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List of Contributors XXI
Preface XXVII
Michel Che and Jacques C. Védrine
General Introduction XXXI
Michel Che and Jacques C. Védrine
Overview on Physical Techniques for Investigating Model Solid Catalysts XLV
Gerhard Ertl
Overview on Physical Techniques for Investigating Porous Catalysts LV
John Meurig Thomas
Volume 1
Part One Molecular/Local Spectroscopies 1
1 Infrared Spectroscopy 3
Frédéric Thibault-Starzyk and Françoise Maugé
1.1 Introduction 3
1.2 Principles of IR Spectroscopy and Basic Knowledge for Its Use 3
1.3 Experimental Considerations 7
1.4 Use of IR Spectroscopy to Characterize Solids 11
1.5 Application to Surface Reactivity: Operando Spectroscopy 39
1.6 Conclusion 45
References 45
2 Raman and UV-Raman Spectroscopies 49
Fengtao Fan, Zhaochi Feng, and Can Li
2.1 Introduction 49
2.2 Characterization of Active Sites and Phase Structure ofMetal Oxides 55
2.3 Characterization of Surface Metal Oxide Species on Supported Metal Oxides 59
2.4 Electron–Phonon Coupling in Nanostructured Materials 63
2.5 Characterization of sp2 Carbon Materials 64
2.6 Characterization of Transition Metal-Containing Microporous and Mesoporous Materials 67
2.7 Synthesis Mechanisms of Molecular Sieves 73
2.8 Conclusions 80
References 81
3 Electronic Spectroscopy: Ultra Violet-visible and Near IR Spectroscopies 89
Friederike C. Jentoft
3.1 Introduction and Overview 89
3.2 UV–vis–NIR Spectra 93
3.3 Experimental Considerations 108
3.4 Formation and Alteration of Solids 120
3.5 Surface Reactivity and Catalysis 130
3.6 Conclusions 139
References 140
4 Photoluminescence Spectroscopy 149
Masaya Matsuoka, Masakazu Saito, and Masakazu Anpo
4.1 Introduction 149
4.2 Basic Principles of Photoluminescence 150
4.3 General Aspects of Photoluminescence Measurements 153
4.4 Characterization of Catalysts by Photoluminescence and Time-Resolved Photoluminescence Spectroscopy 156
4.5 Investigations of the Dynamics of Photocatalysis by Time-Resolved Photoluminescence Spectroscopy 165
4.6 Conclusion 182
References 182
5 Neutron Scattering 185
Hervé Jobic
5.1 Introduction 185
5.2 Introduction to the Theory 186
5.3 Experimental 190
5.4 Structure 192
5.5 Dynamics 194
5.6 Conclusion 208
References 208
6 Sum Frequency Generation and Infrared Reflection Absorption Spectroscopy 211
Karin Föttinger, Christian Weilach, and Günther Rupprechter
6.1 Introduction 211
6.2 Theoretical Background of SFG 213
6.3 Spectrometer Setup 217
6.4 Case Studies 221
6.5 Conclusion 245
References 245
7 Infra Red Reflection Absorption Spectroscopy and Polarisation Modulation-IRRAS 255
Christophe Méthivier and Claire-Marie Pradier
7.1 Introduction 255
7.2 Principle of IRAS 258
7.3 Principle of PM-IRAS 261
7.4 Applications of IRAS and PM-IRAS 263
7.5 Conclusion 285
References 286
8 Nuclear Magnetic Resonance Spectroscopy 289
Lynn F. Gladden, Michal Lutecki, and James McGregor
8.1 Introduction and Historical Perspective 289
8.2 Theory 291
8.3 Popular NMR Techniques for Studying Solids 297
8.4 Characterization of Heterogeneous Catalysts 302
8.5 Porosity, Adsorption, and Transport Processes 308
8.6 ‘‘In Situ’’ NMR 313
8.7 Towards ‘‘Operando’’ Studies 329
8.8 Conclusion and Outlook 331
References 332
9 Electron Paramagnetic Resonance Spectroscopy 343
Piotr Pietrzyk, Zbigniew Sojka, and Elio Giamello
9.1 Introduction 343
9.2 Principles of EPR 345
9.3 Electron–Nucleus Hyperfine Interaction 350
9.4 Experimental Background 356
9.5 Anisotropy of Magnetic Interactions in EPR: the g, A, and D Tensors 359
9.6 EPR Spectra and the Solid State: Single Crystal Versus Powders 366
9.7 Guidelines to Interpretation of EPR Spectra 368
9.8 Computer Simulation of Powder Spectra 378
9.9 Molecular Interpretation of Parameters 380
9.10 Quantum Chemical Calculations of Magnetic Parameters 386
9.11 Advanced EPR Techniques 388
9.12 Characteristics of EPR Techniques in Application to Catalysis and Surfaces 389
9.13 Interfacial and Surface Charge-Transfer Processes 398
9.14 In Situ and Operando EPR Techniques 399
9.15 Conclusions and Prospects 403
References 403
10 Mössbauer Spectroscopy 407
Lorenzo Stievano and Friedrich E. Wagner
10.1 Introduction 407
10.2 The Mössbauer Effect 409
10.3 Radiation Source 411
10.4 Mössbauer Absorbers 414
10.5 Hyperfine Interactions 414
10.6 Experimental Setups 421
10.7 Evaluation of Experimental Data 424
10.8 Theoretical Calculation of Mössbauer Parameters 426
10.9 Common Mössbauer-Active Transitions 427
10.10 Survey of Applications of the Mössbauer Effect in the Study of Catalytic Materials 434
10.11 Conclusion 447
References 448
11 Low Energy Ion Scattering and Secondary Ion Mass Spectrometry 453
Norbert Kruse and Sergey Chenakin
11.1 Introduction 453
11.2 Secondary Ion Mass Spectrometry 457
11.3 Low-Energy Ion Scattering (Ion Scattering Spectroscopy) 461
11.4 Single-Crystal and Polycrystalline Metal Surfaces 465
11.5 Amorphous Metallic Alloys 472
11.6 From Model to Real Catalysts 474
11.7 Conclusion 501
References 502
12 X-ray Absorption Spectroscopy 511
Christophe Geantet and Christophe Pichon
12.1 Introduction 511
12.2 History of X-Ray Absorption Spectroscopy 511
12.3 Principle of X-Ray Absorption Spectroscopy: XANES, EXAFS 512
12.4 Experimentation and Data Processing 515
12.5 Application to Oxide Materials 521
12.6 Applications to the Study of Sulfide Catalysts 524
12.7 Application to Metal Catalysts 527
12.8 Conclusion and Perspectives 533
References 534
13 Auger Electron, X ray and UV Photoelectron Spectroscopies 537
Wolfgang Grünert
13.1 Introduction 537
13.2 Sources of Analytical Information 540
13.3 Instrumentation 567
13.4 Case Studies 571
13.5 Outlook 578
References 579
14 Single Molecule Spectroscopy 585
Timo Lebold, Jens Michaelis, Thomas Bein, and Christoph Bräuchle
14.1 Introduction 585
14.2 Description of the Method 586
14.3 Experimental Considerations and Constraints 591
14.4 Mesoporous Silica Materials 592
14.5 Selected Studies 593
14.6 Conclusion 605
References 605
Volume 2
Part Two Macroscopic Techniques 609
15 X-Ray Diffraction and Small Angle X-Ray Scattering 611
Malte Behrens and Robert Schlögl
16 Transmission Electron Microscopy 655
John Meurig Thomas and Caterina Ducati
17 Scanning Probe Microscopy and Spectroscopy 703
Tomoaki Nishino
18 Thermal Methods 747
Adrien Mekki-Berrada and Aline Auroux
19 Surface Area/Porosity, Adsorption, Diffusion 853
Philip L. Llewellyn, Emily Bloch, and Sandrine Bourrelly
Part Three Characterization of the Fluid Phase (Gas and/or Liquid) 881
20 Mass Spectrometry 883
Sandra Alves and Jean-Claude Tabet
21 Chromatographic Methods 953
Fabrice Bertoncini, Didier Thiebaut, Marion Courtiade, and Thomas Dutriez
22 Transient Techniques: Temporal Analysis of Products and Steady State Isotopic Transient Kinetic Analysis 1013
Angelos M. Efstathiou, John T. Gleaves, and Gregory S. Yablonsky
Part Four Advanced Characterization 1075
23 Techniques Coupling for Catalyst Characterisation 1077
Andrew M. Beale, Matthew G. Ó Brien, and Bert M. Weckhuysen
24 Quantum Chemistry Methods 1119
Philippe Sautet
Conclusions 1147
Michel Che and Jacques C. Védrine
Index 1153
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