Spectroscopy In Catalysis - An Introduction 3E

Superbly organized and of great pedagogic value, Spectroscopy in Catalysis describes the most important modern analytical techniques used to investigate catalytic surfaces. These include electron, ion, and vibrational spectroscopy, mass spectrometry, temperature-programmed techniques, diffraction, and microscopy. With the focus on practical use, rather than theory, each chapter presents current applications to illustrate the type of information that the technique provides and evaluates its possibilities and limitations, allowing selection of the best catalyst and the correct technique to solve a given problem.

This third edition includes significant new developments and case studies, with all the chapters updated by way of recent examples and relevant new literature. For students and for everyone who wants a digestible introduction to catalyst characterization.

From reviews of the previous editions:

"This is a truly valuable book ... very useful for industrial practitioners who need to be aware of the type of information that can be obtained from modern surface spectroscopies .... The book has a superb pedagogic value..."
—Journal of Catalysis

"... this is an excellent text on spectroscopies in catalysis and I highly recommend it for ... introductory courses on heterogeneous catalysis or as a general introductory monograph."
—Journal of the American Chemical Society

J. W. Niemantsverdriet is Professor Physical Chemistry of Surfaces, Director of the Schuit Institute of Catalysis and Dean of the Department of Chemical Engineering and Chemistry. He is (co)author of about 185 scientific papers and of 3 books (see also www.catalysis.nl). Hans has been Editor of the Journal of Catalysis since 1996, and served as Managing Editor of CaTTech between 1996 and 2001. He is member of the Editorial Boards of Applied Surface Science, and Physical Chemistry - Chemical Physics. He served as Chairman of the Netherlands Vacuum Society NEVAC (1997-2000) and as President of the European Federation of Catalysis Societies, EFCATS (1999-2001). His research interests include heterogeneous catalysis and surface reactivity. He frequently presents lectures and short courses based on his books all over the world.

Preface.

List of Acronyms.

1 Introduction.

1.1 Heterogeneous Catalysis.

1.2 The Aim of Catalyst Characterization.

1.3 Spectroscopic Techniques.

1.4 Research Strategies.

References.

2 Temperature-Programmed Techniques.

2.1 Introduction.

2.2 Temperature-Programmed Reduction.

2.2.1 Thermodynamics of Reduction.

2.2.2 Reduction Mechanisms.

2.2.3 Applications.

2.3 Temperature-Programmed Sulfidation.

2.4 Temperature-Programmed Reaction Spectroscopy.

2.5 Temperature-Programmed Desorption.

2.5.1 TPD Analysis.

2.5.2 Desorption in the Transition State Theory.

2.6 Temperature-Programmed Reaction Spectroscopy in UHV.

References.

3 Photoemission and Auger Spectroscopy.

3.1 Introduction.

3.2 X-Ray Photoelectron Spectroscopy (XPS).

3.2.1 XPS Intensities and Sample Composition.

3.2.2 XPS Binding Energies and Oxidation States.

3.2.3 Shake Up, Shake Off, Multiplet Splitting and Plasmon Excitations.

3.2.4 Experimental Aspects of XPS.

3.2.5 Charging and Sample Damage.

3.2.6 Dispersion of Supported Particles from XPS.

3.2.7 Angle-Dependent XPS.

3.2.8 In-Situ and Real Time XPS Studies.

3.3 Ultraviolet Photoelectron Spectroscopy (UPS).

3.3.1 Photoemission of Adsorbed Xenon.

3.4 Auger Electron Spectroscopy.

3.4.1 Energy of Auger Peaks.

3.4.2 Intensity of Auger Peaks.

3.4.3 Application of AES in Catalytic Surface Science.

3.4.4 Scanning Auger Spectroscopy.

3.4.5 Depth-Sensitive Information from AES.

References.

4 The Ion Spectroscopies.

4.1 Introduction.

4.2 Secondary Ion Mass Spectrometry (SIMS).

4.2.1 Theory of SIMS.

4.2.2 Electron and Photon Emission under Ion Bombardment.

4.2.3 Energy Distribution of Secondary Ions.

4.2.4 The Ionization Probability.

4.2.5 Emission of Molecular Clusters.

4.2.6 Conditions for Static SIMS.

4.2.7 Charging of Insulating Samples.

4.2.8 Applications on Catalysts.

4.2.9 Model Catalysts.

4.2.10 Single Crystal Studies.

4.2.11 Concluding Remarks.

4.3 Secondary Neutral Mass Spectrometry (SNMS).

4.4 Ion Scattering: The Collision Process.

4.5 Rutherford Backscattering Spectrometry (RBS).

4.6 Low-Energy Ion Scattering (LEIS).

4.6.1 Neutralization.

4.6.2 Applications of LEIS in Catalysis.

References.

5 Mössbauer Spectroscopy.

5.1 Introduction.

5.2 The Mössbauer Effect.

5.3 Mössbauer Spectroscopy.

5.3.1 Isomer Shift.

5.3.2 Electric Quadrupole Splitting.

5.3.3 Magnetic Hyperfine Splitting.

5.3.4 Intensity.

5.4 Mössbauer Spectroscopy in Catalyst Characterization.

5.4.1 In-Situ Mössbauer Spectroscopy at Cryogenic Temperatures.

5.4.2 Particle Size Determination.

5.4.3 Kinetics of Solid-State Reactions from Single Velocity

Experiments.

5.4.4 In-Situ Mössbauer Spectroscopy Under Reaction Conditions.

5.4.5 Mössbauer Spectroscopy of Elements Other Than Iron.

5.5 Conclusion.

References.

6 Diffraction and Extended X-Ray Absorption Fine Structure (EXAFS).

6.1 Introduction.

6.2 X-Ray Diffraction.

6.2.1 In-Situ XRD: Kinetics of Solid-State Reactions.

6.2.2 Concluding Remarks.

6.3 Low-Energy Electron Diffraction (LEED).

6.4 X-Ray Absorption Fine Structure (XAFS).

6.4.1 EXAFS.

6.4.2 Quick EXAFS for Time-Resolved Studies.

6.4.3 X-Ray Absorption Near Edge Spectroscopy.

References.

7 Microscopy and Imaging.

7.1 Introduction.

7.2 Electron Microscopy.

7.2.1 Transmission Electron Microscopy.

7.2.2 Scanning Electron Microscopy.

7.2.3 Scanning Transmission Electron Microscopy.

7.2.4 Element Analysis in the Electron Microscope.

7.3 Field Emission Microscopy and Ion Microscopy.

7.3.1 Theory of FEM and FIM.

7.4 Scanning Probe Microscopy: AFM and STM.

7.4.1 AFM and SFM.

7.4.1.1 Contact Mode AFM.

7.4.1.2 Non-Contact Mode AFM.

7.4.1.3 Tapping Mode AFM.

7.4.2 AFM Equipment.

7.4.3 Scanning Tunneling Microscopy (STM).

7.4.4 Applications of STM in Catalytic Surface Science.

7.5 Other Imaging Techniques.

7.5.1 Low-Energy Electron Microscopy and Photoemission Electron Microscopy.

References.

8 Vibrational Spectroscopy.

8.1 Introduction.

8.2 Theory of Molecular Vibrations.

8.3 Infrared Spectroscopy.

8.3.1 Equipment.

8.3.2 Applications of Infrared Spectroscopy.

8.3.3 Transmission Infrared Spectroscopy.

8.3.4 Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS).

8.3.5 Attenuated Total Reflection.

8.3.6 Reflection Absorption Infrared Spectroscopy (RAIRS).

8.4 Sum-Frequency Generation.

8.5 Raman Spectroscopy.

8.5.1 Applications of Raman Spectroscopy.

8.6 Electron Energy Loss Spectroscopy (EELS).

8.7 Concluding Remarks.

References.

9 Case Studies in Catalyst Characterization.

9.1 Introduction.

9.2 Supported Rhodium Catalysts.

9.2.1 Preparation of Alumina-Supported Rhodium Model Catalysts.

9.2.2 Reduction of Supported Rhodium Catalysts.

9.2.3 Structure of Supported Rhodium Catalysts.

9.2.4 Disintegration of Rhodium Particles Under CO.

9.2.5 Concluding Remarks.

9.3 Alkali Promoters on Metal Surfaces.

9.4 Cobalt–Molybdenum Sulfide Hydrodesulfurization Catalysts.

9.4.1 Sulfidation of Oxidic Catalysts.

9.4.2 Structure of Sulfided Catalysts.

9.5 Chromium Polymerization Catalysts.

9.6 Concluding Remarks.

References.

Appendix Metal Surfaces and Chemisorption.

A.1 Introduction.

A.2 Theory of Metal Surfaces.

A.2.1 Surface Crystallography.

A.2.2 Surface Free Energy.

A.2.3 Lattice Vibrations.

A.2.4 Electronic Structure of Metal Surfaces.

A.2.5 Work Function.

A.3 Chemisorption on Metals.

A.3.1 Adsorption of Molecules on Jellium.

A.3.2 Adsorption on Metals with d-Electrons.

A.3.3 Concluding Remarks.

References.

Index.