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The cyclic voltammetry, current-time curve at potential step and constant current method were used to investigate the electrochemical behaviour of nickel chloride on the Pt eletrodes in N,N-dimethylformamide (DMF). The experimental results indicate that the reduction of Ni(Ⅱ) is irreversible in two steps, first [Ni(solvent)n](Ⅱ)+2e→[Ni(solvent)n](0) and then is reduced to the metal. The transfer coefficient and diffusion coefficient of Ni(Ⅱ) in DMF were also determined.