Materials Characterization: Introduction to Microscopic and Spectroscopic Methods

Now in its second edition, this continues to serve as an ideal textbook for introductory courses on materials characterization, based on the author?s experience in teaching advanced undergraduate and postgraduate university students. The new edition retains the successful didactical concept of introductions at the beginning of chapters, exercise questions and an online solutions manual. In addition, all the sections have been thoroughly revised, updated and expanded, with two major new topics (electron backscattering diffraction and environmental scanning electron microscopy), as well as fifty additional questions – in total about 20% new content. The first part covers commonly used methods for microstructure analysis, including light microscopy, X–ray diffraction, transmission and scanning electron microscopy, as well as scanning probe microscopy. The second part of the book is concerned with techniques for chemical analysis and introduces X–ray energy dispersive spectroscopy, fluorescence X–ray spectroscopy and such popular surface analysis techniques as photoelectron and secondary ion mass spectroscopy. This section concludes with the two most important vibrational spectroscopies (infra–red and Raman) and the increasingly important thermal analysis. The theoretical concepts are discussed with a minimal involvement of mathematics and physics, and the technical aspects are presented with the actual measurement practice in mind. Making for an easy–to–read text that never loses sight of its intended audience. INDICE: 1 Light Microscopy 1 1.1 Optical Principles 1 1.1.1 Image Formation 1 1.1.2 Resolution 3 1.1.3 Depth of Field 6 1.1.4 Aberrations 7 1.2 Instrumentation 9 1.2.1 Illumination System 9 1.2.2 Objective Lens and Eyepiece 13 1.3 Specimen Preparation 15 1.3.1 Sectioning 16 1.3.2 Mounting 17 1.3.3 Grinding and Polishing 19 1.3.4 Etching 23 1.4 Imaging Modes 26 1.4.1 Bright–Field and Dark–Field Imaging 26 1.4.2 Phase–Contrast Microscopy 27 1.4.3 Polarized–Light Microscopy 30 1.4.4 Nomarski Microscopy 35 1.4.5 Fluorescence Microscopy 37 1.5 Confocal Microscopy 39 1.5.1 Working Principles 39 1.5.2 Three–Dimensional Images 41 References 45 Further Reading 45 2 X–Ray Diffraction Methods 47 2.1 X–Ray Radiation 47 2.1.1 Generation of X–Rays 47 2.1.2 X–Ray Absorption 50 2.2 Theoretical Background of Diffraction 52 2.2.1 Diffraction Geometry 52 2.2.2 Diffraction Intensity 58 2.3 X–Ray Diffractometry 62 2.3.1 Instrumentation 62 2.3.2 Samples and Data Acquisition 65 2.3.3 Distortions of Diffraction Spectra 67 2.3.4 Applications 70 2.4 Wide–Angle X–Ray Diffraction and Scattering 75 2.4.1 Wide–Angle Diffraction 76 2.4.2 Wide–Angle Scattering 79 References 82 Further Reading 82 3 Transmission Electron Microscopy 83 3.1 Instrumentation 83 3.1.1 Electron Sources 84 3.1.2 Electromagnetic Lenses 87 3.1.3 Specimen Stage 89 3.2 Specimen Preparation 90 3.2.1 Prethinning 91 3.2.2 Final Thinning 91 3.3 Image Modes 94 3.3.1 Mass–Density Contrast 95 3.3.2 Diffraction Contrast 96 3.3.3 Phase Contrast 101 3.4 Selected–Area Diffraction (SAD) 107 3.4.1 Selected–Area Diffraction Characteristics 107 3.4.2 Single–Crystal Diffraction 109 3.4.3 Multicrystal Diffraction 114 3.4.4 Kikuchi Lines 114 3.5 Images of Crystal Defects 117 3.5.1 Wedge Fringe 117 3.5.2 Bending Contours 120 3.5.3 Dislocations 122 References 126 Further Reading 126 4 Scanning Electron Microscopy 127 4.1 Instrumentation 127 4.1.1 Optical Arrangement 127 4.1.2 Signal Detection 129 4.1.3 Probe Size and Current 131 4.2 Contrast Formation 135 4.2.1 Electron–Specimen Interactions 135 4.2.2 Topographic Contrast 137 4.2.3 Compositional Contrast 139 4.3 Operational Variables 141 4.3.1 Working Distance and Aperture Size 141 4.3.2 Acceleration Voltage and Probe Current 144 4.3.3 Astigmatism 145 4.4 Specimen Preparation 145 4.4.1 Preparation for Topographic Examination 146 4.4.2 Preparation for Microcomposition Examination 149 4.4.3 Dehydration 149 4.5 Electron Backscatter Diffraction 151 4.5.1 EBSD Pattern Formation 151 4.5.2 EBSD Indexing and Its Automation 153 4.5.3 Applications of EBSD 155 4.6 Environmental SEM 156 4.6.1 ESEM Working Principle 156 4.6.2 Applications 158 References 160 Further Reading 160 5 Scanning Probe Microscopy 163 5.1 Instrumentation 163 5.1.1 Probe and Scanner 165 5.1.2 Control and Vibration Isolation 165 5.2 Scanning Tunneling Microscopy 166 5.2.1 Tunneling Current 166 5.2.2 Probe Tips and Working Environments 167 5.2.3 Operational Modes 168 5.2.4 Typical Applications 169 5.3 Atomic Force Microscopy 170 5.3.1 Near–Field Forces 170 5.3.2 Force Sensors 172 5.3.3 Operational Modes 174 5.3.4 Typical Applications 180 5.4 Image Artifacts 183 5.4.1 Tip 183 5.4.2 Scanner 185 5.4.3 Vibration and Operation 187 References 189 Further Reading 189 6 X–Ray Spectroscopy for Elemental Analysis 191 6.1 Features of Characteristic X–Rays 191 6.1.1 Types of Characteristic X–Rays 193 6.1.2 Comparison of K, L, and M Series 194 6.2 X–Ray Fluorescence Spectrometry 196 6.2.1 Wavelength Dispersive Spectroscopy 199 6.2.2 Energy Dispersive Spectroscopy 203 6.2.3 XRF Working Atmosphere and Sample Preparation 206 6.3 Energy Dispersive Spectroscopy in Electron Microscopes 207 6.3.1 Special Features 208 6.3.2 Scanning Modes 210 6.4 Qualitative and Quantitative Analysis 211 6.4.1 Qualitative Analysis 211 6.4.2 Quantitative Analysis 213 References 219 Further Reading 219 7 Electron Spectroscopy for Surface Analysis 221 7.1 Basic Principles 221 7.1.1 X–Ray Photoelectron Spectroscopy 221 7.1.2 Auger Electron Spectroscopy 222 7.2 Instrumentation 225 7.2.1 Ultrahigh Vacuum System 225 7.2.2 Source Guns 227 7.2.3 Electron Energy Analyzers 229 7.3 Characteristics of Electron Spectra 230 7.3.1 Photoelectron Spectra 230 7.3.2 Auger Electron Spectra 233 7.4 Qualitative and Quantitative Analysis 235 7.4.1 Qualitative Analysis 235 7.4.2 Quantitative Analysis 246 7.4.3 Composition Depth Profiling 247 References 250 Further Reading 251 8 Secondary Ion Mass Spectrometry for Surface Analysis 253 8.1 Basic Principles 253 8.1.1 Secondary Ion Generation 254 8.1.2 Dynamic and Static SIMS 257 8.2 Instrumentation 258 8.2.1 Primary Ion System 258 8.2.2 Mass Analysis System 262 8.3 Surface Structure Analysis 266 8.3.1 Experimental Aspects 266 8.3.2 Spectrum Interpretation 268 8.4 SIMS Imaging 272 8.4.1 Generation of SIMS Images 274 8.4.2 Image Quality 275 8.5 SIMS Depth Profiling 275 8.5.1 Generation of Depth Profiles 276 8.5.2 Optimization of Depth Profiling 276 References 282 9 Vibrational Spectroscopy for Molecular Analysis 283 9.1 Theoretical Background 283 9.1.1 Electromagnetic Radiation 283 9.1.2 Origin of Molecular Vibrations 285 9.1.3 Principles of Vibrational Spectroscopy 286 9.1.4 Normal Mode of Molecular Vibrations 289 9.1.5 Infrared and Raman Activity 292 9.2 Fourier Transform Infrared Spectroscopy 297 9.2.1 Working Principles 298 9.2.2 Instrumentation 300 9.2.3 Examination Techniques 304 9.2.4 Fourier Transform Infrared Microspectroscopy 307 9.3 Raman Microscopy 310 9.3.1 Instrumentation 310 9.3.2 Fluorescence Problem 314 9.3.3 Raman Imaging 315 9.3.4 Applications 316 9.4 Interpretation of Vibrational Spectra 323 9.4.1 Qualitative Methods 323 9.4.2 Quantitative Methods 327 References 331 Further Reading 332 10 Thermal Analysis 333 10.1 Common Characteristics 333 10.1.1 Thermal Events 333 10.1.2 Instrumentation 335 10.1.3 Experimental Parameters 336 10.2 Differential Thermal Analysis and Differential Scanning Calorimetry 337 10.2.1 Working Principles 337 10.2.2 Experimental Aspects 342 10.2.3 Measurement of Temperature and Enthalpy Change 345 10.2.4 Applications 348 10.3 Thermogravimetry 353 10.3.1 Instrumentation 354 10.3.2 Experimental Aspects 355 10.3.3 Interpretation of Thermogravimetric Curves 360 10.3.4 Applications 362 References 365 Further Reading 365 Index 367

• ISBN: 978-3-527-33463-6
• Editorial: Wiley VCH
• Encuadernacion: Cartoné
• Páginas: 392
• Fecha Publicación: 11/09/2013
• Nº Volúmenes: 1
• Idioma: Inglés