In situ XAFS Study of Palladium Electrodeposition at the Liquid/Liquid Interface

Samuel Booth, Sin-Yuen Chang, Akihiro Uehara, Camille La Fontaine, Giannantonio Cibin, Sven L. M. Schroeder, Robert Dryfe

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    We report the use of XAFS (X-ray absorption fine structure) as an in situ method to follow the electrochemically driven deposition of palladium nanoparticles at a liquid/liquid interface. A novel glass/plastic hybrid electrochemical cell was used to enable control of the potential applied to the liquid/liquid interface. In situ measurements indicate that the nucleation of metallic nanoparticles can be triggered through chronoamperometry or cyclic voltammetry. In contrast to spontaneous nucleation at the liquid/liquid interface, whereby fluctuations in Pd oxidation state and concentration are observed, under a fixed interfacial potential the growth process occurs at a steady rate leading to a build-up of palladium at the interface. Raman spectroscopy of the deposit suggests that the organic electrolyte binds directly to the surface of the deposited nanoparticles. It was found that the introduction of citric acid results in the formation of spherical nanoparticles at the interface.
    Original languageEnglish
    Pages (from-to)251-261
    Number of pages11
    JournalElectrochimica Acta
    Early online date14 Mar 2017
    Publication statusPublished - 1 May 2017


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