Oxygen Evolution Reaction at IrO/Ir(Ni) Film Electrodes Prepared by Galvanic Replacement and Anodization: Effect of Precursor Ni Film Thickness.

IrO/Ir(Ni) film electrodes of variable Ni content have been prepared via a galvanic replacement method, whereby surface layers of pre-deposited Ni are replaced by Ir, followed by electrochemical anodization. Electrodeposition of Ni on a glassy carbon electrode support has been carried out at constant potential and the charge of electrodeposited Ni controlled so as to investigate the effect of precursor Ni layer thickness on the electrocatalytic activity of the corresponding IrO/Ir(Ni)/GC electrodes for the oxygen evolution reaction (OER). After their preparation, these electrodes were characterized by microscopic (SEM) and spectroscopic (EDS, XPS) techniques, revealing the formation of Ir deposits on the Ni support and a thin IrO layer on their surfaces. To determine the electroactive surface area of the IrO coatings, cyclic voltammograms were recorded in the potential range between hydrogen and oxygen evolution and the charge under the anodic part of the curves, corresponding to Ir surface oxide formation, served as an indicator of the quantity of active IrO in the film. The electrocatalytic activity of the coatings for OER was investigated by current-potential curves under steady state conditions, revealing that the catalysts prepared from thinner Ni films exhibited enhanced electrocatalytic performance.