Characterization of Solid Materials and Heterogeneous Catalysts

PREFACE
GENERAL INTRODUCTION
OVERVIEW ON PHYSICAL TECHNIQUES FOR INVESTIGATING MODEL SOLID CATALYSTS
OVERVIEW ON PHYSICAL TECHNIQUES FOR INVESTIGATING POROUS CATALYSTS LV

VOLUME 1
PART ONE MOLECULAR/LOCAL SPECTROSCOPIES
INFRARED SPECTROSCOPY
Introduction
Principles of IR Spectroscopy and Basic Knowledge for Its Use
Experimental Considerations
Use of IR Spectroscopy to Characterize Solids
Application to Surface Reactivity: Operando Spectroscopy
Conclusion

RAMAN AND UV-RAMAN SPECTROSCOPIES
Introduction
Characterization of Active Sites and Phase Structure of Metal Oxides
Characterization of Surface Metal Oxide Species on Supported Metal Oxides
Electron-Phonon Coupling in Nanostructured Materials
Characterization of sp2 Carbon Materials
Characterization of Transition Metal-Containing Microporous and Mesoporous Materials
Synthesis Mechanisms of Molecular Sieves
Conclusions

ELECTRONIC SPECTROSCOPY: ULTRA VIOLET-VISIBLE AND NEAR IR SPECTROSCOPIES
Introduction and Overview
UV-vis-NIR Spectra
Experimental Considerations
Formation and Alteration of Solids
Surface Reactivity and Catalysis
Conclusions

PHOTOLUMINESCENCE SPECTROSCOPY
Introduction
Basic Principles of Photoluminescence
General Aspects of Photoluminescence Measurements Characterization of Catalysts by Photoluminescence and Time-Resolved Photoluminescence Spectroscopy
Investigations of the Dynamics of Photocatalysis by Time-Resolved Photoluminescence Spectroscopy
Conclusion

NEUTRON SCATTERING
Introduction
Introduction to the Theory
Experimental
Structure
Dynamics
Conclusion

SUM FREQUENCY GENERATION AND INFRARED REFLECTION ABSORPTION SPECTROSCOPY
Introduction
Theoretical Background of SFG
Spectrometer Setup
Case Studies
Conclusion

INFRA RED REFLECTION ABSORPTION SPECTROSCOPY AND POLARISATION MODULATION-IRRAS
Introduction
Principle of IRAS
Principle of PM-IRAS
Applications of IRAS and PM-IRAS
Conclusion

NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY
Introduction and Historical Perspective
Theory
Popular NMR Techniques for Studying Solids
Characterization of Heterogeneous Catalysts
Porosity, Adsorption, and Transport Processes
"In Situ" NMR
Towards "Operando" Studies
Conclusion and Outlook

ELECTRON PARAMAGNETIC RESONANCE SPECTROSCOPY
Introduction
Principles of EPR
Electron-Nucleus Hyperfine Interaction
Experimental Background
Anisotropy of Magnetic Interactions in EPR: the g, A, and D Tensors
EPR Spectra and the Solid State: Single Crystal Versus Powders
Guidelines to Interpretation of EPR Spectra
Computer Simulation of Powder Spectra
Molecular Interpretation of Parameters
Quantum Chemical Calculations of Magnetic Parameters
Advanced EPR Techniques
Characteristics of EPR Techniques in Application to Catalysis and Surfaces
Interfacial and Surface Charge-Transfer Processes
In Situ and Operando EPR Techniques
Conclusions and Prospects

MÖSSBAUER SPECTROSCOPY
Introduction
The Mössbauer Effect
Radiation Source
Mössbauer Absorbers
Hyperfine Interactions
Experimental Setups
Evaluation of Experimental Data
Theoretical Calculation of Mössbauer Parameters
Common Mössbauer-Active Transitions
Survey of Applications of the Mössbauer Effect in the Study of Catalytic Materials
Conclusion

LOW ENERGY ION SCATTERING AND SECONDARY ION MASS SPECTROMETRY
Introduction
Secondary Ion Mass Spectrometry
Low-Energy Ion Scattering (Ion Scattering Spectroscopy)
Single-Crystal and Polycrystalline Metal Surfaces
Amorphous Metallic Alloys
From Model to Real Catalysts
Conclusion


X-RAY ABSORPTION SPECTROSCOPY
Introduction
History of X-Ray Absorption Spectroscopy
Principle of X-Ray Absorption Spectroscopy: XANES, EXAFS
Experimentation and Data Processing
Application to Oxide Materials
Applications to the Study of Sulfide Catalysts
Application to Metal Catalysts
Conclusion and Perspectives

AUGER ELECTRON, X RAY AND UV PHOTOELECTRON SPECTROSCOPIES
Introduction
Sources of Analytical Information
Instrumentation
Case Studies
Outlook

SINGLE MOLECULE SPECTROSCOPY
Introduction
Description of the Method
Experimental Considerations and Constraints
Mesoporous Silica Materials
Selected Studies
Conclusion


VOLUME 2
PART TWO MACROSCOPIC TECHNIQUES

X-RAY DIFFRACTION AND SMALL ANGLE X-RAY SCATTERING
Introduction
Theoretical Background of X-Ray Diffraction
Experimental Aspects
Application to Phase Identification
Application to Phase Characterization: Ideal Structure
Application for Phase Characterization: Real Structure
X-Ray Diffraction of Catalysts in a Reactive Atmosphere
Small-Angle X-Ray Scattering (SAXS)
Conclusion

TRANSMISSION ELECTRON MICROSCOPY
History and Overview
Introduction
Specimen Preparation and Experimental Considerations
Examples of General Characterization Studies
Examples of Reactivity and Catalysis Studies
Recent Developments and Future Prospects

SCANNING PROBE MICROSCOPY AND SPECTROSCOPY
Introduction
Scanning Tunneling Microscopy
Atomic Force Microscopy
Conclusion

THERMAL METHODS
Main Thermal Methods
Acidity/Basicity
Redox Properties of Solids
Conclusion

SURFACE AREA/POROSITY, ADSORPTION, DIFFUSION
Introduction
Gas Adsorption for the Characterization of Surface Area and Porosity
Diffusion in Porous Solids
Conclusion

PART THREE CHARACTERIZATION OF THE FLUID PHASE (GAS AND/OR LIQUID)

MASS SPECTROMETRY
Linked Atom Theory and the Mass Spectrometry Stories: the Premises of Modern Mass Spectrometry Technology Basics of Mass Spectrometry
Direct Surface Analysis: ImagingMass Spectrometry for Biologists
From Collision Activation to Ion?Surface Chemical Reactions for New Preparative Mass Spectrometry
Petroleomics: Role of Ultra-High Resolution and Data Treatment
Conclusion

CHROMATOGRAPHIC METHODS
Introduction
Analysis at Different Scales
GC _ GC: a Revolutionary Analytical Technique for Detailed Molecular Analysis
Towards Molecular Analysis Systems Highly Coupled Around GC _ GC
Conclusion

TRANSIENT TECHNIQUES: TEMPORAL ANALYSIS OF PRODUCTS AND STEADY STATE ISOTOPIC TRANSIENT KINETIC ANALYSIS
Scope
Temporal Analysis of Products (TAP)
Steady-State Isotopic Transient Kinetic Analysis (SSITKA)
Conclusion

PART FOUR ADVANCED CHARACTERIZATION

TECHNIQUES COUPLING FOR CATALYST CHARACTERISATION
Introduction
Basic Tenets Behind Technique Combining
Illustrations of Setups Combining Multiple In Situ Techniques
Conclusion

QUANTUM CHEMISTRY METHODS
Introduction and Historical Perspective
Building Models of Heterogeneous Catalysts
Electronic Structure Calculations
Application of Total Energy Calculations to the Structure of Catalytic Surfaces Under the Conditions of Catalysis
Conclusions and Outlook

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.

M. Che, University Pierre & Marie Curie, Paris, France; J. C. Vedrine, University Pierre & Marie Curie, Paris, France