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The book consists of a series of edited chapters, each written by an expert in the field and focusing on a particular characterization technique as applied to glass. The book covers a variety of techniques ranging from the very common (like Raman and FTIR) to the most recent (and less well known) ones, like SEM for structural analysis and photoelastic measurements. The level of the chapters make it suitable for researchers and for graduate students about to start their research work. It will also: discuss the technique itself, background, nuances when it comes to looking at glassy materials,…mehr
The book consists of a series of edited chapters, each written by an expert in the field and focusing on a particular characterization technique as applied to glass. The book covers a variety of techniques ranging from the very common (like Raman and FTIR) to the most recent (and less well known) ones, like SEM for structural analysis and photoelastic measurements. The level of the chapters make it suitable for researchers and for graduate students about to start their research work. It will also:
discuss the technique itself, background, nuances when it comes to looking at glassy materials, interpretation of results, case studies, and recent and near-future innovations
Fill a widening gap in modern techniques for glass characterization
Provide much needed updates on the multiple essential characterization techniques
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Autorenporträt
Mario Affatigato, PhD,is currently Professor of Physics at Coe College, Iowa. Prof. Affatigato's research interests include optical properties of glasses and the relationship between those properties and the structure of the glass. He was awarded the Presidential Early Career Award for Scientists and Engineers in 1999, and the Faculty Member Prize for Research in an Undergraduate Institution in 2013 by the American Physical Society. He has published over 80 papers in refereed journals.
Inhaltsangabe
Preface xiii List of Contributors xv 1 DENSITY, THERMAL PROPERTIES, AND THE GLASS TRANSITION TEMPERATURE OF GLASSES 1 Steve Feller Part I: Introduction to Physical Properties and Their Uses 1 Part II: Density 2 1.1 Density: Experimental Background and Theory 2 1.1.1 Overview 2 1.1.2 Experimental Methods and Theory 3 1.1.3 Instrumentation Used for Determining Density 7 1.1.4 Analysis of Data, Extraction of Useful Information, and Other Ways to Express Density 8 1.1.5 Case Studies from Some Glass Systems 13 1.1.6 Conclusion to Density Measurements 19 Part III: Thermal Effects with a Focus on the Glass Transition Temperature 20 1.2 OVERVIEW 20 1.3 EXPERIMENTAL METHODS AND THEORY 20 1.3.2 Differential Thermal Analysis 22 1.4 INSTRUMENTATION USED FOR DETERMINING Tg AND RELATED THERMAL EVENTS 23 1.4.1 DSCs 23 1.4.2 Differential Thermal Analysis 23 1.5 ANALYSIS OF DATA AND EXTRACTION OF USEFUL INFORMATION 25 1.6 CASE STUDIES FROM GLASS SYSTEMS 26 1.6.1 The Glass Transition Temperatures of Barium Borosilicate Glasses [18] 26 1.6.2 Stability Parameters in Lithium Borate Glasses [18] 27 1.7 CONCLUSION TO THERMAL PROPERTIES 30 2 INFRARED SPECTROSCOPY OF GLASSES 32 E.I. Kamitsos 2.1 INTRODUCTION 32 2.2 BACKGROUND AND THEORY 34 2.2.1 Refractive Index and Dielectric Function 34 2.2.2 Reflectance Spectroscopy of Bulk Materials 36 2.2.3 Infrared Spectra of Thin Films 42 2.3 INSTRUMENTATION 44 2.4 ANALYSIS OF INFRARED DATA 48 2.4.1 Bulk Glasses 48 2.4.2 Thin Films of Amorphous Materials 52 2.5 CASE STUDIES 54 2.5.1 Bulk Glasses 54 2.5.2 Glass Thin Films 63 2.6 CONCLUSIONS 68 3 RAMAN SPECTROSCOPY OF GLASSES 74 Rui M. Almeida and Luis F. Santos 3.1 INTRODUCTION 74 3.2 BACKGROUND 76 3.2.1 Theory 76 3.2.2 Selection Rules 78 3.2.3 Depolarization of Raman Lines 79 3.3 INSTRUMENTATION AND DATA ANALYSIS 80 3.3.1 Light Source 81 3.3.2 Sample Compartment 82 3.3.3 Spectrometer 82 3.3.4 Detector 83 3.3.5 Micro-Raman Spectrometers 84 3.3.6 Resolution 85 3.3.7 Data Analysis 86 3.4 CASE STUDIES 87 3.4.1 Structural Effects of Alkali Incorporation in Silicate Glasses 87 3.4.2 Phase Separation Mechanisms in Transition Metal Phosphate Glasses 92 3.4.3 Raman Study of Niobium Germanosilicate Glasses And Glass-Ceramics 96 3.4.4 Raman Spectroscopy of Chalcogenide Glasses 99 3.5 CONCLUSIONS 103 4 BRILLOUIN LIGHT SCATTERING 107 John Kieffer 4.1 INTRODUCTION 107 4.2 BACKGROUND AND THEORY 110 4.3 INSTRUMENTATION 117 4.4 DATA ANALYSIS AND INFORMATION CONTENT 126 4.5 EXAMPLES OF CASE STUDIES 133 4.5.1 Room-Temperature Glass 133 4.5.2 Temperature Dependence, Glass Transition, and Visco-Elasticity 137 4.5.3 Spatially Confined Systems (e.g., Thin Films) 146 4.5.4 Systems Under Pressure 149 4.5.5 Mechanically Fragile Systems, Soft Matter, and Gels 151 4.6 SUMMARY 154 5 NEUTRON DIFFRACTION TECHNIQUES FOR STRUCTURAL STUDIES OF GLASSES 158 Alex C. Hannon 5.1 INTRODUCTION 158 5.2 INSTRUMENTATION 159 5.2.1 The Neutron 159 5.2.2 The Interactions between a Neutron and a Sample 160 5.2.3 Neutron Sources 161 5.2.4 Neutron Diffractometers 164 5.3 THEORETICAL ASPECTS OF NEUTRON DIFFRACTION ON GLASSES 169 5.3.1 The Static Approximation 169 5.3.2 Scattering from a Single Nucleus 169 5.3.3 Scattering from an Assembly of Nuclei 170 5.3.4 Isotropic Samples 171 5.3.5 Coherent and Incoherent (Distinct and Self) Scattering 171 5.3.6 Atomic Vibrations 173 5.3.7 Real-space Correlation Functions 180 5.4 THE APPLICATION OF NEUTRON DIFFRACTION TO STUDIES OF GLASS STRUCTURE 186 5.4.1 Experimental Corrections 186 5.4.2 Resolution 190 5.4.3 Peak Fitting and Integration 194 5.4.4 Normalization of Data 198 5.4.5 Scattering at low Q 200 5.4.6 Sample-Related Difficulties 203 5.4.7 Partial Correlation Functions 209 5.4.8 Interpretation of Results 218 5.4.9 Modeling 226 5.4.10 The PDF Method 229 6 X-RAY DIFFRACTION FROM GLASS 241 Christopher J. Benmore 6.1 INTRODUCTION 241 6.2 BACKGROUND/THEORY 244 6.3 ANALYSIS OF DATA, EXTRACTION OF USEFUL INFORMATION 249 6.4 INSTRUMENTATION 255 6.5 CASE STUDIES 258 6.5.1 SiO2 and Oxide Glasses 258 6.5.2 Chalcogenide Glasses 263 6.5.3 Amorphous Materials, Gels, Foams and Fibers 264 6.6 CONCLUSIONS 264 7 XAFS SPECTROSCOPY AND GLASS STRUCTURE 271 Giuseppe Dalba and Francesco Rocca 7.1 INTRODUCTION 271 7.2 THE ORIGINS OF X-RAY ABSORPTION SPECTRA 272 7.3 XAFS INSTRUMENTATION 274 7.4 THE PHYSICAL MECHANISM OF XAFS 278 7.5 EXAFS 279 7.5.1 EXAFS Formula for Glasses 282 7.6 XAFS DATA ANALYSIS 284 7.6.1 Corrections for Instrumental Errors 284 7.6.2 Pre-edge Background Subtraction 284 7.6.3 Post-edge Background Subtraction 285 7.6.4 Normalization 286 7.6.5 Conversion to k-Space, Choice of Threshold Energy E0 and Weighting 286 7.6.6 Transformation from k-Space to R-Space 286 7.6.7 Fourier Filtering: Reverse Transformation: from R-Space to k-Space 287 7.6.8 Log Amplitude Ratio and Phases Difference Method 288 7.6.9 Fitting Procedure 288 7.7 EXAFS ACCURACY AND LIMITATIONS 289 7.8 XANES 290 7.9 XAFS SPECTROSCOPY APPLIED TO GLASS STRUCTURE: SOME EXAMPLES 291 7.9.1 Silicate Glasses 292 7.9.2 Silica Glass 294 7.9.3 Silica at High Temperature 294 7.9.4 Silica and Germania Glasses under High Pressure 297 7.9.5 Nanoparticles Embedded in Glasses 300 7.9.6 Study of Ionic Conductivity in Superionic Conducting Glasses Doped with AgI 307 7.10 SUMMARY AND CONCLUSIONS 309 8 NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY OF GLASSES 315 Scott Kroeker 8.1 INTRODUCTION 315 8.2 THEORETICAL BACKGROUND 316 8.2.1 Zeeman Effect 316 8.2.2 Magnetic Shielding 318 8.2.3 Quadrupolar Interaction 319 8.2.4 Dipolar Interactions 320 8.2.5 High Resolution Methodologies 320 8.3 INSTRUMENTATION 323 8.3.1 Magnet 323 8.3.2 Probe 325 8.3.3 Radiofrequency Components 326 8.3.4 Computer Control 326 8.3.5 Measurement Uncertainty 327 8.4 DATA ANALYSIS AND STRUCTURAL INTERPRETATION 329 8.4.1 Chemical Shift Assignments 329 8.4.2 Information from Quadrupolar Effects 330 8.4.3 Low-gamma Nuclei 332 8.4.4 Paramagnetic Effects 333 8.5 CASE STUDIES 333 8.5.1 Borophosphate Glasses 333 8.5.2 Aluminosilicate Glasses 336 8.5.3 Borosilicate Glasses 337 8.5.4 Modifier Cations in Alkali Borate Glasses 340 8.6 CONCLUSIONS 341 9 ADVANCED DIPOLAR SOLID STATE NMR SPECTROSCOPY OF GLASSES 345 Hellmut Eckert 9.1 INTRODUCTION 345 9.2 THEORETICAL ASPECTS 347 9.2.1 Direct Magnetic Dipole-Dipole Coupling 348 9.2.2 Indirect Magnetic Dipole-Dipole Coupling 349 9.3 HETERONUCLEAR EXPERIMENTS 349 9.3.1 Spin Echo Double Resonance 349 9.3.2 Rotational Echo Double Resonance 350 9.3.3 Rotational Echo Adiabatic Passage Double Resonance 353 9.3.4 Cross-polarization 354 9.3.5 Connectivity Studies Based on the Detection of Indirect Spin-Spin Interactions 358 9.3.6 Instrumental Considerations and Caveats. 358 9.4 HOMONUCLEAR EXPERIMENTS 360 9.4.1 Static Spin Echo Decay Spectroscopy 360 9.4.2 Homonuclear Dipolar Recoupling Experiments 362 9.4.3 Instrumental Considerations and Caveats 369 9.5 CASE STUDIES 370 9.5.1 Spatial Distributions of Mobile Ions in Alkali Silicate and Borate Glasses 370 9.5.2 Connectivity Distribution in 70 SiO2-30 [(Al2 O3)x(P2O5)1-x] Glasses 374 9.5.3 Speciations and Connectivity Distributions in Borophosphate and Thioborophosphate Glasses 380 10 ATOM PROBE TOMOGRAPHY OF GLASSES 391 Daniel Schreiber and Joseph V. Ryan 10.1 INTRODUCTION 391 10.2 BACKGROUND AND THEORY 392 10.3 INSTRUMENTATION 395 10.3.1 APT Specimen Preparation 399 10.3.2 Experimental Procedure and Parameters 401 10.3.3 Data Reconstruction 403 10.4 ANALYSIS METHODS 409 10.4.1 Estimating Error 412 10.5 CASE STUDIES 417 10.5.1 Composition 418 10.5.2 Interfaces 420 10.5.3 Conclusions 424 Index 431
Preface xiii List of Contributors xv 1 DENSITY, THERMAL PROPERTIES, AND THE GLASS TRANSITION TEMPERATURE OF GLASSES 1 Steve Feller Part I: Introduction to Physical Properties and Their Uses 1 Part II: Density 2 1.1 Density: Experimental Background and Theory 2 1.1.1 Overview 2 1.1.2 Experimental Methods and Theory 3 1.1.3 Instrumentation Used for Determining Density 7 1.1.4 Analysis of Data, Extraction of Useful Information, and Other Ways to Express Density 8 1.1.5 Case Studies from Some Glass Systems 13 1.1.6 Conclusion to Density Measurements 19 Part III: Thermal Effects with a Focus on the Glass Transition Temperature 20 1.2 OVERVIEW 20 1.3 EXPERIMENTAL METHODS AND THEORY 20 1.3.2 Differential Thermal Analysis 22 1.4 INSTRUMENTATION USED FOR DETERMINING Tg AND RELATED THERMAL EVENTS 23 1.4.1 DSCs 23 1.4.2 Differential Thermal Analysis 23 1.5 ANALYSIS OF DATA AND EXTRACTION OF USEFUL INFORMATION 25 1.6 CASE STUDIES FROM GLASS SYSTEMS 26 1.6.1 The Glass Transition Temperatures of Barium Borosilicate Glasses [18] 26 1.6.2 Stability Parameters in Lithium Borate Glasses [18] 27 1.7 CONCLUSION TO THERMAL PROPERTIES 30 2 INFRARED SPECTROSCOPY OF GLASSES 32 E.I. Kamitsos 2.1 INTRODUCTION 32 2.2 BACKGROUND AND THEORY 34 2.2.1 Refractive Index and Dielectric Function 34 2.2.2 Reflectance Spectroscopy of Bulk Materials 36 2.2.3 Infrared Spectra of Thin Films 42 2.3 INSTRUMENTATION 44 2.4 ANALYSIS OF INFRARED DATA 48 2.4.1 Bulk Glasses 48 2.4.2 Thin Films of Amorphous Materials 52 2.5 CASE STUDIES 54 2.5.1 Bulk Glasses 54 2.5.2 Glass Thin Films 63 2.6 CONCLUSIONS 68 3 RAMAN SPECTROSCOPY OF GLASSES 74 Rui M. Almeida and Luis F. Santos 3.1 INTRODUCTION 74 3.2 BACKGROUND 76 3.2.1 Theory 76 3.2.2 Selection Rules 78 3.2.3 Depolarization of Raman Lines 79 3.3 INSTRUMENTATION AND DATA ANALYSIS 80 3.3.1 Light Source 81 3.3.2 Sample Compartment 82 3.3.3 Spectrometer 82 3.3.4 Detector 83 3.3.5 Micro-Raman Spectrometers 84 3.3.6 Resolution 85 3.3.7 Data Analysis 86 3.4 CASE STUDIES 87 3.4.1 Structural Effects of Alkali Incorporation in Silicate Glasses 87 3.4.2 Phase Separation Mechanisms in Transition Metal Phosphate Glasses 92 3.4.3 Raman Study of Niobium Germanosilicate Glasses And Glass-Ceramics 96 3.4.4 Raman Spectroscopy of Chalcogenide Glasses 99 3.5 CONCLUSIONS 103 4 BRILLOUIN LIGHT SCATTERING 107 John Kieffer 4.1 INTRODUCTION 107 4.2 BACKGROUND AND THEORY 110 4.3 INSTRUMENTATION 117 4.4 DATA ANALYSIS AND INFORMATION CONTENT 126 4.5 EXAMPLES OF CASE STUDIES 133 4.5.1 Room-Temperature Glass 133 4.5.2 Temperature Dependence, Glass Transition, and Visco-Elasticity 137 4.5.3 Spatially Confined Systems (e.g., Thin Films) 146 4.5.4 Systems Under Pressure 149 4.5.5 Mechanically Fragile Systems, Soft Matter, and Gels 151 4.6 SUMMARY 154 5 NEUTRON DIFFRACTION TECHNIQUES FOR STRUCTURAL STUDIES OF GLASSES 158 Alex C. Hannon 5.1 INTRODUCTION 158 5.2 INSTRUMENTATION 159 5.2.1 The Neutron 159 5.2.2 The Interactions between a Neutron and a Sample 160 5.2.3 Neutron Sources 161 5.2.4 Neutron Diffractometers 164 5.3 THEORETICAL ASPECTS OF NEUTRON DIFFRACTION ON GLASSES 169 5.3.1 The Static Approximation 169 5.3.2 Scattering from a Single Nucleus 169 5.3.3 Scattering from an Assembly of Nuclei 170 5.3.4 Isotropic Samples 171 5.3.5 Coherent and Incoherent (Distinct and Self) Scattering 171 5.3.6 Atomic Vibrations 173 5.3.7 Real-space Correlation Functions 180 5.4 THE APPLICATION OF NEUTRON DIFFRACTION TO STUDIES OF GLASS STRUCTURE 186 5.4.1 Experimental Corrections 186 5.4.2 Resolution 190 5.4.3 Peak Fitting and Integration 194 5.4.4 Normalization of Data 198 5.4.5 Scattering at low Q 200 5.4.6 Sample-Related Difficulties 203 5.4.7 Partial Correlation Functions 209 5.4.8 Interpretation of Results 218 5.4.9 Modeling 226 5.4.10 The PDF Method 229 6 X-RAY DIFFRACTION FROM GLASS 241 Christopher J. Benmore 6.1 INTRODUCTION 241 6.2 BACKGROUND/THEORY 244 6.3 ANALYSIS OF DATA, EXTRACTION OF USEFUL INFORMATION 249 6.4 INSTRUMENTATION 255 6.5 CASE STUDIES 258 6.5.1 SiO2 and Oxide Glasses 258 6.5.2 Chalcogenide Glasses 263 6.5.3 Amorphous Materials, Gels, Foams and Fibers 264 6.6 CONCLUSIONS 264 7 XAFS SPECTROSCOPY AND GLASS STRUCTURE 271 Giuseppe Dalba and Francesco Rocca 7.1 INTRODUCTION 271 7.2 THE ORIGINS OF X-RAY ABSORPTION SPECTRA 272 7.3 XAFS INSTRUMENTATION 274 7.4 THE PHYSICAL MECHANISM OF XAFS 278 7.5 EXAFS 279 7.5.1 EXAFS Formula for Glasses 282 7.6 XAFS DATA ANALYSIS 284 7.6.1 Corrections for Instrumental Errors 284 7.6.2 Pre-edge Background Subtraction 284 7.6.3 Post-edge Background Subtraction 285 7.6.4 Normalization 286 7.6.5 Conversion to k-Space, Choice of Threshold Energy E0 and Weighting 286 7.6.6 Transformation from k-Space to R-Space 286 7.6.7 Fourier Filtering: Reverse Transformation: from R-Space to k-Space 287 7.6.8 Log Amplitude Ratio and Phases Difference Method 288 7.6.9 Fitting Procedure 288 7.7 EXAFS ACCURACY AND LIMITATIONS 289 7.8 XANES 290 7.9 XAFS SPECTROSCOPY APPLIED TO GLASS STRUCTURE: SOME EXAMPLES 291 7.9.1 Silicate Glasses 292 7.9.2 Silica Glass 294 7.9.3 Silica at High Temperature 294 7.9.4 Silica and Germania Glasses under High Pressure 297 7.9.5 Nanoparticles Embedded in Glasses 300 7.9.6 Study of Ionic Conductivity in Superionic Conducting Glasses Doped with AgI 307 7.10 SUMMARY AND CONCLUSIONS 309 8 NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY OF GLASSES 315 Scott Kroeker 8.1 INTRODUCTION 315 8.2 THEORETICAL BACKGROUND 316 8.2.1 Zeeman Effect 316 8.2.2 Magnetic Shielding 318 8.2.3 Quadrupolar Interaction 319 8.2.4 Dipolar Interactions 320 8.2.5 High Resolution Methodologies 320 8.3 INSTRUMENTATION 323 8.3.1 Magnet 323 8.3.2 Probe 325 8.3.3 Radiofrequency Components 326 8.3.4 Computer Control 326 8.3.5 Measurement Uncertainty 327 8.4 DATA ANALYSIS AND STRUCTURAL INTERPRETATION 329 8.4.1 Chemical Shift Assignments 329 8.4.2 Information from Quadrupolar Effects 330 8.4.3 Low-gamma Nuclei 332 8.4.4 Paramagnetic Effects 333 8.5 CASE STUDIES 333 8.5.1 Borophosphate Glasses 333 8.5.2 Aluminosilicate Glasses 336 8.5.3 Borosilicate Glasses 337 8.5.4 Modifier Cations in Alkali Borate Glasses 340 8.6 CONCLUSIONS 341 9 ADVANCED DIPOLAR SOLID STATE NMR SPECTROSCOPY OF GLASSES 345 Hellmut Eckert 9.1 INTRODUCTION 345 9.2 THEORETICAL ASPECTS 347 9.2.1 Direct Magnetic Dipole-Dipole Coupling 348 9.2.2 Indirect Magnetic Dipole-Dipole Coupling 349 9.3 HETERONUCLEAR EXPERIMENTS 349 9.3.1 Spin Echo Double Resonance 349 9.3.2 Rotational Echo Double Resonance 350 9.3.3 Rotational Echo Adiabatic Passage Double Resonance 353 9.3.4 Cross-polarization 354 9.3.5 Connectivity Studies Based on the Detection of Indirect Spin-Spin Interactions 358 9.3.6 Instrumental Considerations and Caveats. 358 9.4 HOMONUCLEAR EXPERIMENTS 360 9.4.1 Static Spin Echo Decay Spectroscopy 360 9.4.2 Homonuclear Dipolar Recoupling Experiments 362 9.4.3 Instrumental Considerations and Caveats 369 9.5 CASE STUDIES 370 9.5.1 Spatial Distributions of Mobile Ions in Alkali Silicate and Borate Glasses 370 9.5.2 Connectivity Distribution in 70 SiO2-30 [(Al2 O3)x(P2O5)1-x] Glasses 374 9.5.3 Speciations and Connectivity Distributions in Borophosphate and Thioborophosphate Glasses 380 10 ATOM PROBE TOMOGRAPHY OF GLASSES 391 Daniel Schreiber and Joseph V. Ryan 10.1 INTRODUCTION 391 10.2 BACKGROUND AND THEORY 392 10.3 INSTRUMENTATION 395 10.3.1 APT Specimen Preparation 399 10.3.2 Experimental Procedure and Parameters 401 10.3.3 Data Reconstruction 403 10.4 ANALYSIS METHODS 409 10.4.1 Estimating Error 412 10.5 CASE STUDIES 417 10.5.1 Composition 418 10.5.2 Interfaces 420 10.5.3 Conclusions 424 Index 431
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