Characterization of Solid Materials and Heterogeneous Catalysts

From Structure to Surface Reactivity
1. Auflage 2012
ISBN: 978-3-527-32687-7
Verlag: WILEY-VCH

Medienkombination, Englisch, 1182 Seiten, 2 Bände, Format (B × H): 170 mm x 240 mm, Gewicht: 2740 g

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.

Autoren/Hrsg.

Che, Michel

Vedrine, Jacques C.

Fachgebiete

• Naturwissenschaften Chemie Physikalische Chemie Chemische Reaktionen, Katalyse
• Naturwissenschaften Physik Thermodynamik Festkörperphysik, Kondensierte Materie
• Naturwissenschaften Physik Elektromagnetismus Mikroskopie, Spektroskopie

Inhaltsverzeichnis

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

Über Autor(innen)

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.