Eckold / Schober / Nagler Studying Kinetics with Neutrons

Prospects for Time-Resolved Neutron Scattering
1. Auflage 2009
ISBN: 978-3-642-03309-4
Verlag: Springer
Format: PDF
Kopierschutz: 1 - PDF Watermark

E-Book, Englisch, Band 161, 272 Seiten

Reihe: Springer Series in Solid-State Sciences

Neutrons are extremely versatile probes for investigating structure and dynamics in condensed matter. Due to their large penetration depth, they are ideal for in-situ measurements of samples situated in sophisticated and advanced environments. The advent of new high-intensity neutron sources and instruments, as well as the development of new real-time techniques, allows the tracking of transformation processes in condensed matter on a microscopic scale. The present volume provides a review of the state of the art of this new and exciting field of kinetics with neutrons.

Autoren/Hrsg.

Eckold, Götz

Schober, Helmut

Nagler, Stephen E.

Inhaltsverzeichnis

1;Studying Kinetics with Neutrons;3
1.1;1 Introduction to Neutron Techniques;15
1.1.1;1.1 Why Neutrons?;15
1.1.2;1.2 Neutron Sources;17
1.1.3;1.3 Techniques;19
1.1.3.1;1.3.1 Three Axis Spectrometers;20
1.1.3.2;1.3.2 Backscattering Spectrometers;21
1.1.3.3;1.3.3 Time-of-Flight Spectrometers;23
1.1.3.4;1.3.4 Fixed Wavelength Diffractometers;25
1.1.3.5;1.3.5 Time-of-Flight Diffractometers;26
1.1.3.6;1.3.6 SANS Instruments;26
1.1.3.7;1.3.7 Reflectometers;28
1.1.3.8;1.3.8 Spin-Echo Spectrometers;29
1.1.4;1.4 … and What About Kinetics?;31
1.1.5;References;31
1.2;2 Systems in Real-time Using Quasielastic and Inelastic Neutron Scattering;32
1.2.1;2.1 Cement Research;32
1.2.1.1;2.1.1 Constituents and Hydration;33
1.2.1.2;2.1.2 Hydration Kinetics;34
1.2.1.3;2.1.3 Research Tools;35
1.2.2;2.2 Studying Hydrating Cement Using Quasielasticand Inelastic Neutron Scattering;36
1.2.2.1;2.2.1 Quasielastic Neutron Scattering of Hydrogenin Cement Systems;39
1.2.2.2;2.2.2 Models for QENS Data;39
1.2.2.2.1;Empirical Diffusion Models: Rotational Dynamics of Water;40
1.2.2.2.2;The Relaxing Cage Model: Translational-Dynamics of Water;45
1.2.2.2.3;Relaxing Cage Model: Combined Translational-Rotational Dynamics of Water;49
1.2.2.2.4;Jump-Diffusion and Rotation-Diffusion Models: Combined Rotational and Translational Dynamics of Water;51
1.2.2.3;2.2.3 Inelastic Neutron Scattering of Hydrogenin Cement Systems;53
1.2.2.3.1;Vibrational Density of State Studies;53
1.2.2.3.2;Combined Inelastic and Quasielastic Neutron Scattering Studies;56
1.2.2.4;2.2.4 Summary of QENS and INS methods;59
1.2.3;2.3 Time-Resolved Quasielastic and Inelastic Neutron Scattering;60
1.2.3.1;2.3.1 Time-evolution of Descriptive Parameters Derivedfrom Quasielastic and Inelastic Neutron Scattering Data;60
1.2.3.1.1;Fractions from Empirical Diffusion Models of QuasielasticNeutron Scattering Data;61
1.2.3.1.2;Parameters from the Relaxing-Cage Model of Quasielastic Neutron Scattering Data;67
1.2.3.1.3;Parameters from Inelastic Neutron Scattering;68
1.2.3.2;2.3.2 Kinetic Models;70
1.2.3.2.1;Arrhenius Behaviour;71
1.2.3.2.2;Nucleation and Growth;71
1.2.3.2.3;Diffusion-Limited Hydration;75
1.2.3.3;2.3.3 The Kinetics of Cementitious Hydration using Quasiand Inelastic Neutron Scattering: Case Studies;78
1.2.3.3.1;Particle-Size Effects;78
1.2.3.3.2;Comparison of Cementitious Components;80
1.2.3.3.3;Combinations of Cementitious Components;82
1.2.3.3.4;Effect of Additives;83
1.2.4;2.4 Conclusions and Outlook;86
1.2.5;References;87
1.3;3 Kinetic Properties of Transformations Between Different Amorphous Ice Structures;89
1.3.1;3.1 Introduction;90
1.3.2;3.2 Experimental;93
1.3.2.1;3.2.1 Sample Preparation and Experimental Procedure;93
1.3.2.2;3.2.2 Data Treatment;95
1.3.3;3.3 Results;95
1.3.3.1;3.3.1 Wide Angle Diffraction;95
1.3.3.2;3.3.2 Small Angle Signal;98
1.3.4;3.4 Discussion;101
1.3.5;3.5 Conclusions;108
1.3.6;References;109
1.4;4 Structure Evolution in Materials Studiedby Time-Dependent Neutron Scattering;112
1.4.1;4.1 Introduction;112
1.4.2;4.2 Kinetics of Phase Transformations;113
1.4.3;4.3 Time-Resolved Neutron Scattering Techniques;114
1.4.3.1;4.3.1 Characteristics Neutron Scattering Techniquesand Measurement Strategies;114
1.4.3.2;4.3.2 Comparison Neutron and Synchrotron Studies;116
1.4.4;4.4 Neutron and X-ray Studies During Solidificationof Aluminium Alloys;117
1.4.4.1;4.4.1 Time Resolved Neutron Scattering Experiments;117
1.4.4.2;4.4.2 Time Resolved X-ray Scattering Experiments;120
1.4.5;4.5 3D Neutron Depolarization Studies;122
1.4.5.1;4.5.1 Time-Resolved Magnetic Domain Wall Movement;123
1.4.5.2;4.5.2 Time-Resolved Phase Transformation Kinetics in Steels;125
1.4.6;4.6 Spin-Echo Small-Angle Neutron Scattering;128
1.4.7;4.7 Conclusions and Prospects;131
1.4.8;References;132
1.5;5 Applications of In Situ Neutron Diffractionto Optimisation of Novel Materials Synthesis;134
1.5.1;5.1 Brief Review of In Situ Diffractionand MAX Phase Synthesis;135
1.5.1.1;5.1.1 Introduction to In Situ Diffraction;135
1.5.1.2;5.1.2 Review of MAX Phases;136
1.5.2;5.2 In situ Neutron Diffraction: Long Time Scales;138
1.5.2.1;5.2.1 Ti3SiC2 Reactive Sintering Synthesis Mechanism;138
1.5.2.2;5.2.2 Ti3AlC2 Reactive Sintering Synthesis Mechanism;140
1.5.2.3;5.2.3 Ti3SiC2 Synthesis Kinetics;141
1.5.3;5.3 In situ Neutron Diffraction: Short Time Scales;143
1.5.3.1;5.3.1 Ti3SiC2 SHS Synthesis Mechanism;143
1.5.3.2;5.3.2 In situ Diffraction Differential Thermal Analysis;145
1.5.4;5.4 Designer Processing Routes from In Situ Neutron Diffraction Analysis;146
1.5.4.1;5.4.1 Inter-Conversion of MAX Phases;146
1.5.4.2;5.4.2 Intercalation of the A Element into a Crystalline Precursor;147
1.5.4.3;5.4.3 Lessons Learned;150
1.5.5;5.5 Design of Future In Situ Diffraction Equipment;151
1.5.5.1;5.5.1 In Situ Diffraction Chamber Design (Institutional);152
1.5.5.2;5.5.2 In Situ Reaction Chamber Design (User Inserts);155
1.5.5.3;5.5.3 Assembled ISRC Design;156
1.5.6;References;158
1.6;6 Time-Resolved, Electric-Field-Induced Domain Switching and Strain in Ferroelectric Ceramics and Crystals;160
1.6.1;6.1 Introduction;160
1.6.1.1;6.1.1 Piezoelectricity, Ferroelectricity, and Device Applications;160
1.6.1.2;6.1.2 Time-Resolved Neutron Scattering;163
1.6.1.3;6.1.3 Stroboscopic Techniques;164
1.6.1.3.1;Poke and Probe;165
1.6.1.3.2;List Mode;165
1.6.2;6.2 Experimental;165
1.6.2.1;6.2.1 Materials Under Investigation;165
1.6.2.2;6.2.2 Instrumentation;166
1.6.3;6.3 Domain Wall Motion in Ferroelectric Ceramics;168
1.6.3.1;6.3.1 Application of Static Electric Fields;168
1.6.3.2;6.3.2 Application of Subcoercive, Periodic Electric Fields;170
1.6.4;6.4 Time-Resolved Studies of Lattice Strain in Ferroelectric Ceramics;172
1.6.5;6.5 Domain Switching and Strain in Ferroelectric RelaxorSingle Crystals;175
1.6.6;6.6 Future Opportunities and Outlook for Time-Resolved Scattering of Ferroelectrics;180
1.6.6.1;6.6.1 Instrumentation Developments;181
1.6.6.2;6.6.2 Application to other Structures and Phenomena;182
1.6.6.3;6.6.3 Correlation Between Macroscopic Properties and Diffraction Measurements;183
1.6.7;References;184
1.7;7 Time-Resolved Phonons as a Microscopic Probefor Solid State Processes;187
1.7.1;7.1 Introduction;187
1.7.2;7.2 Techniques;188
1.7.3;7.3 Kinetics Between Seconds and Years: Demixing Processes in Simple Systems;191
1.7.3.1;7.3.1 Basics of Demixing and Phase Diagramsof Silver-Alkali Halides;191
1.7.3.2;7.3.2 Experimental;194
1.7.3.3;7.3.3 Nucleation and Growth in KCl–NaCl Mixed Crystals;194
1.7.3.4;7.3.4 Spinodal Decomposition in AgCl–NaCl Mixed Crystals;194
1.7.3.5;7.3.5 The Intermediate Case: AgBr–NaBr;204
1.7.3.5.1;7.3.5.1 Spinodal Decomposition at Low Temperatures;204
1.7.3.5.2;Diffraction and Small Angle Scattering;204
1.7.3.5.3;Inelastic Scattering from Phonons in Single Crystals;206
1.7.3.5.4;Phonon Density of States from Powder Experiments;210
1.7.3.5.5;Nucleation at Elevated Temperature;211
1.7.4;7.4 Kinetics in the Microsecond Regime: Phase Transitions in Ferroelectrics;213
1.7.4.1;7.4.1 Modulated Ferroelectrics and Softmode Transitions;213
1.7.4.2;7.4.2 Experimental;214
1.7.4.3;7.4.3 The Lock-in Transition in K 2SeO4;215
1.7.4.4;7.4.4 The Ferroelectric Phase in SrTiO3;217
1.7.5;7.5 Concluding Remarks and Future Prospects for Time-Resolved Inelastic Scattering;218
1.7.6;References;220
1.8;8 Small Angle Neutron Scattering as a Tool to StudyKinetics of Block Copolymer Micelles;222
1.8.1;8.1 Introduction;222
1.8.2;8.2 Theoretical Background;225
1.8.2.1;8.2.1 Brief Introduction of Thermodynamics and Scaling Laws;225
1.8.2.2;8.2.2 Aniansson and Wall Mechanism;226
1.8.2.3;8.2.3 Scaling Theory – Halperin and Alexander ;227
1.8.2.4;8.2.4 Other Theories;229
1.8.3;8.3 Experimental Background: Small Angle Neutron Scattering;230
1.8.3.1;8.3.1 Structure with SANS: Core-Shell Model;230
1.8.3.2;8.3.2 Equilibrium Kinetics and Time Resolved SANS;233
1.8.4;8.4 Results – Equilibrium Micellar Kinetics;235
1.8.4.1;8.4.1 Low Molecular Weight Surfactant Micelles;235
1.8.4.2;8.4.2 Block Copolymer Micelles;236
1.8.4.3;8.4.3 Amphiphilic Diblock Copolymer Micellesin Aqueous Solutions;237
1.8.4.4;8.4.4 Diblock Copolymer Micelles in Organic Solvents;242
1.8.4.5;8.4.5 Triblock Copolymer Micelles in Organic Solvents;244
1.8.5;8.5 Concluding Remarks and Outlook;245
1.8.6;References;247
1.9;9 Stroboscopic Small Angle Neutron Scattering Investigations of Microsecond Dynamics in Magnetic Nanomaterials;250
1.9.1;9.1 Introduction;250
1.9.2;9.2 Stroboscopic SANS Techniques;251
1.9.3;9.3 Experimental;254
1.9.4;9.4 Scattering Cross-Sections;255
1.9.5;9.5 Results;257
1.9.5.1;9.5.1 Relaxation of Magnetic Correlations Toward Equilibrium in Cobalt-FF;257
1.9.5.2;9.5.2 Response on Oscillating Field in ContinuousStroboscopic SANS;261
1.9.5.3;9.5.3 Response from Pulsed Stroboscopic Technique TISANE;264
1.9.5.4;9.5.4 Temperature and Frequency Dependence;265
1.9.5.5;9.5.5 Co-Precipitates in Solid CuCo Alloy;269
1.9.6;9.6 Discussion;270
1.9.7;9.7 Conclusion;271
1.9.8;References;271
1.10;Index;273