Table of Contents
1 Introduction to Neutron Techniques Götz Eckold Helmut Schober 1
1.1 Why Neutrons? 1
1.2 Neutron Sources 3
1.3 Techniques 5
1.3.1 Three Axis Spectrometers 6
1.3.2 Backscattering Spectrometers 7
1.3.3 Time-of-Flight Spectrometers 9
1.3.4 Fixed Wavelength Diffractometers 11
1.3.5 Time-of-Flight Diffractometers 12
1.3.6 SANS Instruments 12
1.3.7 Reflectometers 14
1.3.8 Spin-Echo Spectrometers 15
1.4 ... and What About Kinetics? 17
References 17
2 Studying the Hydration of Cement Systems in Real-time Using Quasielastic and Inelastic Neutron Scattering Vanessa K. Peterson 19
2.1 Cement Research 19
2.1.1 Constituents and Hydration 20
2.1.2 Hydration Kinetics 21
2.1.3 Research Tools 22
2.2 Studying Hydrating Cement Using Quasielastic and Inelastic Neutron Scattering 23
2.2.1 Quasielastic Neutron Scattering of Hydrogen in Cement Systems 26
2.2.2 Models for QENS Data 26
2.2.3 Inelastic Neutron Scattering of Hydrogen in Cement Systems 40
2.2.4 Summary of QENS and INS methods 46
2.3 Time-Resolved Quasielastic and Inelastic Neutron Scattering 47
2.3.1 Time-evolution of Descriptive Parameters Derived from Quasielastic and Inelastic Neutron Scattering Data 47
2.3.2 Kinetic Models 57
2.3.3 The Kinetics of Cementitious Hydration using Quasi and Inelastic Neutron Scattering: Case Studies 65
2.4 Conclusions and Outlook 73
References 74
3 Kinetic Properties of Transformations Between Different Amorphous Ice Structures Michael Marek Koza Thomas Hansen Roland P. May Helmut Schober 77
3.1 Introduction 78
3.2 Experimental 81
3.2.1 Sample Preparation and Experimental Procedure 81
3.2.2 Data Treatment 83
3.3 Results 83
3.3.1 Wide Angle Diffraction 83
3.3.2 Small Angle Signal 86
3.4 Discussion 89
3.5 Conclusions 96
References 97
4 Structure Evolution in Materials Studied by Time-Dependent Neutron Scattering N.H. van Dijk 101
4.1 Introduction 101
4.2 Kinetics of Phase Transformations 102
4.3 Time-Resolved Neutron Scattering Techniques 103
4.3.1 Characteristics Neutron Scattering Techniques and Measurement Strategies 103
4.3.2 Comparison Neutron and Synchrotron Studies 105
4.4 Neutron and X-ray Studies During Solidification of Aluminium Alloys 106
4.4.1 Time Resolved Neutron Scattering Experiments 106
4.4.2 Time Resolved X-ray Scattering Experiments 109
4.5 3D Neutron Depolarization Studies 111
4.5.1 Time-Resolved Magnetic Domain Wall Movement 112
4.5.2 Time-Resolved Phase Transformation Kinetics in Steels 114
4.6 Spin-Echo Small-Angle Neutron Scattering 117
4.7 Conclusions and Prospects 120
References 121
5 Applications of In Situ Neutron Diffraction to Optimisation of Novel Materials Synthesis D.P. Riley E.H. Kisi E. Wu T. Hansen P. Henry 123
5.1 Brief Review of In Situ Diffraction and MAX Phase Synthesis 124
5.1.1 Introduction to In Situ Diffraction 124
5.1.2 Review of MAX Phases 125
5.2 In situ Neutron Diffraction: Long Time Scales 127
5.2.1 Ti3SiC2 Reactive Sintering Synthesis Mechanism 127
5.2.2 Ti3AlC2 Reactive Sintering Synthesis Mechanism 129
5.2.3 Ti3SiC2 Synthesis Kinetics 130
5.3 In situ Neutron Diffraction: Short Time Scales 132
5.3.1 Ti3SiC2 SHS Synthesis Mechanism 132
5.3.2 In situ Diffraction Differential Thermal Analysis 134
5.4 Designer Processing Routes from In Situ Neutron Diffraction Analysis 135
5.4.1 Inter-Conversion of MAX Phases 135
5.4.2 Intercalation of the A Element into a Crystalline Precursor 136
5.4.3 Lessons Learned 139
5.5 Design of Future In Situ Diffraction Equipment 140
5.5.1 In Situ Diffraction Chamber Design (Institutional) 141
5.5.2 In Situ Reaction Chamber Design (User Inserts) 144
5.5.3 Assembled ISRC Design 145
References 147
6 Time-Resolved, Electric-Field-Induced Domain Switching and Strain in Ferroelectric Ceramics and Crystals Jacob L. Jones Juan C. Nino Abhijit Pramanick John E. Daniels 149
6.1 Introduction 149
6.1.1 Piezoelectricity, Ferroelectricity, and Device Applications 149
6.1.2 Time-Resolved Neutron Scattering 152
6.1.3 Stroboscopic Techniques 153
6.2 Experimental 154
6.2.1 Materials Under Investigation 154
6.2.2 Instrumentation 155
6.3 Domain Wall Motion in Ferroelectric Ceramics 157
6.3.1 Application of Static Electric Fields 157
6.3.2 Application of Subcoercive, Periodic Electric Fields 159
6.4 Time-Resolved Studies of Lattice Strain in Ferroelectric Ceramics 161
6.5 Domain Switching and Strain in Ferroelectric Relaxor Single Crystals 164
6.6 Future Opportunities and Outlook for Time-Resolved Scattering of Ferroelectrics 169
6.6.1 Instrumentation Developments 170
6.6.2 Application to other Structures and Phenomena 171
6.6.3 Correlation Between Macroscopic Properties and Diffraction Measurements 172
References 173
7 Time-Resolved Phonons as a Microscopic Probe for Solid State Processes Götz Eckold 177
7.1 Introduction 177
7.2 Techniques 178
7.3 Kinetics Between Seconds and Years: Demixing Processes in Simple Systems 181
7.3.1 Basics of Demixing and Phase Diagrams of Silver-Alkali Halides 181
7.3.2 Experimental 184
7.3.3 Nucleation and Growth in KCl-NaCl Mixed Crystals 184
7.3.4 Spinodal Decomposition in AgCl-NaCl Mixed Crystals 184
7.3.5 The Intermediate Case: AgBr-NaBr 194
7.4 Kinetics in the Microsecond Regime: Phase Transitions in Ferroelectrics 203
7.4.1 Modulated Ferroelectrics and Softmode Transitions 203
7.4.2 Experimental 204
7.4.3 The Lock-in Transition in K2SeO4 205
7.4.4 The Ferroelectric Phase in SrTiO3 207
7.5 Concluding Remarks and Future Prospects for Time-Resolved Inelastic Scattering 208
References 210
8 Small Angle Neutron Scattering as a Tool to Study Kinetics of Block Copolymer Micelles Reidar Lund 213
8.1 Introduction 213
8.2 Theoretical Background 216
8.2.1 Brief Introduction of Thermodynamics and Scaling Laws 216
8.2.2 Aniansson and Wall Mechanism 217
8.2.3 Scaling Theory - Halperin and Alexander 218
8.2.4 Other Theories 220
8.3 Experimental Background: Small Angle Neutron Scattering 221
8.3.1 Structure with SANS: Core-Shell Model 221
8.3.2 Equilibrium Kinetics and Time Resolved SANS 224
8.4 Results - Equilibrium Micellar Kinetics 226
8.4.1 Low Molecular Weight Surfactant Micelles 226
8.4.2 Block Copolymer Micelles 227
8.4.3 Amphiphilic Diblock Copolymer Micelles in Aqueous Solutions 228
8.4.4 Diblock Copolymer Micelles in Organic Solvents 233
8.4.5 Triblock Copolymer Micelles in Organic Solvents 235
8.5 Concluding Remarks and Outlook 236
References 238
9 Stroboscopic Small Angle Neutron Scattering Investigations of Microsecond Dynamics in Magnetic Nanomaterials A. Wiedenmann R. Gähler R. P. May U. Keiderling K. Habicht S. Prévost M. Klokkenburg B. Erné J. Kohlbrecher 241
9.1 Introduction 241
9.2 Stroboscopic SANS Techniques 242
9.3 Experimental 245
9.4 Scattering Cross-Sections 246
9.5 Results 248
9.5.1 Relaxation of Magnetic Correlations Toward Equilibrium in Cobalt-FF 248
9.5.2 Response on Oscillating Field in Continuous Stroboscopic SANS 252
9.5.3 Response from Pulsed Stroboscopic Technique TISANE 255
9.5.4 Temperature and Frequency Dependence 256
9.5.5 Co-Precipitates in Solid CuCo Alloy 260
9.6 Discussion 261
9.7 Conclusion 262
References 262
Index 265
