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The electrochemical behaviours of the hydrogen evolution reaction (HER) on electrodes prepared by composite coating of nanocrystalline Ni-Mo alloy particle which was formed by ball milling on nickel base has been studied by steady-state polarization and ac impedance techniques. The microstructure and the particle size of Ni-Mo alloy nanocrystals and the morphology of the composite-coated surface of the electrodes were examined by XRD, TEM and SEM. The mechanism of HER on the composite electrodes has been investigated as well. Results showed that for HER electrocatalytic activity which was enhanced with increasing milling time. The reaction rate of HER on the electrodes was proved to be controlled by electrodesorption. The direct composite coating of highly electroactive particles onto the surface may serve as a new approach to the preparation of electrode materials.

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