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Characterization of Catalytic Materials

Book Description

Catalytic materials are essential to nearly every commercial and industrial chemical process in order to make reaction times faster and more efficient. Understanding the microstructure of such materials is essential to designing improved catalytic properties. This volume in the materials characterization series reviews the more common types characterization methods used for understanding surface and structural properties of most types of commercially used catalytic materials. -- Covers both bulk metals and alloys as well as supported metals metal oxides and metal sulfides -- Characterization techniques for zeolites and molecular sieves as well as alumina pillared clays -- Concise summaries of major characterization technologies for catalytic materials, including Auger Electron Spectroscopy, Energy-Dispersive X-Ray Spectroscopy, Neutron Activation Analysis, Scanning Electron Microscopy, and Transmission Electron Spectroscopy

Table of Contents

  1. Cover Page
  2. Title Page
  3. Copyright
  4. Materials Characterization Series
  5. Contents
  6. Preface to the Reissue of the Materials Characterization Series
  7. Preface to Series
  8. Preface to the Reissue of Characterization of Catalytic Materials
  9. Preface
  10. Contributors
  11. Bulk Metals and Alloys
    1. 1.1 Introduction
      1. The Role of Metals and Alloys in Catalysis
    2. 1.2 Preparation of Bulk Alloy or Bimetallic Catalysts
    3. 1.3 Bulk Metal Characterization Methods
      1. Bulk Chemical Analysis,
      2. Determination of Crystal Structure,
      3. Morphology and Microstructure,
      4. Quantification of Surface Area,
      5. Surface Composition,
      6. Gas–Surface Interactions,
      7. Surface Structure of Single Crystals and Metal Films
    4. 1.4 Surface Composition–Structure and Catalysis Relationship
  12. Supported Metals
    1. 2.1 Introduction
      1. Characteristics of Supported Metals,
      2. Conditions of Characterization of Supported Metals
    2. 2.2 Typical Approaches to Metals Characterization
      1. Chemisorption,
      2. Methods of Measuring Chemisorption
    3. 2.3 Reaction Studies of Supported Metals
    4. 2.4 X-ray Diffraction and Scattering Methods
      1. Particle Sizes from Line-Broadening,
      2. Small-Angle X-ray Scattering
    5. 2.5 Electron Microscopy
    6. 2.6 X-ray Absorption Spectroscopy
      1. Preparation for Measurements,
      2. Interpretation of Information,
      3. Strengths and Weaknesses of XAS
    7. 2.7 Mössbauer Spectroscopy
    8. 2.8 Photoelectron/Photoemission Spectroscopy
    9. 2.9 Magnetic Methods
    10. 2.10 Summary
  13. Bulk Metal Oxides
    1. 3.1 Introduction
      1. Oxides as Catalysts,
      2. Mechanistic Features of Oxide Catalyzed Reactions
    2. 3.2 Synthesis Methods
    3. 3.3 Properties of Oxides and Their Relation to Catalytic Behavior
      1. Determination of Bulk Structure,
      2. Bulk Composition,
      3. Metal Oxidation State and Local Structural Environment,
      4. Characterization by Electron Microscopy,
      5. Surface Characterization Using Molecular Probes,
      6. Surface Characterization Using Spectroscopic Analyses,
      7. Reducibility and Oxide Ion Mobility,
      8. Magnetic and Electronic Properties
    4. 3.4 Summary
  14. Supported Metal Oxides
    1. 4.1 Introduction
    2. 4.2 Synthesis Methods
    3. 4.3 Characterization
      1. Structure of the Supported Metal Oxide Phase,
      2. Surface Coverage of the Supported Metal Oxide Phase,
      3. Oxidation States and Local Structural Environments of Supported Metal Oxide Phases,
      4. Morphology of the Supported Metal Oxide Phase,
      5. Surface Chemistry of Supported Metal Oxides,
      6. Characterization Summary
    4. 4.4 Impregnating Solution Chemistry
    5. 4.5 Supported Metal Oxide Catalysts Under Ambient Conditions
    6. 4.6 Supported Metal Oxide Catalysts Under In Situ Conditions
    7. 4.7 Catalysis and Structure–Reactivity Relationship
    8. 4.8 Summary
  15. Bulk Metal Sulfides
    1. 5.1 Introduction
    2. 5.2 Preparation of Bulk TMS Catalysts
      1. Binary Sulfides,
      2. Mixed Metal Sulfides
    3. 5.3 Bulk Characterization
      1. Structures of TMS and Stable Catalytic Phases,
      2. Morphology, Particle Size, and Surface Area,
      3. Metal Oxidation State and Structural Environment
    4. 5.4 Surface Composition
      1. Chemisorption and Molecular Probes,
      2. Surface Characterization Using Spectroscopic Techniques
    5. 5.5 Structure–Function Relationships
      1. Importance of the Electronic Structure,
      2. Effect of the Crystallographic Structure,
      3. Effect of the Sulfur Vacancies
    6. 5.6 Summary
  16. Supported Metal Sulfides
    1. 6.1 Introduction
    2. 6.2 Structure of the Oxidic Catalyst
    3. 6.3 Structure of the Sulfidic Catalyst
      1. Structure of Molybdenum,
      2. Structure of Cobalt and Nickel
    4. 6.4 Specific Surface Area
    5. 6.5 Structure–Reactivity Relationships
      1. Role of Molybdenum,
      2. Role of the Promoter,
      3. Role of Phosphate
    6. 6.6 Summary
  17. Zeolites and Molecular Sieves
    1. 7.1 Introduction
    2. 7.2 Structure of Zeolites and Molecular Sieves
    3. 7.3 X-ray, Neutron, and Electron Diffraction
      1. Identification of Zeolites,
      2. Compositional and Phase Changes,
      3. Structure Determination by Diffraction Techniques
    4. 7.4 High-Resolution Electron Microscopy
    5. 7.5 Solid State NMR Spectroscopy
      1. Framework Composition,
      2. Tetrahedral Atom Ordering,
      3. New Developments
    6. 7.6 Adsorption
      1. Void Volume,
      2. Pore Size
    7. 7.7 Structure and Catalytic Behavior
    8. 7.8 Summary
  18. Alumina Pillared Clays:Methods of Preparation and Characterization
    1. 8.1 Introduction
    2. 8.2 Synthesis Methods
    3. 8.3 Properties of Pillared Clays
      1. X-ray Diffraction Pattern,
      2. Elemental Analysis,
      3. Electron Microscopy,
      4. Pore Structure by Adsorption–Desorption Techniques,
      5. Surface Acidity,
      6. 29Si and 27Al MAS-NMR,
      7. Pillared Clays As Catalysts
    4. 8.4 Summary
  19. Appendixes: Techniques Summaries
    1. 1 Auger Electron Spectroscopy (AES)
    2. 2 Dynamic Secondary Ion Mass Spectrometry (D-SIMS)
    3. 3 Electron Energy-Loss Spectroscopy in the Transmission Electron Microscope (EELS)
    4. 4 Electron Paramagnetic Resonance/Electron Spin Resonance
    5. 5 Electron Probe X-Ray Microanalysis (EPMA)
    6. 6 Energy-Dispersive X-Ray Spectroscopy (EDS)
    7. 7 Extended X-Ray Absorption Fine Structure (EXAFS)
    8. 8 Fourier Transform Infrared Spectroscopy (FTIR)
    9. 9 High-Resolution Electron Energy Loss Spectroscopy (HREELS)
    10. 10 Inductively Coupled Plasma Mass Spectrometry (ICPMS)
    11. 11 Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES)
    12. 12 Ion Scattering Spectroscopy (ISS)
    13. 13 Low-Energy Electron Diffraction (LEED)
    14. 14 Mössbauer Spectroscopy
    15. 15 Neutron Activation Analysis (NAA)
    16. 16 Neutron Diffraction
    17. 17 Physical and Chemical Adsorption for the Measurement of Solid State Areas
    18. 18 Raman Spectroscopy
    19. 19 Scanning Electron Microscopy (SEM)
    20. 20 Scanning Transmission Electron Microscopy (STEM)
    21. 21 Scanning Tunneling Microscopy and Scanning Force Microscopy (STM and SFM)
    22. 22 Solid State Nuclear Magnetic Resonance (NMR)
    23. 23 Static Secondary Ion Mass Spectrometry (Static SIMS)
    24. 24 Temperature Programmed Techniques
    25. 25 Transmission Electron Microscopy (TEM)
    26. 26 Ultraviolet Photoelectron Spectroscopy (UPS)
    27. 27 X-Ray Diffraction (XRD)
    28. 28 X-Ray Fluorescence (XRF)
    29. 29 X-Ray Photoelectron and Auger Electron Diffraction (XPD and AED)
    30. 30 X-Ray Photoelectron Spectroscopy (XPS)
  20. Index