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Title: Exploring electrochemical deposition in aqueous and non-aqueous solvents using boron doped diamond electrodes
Author: Hussein, Haytham E. M.
ISNI:       0000 0004 7972 4094
Awarding Body: University of Warwick
Current Institution: University of Warwick
Date of Award: 2018
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In this thesis, we use boron doped diamond (BDD) because of its unique properties such as: a high thermal conductivity, a good resistance to chemical and electrochemical attack, a very large potential window, and low background currents to investigate electrochemical deposition of the platinum group metals. We first explore the effects of deposition potential and time, in tandem with temperature control, on the morphology of Pt nanostructures created. In this way, we managed to make porous Pt nanoparticles (NPs) via a one-step deposition. We then further use electrochemistry as a diagnostic and analytical technique for characterisation of their electrocatalytic properties, using Pt NPs for studying methanol oxidation for energy conversion applications. Having realised the power of the transmission electron microscope (TEM) as an analytical and a quantitative tool. We made thin BDD (few nm thickness), to provide an electrode, which is electron transparent. Using this dual function BDD in combination with complimentary high-resolution electron microscopy techniques, it was possible to investigate the nucleation and growth of Au at the atomic level. By taking time snapshots, we can provide information about the mechanisms of early stage phase formation and the transition of amorphous nanostructures to crystalline NPs. Finally, we carry out spectroscopic, analytical and electrochemical studies to understand ion-ion, ion-solvent and solvent-solvent interactions, which then aid the utilisation of electrodeposition for the recovery of Pd from industrial-like solutions. We show that the addition of water to acetonitrile switches on the Pd electrodeposition from its Pd-acetate compound. Moreover, we provide proof of concept measurements for the electrochemical recovery of Pd from an organic synthesis solution, without impacting the organic molecules or the active pharmaceutical ingredients. In general, BDD holds a great avenue for nucleation and growth studies, provides features that allow controlling the metal electrodeposition and can be used to make specific nanostructures and catalysers.
Supervisor: Not available Sponsor: Engineering and Physical Sciences Research Council ; University of Warwick
Qualification Name: Thesis (Ph.D.) Qualification Level: Doctoral
EThOS ID:  DOI: Not available
Keywords: QD Chemistry