Introduction to Crystal Growth: Principles and Practice teaches readers about crystals and their origins. It offers a historical perspective of the subject and includes background information whenever possible.
The first section of this introductory book takes readers through the historical development and motivation of the field of crystal growth. With more than 40 years of experience in the field, the author covers nucleation, two-dimensional layer growth mechanism, defects in crystals, and screw dislocation theory of crystal growth. He also explains some aspects of the important subject of phase diagrams.
The second section focuses on the experimental techniques of crystal growth. For practicing crystal growers, the book provides nuts-and-bolts techniques and tips. It discusses the major techniques categorized by solid–solid, liquid–solid, and vapor–solid equilibria and describes characterization techniques essential to measuring the quality of grown crystals.

Preface xv

Author xvii

Section I Principles

1. Introduction 3

What Are Crystals? 3

Why Single Crystals? 4

Why Should One Grow Crystals? 6

Historical Perspective 6

Organization of the Book 10

References 11

2. Nucleation Phenomena 13

Critical Supersaturation 13

Homogeneous (Spontaneous) Nucleation 15

Heterogeneous Nucleation 19

Nucleation on a Substrate 20

Nucleation of a Crystalline Material 21

Equilibrium Shape of Anisotropic Nuclei 22

References 23

3. Crystal Growth Mechanisms 25

Early Theories 25

Two-Dimensional Layer Growth Mechanism 28

Surface Nucleation 32

Verifcation 35

References 36

4. Defects in Crystals 37

Point Defects 37

      Vacancy 38

      Schottky Defect 39

      Frenkel Defect 39

      Interstitial Defect 40

      Substitutional Defect 40

      Color Centers 40

Line Defects or Dislocations 41

      Theoretical Estimation of Critical Shear Stress 43

      Refnement in Calculation of Critical Shear Stress 45

      Edge Dislocation 46

      Screw Dislocation 48

      Mixed Dislocation 49

      Burgers Vector 49

      Motion of Dislocations 50

      Energy of a Straight Screw Dislocation 51

      The Force on a Dislocation When a Shear Stress Is Applied 54

      Dislocation Multiplication 56

      Low-Angle Grain Boundaries 57

Planar Defects 58

      Stacking Faults 58

      Twin Boundaries 60

      Grain Boundaries in Polycrystals 61

Bulk Defects 61

References 62

5. Dislocations and Crystal Growth 65

Screw Dislocation Theory of Crystal Growth 65

      The Theory 66

      Experimental Verifcation 68

      Growth from Solution 69

      Shape of Growth Spirals 71

      Interaction of Growth Spirals 72

Vapor–Liquid–Solid Mechanism of Crystal Growth 72

Dendritic Growth 75

References 76

6. Phase Diagrams and Crystal Growth 79

Latent Heat 79

Gibbs’s Free Energy 80

Chemical Potential 81

Gibbs’s Phase Rule 82

Phase Diagrams 83

      Single-Component Systems 83

      Water 84

      Diamond 85

      Two-Component Systems 86

      Two-Component Solid Solutions 86

      Lever Rule 87

      Crystallization Path 88

      Two-Component Eutectic Systems 89

      Two-Component Peritectic Systems 91

      Three-Component Systems 91

      Concentration–Temperature Phase Diagrams (Solubility Curves) 94

Typical Phase Diagrams 96

      Sodium p-Nitrophenolate 96

      Gallium Antimonide 98

      Lithium Niobate 101

      Cesium Lithium Borate 101

      Potassium Titanyl Phosphate (K 2 O–P 2 O 5 –TiO 2 System) 104

References 105

Section II Practice

7. Growth from the Solid Phase 111

Introduction 111

Solid–Solid Growth Methods 112

      Grain Growth 112

      Strain-Annealing Technique 116

      Solid-State Phase Transformation 120

General Conclusions 121

References 122

8. Growth from the Melts 123

Introduction 123

Bridgman–Stockbarger and Related Techniques 124

      General Considerations 124

      Vertical Bridgman Method 124

      Vertical Gradient Freeze Technique 125

      Horizontal Bridgman Method 126

      Equipment 127

      Furnaces 127

      Electrodynamic Gradient Freeze Furnace 128

      Crucibles 129

      Mechanical Movement 130

      Melt–Solid Interface Shape 131

      Examples 133

      Growth of Indium Antimonide 134

      Materials Synthesis 135

      Crystal Growth 135

      Limitations 139

Czochralski and Related Techniques 140

      Equipment 142

      Crucibles 143

      Heaters 144

      Diameter Control 144

      Example 145

      Growth of Congruent Lithium Niobate Crystals 146

      Refned Processes 148

      Growth of Stoichiometric Lithium Niobate 149

      Liquid Encapsulation Technique 149

      Shaped Crystal Growth 151

      Stepanov Method 152

      Edge-Defned, Film-Fed Growth 153

      Micro-Pulling-Down Method 153

Zone-Melting Techniques 155

      Normal and Equilibrium Freezing 155

      Principle of Zone Refning 159

      Segregation due to Single-Zone Pass 159

      Segregation due to Multiple-Zone Passes 160

      Zone Leveling 161

      Zone Freezing 161

      Zone Refning as a Technique for Crystal Growth 162

      Horizontal Confguration 162

      Material Transport 163

      Vertical Confguration: Floating Zone Technique 164

      Zone Stability 165

      Example 166

      Material Synthesis and Preparation of Ingots 166

      Typical Growth Run 167

Flame Fusion Technique 170

      Technical Considerations 172

      Seed Preparation 172

      Burner Design 172

      Powder Preparation and Feeding 173

      Growth Chamber 174

      Typical Crystals Grown 174

Crystal Growth by the Arc Fusion Technique 175

Growth by the Skull-Melting Technique 176

References 178

9. Growth from Liquid Solutions 183

Introduction 183

Growth from Aqueous Solution 183

      Solution and Solubility 184

      Choice of Solvent 185

      Additives 187

      Nucleation 187

      Achievement of Supersaturation 188

      Apparatus 188

      Mason-Jar Method 188

      Holden’s Rotary Crystallizer 190

      Temperature Differential Method 193

      Growth by Fast Crystallization 195

      Growth from Silica Gel 198

      Gel Preparation 199

      Gelling Mechanism and Structure 201

      Apparatus and the Techniques 202

      Kinetics and Mechanism of Growth 204

      Nucleation Control 205

      Hydrothermal Growth 207

      Autoclaves 208

      Full Bridgman 210

      Modifed Bridgman 211

      Heating and Temperature Control 211

      Pressure Measurements 212

      Hydrothermal Growth of Quartz 213

      Growth of Other Materials 214

      Merits and Demerits 214

Flux Growth 215

      Principle 216

      Solvents and Solubility 217

      Apparatus 219

      Crucibles 219

      Furnaces 219

      Temperature Control .220

      Stirring 220

      Techniques of Growth 220

      Growth by Slow Cooling 221

      Growth by Evaporation 222

      Nucleation Control 224

      Growth by Thermal Gradient 225

      Top-Seeded Solution Growth 225

      Traveling Heater/Solvent Method 228

      General Characteristics of Flux-Grown Crystals 229

      Advantages and Disadvantages 231

High-Pressure, High-Temperature Growth 232

      Diamond 232

      Cubic Boron Nitride 235

References 235

10. Crystal Growth from the Vapor Phase 241

Introduction 241

Classifcation 242

Vapor Transport Mechanisms 242

      Convective Flow 242

      Laminar Flow 243

      Diffusion 243

      Thermodiffusion (Soret Effect) 244

      Total Flux 244

Nucleation Control 245

Furnaces 246

Experimental Techniques 246

      Direct Vapor Transport 246

      Closed-Tube System 247

      Growth of Silicon Carbide .248

      Open-Tube System 250

      Chemical Vapor Transport 252

      Growth by Reversible Reaction 252

      Growth by Irreversible Reaction 254

Concluding Remarks 255

References 255

11. Growth of Thin Films 257

Introduction 257

Epitaxial Growth 257

Growth of Thin Films from the Vapor Phase 259

      Vacuum Deposition 259

      Sputtering 260

      Pulsed Laser Deposition 262

      Chemical Vapor Deposition 263

      Metal-Organic Chemical Vapor Deposition 265

      Growth of Diamond Films by the CVD Process 267

      Molecular Beam Epitaxy 268

      Liquid Phase Epitaxy 269

      Tipping Technique 271

      Dipping Technique 272

      Sliding Boat Technique 273

      Surface Morphology 274

Solid Phase Epitaxy 275

References 276

12. Crystal Characterization 279

Introduction 279

Nomenclature 279

Chemical Composition 280

      CHN Analysis 281

      Energy-Dispersive x-Ray Analysis 282

      Inductively Coupled Plasma Atomic Emission Spectroscopy 283

Dopants and Impurities 284

Compositional Inhomogeneities 284

Morphology and Orientation 285

      Goniometry 286

      x-Ray Diffraction 288

Dislocation Content 290

      Chemical Etching 290

      Decoration Technique 291

      x-Ray Topography 292

      Berg–Barrett Technique 293

      Lang Technique 293

      Electron Microscopy 296

Low-Angle Grain Boundaries 297

Twins 298

Inclusions 298

References 300

Appendix I 303

Appendix II 305

Appendix III 309

Appendix IV 311

Index 313

H. L. BHAT obtained his BSc degree from Mysore University and both MSc and PhD degrees from Sardar Patel University, Gujarat, India. He obtained his post Doctoral research training from Strathclyde University, Glasgow, UK. Dr. Bhat joined the Physics department of Indian Institute of Science, Bangalore as a Research Associate in 1973, and progressed steadily to become a professor in 1993. He was the chairman of this department during 2002-06. During 2006-08 he was a CSIR emeritus Scientist. Currently hs is a visiting professor at Centre for Nano and Soft Matter Sciences, Bangalore. His research interests include crystal growth and crystal physics with special reference to ferroelectric, nonlinear optical, semiconductor and magnetic materials. He has over 200 research publications and produced 28 PhDs. He is a member of many professional bodies and currently the Joint Secretary of Materials Research Society of India.

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