About the Book
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. Vedrine, 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.
Table of Contents:
About the Editors XIX List of Contributors XXI Preface XXVII Michel Che and Jacques C. Vedrine General Introduction XXXI Michel Che and Jacques C. Vedrine 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 Frederic Thibault-Starzyk and Francoise Mauge 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 Herve 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 Fottinger, Christian Weilach, and Gunther 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 Methivier 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 Mossbauer Spectroscopy 407 Lorenzo Stievano and Friedrich E. Wagner 10.1 Introduction 407 10.2 The Mossbauer Effect 409 10.3 Radiation Source 411 10.4 Mossbauer Absorbers 414 10.5 Hyperfine Interactions 414 10.6 Experimental Setups 421 10.7 Evaluation of Experimental Data 424 10.8 Theoretical Calculation of Mossbauer Parameters 426 10.9 Common Mossbauer-Active Transitions 427 10.10 Survey of Applications of the Mossbauer 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 Grunert 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 Brauchle 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 Schlogl 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. O Brien, and Bert M. Weckhuysen 24 Quantum Chemistry Methods 1119 Philippe Sautet Conclusions 1147 Michel Che and Jacques C. Vedrine Index 1153
About the Author :
Michel Che studied chemistry and, after recruitment by CNRS, obtained his Doctorat es 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. Vedrine studied chemistry and, after recruitment by CNRS, obtained his Doctorat es 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.
