The cyclic voltammetry and chronoamperometry were used to investigate the electrochemical behaviors of Er(Ⅲ) and Ni(Ⅱ) in LiClO4-DMSO(dimethylsufoxide) system on Pt and Cu electrodes. Experimental results indicated that the reduction of Er(Ⅲ) to Er and Ni(Ⅱ) to Ni were irreversible in one step on Pt and Cu electrodes. The diffusion coefficient and electron transfer coefficient of Er(Ⅲ) in 0.01 mol*L-1 ErCl3 -0.1 mol*L-1 LiClO4-DMSO system at 303K were 1.47×10-10 m2*s-1 and 0.108 respectively, and the diffusion coefficient and electron transfer coefficient of Ni(Ⅱ) in 0.01 mol*L-1 NiCl2-0.1 mol*L-1 LiClO4-DMSO system at 303K were 3.38×10-10 m2*s-1 and 0.160 respectively. The homogeneous, strong adhesive Er-Ni alloy films with metallic lu- stre was prepared by potentiostatic electrolysis on Cu electrode in ErCl3-NiCl2-LiClO4-DMSO system at -1.90～-2.55 V (vs SCE).
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