Nickel and nickel-copper alloy modified glassy carbon electrodes (GC/Ni and GC/NiCu) prepared by galvanostatic deposition were examined for their redox process and electrocatalytic activities towards the oxidation of methanol in alkaline solutions. The methods of cyclic voltammetery (CV) and chronoamperometry (CA) were employed. The cyclic voltammogram of NiCu alloy demonstrates the formation of beta/beta crystallographic forms of the nickel oxyhydroxide under prolonged repetitive potential cycling in alkaline solution. in CV studies, in the presence of methanol NiCu alloy modified electrode shows a significantly higher response for methanol oxidation. The peak current of the oxidation of nickel hydroxide increase is followed by a decrease in the corresponding cathodic current in presence of methanol. The anodic peak currents show linear dependency with the square root of scan rate. This behavior is the characteristic of a diffusion controlled process. Under the CA regime the reaction followed a Cottrellian behavior and the diffusion coefficient of methanol was found to be 2 x 10(-6) cm(2) s (1) in agreement with the values obtained from CV measurements. (C) 2008 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.