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Electrochemical analysis of nanostructured iron oxides using cyclic voltammetry and scanning electrochemical microscopy
Electrochimica Acta, vol. 222, pp. 1326-1334
Iron oxides in general and especially hematite, α-Fe2O3, have become promising materials for the alkaline water electrolysis and photoelectrochemical water splitting, respectively. In the present study electrocatalytic electrodes with a thin film of α-Fe2O3 and with vertically aligned α-Fe2O3 nanowires were prepared. Cyclic voltammograms of the α-Fe2O3 nanowires revealed differences including a series of three unreported cathodic signals when compared to previously published voltammograms for polycrystalline iron oxides. The generation-collection mode of scanning electrochemical microscopy (SECM) using nanostructured Pt microdisc probes was exploited to detect soluble reaction products formed at the voltammetric peaks of the α-Fe2O3 electrode. SECM tip-substrate voltammetry unexpectedly showed that the reduction of FeVI to FeIII on the cathodic sweep is accompanied by significant O2 evolution.