In-situ X-ray diffraction of electrochemical systems
In-situ X-ray diffraction of electrochemical systems
The work presented in this thesis is aimed at the development of X-ray diffraction procedures to the stage where they can provide an in-situ structural technique for the investigation of the solid/solution interphase. A review of non-traditional in-situ techniques for investigating the electrochemical interphase is first presented and the range of data made available discussed. It is shown that none of the currently available in-situ methods can provide long or short range order parameters. A brief overview of ex-situ techniques is also given to show the kind of surface probe that enables such parameters to be obtained. A critical assessment of design criteria for the in-situ X-ray diffraction [INSEX] experiment is then given, drawing particular attention to methods of detection, electrode construction and cell design. To show the applicability of INSEX to the study of the solid/solution interphase, several systems have been studied from diverse areas of surface chemistry and electrochemistry; the intercalation and adsorption of halogens and interhalogen compounds by high surface area graphite (Papyex), structural changes in the Ni(OH)2 electrode during charging, the formation of nickel hydrides during the deposition of nickel from Watts type bathe and the ordering of the lead monolayer and double layer in the underpotential deposition region ofthe Pb2+/Ag couple.The information from each of these systems is then assessed and areas of future work with INSEX, of interest to electrochemists, given. Finally, suggestions for increasing technique sensitivity and data reliability by improvements to the experimental equipment are discussed.
University of Southampton
1983
Oliver, Alan John
(1983)
In-situ X-ray diffraction of electrochemical systems.
University of Southampton, Doctoral Thesis.
Record type:
Thesis
(Doctoral)
Abstract
The work presented in this thesis is aimed at the development of X-ray diffraction procedures to the stage where they can provide an in-situ structural technique for the investigation of the solid/solution interphase. A review of non-traditional in-situ techniques for investigating the electrochemical interphase is first presented and the range of data made available discussed. It is shown that none of the currently available in-situ methods can provide long or short range order parameters. A brief overview of ex-situ techniques is also given to show the kind of surface probe that enables such parameters to be obtained. A critical assessment of design criteria for the in-situ X-ray diffraction [INSEX] experiment is then given, drawing particular attention to methods of detection, electrode construction and cell design. To show the applicability of INSEX to the study of the solid/solution interphase, several systems have been studied from diverse areas of surface chemistry and electrochemistry; the intercalation and adsorption of halogens and interhalogen compounds by high surface area graphite (Papyex), structural changes in the Ni(OH)2 electrode during charging, the formation of nickel hydrides during the deposition of nickel from Watts type bathe and the ordering of the lead monolayer and double layer in the underpotential deposition region ofthe Pb2+/Ag couple.The information from each of these systems is then assessed and areas of future work with INSEX, of interest to electrochemists, given. Finally, suggestions for increasing technique sensitivity and data reliability by improvements to the experimental equipment are discussed.
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Published date: 1983
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Local EPrints ID: 460169
URI: http://eprints.soton.ac.uk/id/eprint/460169
PURE UUID: b7d85f34-2da6-49e6-9d37-fe683c42383f
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Date deposited: 04 Jul 2022 18:05
Last modified: 04 Jul 2022 18:05
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Author:
Alan John Oliver
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