Practical Materials Characterization

Practical Materials Characterization covers the most common materials analysis techniques in a single volume. It stands as a quick reference for experienced users, as a learning tool for students, and as a guide for the understanding of typical data interpretation for anyone looking at results from a range of analytical techniques. The book includes analytical methods covering microstructural, surface, morphological, and optical characterization of materials with emphasis on microscopic structural, electronic, biological, and mechanical properties. Many examples in this volume cover cutting-edge technologies such as nanomaterials and life sciences. Preface 6 Contents 8 Chapter 1: X-Ray Diffraction and Reflectivity 9 1.1 Introduction 9 1.2 Basics of Diffraction 10 1.3 Instrumentation and Basic Analytical Configurations 13 1.4 Comparison Between 2Theta/Omega and Omega Scans 18 1.5 Basic Information from XRD Diffractograms 20 1.6 Basic XRD Analysis Methods 22 1.7 Quantitative Analysis 24 1.8 Preferred Orientation, Lattice Constants and Crystallite Size Determination 25 1.9 Structure Refinement by the Rietveld Method 27 1.10 Analysis of Thin Films and Bulk Materials with Preferred Orientation 28 1.11 Texture Analysis 31 1.12 Glancing Incidence X-Ray Diffraction 35 1.13 High-Resolution X-Ray Diffraction 36 1.14 Reciprocal Lattice Mapping 40 1.15 X-Ray Reflectivity 44 1.16 Summary and Comparison with Other Analytical Techniques 48 References 49 Chapter 2: Introduction to Optical Characterization of Materials 50 2.1 Introduction 50 2.2 About Light 51 2.2.1 Polarization 52 2.2.2 Light-Matter Interaction: The Basics 53 2.2.2.1 Absorption 55 2.2.2.2 Light Scattering 56 2.3 Spectrophotometry (UV-VIS-NIR) 57 2.3.1 Instrumentation 58 2.3.2 Transmittance 59 2.3.2.1 Data Acquisition Strategies 60 2.3.3 Specular Reflectance 61 2.3.3.1 Data Acquisition Strategies 63 2.3.4 Diffuse Reflectance 63 2.3.5 Diffuse Transmittance 65 2.3.6 Absorbance 65 2.3.6.1 Beer-Lambert Law 66 2.3.7 Applications 66 2.3.7.1 Application Example: Thin Films Thickness Determination 68 2.3.8 Strengths and Limitations 70 2.4 Fourier Transform Infra-Red Spectroscopy (FTIR) 70 2.4.1 Instrumentation 71 2.4.2 Transmittance 73 2.4.2.1 KBr Pellets 73 2.4.2.2 Nujol Method 74 2.4.2.3 IR Sample Cards 74 2.4.2.4 Data Acquisition Strategies 74 2.4.3 Specular Reflectance 75 2.4.4 Diffuse Reflectance 75 2.4.4.1 Data Acquisition Strategies 76 2.4.5 ATR 76 2.4.6 Applications 77 2.4.6.1 Application Example: Material Identification by FTIR 77 2.4.7 Strengths and Limitations 80 2.5 Ellipsometry 82 2.5.1 Instrumentation 83 2.5.1.1 The Null Ellipsometer 85 2.5.1.2 The Photometric Ellipsometers 85 2.5.2 Analysis 86 2.5.3 Data Acquisition Strategies 89 2.5.4 Applications 89 2.5.4.1 Application Example: Thickness and Optical Constants of a Thin TiO2 Film on Si 90 2.5.5 Strengths and Limitations 91 2.6 Raman Spectroscopy 92 2.6.1 Instrumentation 94 2.6.2 Applications 94 2.6.2.1 Application Example: Raman Spectroscopy of Carbon Incorporation in Cubic GaN 95 2.6.3 Strengths and Limitations 96 2.7 Summary 97 References 97 Chapter 3: X-Ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES) 100 3.1 X-Ray Photoelectron Spectroscopy (XPS) 101 3.2 Photoelectron and Auger Electron Emission 101 3.3 The Fermi Level 102 3.4 The Finite Potential and Work Function 103 3.5 Electron Attenuation and Surface Sensitivity 104 3.6 Instrumentation 106 3.7 Elemental and Chemical Shifts 107 3.8 Spin-Orbit Splitting 112 3.9 Energy Loss and Final-State Structures 113 3.10 Ultraviolet Photoelectron Spectroscopy (UPS) 115 3.11 Work Function Measurement 116 3.12 Quantitative Analysis 117 3.13 Angle-Resolved XPS and Thickness Measurement 119 3.14 Ion Sputtering and Depth Profiling 122 3.15 XPS Imaging and Spectroscopy 125 3.16 Auger Electron Spectroscopy (AES) 126 3.17 Instrumentation 127 3.18 Elemental Shifts 128 3.19 Chemical State/Matrix Effects 131 3.20 Quantitative Analysis 132 3.21 Depth Profiling 134 3.22 Imaging and Spectroscopy 135 3.23 Imaging and Auger Mapping 136 3.24 Summary 137 References 137 Chapter 4: Secondary Ion Mass Spectrometry 140 4.1 Introduction 140 4.2 Ion Beam Bombardment and Sputtering 140 4.3 Instrumentation 145 4.3.1 Components 145 4.3.2 Vacuum 146 4.3.3 Ion Sources 146 4.3.4 Mass Analyzers 148 4.3.4.1 Quadrupole 149 4.3.4.2 Magnetic Sector 149 4.3.4.3 Time of Flight (TOF) 151 4.3.5 Detectors 153 4.3.6 Data Acquisition and Analysis 153 4.3.7 Oxygen Leak 153 4.3.8 Sample Stages 154 4.3.9 Electron Gun 154 4.4 Analytical Considerations 154 4.4.1 Analysis of Insulators 154 4.4.2 Static and Dynamic SIMS 155 4.4.3 Mass Spectra and Interferences 156 4.4.3.1 Mass Resolution 156 4.4.3.2 Energy Offset 158 4.4.4 Detectors 159 4.4.5 Quantitative Analysis 160 4.4.5.1 Ion Implants as Standards 160 4.4.5.2 Relative Sensitivity Factors 161 4.4.5.3 Buried Interfaces 163 4.4.5.4 MCs+ Quantitative Analysis of Major Constituents 164 4.4.5.5 Shallow Implant Quantification 164 4.5 Analysis with Mass Spectra 164 4.6 Analysis with Depth Profiles 166 4.6.1 Primary and Secondary Ion Selection 166 4.6.2 Detection Limits 170 4.6.3 Depth Resolution 172 4.6.3.1 Measurement of Depth Resolution and Dynamic Range 172 4.6.3.2 Sputtered Craters and Data Selection 173 4.6.3.3 Crater Topography 173 4.6.3.4 Primary Beam Energy and Angle of Incidence 176 4.6.3.5 Shallow Implants 179 4.6.4 Crystal Orientation and Effect on Ion Yields in Depth Profiles 179 4.6.5 Ion Yields at Interfaces 180 4.6.6 Applications of Depth Profiling 183 4.7 Analysis with Ion Imaging 183 4.7.1 Applications of Ion Imaging 185 4.8 Three-Dimensional Analysis with Ion Imaging and Depth Profiling 186 4.9 Combination with Other Techniques 189 4.10 Conclusion 189 References 190 Chapter 5: Transmission Electron Microscopy 195 5.1 Introduction to Transmission Electron Microscopy 195 5.2 Electron Beam Interaction with Matter 196 5.3 Instrument 197 5.3.1 Transmission Electron Microscope 197 5.3.2 Vacuum System 198 5.3.3 CCD Camera 198 5.4 Specimen Preparation 199 5.5 Basic Operation of a Transmission Electron Microscope 201 5.5.1 Loading Specimens on TEM Holders 201 5.5.2 Basic TEM Alignment 201 5.5.3 Tilting the Specimen 204 5.6 TEM Imaging 205 5.6.1 Thickness-Mass Contrast 205 5.6.2 Diffraction Contrast 205 5.6.2.1 Diffraction Contrast Theory 206 5.6.2.2 Defects Analysis 206 5.6.2.3 Weak-Beam Dark-Field Imaging 208 5.6.3 High-Resolution TEM Imaging (Phase Contrast) 209 5.7 Diffraction 210 5.7.1 Basic Alignment 211 5.7.2 Selected-Area Electron Diffraction 212 5.7.3 Nano-Beam Electron Diffraction 212 5.7.4 Convergent-Beam Electron Diffraction 214 5.8 Scanning TEM 217 5.8.1 The Ronchigram 217 5.8.2 HAADF 219 5.8.3 STEM-BF 220 5.9 Spectroscopy 221 5.9.1 X-Ray Energy Dispersive Spectroscopy 221 5.9.2 Electron Energy-Loss Spectroscopy 222 5.9.3 Energy-Filtered TEM Imaging 224 5.9.4 Spectrum Imaging 226 5.10 Aberration-Corrected TEM/STEM 227 5.10.1 Aberration-Corrected STEM 229 5.10.2 Atomic Column EELS Spectrum Imaging 229 5.10.3 Negative Cs Image Method 231 5.10.4 Atomic Column Selective Contrast Imaging Method 231 5.10.5 Chromatic Aberration-Corrected EFTEM Imaging 233 References 233 Index 236 This unique book covers the most common materials analysis techniques, such as transmission electron microscopy, x-ray diffraction and reflectivity, auger electron spectroscopy, secondary ion mass spectrometry, photoelectron spectroscopy, and several optical characterization methods. It stands as a quick reference for experienced users, as a learning tool for students, and as a guide for the understanding of typical data interpretation for anyone looking at results from a range of analytical techniques. The book includes analytical methods covering microstructural, surface, morphological, and optical characterization of materials with emphasis on microscopic structural, electronic, biological, and mechanical properties. Many examples in this volume cover cutting-edge technologies such as nanomaterials and life sciences. This book also: · Presents cross-comparison between materials characterization techniques, including x-ray diffraction and reflectivity, x-ray photoelectron spectroscopy, secondary ion mass spectrometery, ellipsometry, Raman spectroscopy, and more · Includes clear specifications of strengths and limitations of each technique for specific materials characterization problem · Focuses on applications and clear data interpretation without extensive mathematics This unique book covers the most common materials analysis techniques, such as transmission electron microscopy, x-ray diffraction and reflectivity, auger electron spectroscopy, secondary ion mass spectrometry, photoelectron spectroscopy, and several optical characterization methods. It stands as a quick reference for experienced users, as a learning tool for students, and as a guide for the understanding of typical data interpretation for anyone looking at results from a range of analytical techniques. The book includes analytical methods covering microstructural, surface, morphological, and optical characterization of materials with emphasis on microscopic structural, electronic, biological, and mechanical properties. Many examples in this volume cover cutting-edge technologies such as nanomaterials and life sciences. This book also: {middot} Presents cross-comparison between materials characterization techniques, including x-ray diffraction and reflectivity, x-ray photoelectron spectroscopy, secondary ion mass spectrometery, ellipsometry, Raman spectroscopy, and more {middot} Includes clear specifications of strengths and limitations of each technique for specific materials characterization problem {middot} Focuses on applications and clear data interpretation without extensive mathematics Presents cross-comparison between materials characterization techniques Includes clear specifications of strengths and limitations of each technique for specific materials characterization problem Focuses on applications and clear data interpretation without extensive mathematics This unique book covers the most common materials analysis techniques, such as transmission electron microscopy, x-ray diffraction and reflectivity, auger electron spectroscopy, secondary ion mass spectrometry, photoelectron spectroscopy, and several optical characterization methods. It stands as a quick Front Matter....Pages i-vii X-Ray Diffraction and Reflectivity....Pages 1-41 Introduction to Optical Characterization of Materials....Pages 43-92 X-Ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES)....Pages 93-132 Secondary Ion Mass Spectrometry....Pages 133-187 Transmission Electron Microscopy....Pages 189-229 Back Matter....Pages 231-237