Inorganic materials show a diverse range of important properties that are desirable for many contemporary, real-world applications. Good examples include recyclable battery cathode materials for energy storage and transport, porous solids for capture and storage of gases and molecular complexes for use in electronic devices. An understanding of the function of these materials is necessary in order to optimise their behaviour for real applications, hence the importance of 'structure-property relationships'.

The chapters presented in this volume deal with recent advances in the characterisation of crystalline materials. They include some familiar diffraction methods, thoroughly updated with modern advances. Also included are techniques that can now probe details of the three-dimensional arrangements of atoms in nanocrystalline solids, allowing aspects of disorder to be studied. Small-angle scattering, a technique that is often overlooked, can probe both ordered and disordered structures of materials at longer length scales than those probed by powder diffraction methods.

Addressing both physical principals and recent advances in their applications, Structure from Diffraction Methods covers:

• Powder Diffraction
• X-Ray and Neutron Single-Crystal Diffraction
• PDF Analysis of Nanoparticles
• Electron Crystallography
• Small-Angle Scattering

Ideal as a complementary reference work to other volumes in the series (Local Structural Characterisation and Multi Length-Scale Characterisation), or as an examination of the specific characterisation techniques in their own right, Structure from Diffraction Methods is a valuable addition to the Inorganic Materials Series.

Autorentext

I have truly come a long way without rest. Born into a humble background, I now appreciate the taste of gradually achieving success in life. If everything had been accomplished from the beginning, what fun would life have held? The author of this book, Lawyer Bruce Yoon, worked as a Foreign Affairs Detective in Korea for five years before studying abroad in Australia, where he began studying computer science. He then explored software development and consulting while searching for his purpose. During that time, he pursued theological studies and later participated in M&A projects. Following his involvement in IT/BT businesses, he enrolled in law school and became an attorney.

Inhalt

Inorganic Materials Series Preface xi Preface xiii

List of Contributors xv

1 Powder Diffraction 1
Kenneth D. M. Harris and Andrew Williams

1.1 Introduction 1

1.2 The Similarities and Differences Between Single-Crystal nd Powder XRD 2

1.3 Qualitative Aspects of Powder XRD: 'Fingerprinting' of Crystalline Phases 6

1.4 Quantitative Aspects of Powder XRD: Some reliminaries Relevant to Crystal Structure Determination 8

1.4.1 Relationship between a Crystal Structure and its Diffraction Pattern 8

1.4.2 Comparison of Experimental and Calculated Powder XRD Patterns 10

1.5 Structure Determination from Powder XRD Data 12

1.5.1 Overview 12

1.5.2 Unit Cell Determination (Indexing) 14

1.5.3 Preparing the Intensity Data for Structure Solution: Profile Fitting 15

1.5.4 Structure Solution 16

1.5.5 Structure Refinement 21

1.6 Some Experimental Considerations in Powder XRD 22

1.6.1 Synchrotron versus Laboratory Powder XRD Data 22

1.6.2 Preferred Orientation 24

1.6.3 Phase Purity of the Powder Sample 25

1.6.4 Analysis of Peak Widths in Powder XRD Data 26

1.6.5 Applications of Powder XRD for In Situ Studies of Structural Transformations and Chemical Processes 28

1.7 Powder Neutron Diffraction versus Powder XRD 30

1.8 Validation of Procedures and Results in Structure Determination from Powder XRD Data 33

1.8.1 Overview 33

1.8.2 Validation before Direct-Space Structure Solution 34

1.8.3 Aspects of Validation following Structure Refinement 36

1.9 A more Detailed Consideration of the Application of Powder XRD as a 'Fingerprint' of Crystalline Phases 40

1.10 Examples of the Application of Powder XRD in Chemical Contexts 45

1.10.1 Overview 45

1.10.2 Structure Determination of Zeolites and Other Framework Materials 46

1.10.3 In Situ Powder XRD Studies of Materials Synthesis 48

1.10.4 Structure Determination of New Materials Produced by Solid-State Mechanochemistry 50

1.10.5 In Situ Powder XRD Studies of Solid-State Mechanochemical Processes 53

1.10.6 In Situ Powder XRD Studies of a Polymorphic Transformation 55

1.10.7 In Situ Powder XRD Studies of a Solid-State Reaction 58

1.10.8 Establishing Details of a Hydrogen-Bonding Arrangement by Powder Neutron Diffraction 58

1.10.9 Structure Determination of a Material Produced by Rapid Precipitation from Solution 60

1.10.10 Structure Determination of Intermediates in a Solid-State Reaction 62

1.10.11 Structure Determination of a Novel Aluminium Methylphosphonate 62

1.10.12 Structure Determination of Materials Prepared by Solid-State Dehydration/Desolvation Processes 63

1.10.13 Structure Determination of the Product Material from a Solid-State Photopolymerisation Reaction 66

1.10.14 Exploiting Anisotropic Thermal Expansion in Structure Determination 68

1.10.15 Rationalisation of a Solid-State Reaction 69

1.10.16 Structure Determination of Organometallic Complexes 71

1.10.17 Examples of Structure Determination of Some Polymeric Materials 72

1.10.18 Structure Determination of Pigment Materials 73

1.11 Conclusion 74

References 75

2 X-Ray and Neutron Single-Crystal Diffraction 83
William Clegg

2.1 Introduction 83

2.2 Solid-State Fundamentals 86

2.2.1 Translation Symmetry 87

2.2.2 Other Symmetry 91

2.2.3 An Introduction to Non-Ideal Behaviour 98

2.3 Scattering and Diffraction 101

2.3.1 Fundamentals of Radiation and Scattering 102

2.3.2 Diffraction of Monochromatic X-Rays 103

2.3.3 Diffraction of Polychromatic X-Rays 110

2.3.4 Diffraction of Neutrons 111

2.3.5 Some Competing and Complicating Effects 114

2.4 Experimental Methods 119

2.4.1 Radiation Sources 119

2.4.2 Single Crystals 124

2.4.3 Measuring the Diffraction Pattern 126

2.4.4 Correcting for Systematic Errors 127

2.5 Structure Solution 128

2.5.1 Direct Methods 130

2.5.2 Patterson Synthesis 131

2.5.3 Symmetry Arguments 132

2.5.4 Charge Flipping 133

2.5.5 Completing a Partial Structure Model 134

2.6 Structure Refinement 138

2.6.1 Minimisation and Weights 139

2.6.2 Parameters, Constraints and Restraints 139

2.6.3 Refinement Results 140

2.6.4 Computer Programs for Structure Solution and Refinement 141

2.7 Problem Structures, Special Topics, Validation and Interpretation 142

2.7.1 Disorder 142

2.7.2 Twinning 143

2.7.3 Pseudosymmetry, Superstructures and Incommensurate Structures 145

2.7.4 Absolute Structure 147

2.7.5 Distinguishing Element Types, Oxidation States and Spin States 148

2.7.6 Valence Effects 149

2.7.7 Diffraction Experiments under Non-Ambient Conditions 150

2.7.8 Issues of Interpretation and Validation 151

Software Acknowledgements 153

References 153

3 PDF Analysis of Nanoparticles 155
Reinhard B. Neder

3.1 Introduction 155

3.2 Pair Distribution Function 160

3.3 Data Collection Strategies 168

3.4 Data Treatment 170

3.4.1 Calculation of G(r) from a Structural Model 175

3.4.2 Data Modelling 183

3.5 Examples 184

3.5.1 Local Disorder versus Long-Range Average Order 185

3.5.2 ZnSe Nanoparticle 189

3.5.3 Decorated ZnO Nanoparticle 194

3.6 Complementary Techniques 197

References 199

4 Electron Crystallography 201
Lu Han, Keiichi Miyasaka and Osamu Terasaki

4.1 Introduction 201

4.2 Crystal Description 203

4.2.1 Fourier Transformation and Related Functions 203

4.2.2 Lattices 204

4.2.3 Crystals and Crystal Structure Factors 205

4.2.4 Simple Description of Babinet's Principle 206

4.3 Electron Microscopy 208

4.3.1 Interaction between Electrons and M…