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xiii | |
| Preface |
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xvii | |
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Part I Basics and Methods |
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1 | (122) |
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1 Introduction to Scanning Electron Microscopy |
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3 | (36) |
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1.1 Components of the Scanning Electron Microscope |
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4 | (12) |
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6 | (3) |
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1.1.2 Electromagnetic Lenses |
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9 | (4) |
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13 | (1) |
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13 | (1) |
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1.1.4.1 Everhart-Thornley Detector |
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13 | (2) |
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1.1.4.2 Scintillator Detector |
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15 | (1) |
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1.1.4.3 Solid-State Detector |
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16 | (1) |
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1.1.4.4 In-Lens or Through-the-Lens Detectors |
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16 | (1) |
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1.2 Electron-Matter Interaction |
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16 | (12) |
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1.2.1 Backscattered Electrons (BSEs) |
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20 | (2) |
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1.2.2 Secondary Electrons (SEs) |
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22 | (3) |
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1.2.3 Auger Electrons (AEs) |
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25 | (1) |
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1.2.4 Emission of Photons |
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25 | (1) |
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1.2.4.1 Emission of X-Rays |
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25 | (1) |
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1.2.4.2 Emission of Visible light |
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26 | (1) |
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1.2.5 Interaction Volume and Resolution |
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26 | (1) |
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1.2.5.1 Secondary Electrons |
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27 | (1) |
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1.2.5.2 Backscattered Electrons |
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27 | (1) |
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27 | (1) |
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28 | (3) |
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1.3.1 Topographic Contrast |
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28 | (3) |
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1.3.2 Composition Contrast |
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31 | (1) |
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1.3.3 Channeling Contrast |
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31 | (1) |
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1.4 Electron Backscattered Diffraction (EBSD) |
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31 | (3) |
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1.5 Dispersive X-Ray Spectroscopy |
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34 | (2) |
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36 | (1) |
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36 | (3) |
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37 | (2) |
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2 Conventional and Advanced Electron Transmission Microscopy |
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39 | (32) |
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39 | (9) |
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2.1.1 Introductory Remarks |
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39 | (1) |
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2.1.2 Instrumentation and Basic Electron Optics |
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40 | (2) |
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2.1.3 Theory of Electron-Specimen Interaction |
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42 | (6) |
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2.2 High-Resolution Transmission Electron Microscopy |
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48 | (6) |
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2.3 Conventional TEM of Defects in Crystals |
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54 | (1) |
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55 | (2) |
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2.5 Off-Axis and Inline Electron Holography |
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57 | (2) |
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2.6 Electron Diffraction Techniques |
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59 | (2) |
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2.6.1 Fundamentals of Electron Diffraction |
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59 | (2) |
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2.7 Convergent Beam Electron Diffraction |
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61 | (2) |
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2.7 A Large-Angle Convergent Beam Electron Diffraction |
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63 | (1) |
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2.7.2 Characterization of Amorphous Structures by Diffraction |
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63 | (1) |
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2.8 Scanning Transmission Electron Microscopy and Z-Contrast |
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63 | (3) |
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66 | (5) |
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67 | (4) |
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3 Dynamic Transmission Electron Microscopy |
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71 | (28) |
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71 | (1) |
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3.2 How Does Single-Shot DTEM Work? |
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72 | (10) |
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3.2.1 Current Performance |
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74 | (1) |
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3.2.2 Electron Sources and Optics |
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75 | (5) |
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3.2.3 Arbitrary Waveform Generation Laser System |
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80 | (1) |
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3.2.4 Acquiring High Time Resolution Movies |
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81 | (1) |
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3.3 Experimental Applications of DTEM |
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82 | (6) |
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3.3.1 Diffusionless First-Order Phase Transformations |
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82 | (3) |
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3.3.2 Observing Transient Phenomena in Reactive Multilayer Foils |
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85 | (3) |
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3.4 Crystallization Under Far-from-Equilibrium Conditions |
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88 | (2) |
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3.5 Space Charge Effects in Single-Shot DTEM |
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90 | (1) |
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3.5.1 Global Space Charge |
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90 | (1) |
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3.5.2 Stochastic Blurring |
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91 | (1) |
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91 | (3) |
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3.6.1 Novel Electron Sources |
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91 | (1) |
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92 | (1) |
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93 | (1) |
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3.6.4 Aberration Correction |
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93 | (1) |
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94 | (5) |
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95 | (4) |
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4 Formation of Surface Patterns Observed with Reflection Electron Microscopy |
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99 | (24) |
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99 | (3) |
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4.2 Reflection Electron Microscopy |
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102 | (5) |
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4.3 Silicon Substrate Preparation |
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107 | (2) |
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109 | (2) |
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111 | (3) |
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4.6 Surface Reconstructions |
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114 | (1) |
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115 | (1) |
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4.8 Thermal Oxygen Etching |
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116 | (3) |
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119 | (4) |
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Part II Growth and Interactions |
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123 | (86) |
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5 Electron and Ion Irradiation |
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125 | (20) |
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125 | (1) |
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5.2 The Physics of Irradiation |
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126 | (3) |
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5.2.1 Scattering of Energetic Particles in Solids |
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126 | (2) |
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5.2.2 Scattering of Electrons |
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128 | (1) |
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129 | (1) |
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5.3 Radiation Defects in Solids |
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129 | (2) |
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5.3.1 The Formation of Defects |
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129 | (1) |
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5.3.2 The Migration of Defects |
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130 | (1) |
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5.4 The Setup in the Electron Microscope |
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131 | (1) |
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5.4.1 Electron Irradiation |
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131 | (1) |
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132 | (1) |
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132 | (9) |
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5.5.1 Electron Irradiation |
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133 | (7) |
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140 | (1) |
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141 | (4) |
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142 | (3) |
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6 Observing Chemical Reactions Using Transmission Electron Microscopy |
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145 | (27) |
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145 | (1) |
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146 | (4) |
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6.3 Types of Chemical Reaction Suitable for TEM Observation |
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150 | (4) |
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6.3.1 Oxidation and Reduction (Redox) Reactions |
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150 | (1) |
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6.3.2 Phase Transformations |
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151 | (1) |
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152 | (1) |
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152 | (1) |
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6.3.5 Hydroxylation and Dehydroxylation |
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152 | (1) |
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6.3.6 Nucleation and Growth of Nanostructures |
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153 | (1) |
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154 | (3) |
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6.4.1 Reaction of Ambient Environment with Various TEM Components |
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154 | (1) |
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6.4.2 Reaction of Grid/Support Materials with the Sample or with Each Other |
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154 | (1) |
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6.4.3 Temperature and Pressure Considerations |
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155 | (1) |
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6.4.4 Selecting Appropriate Characterization Technique(s) |
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156 | (1) |
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156 | (1) |
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6.4.6 Independent Verification of the Results, and the Effects of the Electron Beam |
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157 | (1) |
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6.5 Available Information Under Reaction Conditions |
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157 | (7) |
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6.5.1 Structural Modification |
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158 | (1) |
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6.5.1.1 Electron Diffraction |
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158 | (1) |
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6.5.1.2 High-Resolution Imaging |
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158 | (4) |
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162 | (2) |
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6.5.3 Reaction Rates (Kinetics) |
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164 | (1) |
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6.6 Limitations and Future Developments |
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164 | (8) |
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165 | (7) |
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7 In-Situ TEM Studies of Vapor- and Liquid-Phase Crystal Growth |
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172 | (20) |
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171 | (1) |
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7.2 Experimental Considerations |
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172 | (3) |
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7.2.1 What Crystal Growth Experiments are Possible? |
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172 | (1) |
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7.2.2 How Can These Experiments be Made Quantitative? |
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173 | (2) |
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7.2.3 How Relevant Can These Experiments Be? |
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175 | (1) |
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7.3 Vapor-Phase Growth Processes |
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175 | (8) |
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7.3.1 Quantum Dot Growth Kinetics |
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176 | (1) |
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7.3.2 Vapor-Liquid-Solid Growth of Nanowires |
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177 | (3) |
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7.3.3 Nucleation Kinetics in Nanostructures |
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180 | (3) |
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7.4 Liquid-Phase Growth Processes |
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183 | (4) |
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7.4.1 Observing Liquid Samples Using TEM |
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183 | (1) |
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7.4.2 Electrochemical Nucleation and Growth in the TEM System |
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184 | (3) |
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187 | (5) |
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188 | (4) |
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8 In-Situ TEM Studies of Oxidation |
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192 | (17) |
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191 | (1) |
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8.2 Experimental Approach |
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192 | (4) |
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8.2.1 Environmental Cells |
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192 | (1) |
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8.2.2 Surface and Environmental Conditions |
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193 | (1) |
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8.2.3 Gas-Handling System |
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194 | (1) |
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195 | (1) |
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196 | (9) |
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8.3.1 Surface Reconstruction |
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196 | (1) |
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8.3.2 Nucleation and Initial Oxide Growth |
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197 | (1) |
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8.3.3 Role of Surface Defects on Surface Oxidation |
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198 | (1) |
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8.3.4 Shape Transition During Oxide Growth in Alloy Oxidation |
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199 | (3) |
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8.3.5 Effect of Oxygen Pressure on the Orientations of Oxide Nuclei |
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202 | (1) |
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8.3.6 Oxidation Pathways Revealed by High-Resolution TEM Studies of Oxidation |
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203 | (2) |
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205 | (1) |
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206 | (3) |
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206 | (3) |
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Part III Mechanical Properties |
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209 | (70) |
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9 Mechanical Testing with the Scanning Electron Microscope |
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211 | (16) |
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211 | (1) |
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9.2 Technical Requirements and Specimen Preparation |
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212 | (2) |
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9.3 In-Situ Loading of Macroscopic Samples |
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214 | (3) |
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9.3.1 Static Loading in Tension, Compression, and Bending |
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214 | (2) |
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9.3.2 Dynamic Loading in Tension, Compression, and Bending |
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216 | (1) |
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9.3.3 Applications of In-Situ Testing |
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216 | (1) |
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9.4 In-Situ Loading of Micron-Sized Samples |
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217 | (6) |
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9.4.1 Static Loading of Micron-Sized Samples in Tension, Compression, and Bending |
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218 | (2) |
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9.4.2 Applications of In-Situ Testing of Small-Scale Samples |
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220 | (2) |
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9.4.3 In-Situ Microindentation and Nanoindentation |
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222 | (1) |
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223 | (4) |
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223 | (4) |
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10 In-Situ TEM Straining Experiments: Recent Progress in Stages and Small-Scale Mechanics |
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227 | (28) |
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227 | (1) |
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10.2 Available Straining Techniques |
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228 | (5) |
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228 | (1) |
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10.2.2 Mechanical Straining |
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229 | (1) |
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10.2.3 Instrumented Stages and MEMS/NEMS Devices |
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230 | (3) |
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10.3 Dislocation Mechanisms in Thermally Strained Metallic Films |
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233 | (6) |
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233 | (2) |
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10.3.2 Dislocation Motion in Single Crystalline Films and Near Interfaces |
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235 | (1) |
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10.3.3 Dislocation Nucleation and Multiplication in Thin Films |
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236 | (3) |
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10.3.4 Diffusion-Induced Dislocation Plasticity in Polycrystalline Cu Films |
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239 | (1) |
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10.4 Size-Dependent Dislocation Plasticity in Metals |
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239 | (8) |
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10.4.1 Plasticity in Geometrically Confined Single Crystal fee Metals |
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241 | (2) |
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10.4.2 Size-Dependent Transitions in Dislocation Plasticity |
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243 | (1) |
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10.4.3 Plasticity by Motion of Grain Boundaries |
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244 | (1) |
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10.4.4 Influence of Grain Size Heterogeneities |
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245 | (2) |
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10.5 Conclusions and Future Directions |
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247 | (8) |
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248 | (7) |
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11 In-Situ Nanoindentation in the Transmission Electron Microscope |
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255 | (24) |
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255 | (5) |
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11.1.1 The Evolution of In-Situ Mechanical Probing in a TEM |
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255 | (1) |
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11.1.2 Introduction to Nanoindentation |
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256 | (4) |
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11.2 Experimental Methodology |
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260 | (3) |
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263 | (9) |
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11.3.1 In-Situ TEM Nanoindentation of Silicon |
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263 | (6) |
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11.3.2 In-Situ TEM Nanoindentation of Al Thin Films |
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269 | (3) |
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272 | (7) |
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274 | (5) |
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Part IV Physical Properties |
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279 | (92) |
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12 Current-Induced Transport: Electromigration |
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281 | (22) |
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281 | (2) |
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12.2 Transmission Electron Microscopy |
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283 | (6) |
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283 | (5) |
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288 | (1) |
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12.2.3 Convergent Beam Electron Diffraction (CBED): Measurements of Elastic Strain |
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288 | (1) |
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12.3 Secondary Electron Microscopy |
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289 | (3) |
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289 | (2) |
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12.3.2 Elemental Analysis |
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291 | (1) |
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12.3.3 Electron Backscatter Diffraction (EBSD) |
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292 | (1) |
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12.4 X-Radiography Studies |
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292 | (3) |
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12.4.1 Microscopy and Tomography |
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292 | (1) |
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293 | (1) |
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294 | (1) |
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294 | (1) |
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12.5 Specialized Techniques |
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295 | (2) |
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295 | (1) |
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12.5.2 Reflective High-Energy Electron Diffraction (RHEED) |
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296 | (1) |
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12.5.3 Scanning Probe Methods |
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296 | (1) |
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12.6 Comparison of M-Situ Methods |
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297 | (6) |
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299 | (4) |
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13 Cathodoluminescence in Scanning and Transmission Electron Microscopies |
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303 | (18) |
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303 | (1) |
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13.2 Principles of Cathodoluminsecence |
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304 | (3) |
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13.2.1 The Generation and Recombination of Electron-Hole Pairs |
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304 | (1) |
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13.2.2 Characteristic of CL Spectroscopy |
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305 | (1) |
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13.2.3 CL Imaging and Contrast Analysis |
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306 | (1) |
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13.2.4 Spatial Resolution of CL Imaging and Spectroscopy |
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306 | (1) |
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13.2.5 CL Detection Systems |
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307 | (1) |
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13.3 Applications of CL in Scanning and Transmission Electron Microscopies |
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307 | (6) |
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13.3.1 Assessments of Group III-V Compounds |
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308 | (1) |
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308 | (1) |
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13.3.1.2 III-V Compounds Except Nitrides |
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309 | (1) |
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13.3.2 Group II---VI Compounds and Related Materials |
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310 | (1) |
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310 | (2) |
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13.3.2.2 Group II-VI Compounds, Except Oxides |
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312 | (1) |
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13.3.3 Group IV and Related Materials |
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313 | (1) |
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313 | (8) |
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313 | (8) |
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14 In-Situ TEM with Electrical Bias on Ferroelectric Oxides |
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321 | (26) |
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321 | (2) |
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14.2 Experimental Details |
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323 | (1) |
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14.3 Domain Polarization Switching |
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324 | (2) |
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14.4 Grain Boundary Cavitation |
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326 | (5) |
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14.5 Domain Wall Fracture |
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331 | (4) |
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14.6 Antiferroelectric-to-Ferroelectric Phase Transition |
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335 | (6) |
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14.7 Relaxor-to-Ferroelectric Phase Transition |
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341 | (6) |
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345 | (2) |
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347 | (24) |
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347 | (3) |
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15.2 The In-Situ Creation of Magnetic Fields |
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350 | (12) |
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15.2.1 Combining the Objective Lens Field with Specimen Tilt |
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351 | (1) |
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15.2.2 Magnetizing Stages Using Coils and Pole-Pieces |
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352 | (4) |
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15.2.3 Magnetizing Stages Without Coils |
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356 | (1) |
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356 | (2) |
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15.2.3.2 Spin Torque Applications |
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358 | (3) |
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15.2.3.3 Self-Driven Devices |
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361 | (1) |
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362 | (4) |
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15.3.1 Demagnetization and Magnetization of Ring Structures |
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362 | (2) |
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15.3.2 Determination of Wall Velocities |
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364 | (1) |
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15.3.3 Determination of Stray Fields |
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365 | (1) |
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366 | (1) |
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367 | (4) |
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367 | (4) |
| Index |
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371 | |