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The hexagonal closed packed (hcp) nanocrystalline nickel (Ni), with an average diameter of 9.7 ± 2.27 nm was deposited uniformly on composite graphite (CG) by the rapid scanning (6,500 mVs–1) voltammetry technique. The hcp‐nano Ni‐modified CG electrode was investigated for the catalytic oxidation of methanol in alkaline medium through the formation of NiOOH. A high anodic current was obtained at peak potential of +570 mV vs Ag/AgCl. Both the scan rate and the methanol concentration affected the oxidation of methanol. The results showed that catalytic activity had increased with decrease in Ni particle diameter. It was also shown that the hcp‐nano Ni/CG modified electrode was the most efficient catalyst in the oxidation of methanol.

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