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Preface to the Reissue of the Materials Characterization Series

Preface to Series

Preface to the Reissue of Characterization of Catalytic Materials

Preface

Contributors

BULK METALS AND ALLOYS

1.1 Introduction

The Role of Metals and Alloys in Catalysis

1.2 Preparation of Bulk Alloy or Bimetallic Catalysts

1.3 Bulk Metal Characterization Methods

Bulk Chemical Analysis 4, Determination of Crystal

Structure 5, Morphology and Microstructure 6, Quantification

of Surface Area 8, Surface Composition 9, Gas-Surface

Interactions 11, Surface Structure of Single Crystals and Metal Films

1.4 Surface Composition-Structure and Catalysis Relationship

SUPPORTED METALS

2.1 Introduction

Characteristics of Supported Metals 18, Conditions

of Characterization of Supported Metals

2.2 Typical Approaches to Metals Characterization

Chemisorption 19, Methods of Measuring Chemisorption

2.3 Reaction Studies of Supported Metals

2.4 X-ray Diffraction and Scattering Methods

Particle Sizes from Line-Broadening 27, Small-Angle X-ray Scattering

2.5 Electron Microscopy

2.6 X-ray Absorption Spectroscopy

Preparation for Measurements 32, Interpretation of

Information 32, Strengths and Weaknesses of XAS

2.7 Massbauer Spectroscopy

2.8 PhotoelectronPhotoemission Spectroscopy

2.9 Magnetic Methods

2.10 Summary

BULK METAL OXIDES

3.1 Introduction

Oxides as Catalysts 47, Mechanistic Features of Oxide Catalyzed Reactions

3.2 Synthesis Methods

3.3 Properties of Oxides and Their Relation to Catalytic Behavior 51

Determination of Bulk Structure 51, Bulk Composition 57, Metal Oxidation

State and Local Structural Environment 57, Characterization by Electron

Microscopy 60, Surface Characterization Using Molecular Probes 61,

Surface Characterization Using Spectroscopic Analyses 63, Reducibility

and Oxide Ion Mobility 64, Magnetic and Electronic Properties 65

3.4 Summary

SUPPORTED METAL OXIDES

4.1 Introduction

4.2 Synthesis Methods

4.3 Characterization

Structure of the Supported Metal Oxide Phase 71, Surface Coverage

of the Supported Metal Oxide Phase 73, Oxidation States and Local

Structural Environments of Supported Metal Oxide Phases 75, Morphology

of the Supported Metal Oxide Phase 77, Surface Chemistry of

Supported Metal Oxides 77, Characterization Summary

4.4 Impregnating Solution Chemistry

4.5 Supported Metal Oxide Catalysts Under Ambient Conditions

4.6 Supported Metal Oxide Catalysts Under In Situ Conditions

4.7 Catalysis and Structure-Reactivity Relationship

4.8 Summary

5.1 Introduction

5.2 Preparation of Bulk TMS Catalysts

Binary Sulfides 90, Mixed Metal Sulfides

5.3 Bulk Characterization

Structures of TMS and Stable Catalytic Phases 92, Morphology, Particle Size,

and Surface Area 94, Metal Oxidation State and Structural Environment

5.4 Surface Composition

Chemisorption and Molecular Probes 96, Surface

Characterization Using Spectroscopic Techniques

5.5 Structure-Function Relationships

Importance of the Electronic Structure 100, Effect of the Crystallographic

Structure 102, Effect of the Sulfur Vacancies

5.6 Summary

SUPPORTED METAL SULFIDES

6.1 Introduction

6.2 Structure of the Oxidic Catalyst

6.3 Structure of the Sulfidic Catalyst

Structure of Molybdenum 114, Structure of Cobalt and Nickel

6.4 Specific Surface Area

6.5 Structure-Reactivity Relationships

Role of Molybdenum 121, Roleofthe Promoter 122, Role of Phosphate

6.6 Summary

ZEOLITES AND MOLECULAR SIEVES

7.1 Introduction

7.2 Structure of Zeolites and Molecular Sieves

7.3 X-ray, Neutron, and Electron Diffraction

Identification of Zeolites 134, Compositional and Phase

Changes 135, Structure Determination by Diffraction Techniques

7.4 High-Resolution Electron Microscopy

7.5 Solid State NMR Spectroscopy

Framework Composition 139, Tetrahedral Atom

Ordering 141, New Developments

7.6 Adsorption

Void Volume 142, Pore Size

7.7 Structure and Catalytic Behavior

7.8 Summary

ALUMINA PILLARED CLAYS:

METHODS OF PREPARATION AND CHARACTERIZATION

8.1 Introduction

8.2 Synthesis Methods

8.3 Properties of Pillared Clays

X-ray Diffraction Pattern 152, Elemental Analysis 153, Electron

Microscopy 154, Pore Structure by Adsorption-Desorption

Techniques 155, Surface Acidity 158, 29Si and 27A1 MAS-

NMR 158, Pillared Clays As Catalysts

8.4 Summary

APPENDIXES: TECHNIQUES SUMMARIES

1 Auger Electron Spectroscopy (AES)

2 Dynamic Secondary Ion Mass Spectrometry (D-SIMS)

3 Electron Energy-Loss Spectroscopy in the Transmission Electron Microscope (EELS)

4 Electron Paramagnetic ResonanceElectron Spin Resonance

5 Electron Probe X-Ray Microanalysis (EPMA)

6 Energy-Dispersive X-Ray Spectroscopy (EDS)

7 Extended X-Ray Absorption Fine Structure (EXAFS)

8 Fourier Transform Infrared Spectroscopy (FTIR)

9 High-Resolution Electron Energy Loss Spectroscopy (HREELS)

10 Inductively Coupled Plasma Mass Spectrometry (ICPMS)

11 Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES)

12 Ion Scattering Spectroscopy (ISS)

13 Low-Energy Electron Diffraction (LEED)

14 M6ssbauer Spectroscopy

15 Neutron Activation Analysis (NAA)

16 Neutron Diffraction

17 Physical and Chemical Adsorption for the Measurement of Solid State Areas

18 Raman Spectroscopy

19 Scanning Electron Microscopy (SEM)

20 Scanning Transmission Electron Microscopy (STEM)

21 Scanning Tunneling Microscopy and Scanning Force Microscopy (STM and SFM)

22 Solid State Nuclear Magnetic Resonance (NMR)

23 Static Secondary Ion Mass Spectrometry (Static SIMS)

24 Temperature Programmed Techniques

25 Transmission Electron Microscopy (TEM)

26 Ultraviolet Photoelectron Spectroscopy (UPS)

27 X-Ray Diffraction (XRD)

28 X-Ray Fluorescence (XRF)

29 X-Ray Photoelectron and Auger Electron Diffraction (XPD and AED)

30 X-Ray Photoelectron Spectroscopy (XPS)

Index

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