Characterization and Chemical Modification of the Silica Surface (eBook)

Cover 1
Table of contents 10
PART I: CHARACTERIZATION OF THE SILICA SURFACE 18
CHAPTER 1. SILICA: PREPARATION AND PROPERTIES 20
1. Introduction: natural and synthetic silica 20
2. Preparation of amorphous silica 21
3. The effect of particle packing on the surface area 30
4. The sol - gel process 32
5. Applications of pure silicas and powders 44
References 46
CHAPTER 2. PHYSICAL CHARACTERIZATION OF THE SILICA SURFACE 48
1. The isotherm 49
2. Determination of the specific surface area 51
3. Pore size characterization 54
References 72
CHAPTER 3. THE SURFACE CHEMISTRY OF SILICA 76
1. Surface species 76
2. The hydroxylated surface 79
3. Dehydroxylation and rehydroxylation 79
4. Infrared study of the silica surface 82
5. Deuteration 85
References 91
CHAPTER 4. QUANTIFICATION OF THE SILANOL NUMBER 96
1. Introduction 96
2. The silanol number- a physicochemical constant 98
3. Hexamethyldisilazane as a silanol titrator 100
4. Conclusion 105
References 106
CHAPTER 5. THE DISTRIBUTION OF THE SILANOL TYPES AND THEIR DESORPTION ENERGIES 110
1. The infrared models 111
2. The NMR models 121
3. TPD- models 126
4. Zhuravlev's model 135
5. Comparison and conclusion 139
References 142
CHAPTER 6. THE EFFECT OF SURFACE MORPHOLOGY ON THE DEHYDROXYLATION BEHAVIOUR 144
References 148
CHAPTER 7. RELATED MATERIALS: SILICATES 150
1. Simple orthosilicates 150
2. Other discrete, noncyclic silicate anions 150
3. Cyclic silicate anions 151
4. Infinite chain anions 151
5. Infinite sheet anions 152
6. Minerals 152
References 162
PART II: CHEMICAL MODIFICATION OF THE SILICA SURFACE 164
CHAPTER 8. CHEMICAL MODIFICATION OF SILICA: APPLICATIONS AND PROCEDURES 166
1. Applications of modified silica gel 166
2. Modification procedures 189
References 204
CHAPTER 9. MODIFICATION WITH SILICON COMPOUNDS: MECHANISTIC STUDIES 210
1. Modification with aminosilanes 211
2. Modification with chlorosilanes 283
3. Modification with other silicon compounds 305
References 309
CHAPTER 10. MODIFICATION WITH BORON COMPOUNDS 316
1. Introduction 316
2. Modification with boronhalides 317
3. Modification of the silica surface with diborane 336
References 370
CHAPTER 11. MODIFICATION WITH OTHER COMPOUNDS 374
1. Modification with Ti- compounds 374
2. Modification with Al- compounds 381
3. Modification with P - compounds 387
4. Modification with transition metal compounds 392
References 395
CHAPTER 12. AMMONIATION OF MODIFIED SILICA: INTRODUCTION OF FUNCTIONAL GROUPS 400
1. Introduction 400
2. Ammoniation of the unmodified silica 401
3. Ammoniation of halogenated silica 407
4. Ammoniation of chlorosilylated silica 410
5. Ammoniation of silica, activated with boron compounds 435
PART III: CHEMICAL SURFACE COATING 452
CHAPTER 13. COATING TECHNIQUES 454
1. Chemical Vapour Deposition (CVD) 454
2. Physical Vapour Deposition (PVD) 466
3. Atomic Layer Epitaxy 470
4. Molecular Layering 472
5. Chemical Surface Coating 475
References 475
CHAPTER 14. CHEMICAL SURFACE COATING 478
1. Principles of Chemical Surface Coating 478
2. Gas-phase modification 480
3. Liquid phase CSC 493
References 502
APPENDICES SURFACE ANALYSIS TECHNIQUES 504
APPENDIX A. FTIR-PAS Fourier Transform Infrared Spectroscopy with Photoacoustic detection 506
1. Introduction 506
2. Fourier Transform Infrared Spectroscopy 508
3. Photoacoustic spectroscopy 513
Bibliography 516
APPENDIX B. XPS X-Ray Photoelectron Spectroscopy 518
1. Principles 518
2. Instrumentation 520
Bibliography 521
APPENDIX C. 29Si CP MAS NMR Cross Polarization Magic Angle Nuclear Magnetic Resonance 522
1. Principles 522
2. Magic Angle Spinning 524
3. Cross Polarization 526
Bibliography 527
APPENDIX D. SURFACE SCIENCE TECHNIQUES 528
AUTHOR INDEX 546
SUBJECT INDEX 560
Studies in Surface Science and Catalysis 568