We prepared a simple, one-step synthesis of Pt-M (M = Co, Cu & Fe)/C supported on Vulcan-XC-72 carbon using the polyol reduction method. The morphology, structure and elemental composition of the prepared catalysts were confirmed by transmission electron microscopy (TEM), X-ray diffraction (XRD) and energy dispersive X-ray spectroscopy (EDX). Electrochemical characterization including electrochemical impedance, cyclic voltammetry and chronoamperometry were studied to compare the electrochemical activity of the as-prepared catalyst with standard 20 wt % Pt/C. From transmission electron microscopy studies, the estimated average particle size for PtFe/C, PtCo/C and PtCu/C were 16, 12 and 10 nm respectively. In cyclic voltammetry studies, the PtFe/C catalyst exhibited the maximum current density for electrooxidation of methanol (14.88 mA cm−2), compared to PtCu/C (9.96 mA cm−2), PtCo/C (4.66 mA cm−2) and Pt/C (2.34 mA cm−2). Also, the negative sweep onset potential and greater If/Ib ratio verified the enhanced activity of the PtFe/C catalyst. The stability of the catalyst was studied using chronoamperometric methods, which reveals the slow decay of the prepared catalyst and higher current density for initial and final time intervals. Impedance studies confirm that the PtFe/C catalyst exhibits the smallest semicircle, suggesting a significantly higher electrooxidation rate in comparison to the other catalysts. The electrocatalytic activity of the prepared catalyst follows the order: PtFe/C > PtCu/C > PtCo/C > Pt/C.
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