X-Ray Absorption and X-Ray Emission Spectroscopy
Theory and Applications
1. Edition March 2016
890 Pages, Hardcover
Wiley & Sons Ltd
ISBN:
978-1-118-84423-6
John Wiley & Sons
During the last two decades, remarkable and often spectacular progress has been made in the methodological and instrumental aspects of x-ray absorption and emission spectroscopy. This progress includes considerable technological improvements in the design and production of detectors especially with the development and expansion of large-scale synchrotron reactors All this has resulted in improved analytical performance and new applications, as well as in the perspective of a dramatic enhancement in the potential of x-ray based analysis techniques for the near future. This comprehensive two-volume treatise features articles that explain the phenomena and describe examples of X-ray absorption and emission applications in several fields, including chemistry, biochemistry, catalysis, amorphous and liquid systems, synchrotron radiation, and surface phenomena. Contributors explain the underlying theory, how to set up X-ray absorption experiments, and how to analyze the details of the resulting spectra.
X-Ray Absorption and X-ray Emission Spectroscopy: Theory and Applications:
* Combines the theory, instrumentation and applications of x-ray absorption and emission spectroscopies which offer unique diagnostics to study almost any object in the Universe.
* Is the go-to reference book in the subject for all researchers across multi-disciplines since intense beams from modern sources have revolutionized x-ray science in recent years
* Is relevant to students, postdocurates and researchers working on x-rays and related synchrotron sources and applications in materials, physics, medicine, environment/geology, and biomedical materials
VOLUME I
List of Contributors
Foreword
I INTRODUCTION: HISTORY, XAS, XES, AND THEIR IMPACT ON SCIENCE
1 Introduction: Historical Perspective on XAS
Jeroen A. van Bokhoven and Carlo Lamberti
1.1 Historical Overview of 100 Years of X-Ray Absorption: A Focus on the Pioneering 1913.1971 Period
1.2 About the Book: A Few Curiosities, Some Statistics, and a Brief Overview
References
II EXPERIMENTAL AND THEORY
2 From Synchrotrons to FELs: How Photons Are Produced; Beamline Optics and Beam Characteristics
Giorgio Margaritondo
2.1 Photon Emission by Accelerated Charges: from the Classical Case to the
Relativistic Limit
2.2 Undulators, Wigglers, and Bending Magnets
2.3 The Time Structure of Synchrotron Radiation
2.4 Elements of Beamline Optics
2.5 Free Electron Lasers
References
3 Real-Space Multiple-Scattering Theory of X-ray Spectra
Joshua J. Kas, Kevin Jorisson and John J. Rehr
3.1 Introduction
3.2 Theory
3.3 Applications
3.4 Conclusion
References
4 Theory of X-ray Absorption Near Edge Structure
Yves Joly and Stephane Grenier
4.1 Introduction
4.2 The x-ray Absorption Phenomena
4.3 X-ray Matter Interaction
4.4 XANES General Formulation
4.5 XANES Simulations in the Mono-Electronic Scheme
4.6 Multiplet Ligand Field Theory
4.7 Current Theoretical Developments
4.8 Tensorial Approaches
4.9 Conclusion
References
5 How to Start an XAS Experiment
Diego Gianolio
5.1 Introduction
5.3 Prepare the Experiment
5.4 Perform the Experiment
References
6 Hard X-ray Photon-in/Photon-out Spectroscopy: Instrumentation, Theory and Applications
Pieter Glatzel, Roberto Alonso-Mori, and Dimosthenis Sokaras
6.1 Introduction
6.2 History
6.3 Basic Theory of XES
6.4 Chemical Sensitivity of X-ray Emission
6.5 HERFD and RIXS
6.6 Experimental X-ray Emission Spectroscopy
6.7 Conclusion
References
7 QEXAFS: Techniques and Scientific Applications for Time-Resolved XAS
Maarten Nachtegaal, Oliver Muller, Christian Konig and Ronald Frahm
7.1 Introduction
7.2 History and Basics of QEXAFS
7.3 Monochromators and Beamlines for QEXAFS
7.4 Detectors and Readout Systems
7.5 Applications of QEXAFS in Chemistry
7.6 Conclusion
Acknowledgements
References
8 Time-Resolved XAS Using an Energy Dispersive Spectrometer: Techniques and Applications
Olivier Mathon, Innokenty Kantor and Sakura Pascarelli
8.1 Introduction
8.2 Energy Dispersive X-Ray Absorption Spectroscopy
8.3 From the Minute Down to the Ms: Filming a Chemical Reaction in Situ
8.4 Down to the s Regime: Matter under Extreme Conditions
8.5 Playing with a 100 ps Single Bunch
8.6 Conclusion
References
9 X-Ray Transient Absorption Spectroscopy
Lin X. Chen
9.1 Introduction
9.2 Pump-Probe Spectroscopy
9.3 Experimental Considerations
9.4 Transient Structural Information Investigated by XTA
9.5 X-Ray Pump-Probe Absorption Spectroscopy: Examples
9.6 Perspective of Pump-Probe X-Ray Spectroscopy
Acknowledgments
References
10 Space-Resolved XAFS, Instrumentations and Applications
Yoshio Suzuki and Yasuko Terada
10.1 Space-Resolving Techniques for XAFS
10.2 Beam-Focusing Instrumentation for Microbeam Production
10.3 Examples of Beam-Focusing Instrumentation
10.4 Examples of Applications of Microbeam-XAFS Technique to Biology and nenvironmental Science
10.5 Conclusion and Outlook
References
11 Quantitative EXAFS Analysis
Bruce Ravel
11.1 A Brief History of EXAFS Theory
11.2 Theoretical Calculation of EXAFS Scattering Factors
11.3 Practical Examples of EXAFS Analysis
11.4 Conclusion
References
12 XAS Spectroscopy: Related Techniques and Combination with Other Spectroscopic and Scattering Methods
Carlo Lamberti, Elisa Borfecchia, Jeroen A. van Bokhoven and Marcos Fern´andez-Garcia
12.1 Introduction
12.2 Atomic Pair Distribution Analysis of Total Scattering Data
12.3 Diffraction Anomalous Fine Structure (DAFS)
12.4 Inelastic Scattering Techniques
12.5 -Environmental Fine Structure (BEFS)
12.6 Combined Techniques
12.7 Conclusion
Acknowledgments
References
VOLUME II
List of Contributors
Foreword
III APPLICATIONS: FROM SEMICONDUCTORS TO MEDICINE TO NUCLEAR
MATERIALS
13 X-Ray Absorption and Emission Spectroscopy for Catalysis
Jeroen A. van Bokhoven and Carlo Lamberti
13.1 Introduction
13.2 The Catalytic Process
13.3 Reaction Kinetics from Time-Resolved XAS
13.4 Sub-Micrometer Space Resolved Measurements
13.5 Emerging Methods
13.6 Conclusion and outlook
References
14 High Pressure XAS, XMCD and IXS 383
Jean-Paul Itie, Francois Baudelet and Jean-Pascal Rueff
14.1 Introduction
14.2 High Pressure EXAFS and XANES
14.3 High-Pressure Magnetism and XMCD
14.4 High Pressure Inelastic X-Ray Scattering
14.5 Conclusion
References
15 X-Ray Absorption and RIXS on Coordination Complexes
Thomas Kroll, Marcus Lundberg and Edward I. Solomon
15.1 Introduction
15.2 Metal K-Edges
15.3 Metal L-Edges
15.4 Resonant Inelastic X-Ray Scattering
15.5 Conclusion
Acknowledgments
References
16 Semiconductors
Federico Boscherini
16.1 Introduction
16.2 XAS Instrumental Aspects
16.3 Applications
16.4 Conclusion
References
17 XAS Studies on Mixed Valence Oxides
Joaqu?n Garc?a, Gloria Sub?as and Javier Blasco
17.1 Introduction
17.2 Solid State Applications (Mixed Valence Oxides)
17.3 Conclusion
References
18 Novel XAS Techniques for Probing Fuel Cells and Batteries
David E. Ramaker
18.1 Introduction
18.2 XANES Techniques
18.3 In Operando Measurements
18.4 Future Trends
18.5 Appendix
References
19 X-ray Spectroscopy in Studies of the Nuclear Fuel Cycle
Melissa A. Denecke
19.1 Background
19.2 Application Examples
19.3 Conclusion and Outlook
References
20 Planetary, Geological and Environmental Sciences
Francois Farges and Max Wilke
20.1 Introduction
20.2 Planetary and Endogenous Earth Sciences
20.3 Environmental Geosciences
20.4 Conclusion
Acknowledgments
References
21 X-Ray Absorption Spectroscopy and Cultural Heritage: Highlights and Perspectives
Franc¸ois Farges and Marine Cotte
21.1 Introduction
21.2 Instrumentation: Standard and Recently Developed Approaches
21.3 Some Applications
21.4 Conclusion
Acknowledgments
References
22 X-ray Spectroscopy at Free Electron Lasers
Wojciech Gawelda, Jakub Szlachetko and Christopher J. Milne
22.1 Introduction to X-ray Free Electron Lasers in Comparison to Synchrotrons
22.2 Current Implementations of X-Ray Spectroscopy Techniques at XFELs
22.3 Examples of Time-Resolved X-Ray Spectroscopy at XFELs
22.4 Examples of Nonlinear X-Ray Spectroscopy at XFELs
22.5 Conclusion and Outlook
References
23 X-ray Magnetic Circular Dichroism
Andrei Rogalev, Katharina Ollefs and Fabrice Wilhelm
23.1 Historical Introduction
23.2 Physical Content of XMCD and the Sum Rules
23.3 Experimental Aspects and Data Analysis
23.4 Examples of Recent Research
23.5 Conclusion and Outlook
Acknowledgments
References
24 Industrial Applications
Simon R. Bare and Jeffrey Cutler
24.1 Introduction
24.2 The Patent Literature
24.3 The Open Literature
24.4 Examples of Applications from Light Sources
24.5 Examples of Applications from Companies
24.6 Conducting Industrial Research at Light Sources
24.7 Conclusion and Outlook
Acknowledgements
References
25 XAS in Liquid Systems
Adriano Filipponi and Paola D'Angelo
25.1 The Liquid State of Matter
25.2 Computer Modelling of Liquid Structures
25.3 XAFS Calculations in Liquids/Disordered Systems
25.4 Experimental and Data-Analysis Approaches
25.5 Examples of Data Analysis Applications
References
26 Surface Metal Complexes and Their Applications
Joseph D. Kistler, Pedro Serna, Kiyotaka Asakura and Bruce C. Gates
26.1 Introduction
26.2 Aim of the Chapter
26.3 Mononuclear Iridium Complexes Supported on Zeolite HSSZ-53: Illustration of EXAFS
Data Fitting and Model Discrimination
26.4 Iridium Complexes Supported on MgO and on Zeolites: Precisely Synthesized Isostructural Metal Complexes on Supports with Contrasting Properties as Ligands
26.5 Supported Chromium Complex Catalysts for Ethylene Polymerization Characterization of Samples Resembling Industrial Catalysts
26.6 Copper Complexes on Titania: Insights Gained from Samples Incorporating Single-Crystal Supports
26.7 Gold Complexes Supported on Zeolite NaY: Determining Crystallographic Locations of Metal Complexes on a Support by Combining EXAFS Spectroscopy and TEM
26.8 Gold Supported on CeO2: Conversion of Gold Complexes into Clusters in a CO Oxidation Catalyst Characterized by Transient XAFS Spectroscopy
26.9 Mononuclear Rhodium Complexes and Dimers on MgO: Discovery of a Catalyst for Selective Hydrogenation of 1,3-Butadiene
26.10 Osmium Complexes Supported on MgO: Determining Structure of the Metal-Support Interface and the Importance of Support Surface Defect Sites
26.11 Conclusion
Acknowledgments
References
27 Nanostructured Materials
Alexander V. Soldatov and Kirill A. Lomachenko
27.1 Introduction
27.2 Small Nanoclusters
27.3 XAS and XES for the Study of Nanoparticles
27.4 Nanostructures and Defects in Solids
27.5 Conclusion and Outlook
References
Index
List of Contributors
Foreword
I INTRODUCTION: HISTORY, XAS, XES, AND THEIR IMPACT ON SCIENCE
1 Introduction: Historical Perspective on XAS
Jeroen A. van Bokhoven and Carlo Lamberti
1.1 Historical Overview of 100 Years of X-Ray Absorption: A Focus on the Pioneering 1913.1971 Period
1.2 About the Book: A Few Curiosities, Some Statistics, and a Brief Overview
References
II EXPERIMENTAL AND THEORY
2 From Synchrotrons to FELs: How Photons Are Produced; Beamline Optics and Beam Characteristics
Giorgio Margaritondo
2.1 Photon Emission by Accelerated Charges: from the Classical Case to the
Relativistic Limit
2.2 Undulators, Wigglers, and Bending Magnets
2.3 The Time Structure of Synchrotron Radiation
2.4 Elements of Beamline Optics
2.5 Free Electron Lasers
References
3 Real-Space Multiple-Scattering Theory of X-ray Spectra
Joshua J. Kas, Kevin Jorisson and John J. Rehr
3.1 Introduction
3.2 Theory
3.3 Applications
3.4 Conclusion
References
4 Theory of X-ray Absorption Near Edge Structure
Yves Joly and Stephane Grenier
4.1 Introduction
4.2 The x-ray Absorption Phenomena
4.3 X-ray Matter Interaction
4.4 XANES General Formulation
4.5 XANES Simulations in the Mono-Electronic Scheme
4.6 Multiplet Ligand Field Theory
4.7 Current Theoretical Developments
4.8 Tensorial Approaches
4.9 Conclusion
References
5 How to Start an XAS Experiment
Diego Gianolio
5.1 Introduction
5.3 Prepare the Experiment
5.4 Perform the Experiment
References
6 Hard X-ray Photon-in/Photon-out Spectroscopy: Instrumentation, Theory and Applications
Pieter Glatzel, Roberto Alonso-Mori, and Dimosthenis Sokaras
6.1 Introduction
6.2 History
6.3 Basic Theory of XES
6.4 Chemical Sensitivity of X-ray Emission
6.5 HERFD and RIXS
6.6 Experimental X-ray Emission Spectroscopy
6.7 Conclusion
References
7 QEXAFS: Techniques and Scientific Applications for Time-Resolved XAS
Maarten Nachtegaal, Oliver Muller, Christian Konig and Ronald Frahm
7.1 Introduction
7.2 History and Basics of QEXAFS
7.3 Monochromators and Beamlines for QEXAFS
7.4 Detectors and Readout Systems
7.5 Applications of QEXAFS in Chemistry
7.6 Conclusion
Acknowledgements
References
8 Time-Resolved XAS Using an Energy Dispersive Spectrometer: Techniques and Applications
Olivier Mathon, Innokenty Kantor and Sakura Pascarelli
8.1 Introduction
8.2 Energy Dispersive X-Ray Absorption Spectroscopy
8.3 From the Minute Down to the Ms: Filming a Chemical Reaction in Situ
8.4 Down to the s Regime: Matter under Extreme Conditions
8.5 Playing with a 100 ps Single Bunch
8.6 Conclusion
References
9 X-Ray Transient Absorption Spectroscopy
Lin X. Chen
9.1 Introduction
9.2 Pump-Probe Spectroscopy
9.3 Experimental Considerations
9.4 Transient Structural Information Investigated by XTA
9.5 X-Ray Pump-Probe Absorption Spectroscopy: Examples
9.6 Perspective of Pump-Probe X-Ray Spectroscopy
Acknowledgments
References
10 Space-Resolved XAFS, Instrumentations and Applications
Yoshio Suzuki and Yasuko Terada
10.1 Space-Resolving Techniques for XAFS
10.2 Beam-Focusing Instrumentation for Microbeam Production
10.3 Examples of Beam-Focusing Instrumentation
10.4 Examples of Applications of Microbeam-XAFS Technique to Biology and nenvironmental Science
10.5 Conclusion and Outlook
References
11 Quantitative EXAFS Analysis
Bruce Ravel
11.1 A Brief History of EXAFS Theory
11.2 Theoretical Calculation of EXAFS Scattering Factors
11.3 Practical Examples of EXAFS Analysis
11.4 Conclusion
References
12 XAS Spectroscopy: Related Techniques and Combination with Other Spectroscopic and Scattering Methods
Carlo Lamberti, Elisa Borfecchia, Jeroen A. van Bokhoven and Marcos Fern´andez-Garcia
12.1 Introduction
12.2 Atomic Pair Distribution Analysis of Total Scattering Data
12.3 Diffraction Anomalous Fine Structure (DAFS)
12.4 Inelastic Scattering Techniques
12.5 -Environmental Fine Structure (BEFS)
12.6 Combined Techniques
12.7 Conclusion
Acknowledgments
References
VOLUME II
List of Contributors
Foreword
III APPLICATIONS: FROM SEMICONDUCTORS TO MEDICINE TO NUCLEAR
MATERIALS
13 X-Ray Absorption and Emission Spectroscopy for Catalysis
Jeroen A. van Bokhoven and Carlo Lamberti
13.1 Introduction
13.2 The Catalytic Process
13.3 Reaction Kinetics from Time-Resolved XAS
13.4 Sub-Micrometer Space Resolved Measurements
13.5 Emerging Methods
13.6 Conclusion and outlook
References
14 High Pressure XAS, XMCD and IXS 383
Jean-Paul Itie, Francois Baudelet and Jean-Pascal Rueff
14.1 Introduction
14.2 High Pressure EXAFS and XANES
14.3 High-Pressure Magnetism and XMCD
14.4 High Pressure Inelastic X-Ray Scattering
14.5 Conclusion
References
15 X-Ray Absorption and RIXS on Coordination Complexes
Thomas Kroll, Marcus Lundberg and Edward I. Solomon
15.1 Introduction
15.2 Metal K-Edges
15.3 Metal L-Edges
15.4 Resonant Inelastic X-Ray Scattering
15.5 Conclusion
Acknowledgments
References
16 Semiconductors
Federico Boscherini
16.1 Introduction
16.2 XAS Instrumental Aspects
16.3 Applications
16.4 Conclusion
References
17 XAS Studies on Mixed Valence Oxides
Joaqu?n Garc?a, Gloria Sub?as and Javier Blasco
17.1 Introduction
17.2 Solid State Applications (Mixed Valence Oxides)
17.3 Conclusion
References
18 Novel XAS Techniques for Probing Fuel Cells and Batteries
David E. Ramaker
18.1 Introduction
18.2 XANES Techniques
18.3 In Operando Measurements
18.4 Future Trends
18.5 Appendix
References
19 X-ray Spectroscopy in Studies of the Nuclear Fuel Cycle
Melissa A. Denecke
19.1 Background
19.2 Application Examples
19.3 Conclusion and Outlook
References
20 Planetary, Geological and Environmental Sciences
Francois Farges and Max Wilke
20.1 Introduction
20.2 Planetary and Endogenous Earth Sciences
20.3 Environmental Geosciences
20.4 Conclusion
Acknowledgments
References
21 X-Ray Absorption Spectroscopy and Cultural Heritage: Highlights and Perspectives
Franc¸ois Farges and Marine Cotte
21.1 Introduction
21.2 Instrumentation: Standard and Recently Developed Approaches
21.3 Some Applications
21.4 Conclusion
Acknowledgments
References
22 X-ray Spectroscopy at Free Electron Lasers
Wojciech Gawelda, Jakub Szlachetko and Christopher J. Milne
22.1 Introduction to X-ray Free Electron Lasers in Comparison to Synchrotrons
22.2 Current Implementations of X-Ray Spectroscopy Techniques at XFELs
22.3 Examples of Time-Resolved X-Ray Spectroscopy at XFELs
22.4 Examples of Nonlinear X-Ray Spectroscopy at XFELs
22.5 Conclusion and Outlook
References
23 X-ray Magnetic Circular Dichroism
Andrei Rogalev, Katharina Ollefs and Fabrice Wilhelm
23.1 Historical Introduction
23.2 Physical Content of XMCD and the Sum Rules
23.3 Experimental Aspects and Data Analysis
23.4 Examples of Recent Research
23.5 Conclusion and Outlook
Acknowledgments
References
24 Industrial Applications
Simon R. Bare and Jeffrey Cutler
24.1 Introduction
24.2 The Patent Literature
24.3 The Open Literature
24.4 Examples of Applications from Light Sources
24.5 Examples of Applications from Companies
24.6 Conducting Industrial Research at Light Sources
24.7 Conclusion and Outlook
Acknowledgements
References
25 XAS in Liquid Systems
Adriano Filipponi and Paola D'Angelo
25.1 The Liquid State of Matter
25.2 Computer Modelling of Liquid Structures
25.3 XAFS Calculations in Liquids/Disordered Systems
25.4 Experimental and Data-Analysis Approaches
25.5 Examples of Data Analysis Applications
References
26 Surface Metal Complexes and Their Applications
Joseph D. Kistler, Pedro Serna, Kiyotaka Asakura and Bruce C. Gates
26.1 Introduction
26.2 Aim of the Chapter
26.3 Mononuclear Iridium Complexes Supported on Zeolite HSSZ-53: Illustration of EXAFS
Data Fitting and Model Discrimination
26.4 Iridium Complexes Supported on MgO and on Zeolites: Precisely Synthesized Isostructural Metal Complexes on Supports with Contrasting Properties as Ligands
26.5 Supported Chromium Complex Catalysts for Ethylene Polymerization Characterization of Samples Resembling Industrial Catalysts
26.6 Copper Complexes on Titania: Insights Gained from Samples Incorporating Single-Crystal Supports
26.7 Gold Complexes Supported on Zeolite NaY: Determining Crystallographic Locations of Metal Complexes on a Support by Combining EXAFS Spectroscopy and TEM
26.8 Gold Supported on CeO2: Conversion of Gold Complexes into Clusters in a CO Oxidation Catalyst Characterized by Transient XAFS Spectroscopy
26.9 Mononuclear Rhodium Complexes and Dimers on MgO: Discovery of a Catalyst for Selective Hydrogenation of 1,3-Butadiene
26.10 Osmium Complexes Supported on MgO: Determining Structure of the Metal-Support Interface and the Importance of Support Surface Defect Sites
26.11 Conclusion
Acknowledgments
References
27 Nanostructured Materials
Alexander V. Soldatov and Kirill A. Lomachenko
27.1 Introduction
27.2 Small Nanoclusters
27.3 XAS and XES for the Study of Nanoparticles
27.4 Nanostructures and Defects in Solids
27.5 Conclusion and Outlook
References
Index
