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

DOI: 10.1016/j.electacta.2017.03.059 DOI Help

Authors: Samuel G. Booth (University of Manchester) , Sin-yuen Chang (Diamond Light Source) , Akihiro Uehara (Kyoto University) , Camille La Fontaine (Synchrotron Soleil) , Giannantonio Cibin (Diamond Light Source) , Sven Schroeder (Diamond Light Source; University of Leeds) , Robert A. W. Dryfe (University of Manchester)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Electrochimica Acta

State: Published (Approved)
Published: March 2017
Diamond Proposal Number(s): 13953

Abstract: 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.

Journal Keywords: Palladium; Electrodeposition; XANES; Nanoparticles

Subject Areas: Chemistry, Technique Development

Instruments: B18-Core EXAFS