Scanning Electrochemical Microscopy (SECM) is a unique technique for studying fast heterogeneous kinetics and to map reactivity gradients along the surface of an electrocatalyst, especially when it involves multiple surface sites of varying reactivity. It combines the dual advantages offered by ultramicroelectrode (UME) voltammetry in terms of reduced ohmic drop and insignificant double layer charging contribution with the advantages of imaging by rastering the UME across an electro-active surface. In this work, we demonstrate these distinctive features of SECM in evaluating reactivity gradients on catalyst (Pt/C) coated Nafion® films towards hydrogen oxidation activity, a reaction of immense technological relevance. Imaging has been performed in the feedback mode by allowing H2 evolution at the tip (25 𝜇m Pt UME), which is reoxidized at the substrate electrode containing Pt/C-Nafion film. Interesting distribution in H2 oxidation activity has been observed as a function of potential applied to the Pt/CNafion film. In addition, a plot of normalized tip current versus the substrate electrode potential indicates the effect of potential-induced reactivity change in the catalyst-coated membranes. The results of the present investigation are believed to be useful to H2/O2 PEM fuel cells with respect to evaluating reactivity gradients of catalyst-coated polymer electrolyte membranes, which is important to rectify problems related to catalyst utilization.
Volume 134, 2022
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