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Nanocrystalline nickel with an average diameter of about 16 nm and a face-centered cubic (fcc)structure was uniformly attached to the surface of carbon nanotubes (CNT) by wet chemistry.The sample was characterized by X-ray powder diffraction and transmission electron microscopy (TEM).A glass carbon electrode modified with nickel-modified multi-wall carbon nanotubes (MWCNTs-Ni/GCE) was prepared.The electrochemical behavior of the MWCNTs-Ni/GCE and the electrocatalytic oxidation of methanol at the MWCNTsNi/GCE were investigated by cyclic voltammetry in 1.0 mol/L NaOH solution.The cyclic voltammograms showed that the electron transfer between β-Ni(OH)2 and β-NiOOH is mainly a diffusion-controlled quasireversible process,and that the electrode has high catalytic activity for the electrooxidation of methanol in alkaline medium,revealing its potential application in alkaline rechargeable batteries and fuel cells.