A facile one‐step electrochemical codeposition of platinum‐gold (PtAu) alloy materials embedded in N‐[3‐(trimethoxysilyl)propyl] ethylenediamine (EDAS) silicate sol‐gel on indium‐tin‐oxide electrode (ITO/EDAS‐PtAu) is reported. The x‐ray diffraction patterns, X‐ray photoelectron spectroscopy analysis, scanning electron microscopy, energy dispersive X‐ray analysis, elemental mapping, line scan spectra and cyclic voltammetric studies showed the formation of PtAu bimetallic microstructures at the ITO/EDAS‐PtAu electrodes. The electrochemically codeposited PtAu alloy microstructures materials showed profound enhancement for methanol oxidation reaction in alkaline medium. The observed results revealed that the present facile synthetic methodology for the preparation of PtAu alloy microstructures materials embedded in silicate sol‐gel (ITO/EDAS‐PtAu) modified electrode is a promising approach and the modified electrode showed enhanced mass activity and stability towards methanol oxidation reaction.
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