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 Photoelectron/Photoemission 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 Resonance/Electron 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