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In-situ Electron Microscopy: Applications in Physics, Chemistry and Materials Science

Gerhard Dehm (Editor), James M. Howe (Editor), Josef Zweck (Editor)
ISBN: 978-3-527-31973-2
402 pages
May 2012
In-situ Electron Microscopy: Applications in Physics, Chemistry and Materials Science (3527319735) cover image
Adopting a didactical approach from fundamentals to actual experiments and applications, this handbook and ready reference covers
real-time observations using modern scanning electron microscopy and transmission electron microscopy, while also providing information
on the required stages and samples. The text begins with introductory material and the basics, before describing advancements and applications in dynamic transmission electron microscopy and reflection electron microscopy. Subsequently, the techniques needed to determine growth processes, chemical reactions and oxidation, irradiation effects, mechanical, magnetic, and ferroelectric properties as well as cathodoluminiscence and electromigration are discussed.
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List of Contributors XIII

Preface XVII

Part I Basics and Methods 1

1 Introduction to Scanning Electron Microscopy 3
Christina Scheu and Wayne D. Kaplan

1.1 Components of the Scanning Electron Microscope 4

1.2 Electron–Matter Interaction 16

1.3 Contrast Mechanisms 28

1.4 Electron Backscattered Diffraction (EBSD) 31

1.5 Dispersive X-Ray Spectroscopy 34

1.6 Other Signals 36

1.7 Summary 36

2 Conventional and Advanced Electron Transmission Microscopy 39
Christoph Koch

2.1 Introduction 39

2.2 High-Resolution Transmission Electron Microscopy 48

2.3 Conventional TEM of Defects in Crystals 54

2.4 Lorentz Microscopy 55

2.5 Off-Axis and Inline Electron Holography 57

2.6 Electron Diffraction Techniques 59

2.7 Convergent Beam Electron Diffraction 61

2.8 Scanning Transmission Electron Microscopy and Z-Contrast 63

2.9 Analytical TEM 66

3 Dynamic Transmission Electron Microscopy 71
Thomas LaGrange, Bryan W. Reed, Wayne E. King, Judy S. Kim, and Geoffrey H. Campbell

3.1 Introduction 71

3.2 How Does Single-Shot DTEM Work? 72

3.3 Experimental Applications of DTEM 82

3.4 Crystallization Under Far-from-Equilibrium Conditions 88

3.5 Space Charge Effects in Single-Shot DTEM 90

3.6 Next-Generation DTEM 91

3.7 Conclusions 94

4 Formation of Surface Patterns Observed with Reflection Electron Microscopy 99
Alexander V. Latyshev

4.1 Introduction 99

4.2 Reflection Electron Microscopy 102

4.3 Silicon Substrate Preparation 107

4.4 Monatomic Steps 109

4.5 Step Bunching 111

4.6 Surface Reconstructions 114

4.7 Epitaxial Growth 115

4.8 Thermal Oxygen Etching 116

4.9 Conclusions 119

Part II Growth and Interactions 123

5 Electron and Ion Irradiation 125
Florian Banhart

5.1 Introduction 125

5.2 The Physics of Irradiation 126

5.3 Radiation Defects in Solids 129

5.4 The Setup in the Electron Microscope 131

5.5 Experiments 132

5.6 Outlook 141

6 Observing Chemical Reactions Using Transmission Electron Microscopy 145
Renu Sharma

6.1 Introduction 145

6.2 Instrumentation 146

6.3 Types of Chemical Reaction Suitable for TEM Observation 150

6.4 Experimental Setup 154

6.5 Available Information Under Reaction Conditions 157

6.6 Limitations and Future Developments 164

7 In-Situ TEM Studies of Vapor- and Liquid-Phase Crystal Growth 171
Frances M. Ross

7.1 Introduction 171

7.2 Experimental Considerations 172

7.3 Vapor-Phase Growth Processes 175

7.4 Liquid-Phase Growth Processes 183

7.5 Summary 187

8 In-Situ TEM Studies of Oxidation 191
Guangwen Zhou and Judith C. Yang

8.1 Introduction 191

8.2 Experimental Approach 192

8.3 Oxidation Phenomena 196

8.4 Future Developments 205

8.5 Summary 206

Part III Mechanical Properties 209

9 Mechanical Testing with the Scanning Electron Microscope 211
Christian Motz

9.1 Introduction 211

9.2 Technical Requirements and Specimen Preparation 212

9.3 In-Situ Loading of Macroscopic Samples 214

9.4 In-Situ Loading of Micron-Sized Samples 217

9.5 Summary and Outlook 223

10 In-Situ TEM Straining Experiments: Recent Progress in Stages and Small-Scale Mechanics 227
Gerhard Dehm, Marc Legros, and Daniel Kiener

10.1 Introduction 227

10.2 Available Straining Techniques 228

10.3 Dislocation Mechanisms in Thermally Strained Metallic Films 233

10.4 Size-Dependent Dislocation Plasticity in Metals 239

10.5 Conclusions and Future Directions 247

11 In-Situ Nanoindentation in the Transmission Electron Microscope 255
Andrew M. Minor

11.1 Introduction 255

11.2 Experimental Methodology 260

11.3 Example Studies 263

11.4 Conclusions 272

Part IV Physical Properties 279

12 Current-Induced Transport: Electromigration 281
Ralph Spolenak

12.1 Principles 281

12.2 Transmission Electron Microscopy 283

12.3 Secondary Electron Microscopy 289

12.4 X-Radiography Studies 292

12.5 Specialized Techniques 295

12.6 Comparison of In-Situ Methods 297

13 Cathodoluminescence in Scanning and Transmission Electron Microscopies 303
Yutaka Ohno and Seiji Takeda

13.1 Introduction 303

13.2 Principles of Cathodoluminsecence 304

13.3 Applications of CL in Scanning and Transmission Electron Microscopies 307

13.4 Concluding Remarks 313

14 In-Situ TEM with Electrical Bias on Ferroelectric Oxides 321
Xiaoli Tan

14.1 Introduction 321

14.2 Experimental Details 323

14.3 Domain Polarization Switching 324

14.4 Grain Boundary Cavitation 326

14.5 Domain Wall Fracture 331

14.6 Antiferroelectric-to-Ferroelectric Phase Transition 335

14.7 Relaxor-to-Ferroelectric Phase Transition 341

15 Lorentz Microscopy 347
Josef Zweck

15.1 Introduction 347

15.2 The In-Situ Creation of Magnetic Fields 350

15.3 Examples 362

15.4 Problems 366

15.5 Conclusions 367

References 367

Index 371

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Professor Gerhard Dehm is the department head of Materials Physics at the Montanuniversität Leoben, Austria, and director of the Erich Schmid Institute of Materials Science from the Austrian Academy of Sciences. He has worked previously at the Max-Planck-Institute for Metals Research in Stuttgart and the Department of Materials Engineering at the Technion in Haifa. Gerhard Dehm has authored about 200 scientific publications and organized several international symposia in the field of in situ characterization. He received several scientific awards including the Masing Award from the German Society of Materials Science (DGM) and the award for Nanosciences and Nanotechnology from the State of Styria (Austria).

James M. Howe is the Thomas Goodwin Digges Chaired Professor and Director of the Nanoscale Materials Characterization Facility in the Department of Materials Science and Engineering at the University of Virginia (USA). He has been a visiting professor at the University of Vienna and Osaka University. Dr. Howe has published over 200 technical papers, four book chapters and four symposium proceedings, and is author of the textbook 'Interfaces in Materials' and co-author of the textbook 'Transmission Electron Microscopy and Diffractometry of Materials'. For his research, he has received several awards including a von Humboldt Senior Research Award, the ASM Materials Science Research Silver Medal, and the TMS Champion H. Mathewson Medal.

Professor Josef Zweck is head of the electron microscopy group at the University of Regensburg's physics faculty (Germany). An important branch of his work specializes in imaging of intrinsic magnetic and electrostatic fields and their in-situ manipulation by specialized specimen holders. He is board member of Germany's society for electron microscopy (DGE) since 1996 and presides it in the years 2012 and 2013. He has authored well over 100 scientific publications and is referee for numerous scientific journals. He was involved in numerous organizations of the German Physical society's (DPG, Deutsche Physikalische Gesellschaft) annual meetings, as well as national and international congresses on electron microscopy, especially in 1997 when he hosted the 'Dreiländertagung' ('three countries conference', Austria, Switzerland and Germany) in Regensburg. This congress will return to Regensburg in 2013 as a multinational conference with now 10 countries involved.
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