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Characterization of Solid Materials and Heterogeneous Catalysts: From Structure to Surface Reactivity, 2 Volume Set

Michel Che (Editor), Jacques C. Vedrine (Editor)
ISBN: 978-3-527-32687-7
1284 pages
May 2012
Characterization of Solid Materials and Heterogeneous Catalysts: From Structure to Surface Reactivity, 2 Volume Set (3527326871) cover image


This two-volume book provides an overview of physical techniques used to characterize the structure of solid materials, on the one hand,
and to investigate the reactivity of their surface, on the other. Therefore this book is a must-have for anyone working in fields related to surface
reactivity. Among the latter, and because of its most important industrial impact, catalysis has been used as the directing thread of the book.
After the preface and a general introduction to physical techniques by M. Che and J.C. Védrine, two overviews on physical techniques are
presented by G. Ertl and Sir J.M. Thomas for investigating model catalysts and porous catalysts, respectively.
The book is organized into four parts: Molecular/Local Spectroscopies, Macroscopic Techniques, Characterization of the Fluid Phase (Gas and/
or Liquid), and Advanced Characterization. Each chapter focuses upon the following important themes: overview of the technique, most important parameters to interpret the experimental data, practical details, applications of the technique, particularly during chemical processes,
with its advantages and disadvantages, conclusions.
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Table of Contents

About the Editors XIX

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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Author Information

Michel Che studied chemistry and, after recruitment by CNRS, obtained his Doctorat ès Sciences (University of Lyon, F) in 1968. He worked as post-doc at Princeton University (USA) (1969-1971) and then as frequent visiting scientist at the Atomic Energy Research Establishment,
Harwell (UK) (1972-1982). He became Professor at the University Pierre & Marie Curie, Paris in 1975 and Boris Imelik Chair Professor of Institut Universitaire de France in 1995. His research concerns spectroscopy, surface reactivity and heterogeneous catalysis. He was President-Founder of the European Federation of Catalysis Societies (starting the biennial Europacat congresses) and later of the International Association of Catalysis Societies. His scientific and educational work earned him several international awards, lectureships and honorary doctorates.

Jacques C. Védrine studied chemistry and, after recruitment by CNRS, obtained his Doctorat ès Sciences (University of Lyon, F) in 1968. He worked as post-doc in USA at Varian Associates, Palo-Alto (1969-70) and at Princeton University (1970-71). He was deputy director of
the Institut de Recherches sur la Catalyse, CNRS in Lyon (1988-1998) and Chair Professor at Liverpool University, UK (1998-2003). He is one of the Editors of Appl. Catal. A: General. His research field covers physical techniques of catalyst characterization and heterogeneous catalysis for acid- and selective oxidation-type reactions on zeolites and mixed metal oxides. He was President of the European Federation of Catalysis Societies and of the Acid-Base World Organization. His scientific and educational work earned him several awards, and an honorary doctorate.
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