A comprehensive and accessible introduction to the characterization of condensed materials
The characterization of condensed materials is a crucial aspect of materials science. The science underlying this area of research and analysis is interdisciplinary, combining electromagnetic spectroscopy, surface and interface testing methods, physiochemical analysis methods, and more. All of this must be brought to bear in order to understand the relationship between microstructures and larger-scale properties of condensed matter.
Characterization of Condensed Matter: An Introduction to Composition, Microstructure, and Surface Methods introduces the technologies involved in the characterization of condensed matter and their many applications. It incorporates more than a decades’ experience in teaching a successful undergraduate course in the subject and emphasizes accessibility and continuously reinforced learning. The result is a survey which promises to equip students with both underlying theory and real experimental instances of condensed matter characterization.
Characterization of Condensed Matter readers will also find:
- Detailed treatment of techniques including electromagnetic spectroscopy, X-ray diffraction, X-ray absorption, electron microscopy, surface and element analysis, and more
- Incorporation of concrete experimental examples for each technique
- Exercises at the end of each chapter to facilitate understanding
Characterization of Condensed Matter is a useful reference for undergraduates and early-career graduate students seeking a foundation and reference for these essential techniques.
Table of Contents
Part I Fundamental of Universe, Matter, Condensed Matter and Materials 1
1 Universe, Matter, Condensed Matter and Materials 3
1.1 Features of the Universe and Fundamental Constants 4
1.2 Structure and Composition of Matter 9
1.2.1 Classification and Characteristics of Matter (Radiation Coupling and Energy Conservation) 9
1.2.2 Fundamental Particles 9
1.2.3 Fundamental Forces 11
1.3 Fundamental Constants Describing the Universe and Matter 15
1.4 Experiments to Study Fundamental Particles and Forces 20
1.5 Introduction to Condensed Matter and Materials 27
1.5.1 Classification of Condensed Matter 28
1.5.2 Structures and Compositions of Condensed Matter or Materials 30
1.5.3 Intrinsic Properties of Condensed Matter and Materials 32
1.6 Main Research Areas in Condensed Matter Physics 33
Questions for Thinking 34
References 34
2 The Laser Interferometer Gravitational-Wave Observatory 37
2.1 A Brief History of Gravitational and Gravitational-Wave Measurements 37
2.2 Fundamentals of LIGO and Related Facility Development 39
2.2.1 Detecting Gravitational Waves 41
2.2.2 Educational Analogy Experiments 44
2.2.2.1 Herriott Delay Line 45
2.3 Key Components of the LIGO Facility 47
2.3.1 Coherent Laser Source and Laser 47
2.3.2 The Laser Interferometer Detector 47
2.3.3 Fourier Transform and Signal Processing System 48
2.4 Application of LIGO 49
2.4.1 Detection of a Supernova Explosion 49
2.4.2 Detection of Black Hole Fusion 50
Questions for Thinking 51
List of Abbreviations 51
References 51
3 Fundamentals of Crystallography: Microstructures and Crystal Phases of Condensed Matter 55
3.1 The Microstructure of Condensed Matter and Materials 55
3.1.1 The Microscale 55
3.1.2 The Hard-Sphere Model 56
3.1.3 Energy and Packing 57
3.1.4 Crystals, Quasicrystals and Amorphous Structures 58
3.2 The Unit Cell 60
3.2.1 Lattice and Motif 60
3.2.2 Lattice and Crystal Structure 61
3.2.3 Unit Cell and Unit Vectors 61
3.2.4 Unit Cells, Bravais Lattices and Crystal Systems 63
3.2.5 Unit Cells and Their Parameters 65
3.3 Crystal Structures (Phases) 65
3.3.1 Close Packing and Stacking 65
3.3.2 The Face-Centered Cubic (FCC) Lattice and its Parameters 67
3.3.3 The Body-Centered Cubic (BCC) Lattice and its Parameters 69
3.3.4 The Hexagonal Close-Packed (HCP) Lattice and its Parameters 70
3.3.5 Point Coordinates and Crystallographic Directions 71
3.3.6 Crystallographic Families and Symmetry 72
3.3.7 Coordinate Transformations 72
3.3.8 Crystallographic Planes and Miller Indices 73
3.3.9 Linear Density, Planar Density and Crystal Density 74
3.4 Quasicrystals 77
3.4.1 A Brief History of Quasicrystals 77
3.4.2 Phase and Structure Characteristics of Quasicrystals 79
Questions for Thinking 79
References 80
Part II Electromagnetic Spectroscopy 81
4 Elements of X-Ray Diffraction 83
4.1 Diffraction of X-Rays 83
4.1.1 The Kinematical Theory of Diffraction 85
4.1.2 The Dynamical Diffraction Theory 85
4.1.3 The Mechanism of the Interaction between X-Rays and the Unit Cell 86
4.1.4 Scattering of X-Rays and the Structure Factor of the Unit Cell 86
4.2 Development of X-Ray Diffraction 88
4.3 Generation of X-Rays 91
4.3.1 X-Ray Tubes: Cathode Ray Tube Structure 91
4.3.2 The Interaction of X-Rays with Matter 92
4.3.2.1 Scattering of X-Rays 92
4.3.2.2 Absorption of X-Rays by Matter 93
4.4 Applications 94
4.4.1 Crystal Phase Analysis 94
4.4.2 Determination of Inner Stress of Condensed Samples 97
4.4.2.1 Measurement of Residual Stress in Polycrystalline Materials 98
4.4.2.2 Measurement of Residual Stress in Single-Crystalline Materials 100
Questions for Thinking 101
References 101
5 X-Ray Fluorescence Spectroscopy (XRF) 103
5.1 Theoretical Foundations 103
5.2 General Setup of an XRF Spectrometer 104
5.3 Types of XRF Analyzers 107
5.4 History and Current Status of XRF 108
5.5 Applications 109
5.6 Appendix 112
5.6.1 Analysis of XRF Spectra 112
5.6.2 Total Reflection XRF, Proton-Excited XRF and Synchrotron Radiation XRF Spectrometry 113
Questions for Thinking 114
References 114
6 X-Ray Emission Spectroscopy (XES) 115
6.1 Principles of XAS and XES 115
6.2 Classification of XES 118
6.3 History of XES and Common XES Spectrometers 119
6.4 Applications 119
Questions for Thinking 121
References 121
7 X-Ray Absorption Spectroscopy (XAS) 123
7.1 The Physics of XAS 123
7.1.1 The Principle of X-Ray Absorption Near-Edge Structure (XANES) Spectroscopy 123
7.1.2 The Principle of Extended X-Ray Absorption Fine Structure (EXAFS) Spectroscopy 124
7.2 Generation of X-Ray Synchrotron Radiation 125
7.2.1 The Structure of Synchrotron Radiation Facilities 126
7.2.2 Synchrotron Radiation Facilities Around the World 127
7.3 Applications of XANES Spectroscopy 132
7.4 Applications of EXAFS Spectroscopy 133
7.5 Differences Between EXAFS and XANES 133
Questions for Thinking 134
References 134
8 X-Ray Raman Scattering (XRS) 137
8.1 Interaction of Light and Matter in XRS 137
8.2 A Brief History of XRS Spectrometers 139
8.3 Components of an XRS Spectrometer 141
8.3.1 X-Ray Scattering Crystal Detector 141
8.3.2 High-Resolution Crystal Detector 142
8.3.3 A Superlattice Thin-Film Mirror Surface as a Double Multilayer Monochromator 142
8.3.4 The Detection of Scattered Photons in XRS 143
8.4 Applications of XRS 143
8.4.1 Chemistry 143
8.4.2 Polymer Science 143
8.4.3 Materials Science 144
8.4.4 Biology 145
8.4.5 Chinese Herbal Medicine 146
8.4.6 Gem Research 146
8.4.7 Investigation of Cultural Relics 147
8.5 Summary and Outlook 147
Questions for Thinking 148
References 148
9 Fourier-Transform Infrared (FTIR) Spectroscopy 149
9.1 General Scope of FTIR Spectroscopy 149
9.2 A Brief History of IR Spectrometers 150
9.3 Basic Concepts 150
9.4 Setup of a Standard FTIR Instrument 153
9.5 Advantages of FTIR Spectroscopy 155
9.5.1 Signal-to-Noise Ratio and Linearity 155
9.5.2 Accuracy 155
9.5.3 Data Handling Facility 155
9.5.4 Mechanical Simplicity 155
9.6 Key Elements of an FTIR Spectrometer 156
9.6.1 IR Light Source and Laser 156
9.6.2 Michelson Interferometer and Beam Splitter 156
9.6.2.1 Michelson Interferometer 156
9.6.2.2 Measuring and Processing the Interferogram 158
9.6.2.3 Beamsplitter 160
9.6.3 Infrared Photodetector 160
9.6.4 Fourier Transform and Signal Processing System 161
9.7 Spectral Range 161
9.7.1 Far Infrared 161
9.7.2 Mid Infrared 161
9.7.3 Near Infrared 161
9.8 Application of FTIR Spectroscopy 162
9.8.1 Biological Materials 162
9.8.2 Microscopy and Imaging 162
9.8.3 Studies at the Nanoscale and Spectroscopy Below the Diffraction Limit 162
9.8.4 FTIR Systems as Detectors in Chromatography 162
9.8.5 Thermogravimetric Analysis 163
9.8.6 Emission Spectroscopy and IR Chemiluminescence 163
9.8.7 Kinetics of Chemical Reactions and Spectra of Transient Species 163
Questions for Thinking 164
References 164
10 Energy-Dispersive X-Ray (EDX) Spectroscopy of Elements 167
10.1 Principles of EDX Spectroscopy 167
10.1.1 Production of Characteristic X-Rays 167
10.2 A Brief History of EDX Spectrometer Development 169
10.3 Key Components of EDX Spectrometers 170
10.3.1 The X-Ray Generator 170
10.3.2 The Vacuum System 170
10.3.3 The X-Ray Detector 171
10.3.3.1 The Semiconductor Detectors 171
10.3.3.2 The Direct Detectors 172
10.3.3.3 The Indirect Detectors 172
10.3.4 The Signal Processing System 173
10.4 Applications of EDX Spectroscopy 173
10.4.1 Surface Penetration 173
10.4.2 Elemental Resolution, Reliability, and Errors 173
10.4.3 Characteristics of EDX Energy Spectrometers 174
Questions for Thinking 175
References 176
Part III Characterization Methods Based on the Particle (electron Or Electron Beam, Neutron)-matter Interaction 177
11 Scanning Electron Microscopy (SEM) 179
11.1 Interaction Between the Electron Beam and Matter 180
11.1.1 Elastic Scattering 180
11.1.2 Inelastic Scattering 181
11.2 Signal Detection 182
11.2.1 Primary and Secondary Electrons 183
11.2.2 Backscattered Electrons and Auger Electrons 183
11.2.3 The Relation Between Surface Topography and Secondary Electrons 184
11.2.4 The Relation Between Atomic Number z and Backscattered Electrons 184
11.3 History of SEM Development 185
11.4 Key Components of SEM Devices 186
11.4.1 Electron Beam Sources 186
11.4.1.1 Thermionic Electron Guns 186
11.4.1.2 Field-Emission Electron Guns 187
11.4.2 Electronic Detectors 187
11.4.3 Signal Processing and Imaging System 188
11.5 Application and Expansion of SEM 190
11.5.1 Analysis of Powder Particles 190
11.5.2 Fracture Analysis 190
11.5.3 Observation and Analysis Metallographic Structures 190
11.5.4 Dynamic Study of Fracture Processes 191
Questions for Thinking 191
References 191
12 Transmission Electron Microscopy (TEM) 193
12.1 The Interaction Between Electrons and Atoms 193
12.1.1 Transmitted Electrons and Bright-Field Image 195
12.2 Brief History of EM and TEM Development 195
12.3 Key Components of EM and TEM Instruments 198
12.3.1 The Basic Structure of a TEM 198
12.3.1.1 Illumination System 198
12.3.1.2 Electron Gun 199
12.3.1.3 Electromagnetic Lenses 199
12.3.1.4 Imaging System 201
12.3.1.5 Viewing and Recording System 202
12.4 Applications and Extensions of TEM 202
12.4.1 Analysis of Microstructure and Morphology 202
12.4.2 Element Distribution and Morphology Analysis Using EDX Combined with TEM 203
12.4.3 High-Angle Annular Dark-Field (HAADF) STEM 204
Questions for Thinking 205
References 206
13 Spherical-Aberration-Corrected Transmission Electron Microscopy (sac-tem) 207
13.1 The Principle of Spherical Aberration Correction 207
13.2 History of SAC-TEM and Spherical Aberration Correctors 207
13.2.1 The Development of SAC-TEM 207
13.2.2 Spherical Aberration Correctors 208
13.3 Applications of SAC-TEM or SAC-STEM 210
13.3.1 Atomic Structure Characterization 210
13.3.2 Surface and Interface Study 210
13.3.3 Differentiation of Light Elements 211
Questions for Thinking 213
References 213
14 Environmental Transmission Electron Microscopy (ETEM) 215
14.1 Design of Environmental TEM Instruments 216
14.1.1 Windowed Cell 216
14.1.2 Differential Pumping 217
14.2 Applications of ETEM 219
14.2.1 In-Situ Observation of Vapor-Liquid-Solid Growth in the Formation of Nanowires 219
14.2.2 In-Situ Reduction of Metal Oxides 220
14.2.3 Photocatalytic Splitting of Water 222
14.2.4 Particle Formation and Migration 223
14.2.5 Nucleation and Growth of Nanomaterials in Liquid Solution 224
Questions for Thinking 227
References 227
15 Holography 229
15.1 Principles and Foundations 229
15.1.1 The Holographic Principle 229
15.1.2 Electronic Holography 231
15.1.3 Characteristics of Electronic Holography 233
15.2 History 236
15.3 Applications of Electronic Holography 238
15.3.1 The Principle of Observing Electromagnetic Fields with Electronic Holography 238
15.3.2 Fine Structures of Domain Walls in Magnetic Films 239
15.3.3 Micro-Distribution of Magnetic Fields 240
15.3.4 Observing Recorded Magnetization Patterns 240
15.3.5 Quantitative Measurement of Magnetic Moments Using Electron Holography 241
Questions for Thinking 242
References 242
Part IV Characterization Methods for Hyperfine Structures Related to the Magnetic Properties of Electrons and Nuclei 245
16 Nuclear Magnetic Resonance (NMR) Spectroscopy 247
16.1 Basic Theory and Principles 247
16.1.1 Nuclear Spins and Magnetic Moments 247
16.1.2 Relaxation of Nuclear Magnetic Moments 249
16.2 Pulsed Fourier-Transform (FT) NMR Spectrometry 251
16.2.1 Basic Setup of an NMR Spectrometer 251
16.2.2 Basic Operating Principle 252
16.2.3 Parameters and Performance of NMR Measurements 253
16.3 Acquisition of NMR Signals 255
16.3.1 Magnetic Field Gradients 255
16.3.2 Pulse Sequences in MRI 257
Questions for Thinking 259
References 260
17 Mössbauer Effect and Mössbauer Spectroscopy 261
17.1 Introduction 261
17.2 History and Development 262
17.3 Principles and Fundamentals 263
17.3.1 Mössbauer Effect 263
17.3.2 Mössbauer Spectroscopy 264
17.4 Analysis of Mössbauer Spectra 265
17.4.1 Isomer Shift 265
17.4.2 Quadrupole Splitting 266
17.4.3 Magnetic Hyperfine Splitting or Nuclear Zeeman Effect 267
17.5 Instrumentation and Equipment 268
17.5.1 Actuating Device 268
17.5.2 γ-Ray Sources 269
17.5.3 γ-Ray Detectors 269
17.5.4 Amplifier and Pulse-Height Measuring System 271
17.5.5 Data Collector, Processor, and Analyzer 271
17.6 Applications of the Mössbauer Effect and Mössbauer Spectroscopy 272
17.6.1 Features of the Mössbauer Effect and of Mössbauer Spectroscopy 272
17.6.2 Specific Applications 273
Questions for Thinking 275
References 275
Part V Surface Analysis Method 277
18 Atomic Force Microscopy 279
18.1 Detection of Surface Morphology with AFM 279
18.2 History of AFM 281
18.3 Key Components of an AFM Instrument 281
18.3.1 Cantilever and Laser System 281
18.3.1.1 Laser 281
18.3.1.2 Cantilever 281
18.3.2 Piezoelectric Scanner 282
18.3.3 Operating Modes 283
18.3.3.1 Static or Contact Mode 283
18.3.3.2 Dynamic Mode 283
18.3.3.3 Tapping Mode 284
18.3.3.4 Noncontact Mode 285
18.4 Applications and Extensions of AFM 286
18.4.1 Surface Topography 286
18.4.2 Atomic Force Spectroscopy 287
18.4.3 In-situ Observation of Biomolecular Processes 287
18.5 Recent Progress of AFM 288
18.5.1 Principles and Applications of Scanning Near-Field Ultrasonic Holography Under AFM Platform 288
18.5.2 Ultrasonic AFM for the Detection of Subsurface Morphology 288
18.5.3 Photoacoustic Microscopy 290
Questions for Thinking 291
References 291
19 X-Ray Photoelectron Spectroscopy (XPS) 293
19.1 Brief History of XPS Spectroscopy 293
19.2 Applications of XPS Spectroscopy 293
19.2.1 Surface Sensitivity 293
19.2.2 Element Resolution, Reliability, and Error 294
19.2.3 Typical Analysis of XPS Spectra 295
Questions for Thinking 296
References 296
Part VI Some Progress and Perspective 297
20 New and Recent Experimental Techniques 299
20.1 Methods Based on Interactions Between Electromagnetic Waves and Matter 299
20.1.1 Confocal Laser Scanning Fluorescence Microscopy 299
20.1.2 Two-Photon Microscopy 301
20.1.3 Optical-Mode Photoacoustic Microscopy 302
20.1.4 Multicolor 3D Fluorescence Microscopy 303
20.1.5 Optical Coherence Tomography 305
20.1.6 X-Ray Free-Electron Lasers 307
20.1.7 Femtosecond Lasers 308
20.1.7.1 Applications of Femtosecond Lasers 309
20.2 Methods Based on Interactions Between Electrons and Matter 310
20.2.1 Environmental Scanning Electron Microscopy 310
20.2.1.1 Main Features of ESEM 311
20.2.1.2 Representative Applications of ESEM 312
20.2.2 High-Resolution STEM 313
20.2.3 Transmission Electron Cryomicroscopy 314
20.2.4 Scanning-Probe Microscopy 315
Questions for Thinking 316
References 316
Answers to “Questions for Thinking” 319
Index 349
