The present study employed a simple mechanochemical method followed by 24-h ultrasonication to synthesize oxide-free metallic bismuth (Bi) nanoparticles. This was further used to synthesize a Pt-Bi(x%)/C (NC-x) hybrid electrocatalyst for the hydrogen evolution reaction in alkaline media. X-ray photoelectron spectroscopy and contact angle measurements reveal, Bi modifies the electronic structure and surface morphology of the Pt/C electrocatalyst, thus enhancing reaction kinetics and active site availability. The relative three-electrode study reveals that optimised NC-20 electrocatalyst reduces the overpotentials by 10.44 % and enhances the current density by 53 % compared to commercial Pt/C. The practical applicability of the NC-20 electrocatalyst was studied with the 13 cm2 single cell anion exchange membrane electrolyser. The catalyst demonstrates promising performance where the current density of NC-20//IrO2 relatively increases by 22.6 % compared to standard Pt/ C//IrO2, and shows continuous production and stable performance when monitored for 30 h.

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