Mao, Bingwei (1987) In-situ x-ray diffraction studies of electrochemical interfaces. University of Southampton, Doctoral Thesis.
Abstract
A major objective of the work presented in this thesis has been the improvement of in-situ X-ray diffraction procedures to the stage that they can provide a surface sensitive technique for the investigation of a variety of electrochemical interfacial systems. Comparisons are made in a brief overview between this in-situ X-ray diffraction technique and other techniques applicable to the investigation of electrochemical interfaces. The methodology for the in-situ X-ray diffraction (INSEX) experiments is then given, particular attention being drawn to electrode surface preparation, cell design and detection system maintenance. INSEX has been applied to monitor the structural changes in diverse systems: the ordering of thallium and thallium iodide monolayers in the underpotential deposition region of the Tl+/Ag and TlI/Ag systems; the reconstruction of platinized surfaces induced by hydrogen and carbon monoxide adsorption and structure loss of Pt surfaces in the double layer region and due to the formation of oxide films; structural changes of polyaniline films undergoing oxidation/reduction cycles between the leucoemeraldine and emeraldine forms. The diffraction information from the systems is assessed qualitatively by comparing the diffractograms with diffraction intensities calculated from the equation derived for scattering from monolayer structures. (D80427)
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