A scanning electrochemical microscopic (SECM) observation of oxygen evolution on a polycrystalline titanium electrode during anodic oxidation in 0.1 mol dm−3 H2SO4 was attempted to evaluate the heterogeneity of the electrode surface. The micro probe electrode, which was scanned above the titanium electrode surface, could detect oxygen evolved in parallel with the formation of anodic oxide film. The probe current image corresponding to the distribution of oxygen evolution was in good agreement with the conventional probe current image measured in pH 8.4 borate solution containing K4Fe(CN)6, indicating that the oxygen evolution took place preferentially on the substrate grain covered with the thinner oxide film. It is shown that the SECM measurement of oxygen detection is useful for in-situ evaluation of the heterogeneity of anodic oxide film on the metal electrode during anodic oxidation.
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Fushimi et al. (2000) studied this question.
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