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Ni/multi-walled carbon nanotubes (MWNTs) nanocomposites were successfully synthesised via a simple, rapid and efficient approach. The electrochemical performance of the Ni/MWNTs composites modified glassy carbon electrode (Ni/MWNTs/GCE) was evaluated by using cyclic voltammetry. Direct glucose oxidation at such Ni/MWNTs/GCE was investigated in detail by discussing the effect of the structure and materials of the electrode on electrocatalytic oxidation of glucose. As a result, the authors found that the Ni/MWNTs/GCE exhibited high electrocatalytic activity to glucose oxidation in alkaline solution, and could be used for the development of a non-enzymatic glucose sensor.