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E-raamat: X-ray Absorption Spectroscopy for the Chemical and Materials Sciences

  • Formaat: PDF+DRM
  • Ilmumisaeg: 23-Nov-2017
  • Kirjastus: John Wiley & Sons Inc
  • Keel: eng
  • ISBN-13: 9781118676172
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  • Formaat: PDF+DRM
  • Ilmumisaeg: 23-Nov-2017
  • Kirjastus: John Wiley & Sons Inc
  • Keel: eng
  • ISBN-13: 9781118676172

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This book is a practical guide to help investigators choose the right experiment, carry it out properly and analyse the data to give the best reliable result. It book gives readers insights to extract what they need from the world of large scale experimental facilities like synchrotrons. Key features: * A no-nonsense introduction to the technique and applications of x-ray absorption spectroscopy * XAFS is now an everyday tool for the structural analysis of material science, biology and catalysts * Features Questions and Answers to support the student s learning through the book * Relevant to all working on synchrotron sources and applications in physics, materials, environment/geology, and biomedical materials * Four-colour representation to allow easy interpretation of images and data for the reader
About the Author ix
Preface xi
Acknowledgments xiii
Glossary and Abbreviations xv
1 Introduction to X-Ray Absorption Fine Structure (XAFS)
1(8)
1.1 Materials: Texture and Order
1(1)
1.2 Absorption and Emission of X-Rays
2(1)
1.3 XANES and EXAFS
2(1)
1.4 Information Content
3(1)
1.5 Using X-Ray Sources as They Were
4(1)
1.6 Using Light Sources Now and To Be
5(2)
1.7 Questions
7(2)
References
8(1)
2 Basis of XAFS
9(24)
2.1 Interactions of X-Rays With Matter
9(15)
2.1.1 Absorption Coefficients
9(1)
2.1.2 Absorption Edges
10(2)
2.1.3 XANES and EXAFS
12(1)
2.1.3.1 XANES Features
13(3)
2.1.3.2 Edge Position
16(3)
2.1.3.3 The EXAFS Effect
19(2)
2.1.3.4 EXAFS Quantification
21(3)
2.2 Secondary Emissions
24(6)
2.2.1 X-Ray Fluorescence
26(2)
2.2.2 Electron Emission
28(1)
2.2.3 Resonant Inelastic X-Ray Scattering or Spectroscopy (RIXS)
29(1)
2.3 Effects of Polarization
30(1)
2.3.1 Plane (Linear) Polarization
30(1)
2.3.2 Circular Polarization
30(1)
2.3.3 Magnetic Dichroism
30(1)
2.4 Questions
31(2)
References
32(1)
3 X-Ray Sources and Beamlines
33(28)
3.1 Storage Rings
33(10)
3.1.1 Second-and Third-Generation Sources
33(1)
3.1.2 Bending Magnet Radiation
34(4)
3.1.3 Insertion Devices
38(1)
3.1.3.1 Wavelength Shifters and Multipole Wigglers
38(1)
3.1.3.2 Planar Undulators
38(3)
3.1.3.3 Helical Undulators
41(1)
3.1.4 Time Structure
41(2)
3.2 Other Sources
43(2)
3.2.1 Laboratory Sources
43(1)
3.2.2 Plasma Sources
44(1)
3.2.3 High Harmonic Generation
44(1)
3.2.4 Free Electron Lasers (FELs)
44(1)
3.3 Beamline Architecture
45(12)
3.3.1 Mirrors
48(1)
3.3.2 Monochromators
49(6)
3.3.3 Near-Sample Focusing Elements
55(1)
3.3.3.1 Kirkpatrick-Baez (KB) Mirrors
55(1)
3.3.3.2 X-Ray Lenses
56(1)
3.3.3.3 Zone Plates
56(1)
3.4 Effect of Photon Energy on Experiment Design
57(1)
3.5 Questions
58(3)
References
59(2)
4 Experimental Methods
61(56)
4.1 Sample Characteristics
62(2)
4.1.1 X-Ray Absorption of Samples
62(1)
4.1.2 Classes of Experimental Layouts
63(1)
4.2 Scanning Modes
64(3)
4.2.1 Scanning XAFS
64(2)
4.2.2 Energy Dispersive XAFS
66(1)
4.3 Detection Methods
67(28)
4.3.1 Transmission
67(7)
4.3.2 Electron Yield
74(2)
4.3.3 Fluorescence
76(3)
4.3.3.1 Total Fluorescence Yield
79(7)
4.3.3.2 High-Resolution Fluorescence Detection (HERFD) and X-Ray Emission Spectroscopy (XES)
86(4)
4.3.3.3 Resonant Inelastic X-Ray Scattering or Spectroscopy (RIXS)
90(1)
4.3.3.4 Inelastic X-Ray Raman Scattering (XRS) or Nonresonant Inelastic X-Ray Scattering (NIXS)
91(3)
4.3.4 X-Ray Excited Optical Luminescence (XEOL)
94(1)
4.4 Spatial Resolution
95(8)
4.4.1 Methods of Studying Textured Materials
95(1)
4.4.2 Full-Field Transmission X-Ray Microscopy (TXM)
96(3)
4.4.3 X-Ray Photoelectron Emission Microscopy (X-PEEM)
99(1)
4.4.4 Focused-Beam Microscopies
100(1)
4.4.4.1 Scanning Micro- and Nano-Focus Microscopy
100(2)
4.4.4.2 Scanning (Transmission) X-Ray Microscopy (STXM)
102(1)
4.5 Combining Techniques
103(3)
4.5.1 Two-Color XAFS
103(1)
4.5.2 X-Ray Scattering
104(2)
4.6 X-Ray Free Electron Lasers (XFELs)
106(4)
4.6.1 Laser-Pump Measurements
107(1)
4.6.2 Sampling Environments
108(1)
4.6.3 X-Ray Beam Intensity
109(1)
4.6.4 XAS and XES
109(1)
4.7 Questions
110(7)
References
111(6)
5 Data Analysis and Simulation Methods
117(46)
5.1 Background Subtraction
119(4)
5.1.1 Experimental Considerations
119(2)
5.1.2 Background Subtraction Procedures
121(2)
5.2 Compositional Analysis
123(7)
5.2.1 Single Energy Comparisons
123(1)
5.2.2 Least Squares Analysis
124(2)
5.2.3 Principal Component Analysis
126(3)
5.2.4 Mapping Procedures
129(1)
5.3 Structural Analysis
130(23)
5.3.1 EXAFS Analysis
130(2)
5.3.1.1 Distance Measurement
132(1)
5.3.1.2 Angle Estimation
133(5)
5.3.1.3 Coordination Number Estimation
138(2)
5.3.1.4 Speciation of Back-Scattering Elements
140(3)
5.3.1.5 Goodness of Fit
143(2)
5.3.2 XANES Simulations
145(1)
5.3.2.1 K Edge XANES
145(1)
5.3.2.2 L Edge XANES
146(4)
5.3.3 XES and RIXS Simulations
150(3)
5.4 Present To Future Opportunities
153(1)
5.5 Questions
154(9)
References
155(8)
6 Case Studies
163(34)
6.1 Chemical Processing
164(20)
6.1.1 Liquid Phase Reactions
164(101)
6.1.1.1 Steady State or Slow Reactions (Minutes-Hours)
165(1)
6.1.1.2 Fast Reactions (Ms to Minutes)
166(7)
6.1.1.3 Very Fast Reactions (~100 ps-ms)
173(4)
6.1.1.4 Ultrafast Reactions (fs - ps) 2
177(101)
6.1.2 Reactions of Solid-State Materials
178(101)
6.1.2.1 Steady-State or Slow Reactions (Minutes-Hours)
179(2)
6.1.2.2 Fast Reactions (Ms to Minutes)
181(3)
6.2 Functional Materials
184(2)
6.3 Imaging on Natural, Environmental, and Heritage Materials
186(106)
6.4 Questions
192(1)
References
193(4)
Index 197
JOHN EVANS, PHD, is currently Emeritus Professor in Inorganic Chemistry at the University of Southampton and a visiting scientist at the Diamond Light Source. Previously, he was Science Program Advisor at Diamond. He was awarded the Royal Society of Chemistry Tilden Medal in 1994 and the Royal Society of Chemistry Meldola Medal in 1978.