Surface Analysis - The Principal Techniques
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1 Surface Analysis - The Principal Techniques 2nd Edition Editors johnc.vickerman Manchester Interdisciplinary Biocentre, University of Manchester, UK IAN S. GILMORE National Physical Laboratory, Teddington, UK WILEY A John Wiley and Sons, Ltd., Publication
2 Contents List of Contributors Preface xv xvii 1 Introduction l John C. Vickerman 1.1 How do we Define the Surface? How Many Atoms in a Surface? Information Required Surface Sensitivity Radiation Effects - Surface Damage Complexity of the Data 8 2 Auger Electron Spectroscopy 9 Hans /org Mathieu 2.1 Introduction Principle of the Auger Process Kinetic Energies of Auger Peaks Ionization Cross-Section Comparison of Auger and Photon Emission Electron Backscattering Escape Depth Chemical Shifts Instrumentation Electron Sources Spectrometers Modes of Acquisition Detection Limits Instrument Calibration 30
3 2.4 Quantitative Analysis Depth Profile Analysis Thin Film Calibration Standard Depth Resolution Sputter Rates Preferential Sputtering A-Correction Chemical Shifts in AES Profiles Summary 43 References 44 Problems 45 Electron Spectroscopy for Chemical Analysis 47 Buddy D. Ratner and David G. Castner 3.1 Overview The Basic ESCA Experiment A History of the Photoelectric Effect and ESCA Information Provided by ESCA X-ray Interaction with Matter, the Photoelectron Effect and Photoemission from Solids Binding Energy and the Chemical Shift Koopmans' Theorem Initial State Effects Final State Effects Binding Energy Referencing Charge Compensation in Insulators Peak Widths Peak Fitting Inelastic Mean Free Path and Sampling Depth Quantification Quantification Methods Quantification Standards Quantification Example Spectral Features Instrumentation Vacuum Systems for ESCA Experiments X-ray Sources 82
4 vii Analyzers Data Systems Accessories Spectral Quality Depth Profiling X-Y Mapping and Imaging Chemical Derivatization Valence Band Perspectives Conclusions 100 Acknowledgements 101 References 101 Problems 109 Molecular Surface Mass Spectrometry by SIMS 113 John С Vickerman 4.1 Introduction Basic Concepts The Basic Equation Sputtering Ionization The Static Limit and Depth Profiling Surface Charging Experimental Requirements Primary Beam Mass Analysers Secondary Ion Formation Introduction Models of Sputtering Ionization Influence of the Matrix Effect in Organic Materials Analysis Modes of Analysis Spectral Analysis SIMS Imaging or Scanning SIMS Depth Profiling and 3D Imaging Ionization of the Sputtered Neutrals 183
5 viii CONTENTS Photon Induced Post-Ionization Photon Post-Ionization and SIMS Ambient Methods of Desorption Mass Spectrometry 194 References 199 Problems Dynamic SIMS 207 David McPhail and Mark Dowsett 5.1 Fundamentals and Attributes Introduction Variations on a Theme The Interaction of the Primary Beam with the Sample Depth Profiling Complimentary Techniques and Data Comparison Areas and Methods of Application Dopant and Impurity Profiling Profiling High Concentration Species Use of SIMS in Near Surface Regions Applications of SIMS Depth Profiling in Materials Science Quantification of Data Quantification of Depth Profiles Fabrication of Standards Depth Measurement and Calibration of the Depth Scale Sources of Error in Depth Profiles Novel Approaches Bevelling and Imaging or Line Scanning Reverse-Side Depth Profiling Two-Dimensional Analysis Instrumentation Overview Secondary Ion Optics Dual Beam Methods and ToF Gating 254
6 IX 5.6 Conclusions References Problems Low-Energy Ion Scattering and Rutherford Backscattering Edmund Taglauer Introduction Physical Basis The Scattering Process Collision Kinematics Interaction Potentials and Cross-sections Shadow Cone Computer Simulation Rutherford Backscattering Energy Loss Apparatus Beam Effects Quantitative Layer Analysis Structure Analysis Medium-Energy Ion Scattering (MEIS) The Value of RBS and Comparison to Related Techniques Low-Energy Ion Scattering Neutralization Apparatus Surface Composition Analysis Structure Analysis Conclusions Acknowledgement References Problems Key Facts Vibrational Spectroscopy from Surfaces 333 Martyn E. Pemble and Peter Gardner 7.1 Introduction Infrared Spectroscopy from Surfaces 334
7 7.2.1 Transmission IR Spectroscopy Photoacoustic Spectroscopy Reflectance Methods Electron Energy Loss Spectroscopy (EELS) Inelastic or 'Impact' Scattering Elastic or 'Dipole' Scattering The EELS (HREELS) Experiment The Group Theory of Surface Vibrations General Approach Group Theory Analysis of Ethyne Adsorbed at a Flat, Featureless Surface Group Theory Analysis of Ethyne Adsorbed at a (100) Surface of an FCC Metal The Expected Form of the RAIRS and Dipolar EELS (HREELS) Spectra Laser Raman Spectroscopy from Surfaces Theory of Raman Scattering The Study of Collective Surface Vibrations (Phonons) using Raman Spectroscopy Raman Spectroscopy from Metal Surfaces Spatial Resolution in Surface Raman Spectroscopy Fourier Transform Surface Raman Techniques Inelastic Neutron Scattering (INS) Introduction to INS The INS Spectrum INS Spectra of Hydrodesesulfurization Catalysts Sum-Frequency Generation Methods 383 References 386 Problems Surface Structure Determination by Interference Techniques 391 Christopher A. Lucas 8.1 Introduction Basic Theory of Diffraction - Three Dimensions Extension to Surfaces - Two Dimensions Electron Diffraction Techniques General Introduction 402
8 XI Low Energy Electron Diffraction Reflection High Energy Electron Diffraction (RHEED) X-ray Techniques General Introduction X-ray Adsorption Spectroscopy Surface X-ray Diffraction (SXRD) X-ray Standing Waves (XSWs) Photoelectron Diffraction Introduction Theoretical Considerations Experimental Details Applications of XPD and PhD 470 References Scanning Probe Microscopy 479 Graham ]. Leggett 9.1 Introduction Scanning Tunnelling Microscopy Basic Principles of the STM Instrumentation and Basic Operation Parameters Atomic Resolution and Spectroscopy: Surface Crystal and Electronic Structure Atomic Force Microscopy Basic Principles of the AFM Chemical Force Microscopy Friction Force Microscopy Biological Applications of the AFM Scanning Near-Field Optical Microscopy Optical Fibre Near-Field Microscopy Apertureless SNOM Other Scanning Probe Microscopy Techniques Lithography Using Probe Microscopy Methods STM Lithography AFM Lithography Near-Field Photolithography The 'Millipede' 550
9 xii CONTENTS 9.7 Conclusions 551 References 552 Problems 559 lo The Application of Multivariate Data Analysis Techniques in Surface Analysis 563 Joanna L.S. Lee and Ian S. Gilmore 10.1 Introduction Basic Concepts Matrix and Vector Representation of Data Dimensionality and Rank Relation to Multivariate Analysis Choosing the Appropriate Multivariate Method Factor Analysis for Identification Terminology Mathematical Background Principal Component Analysis Multivariate Curve Resolution Analysis of Multivariate Images Regression Methods for Quantification Terminology Mathematical Background Principal Component Regression Partial Least Squares Regression Calibration, Validation and Prediction Example - Correlating ToF-SIMS Spectra with Polymer Wettability Using PLS Methods for Classification Discriminant Function Analysis Hierarchal Cluster Analysis Artificial Neural Networks Summary and Conclusion 606 Acknowledgements 608 References 608 Problems 611
10 XIII Appendix i Vacuum Technology for Applied Surface Science 613 Rod Wilson Al.l Introduction: Gases and Vapours 613 Al.2 The Pressure Regions of Vacuum Technology and their Characteristics 619 A1.3 Production of a Vacuum 622 Al.3.1 Types of Pump 622 Al.3.2 Evacuation of a Chamber 634 Al.3.3 Choice of Pumping System 635 Al.3.4 Determination of the Size of Backing Pumps 636 Al.3.5 Flanges and their Seals 636 Al.4 Measurement of Low Pressures 637 Al.4.1 Gauges for Direct Pressure Measurement 638 Al.4.2 Gauges Using Indirect Means of Pressure Measurement 640 Al.4.3 Partial Pressure Measuring Instruments 644 Acknowledgement 647 References 647 Appendix 2 Units, Fundamental Physical Constants and Conversions 649 A2.1 Base Units of the SI 649 A2.2 Fundamental Physical Constants 650 A2.3 Other Units and Conversions to SI 651 References 652 Index 653
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