In this work, Ni-Co alloy coating on the surface of glassy carbon (GC) electrode was performed by cyclic voltammetry. The results showed that the deposition of Ni-Co is an anomalous process. The deposition bath was prepared according to the metal ion Ni/Co ratio of 4:1 using NiSO4 center dot 7H(2)O and CoSO4 center dot 8H(2)O, and the total concentration of all solutions was 40.0 mM. The pH of the bath solution was adjusted at 2.0 using boric acid at room temperature. The modified electrode was conditioned by potential recycling in a potential range of 100-700 mV (vs. Ag/AgCl) by cyclic voltammetric method in an alkaline solution. The Ni-Co modified electrode showed a higher activity towards methanol oxidation in the Ni (III) and Co (IV) oxidation states. Cyclic voltammetry was used for the electrochemical characterization of the Ni-Co modified electrode and the mechanism of methanol oxidation is proposed. The result of double steps chronoamperometry shows that the methanol electrooxidation is an irreversible reaction. Moreover, the effects of various parameters such as mole ratio of Ni-Co in the alloy in modification step, potential scan rate, methanol concentration and solution temperature on the electro-oxidation of methanol have also been investigated. (C) 2011 Elsevier Ltd. All rights reserved.