The electrodeposition of Lu+/Ni alloy thin films from Lu(Ⅲ) and Ni(Ⅱ) solutions was studied in a nonaqueous dimethysulfoxide (DMSO). Different substrates have been used (platinum and copper), and the effect of them on the electrochemical behavior of the studied ions is shown. The obtained Lu+/Ni alloy thin films were subjected to scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffraction analysis (XRD). The lutetium content in Lu-/Ni alloy thin films increases as the potential was made more cathodic, reaching a maximum value of 28.77 at.%, and then decreases. The films were amorphous. After heat treatment of crystallization at 520℃ for 1 h, the alloy phase of Lu+/Ni can be found in XRD patterns.