Modern Glass Characterization (eBook, ePUB)
Redaktion: Affatigato, Mario
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Modern Glass Characterization (eBook, ePUB)
Redaktion: Affatigato, Mario
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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
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- Produktdetails
- Verlag: John Wiley & Sons
- Seitenzahl: 464
- Erscheinungstermin: 29. Oktober 2015
- Englisch
- ISBN-13: 9781119051879
- Artikelnr.: 43831660
- Verlag: John Wiley & Sons
- Seitenzahl: 464
- Erscheinungstermin: 29. Oktober 2015
- Englisch
- ISBN-13: 9781119051879
- Artikelnr.: 43831660
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 ACKNOWLEDGMENTS 30 REFERENCES 31 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 ACKNOWLEDGMENTS 69 REFERENCES 69 3 RAMAN SPECTROSCOPY OF GLASSES 74 Rui
M. Almeida and Lü?s 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 ACKNOWLEDGMENTS 103 REFERENCES 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 REFERENCES 155 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 ACKNOWLEDGMENTS 231 REFERENCES 231
FURTHER READING 240 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
ACKNOWLEDGMENTS 266 REFERENCES 267 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 REFERENCES 310 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
ACKNOWLEDGMENTS 342 REFERENCES 342 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 ACKNOWLEDGMENTS 386 REFERENCES 386 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 ACKNOWLEDGMENTS 425 REFERENCES 425 Index 431
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 ACKNOWLEDGMENTS 30 REFERENCES 31 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 ACKNOWLEDGMENTS 69 REFERENCES 69 3 RAMAN SPECTROSCOPY OF GLASSES 74 Rui
M. Almeida and Lü?s 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 ACKNOWLEDGMENTS 103 REFERENCES 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 REFERENCES 155 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 ACKNOWLEDGMENTS 231 REFERENCES 231
FURTHER READING 240 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
ACKNOWLEDGMENTS 266 REFERENCES 267 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 REFERENCES 310 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
ACKNOWLEDGMENTS 342 REFERENCES 342 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 ACKNOWLEDGMENTS 386 REFERENCES 386 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 ACKNOWLEDGMENTS 425 REFERENCES 425 Index 431