X-Ray Studies on Electrochemical Systems: Synchrotron Methods for Energy Materials

Description

This book is your graduate level entrance into battery, fuel cell and solar cell research at synchrotron x-ray sources. Materials scientists find numerous examples for the combination of electrochemical experiments with simple and with highly complex x-ray scattering and spectroscopy methods. Physicists and chemists can link applied electrochemistry with fundamental concepts of condensed matter physics, physical chemistry and surface science. Contents: Introduction Molecular Structure and Electronic Structure Crystal Structure and Microstructure Real Space Imaging and Tomography Resonant Methods and Chemical Contrast Variation Surface Sensitive and Volume Sensitive Methods Organic and Bio-Organic Samples Complex Case Studies / Electrochemical In Situ Studies Correlation of Electronic Structure And Conductivity Radiation Damages Background Subtraction X-Ray Physics Nobel Prizes Synchrotron Centers World Electromagnetic Spectrum Kα,Β X-Ray Energies Periodic Table of Elements Includes investigations of organic materials, bio-electronic interfaces and devices. Covers surface & volume sensitive methods. The first comprehensive treatment for chemical energy storage and conversion devices from the atomic & molecular scale. Preface Acknowledgement Contents 1 Introduction 2 Molecular structure and electronic structure 2.1 X-ray absorption spectroscopy 2.1.1 Hard X-rays: XAS and XANES 2.1.2 Soft X-ray spectroscopy: NEXAFS 2.2 X-ray emission spectroscopy 2.2.1 Hard X-ray emission 2.2.2 Energy-Dispersive X-ray Spectroscopy (EDS, EDX, or XEDS) 2.2.3 Soft X-ray emission spectroscopy 2.3 X-ray photoelectron spectroscopy 2.3.1 Core level spectroscopy 2.3.2 Valence band spectroscopy 3 Crystal structure and microstructure 3.1 X-ray diffraction 3.2 X-ray wide-angle scattering 3.3 Small-angle X-ray scattering (SAXS) 3.3.1 SAXS on GC supercapacitor electrodes 3.3.2 Excursion to ultra small-angle neutron scattering (USANS) 3.3.3 USAXS on aerogel catalysts 3.4 Extended X-ray absorption fine structure (EXAFS) spectroscopy 3.5 X-ray reflectometry 3.5.1 XRR on photoelectrode materials 3.5.2 In situ and operando X-ray and neutron reflectometry on electrochemical systems 3.5.3 Neutron reflectometry on electrochemical systems 4 Real space imaging and tomography 4.1 X-ray imaging and X-ray microscopy 4.1.1 Polymer electrolyte membrane fuel cells 4.1.2 Batteries 4.2 Neutron imaging and radiography 4.2.1 Solid oxide fuel cells 4.3 Complementarity of X-ray and neutron methods 4.4 Tomography 4.4.1 Neutron tomography on SOFC 4.4.2 X-ray tomography on SOFC 4.4.3 Tomography on PEM-FC 4.4.4 Tomography on batteries 4.5 Scanning transmission X-ray microspectroscopy (STXM) 4.5.1 STXM on PEM fuel cells 4.5.2 STXM on lithium ion batteries 4.5.3 STXM on biological samples 4.5.4 STXM on soot from combustion processes 4.5.5 STXM on Liesegang rings 5 Resonant methods and chemical contrast variation 5.1 X-ray tube (Kathodenstrahlen) 5.2 Synchrotron storage rings 5.3 Anomalous X-ray diffraction 5.3.1 Distinguishing W and Cu in CuWO4 photoanodes 5.3.2 Separation of manganite spinel diffractogram from other battery components 5.3.3 Diffraction on substituted protonated ceramic proton conductors 5.4 Anomalous small-angle X-ray scattering 5.4.1 In situ ASAXS on lithium batteries 5.4.2 In situ ASAXS on Pt-based PEM-FC assemblies 5.4.3 ASAXS on SOFC assemblies 5.5 Resonant photoemission spectroscopy 5.5.1 SOFC cathodes 5.5.2 Mn 2p resonant photoelectron spectroscopy for SOFC chromium poisoning 5.5.3 VB PES on photoelectrodes 5.5.4 Lithium ion battery cathodes 5.5.5 Resonant inelastic X-ray scattering 6 Surface-sensitive and volume-sensitive methods 6.1 X-ray Raman spectroscopy 6.2 Hard X-ray XPS and hard X-ray PES (HAX-PES) 6.3 X-ray standing waves for electrochemical double layer studies 6.3.1 Resonant photoemission spectroscopy on thin thermochromic window VO2 films 7 Organic and bio-organic samples 7.1 X-ray studies on polymer electrolyte membranes 7.2 Organic solar cells 7.2.1 Organic dyes for photosensitization 7.3 Proteins, enzymes, bio-catalysts, living cells, and biofilms 7.3.1 Protein crystallography 7.3.2 Reflectometry on proteins and cells 7.3.3 Protein spectroscopy 7.3.4 Bioelectrodes, biofilms, and bioelectricity 7.3.5 Photoelectrochemical studies on cyanobacteria during γ
-irradiation 8 Complex case studies/electrochemical in situ studies 8.1 Lithium ion batteries 8.1.1 Battery cell assembly and ex situ studies on materials and components 8.1.2 Manufacturing and assembly of in situ battery cells at the synchrotron 8.1.3 Operando XANES, anomalous XRD, EXAFS, and ASAXS on a lithium ion battery 8.1.4 Operando X-ray Raman study on a lithium ion battery 8.2 Ceramic fuel cells 8.2.1 Ceramic proton conducting electrolyte membranes 8.2.2 SOFC anode poisoning and sulfur molecular structure 8.3 Photoelectrochemical cells (for solar hydrogen) 8.3.1 Operando NEXAFS spectroscopy during water splitting 8.3.2 Operando photoelectron spectroscopy during water splitting 8.4 Bioelectrochemical systems 8.4.1 Fe 3p resonant VB XPS on phycocyanin adsorbed on iron oxide 8.4.2 Operando NAP-XPS spectroscopy on an illuminated algal biofilm 8.5 Electrochemical double layer capacitors 8.5.1 X-ray diffraction and wide angle scattering on glassy carbon 8.5.2 Small-angle scattering on supercapacitor electrodes with X-rays and with neutrons 8.5.3 NEXAFS spectroscopy on thermally oxidized glassy carbon plates 9 Correlation of electronic structure and conductivity 9.1 Hole conductivity in SOFC cathodes 9.2 SOFC chromium poisoning 9.3 Proton conductivity in IT-SOFC electrolytes 9.4 Lithium ion batteries 9.5 Water splitting photoelectrodes 10 Radiation damages 11 Background subtraction 11.1 Optical absorption spectra of phycocyanin on a photoelectrode 11.2 NEXAFS data on CuWO4 from BESSY-II 11.3 Treatment of optical Raman spectra 11.4 Background subtraction for an empty cell Appendix References Index