Abstract: YNi alloy was prepared by molten salt electrolysis of fluoride system in conventional graphite electrolyzer with Y₂O₃ as raw materials, nickel rod as consumable cathode and graphite plate as anode. The effects of electrolysis time, electrolysis temperature, electrolyte composition and cathode current density on the electrolysis process were studied. The results showed that the optimum technological conditions for preparing yttrium nickel alloy by molten salt electrolysis were as follows. The electrolysis temperature was 1 000 ℃, and the mass ratio of YF₃ to LiF was 85:15. The cathode current density was 10.0 A/cm² and the current efficiency was about 72.8% in normal electrolysis. The Y Content of the prepared yttrium nickel alloy was 52.6%, which was composed of YNi₂ phase and Y-Ni phase. The content of impurity was quite low, which could meet the requirement of rare earth hydrogen storage alloy for raw materials. The research results of this paper provide a feasible way for the large-scale production of Y-Ni alloy.