiling 190 7.6 Polymeric Materials 193 7.7 Adhesion Science 202 7.8 Nanotechnology 210 7.9 Biology 215 7.10 Energy 219
• 8 Comparison of XPS and AES with Other Analytical Techniques 223 Glossary 229 Bibliography 239
• Appendix 1 247 Auger Electron Energies 247
• Appendix 2 249 Table of Binding Energies Accessible with Al K Radiation 250
• Appendix 3 255 Documentary Standards in Surface Analysis 255 The Scope of TC201 255 The Purpose of TC201 255 International Standards Relevant to Electron Spectroscopies 256 Index 259.
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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.
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• Preface.- Scanning Electron Microscopy and Associated Techniques: Overview.- Electron Beam - Specimen Interactions: Interaction Volume.- Backscattered Electrons.- Secondary Electrons.- X-rays.- SEM Instrumentation.- Image Formation.- SEM Image Interpretation.- The Visibility of Features in SEM Images.- Image Defects.- High resolution imaging.- Low Beam Energy SEM.- Variable Pressure Scanning Electron Microscopy (VPSEM).- ImageJ and Fiji.- SEM Imaging checklist.- SEM Case Studies.- Energy Dispersive X-ray Spectrometry: Physical Principles and User-Selected Parameters.- DTSA-II EDS Software.- Qualitative Elemental Analysis by Energy Dispersive X-ray Spectrometry.- Quantitative Analysis: from k-ratio to Composition.- Quantitative analysis: the SEM/EDS elemental microanalysis k-ratio procedure for bulk specimens, step-by-step.- Trace Analysis by SEM/EDS.- Low Beam Energy X-ray Microanalysis.- Analysis of Specimens with Special Geometry: Irregular Bulk Objects and Particles.- Compositional Mapping.- Attempting Electron-Excited X-ray Microanalysis in the Variable Pressure Scanning Electron Microscope (VP-SEM).- Energy Dispersive X-ray Microanalysis Checklist.- X-ray Microanalysis Case Studies.- Cathodoluminescence.- Characterizing crystalline materials in the SEM.- Focused Ion Beam Applications in the SEM laboratory.- Ion Beam Microscopy.- Appendix - A Database of Electron-Solid Interactions.- Index.
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This thoroughly revised and updated Fourth Edition of a time-honored text provides the reader with a comprehensive introduction to the field of scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDS) for elemental microanalysis, electron backscatter diffraction analysis (EBSD) for micro-crystallography, and focused ion beams. Students and academic researchers will find the text to be an authoritative and scholarly resource, while SEM operators and a diversity of practitioners - engineers, technicians, physical and biological scientists, clinicians, and technical managers - will find that every chapter has been overhauled to meet the more practical needs of the technologist and working professional. In a break with the past, this Fourth Edition de-emphasizes the design and physical operating basis of the instrumentation, including the electron sources, lenses, detectors, etc. In the modern SEM, many of the low level instrument parameters are now controlled and optimized by the microscope's software, and user access is restricted. Although the software control system provides efficient and reproducible microscopy and microanalysis, the user must understand the parameter space wherein choices are made to achieve effective and meaningful microscopy, microanalysis, and micro-crystallography. Therefore, special emphasis is placed on beam energy, beam current, electron detector characteristics and controls, and ancillary techniques such as energy dispersive x-ray spectrometry (EDS) and electron backscatter diffraction (EBSD). With 13 years between the publication of the third and fourth editions, new coverage reflects the many improvements in the instrument and analysis techniques. The SEM has evolved into a powerful and versatile characterization platform in which morphology, elemental composition, and crystal structure can be evaluated simultaneously. Extension of the SEM into a "dual beam" platform incorporating both electron and ion columns allows precision modification of the specimen by focused ion beam milling. New coverage in the Fourth Edition includes the increasing use of field emission guns and SEM instruments with high resolution capabilities, variable pressure SEM operation, theory, and measurement of x-rays with high throughput silicon drift detector (SDD-EDS) x-ray spectrometers. In addition to powerful vendor- supplied software to support data collection and processing, the microscopist can access advanced capabilities available in free, open source software platforms, including the National Institutes of Health (NIH) ImageJ-Fiji for image processing and the National Institute of Standards and Technology (NIST) DTSA II for quantitative EDS x-ray microanalysis and spectral simulation, both of which are extensively used in this work. However, the user has a responsibility to bring intellect, curiosity, and a proper skepticism to information on a computer screen and to the entire measurement process. This book helps you to achieve this goal. Realigns the text with the needs of a diverse audience from researchers and graduate students to SEM operators and technical managers Emphasizes practical, hands-on operation of the microscope, particularly user selection of the critical operating parameters to achieve meaningful results Provides step-by-step overviews of SEM, EDS, and EBSD and checklists of critical issues for SEM imaging, EDS x-ray microanalysis, and EBSD crystallographic measurements Makes extensive use of open source software: NIH ImageJ-FIJI for image processing and NIST DTSA II for quantitative EDS x-ray microanalysis and EDS spectral simulation. Includes case studies to illustrate practical problem solving Covers Helium ion scanning microscopy Organized into relatively self-contained modules - no need to "read it all" to understand a topic Includes an online supplement-an extensive "Database of Electron-Solid Interactions"-which can be accessed on SpringerLink, in Chapter 3.
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• Preface. Acknowledgements. Electron Spectroscopy: Some Basic Concepts. Electron Spectrometer Design. The Electron Spectrum: Qualitative and Quantitative Interpretation. Compositional Depth Profiling. Applications of Electron Spectroscopy in Materials Science. Comparison of XPS and AES with Other Analytical Techniques. Glossary. Bibliography.
• Appendix 1. Auger Electron Energies.
• Appendix 2. Table of Binding Energies Accessible with AIKalpha Radiation. Index.
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Extensively revised and updated with additional material included in existing chapters and new material on angle resolved XPS, surface engineering and complimentary methods. Includes an accessible introduction to the key spectroscopic techniques in surface analysis. Provides descriptions of latest instruments and techniques. Includes a detailed glossary of key surface analysis terms.
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Providing a comprehensive introduction to the capabilities and use of scanning electron microscopes (SEM) and x-ray spectrometers, this highly acclaimed text emphasizes practical aspects of imaging and analysis for a broad audience of students and practitioners whose backgrounds span a wide range of science and technology. Topics discussed include user-controlled functions of scanning electron microscopes and x-ray spectrometers, the characteristics of electron beam - specimen interactions, image formation and interpretation, the use of x-rays for qualitative and quantitative analysis and the methodology for structural analysis using electron back-scatter diffraction. SEM sample preparation methods for hard materials, polymers, and biological specimens are covered in separate chapters. In addition, techniques for the elimination of charging in non-conducting specimens are detailed. A database of useful parameters for SEM and X-ray micro-analysis calculations and enhancements to the text chapters are available on an accompanying CD. This third edition has been extensively revised, including new sections on: variable-pressure SEM, electron backscatter diffraction (EBSD), recent developments in x-ray detectors, and expanded coverage of: low-voltage SEM, X-ray mapping, specimen preparation. The text has been used in educating over 3,000 students at the Lehigh Microscopy School SEM short course as well as thousands of undergraduate and graduate students at universities worldwide.
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• Major Symbols. Standard Abbreviations. Introduction and Overview of Electrode Processes. Potentials and Thermodynamics of Cells. Kinetics of Electrode Reactions. Mass Transfer by Migration and Diffusion. Basic Potential Step Methods. Potential Sweep Methods. Polarography and Pulse Voltammetry. Controlled--Current Techniques. Method Involving Forced Convention--Hydrodynamic Methods. Techniques Based on Concepts of Impedance. Bulk Electrolysis Methods. Electrode Reactions with Coupled Homogeneous Chemical Reactions. Double--Layer Structure and Adsorption. Electroactive Layers and Modified Electrodes. Electrochemical Instrumentation. Scanning Probe Techniques. Spectroelectrochemistry and Other Coupled Characterization Methods. Photoelectrochemistry and Electrogenerated Chemiluminescence. Appendix A: Mathematical Methods. Appendix B: Digital Simulations of Electrochemical Problems. Appendix C: Reference Tables. Index.
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This edition is fully revised to reflect the current state off the field. Significant additions include ultramicroelectrodes, modified electrodes, and scanning probe methods. Many chapters have been modified and improved, including electrode kinetics, voltammetric methods, and mechanisms of coupled chemical reactions.
(source: Nielsen Book Data)