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Polyrhodanine/Zinc Oxides (PRh/ZnO) nanocomposites were successfully synthesized through an in‐situ polymerization method. After that, the nanocomposites served as a substrate for bimetallic nickel‐platinum (Ni−Pt) to form PRh/ZnO/Ni/Pt electrocatalyst. Characterization methods including field emission scanning electron microscopy (FESEM), Fourier transform infrared spectroscopy (FTIR) and x‐ray diffraction analysis (XRD) were then employed to investigate the morphology and chemical structure of synthesized samples. Next, the electrochemical activity of fabricated PRh/ZnO/Ni/Pt electrocatalyst in methanol electrooxidation reaction in alkaline media was investigated via cyclic voltammetry (CV) and chronoamperometric (CA) measurements. The experimental results indicated that the addition of Ni to the synthesized PRh/ZnO/Pt led to a higher electrochemically active surface area (EASA). Also, from the CV tests, a desirable amount of maximum anodic current density was achieved for the PRh/ZnO/Ni/Pt, which was as much as 35 mA cm−2. With regard to the density functional theory (DFT) calculations, computational results suggested that utilizing the PRh/ZnO structure beside Ni and Pt resulted in the improvement of the reactivity of catalyst and a decrease in the energy gap which was consistent with the experimental findings.