Reflection extended X-ray absorption fine structure

Reflection extended x-ray absorption fine-structure spectroscopy (RcnEXAFS)... 

Agostini G, Groppo E, Bordiga S, et al Reactivity of Cr species grafted on SiO2/Si(100) surface a reflection extended X-ray absorption fine structure study down to the suh-monolayer regime, J Phys Chem C 111(44) 16437—16444, 2007. 

This chapter contains articles on six techniques that provide structural information on surfaces, interfeces, and thin films. They use X rays (X-ray diffraction, XRD, and Extended X-ray Absorption Fine-Structure, EXAFS), electrons (Low-Energy Electron Diffraction, LEED, and Reflection High-Energy Electron Diffraction, RHEED), or X rays in and electrons out (Surfece Extended X-ray Absorption Fine Structure, SEXAFS, and X-ray Photoelectron Diffraction, XPD). In their usual form, XRD and EXAFS are bulk methods, since X rays probe many microns deep, whereas the other techniques are surfece sensitive. There are, however, ways to make XRD and EXAFS much more surfece sensitive. For EXAFS this converts the technique into SEXAFS, which can have submonolayer sensitivity. 

Alternatives to XRD include transmission electron microscopy (TEM) and diffraction, Low-Energy and Reflection High-Energy Electron Diffraction (LEED and RHEED), extended X-ray Absorption Fine Structure (EXAFS), and neutron diffraction. LEED and RHEED are limited to surfaces and do not probe the bulk of thin films. The elemental sensitivity in neutron diffraction is quite different from XRD, but neutron sources are much weaker than X-ray sources. Neutrons are, however, sensitive to magnetic moments. If adequately large specimens are available, neutron diffraction is a good alternative for low-Z materials and for materials where the magnetic structure is of interest. 

These conclusions from the infrared reflectance spectra recorded with Pt and Pt-Ru bulk alloys were confirmed in electrocatalysis studies on small bimetallic particles dispersed on high surface area carbon powders.Concerning the structure of bimetallic Pt-Ru particles, in situ Extended X-Ray Absorption Fine Structure (EXAFS>XANES experiments showed that the particle is a true alloy. For practical application, it is very important to determine the optimum composition of the R-Ru alloys. Even if there are still some discrepancies, several recent studies have concluded that an optimum composition about 15 to 20 at.% in ruthenium gives the best results for the oxidation of methanol. This composition is different from that for the oxidation of dissolved CO (about 50 at.% Ru), confirming a different spatial distribution of the adsorbed species. 

Final justification for using terms such as inner- or outer-sphere awaits direct spectroscopic confirmation. Electron Spin Resonance, Mossbauer, and Fourier Transform Infrared-Cylindrical Internal Reflection Spectroscopic techniques are being used to establish the structure of surface complexes (see, e.g., McBride, Ambe et al., and Zeltner et al., this volume). The potential for using EXAFS (extended x-ray absorption fine structure) to establish the type of surface complex for Pb + adsorbing onto goethite is currently being undertaken in our laboratory. 

Rutherford Backscattering Spectroscopy Reflection High-Energy Electron Diffraction Scanning Electron Microscopy Surface (Sensitive) Extended X-Ray Absorption Fine Structure... 

Surface Extended X-ray Absorption Fine Structure Surface Integrated Molecular Orbital/Molecular Mechanics Scanning Reflection Electron Microscopy Scanning Tunneling Microscope [or Microscopy]... 

Spectroscopy. - In the following paragraphs we discuss how various spectroscopy tools have been used to illuminate the rich surface chemistry of supported polynuclear metal complexes. These methods include infrared (both diffuse reflectance and transmission), ultraviolet and visible (UV-Vis), x-ray photoelectron spectroscopy (XPS), and x-ray absorption, near edge spectroscopy s (XANES) and extended X-ray absorption fine structure (EXAFS) spectroscopy s. 

Surface analytical techniques. A variety of spectroscopic methods have been used to characterize the nature of adsorbed species at the solid-water interface in natural and experimental systems (Brown et al, 1999). Surface spectroscopy techniques such as extended X-ray absorption fine structure spectroscopy (EXAFS) and attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) have been used to characterize complexes of fission products, thorium, uranium, plutonium, and uranium sorbed onto silicates, goethite, clays, and microbes (Chisholm-Brause et al, 1992, 1994 Dent et al, 1992 Combes et al, 1992 Bargar et al, 2000 Brown and Sturchio, 2002). A recent overview of the theory and applications of synchrotron radiation to the analysis of the surfaces of soils, amorphous materials, rocks, and organic matter in low-temperature geochemistry and environmental science can be found in Fenter et al (2002). 

Ebert M, Mair V, Tessadri R, Hoffmann P, Ortner HM (2000) Total-reflection X-ray fluorescence analysis of geological microsamples. Spectrochim Acta 55 205-212 Eisenberger P, Lengeler (1980) Extended X-ray absorption fine-structure determination of coordination numbers limitations. Phys Rev 22 3551-3562... 

Heald SM, Chen H, Tranquada (1988) Glancing-angle extended X-ray-absorption fine structure and reflectivity studies of interfacial regions. Phys Rev 38 1016-1026... 

Structure of Active Sites. - Klier and others have claimed that the active phase is a Cu" species dissolved in ZnO. Estimating the amount of dissolved Cu" reflected irreversible chemisorption of CO in proportion to the dissolved Cu" ". The existence of Cu in the active state is verified by means of Auger electron spectroscopy (AES), X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS), but it is also pointed out that the Cu" concentration depends upon the total content of Cu in the catalyst. 

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