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The electrochemical properties of Dy(III), Ni(II) and Dy(III)+ Ni(II) in dimethylformamide were studied by cyclic voltammetry on Pt or Cu electrode . Black, metallic lustered, compact and well adhesive Dy-Ni alloy films can be co-deposited on Cu electrode by sweeping-potential-deposition method within some potentials. SEM, EDAX and XRD were used to analyze the alloy films. The Dy content in the Dy-Ni alloy film is up to 56.91%(mass fraction) and the Dy-Ni alloy films are amorphous.