The Ni 5 Zr alloy prepared from the mixture of nickel oxide (NiO) and zirconium oxide (ZrO 2 ) powders by direct electrochemical reduction was conducted in molten lithium chloride (LiCl) at 923 K. The electrochemical reduction behaviors of ZrO 2 and NiO-ZrO 2 mixture were firstly investigated by cyclic voltammetry measurements. The influence of process parameters such as oxide composition, compression force, sintering time, and cell voltage on the electrolysis process have been comprehensively evaluated in terms of the electrochemical reducibility of ZrO 2 . The results demonstrated that the reduction starts with the reduction of NiO to Ni metal, and is followed by the reduction of ZrO 2 on the pre-formed Ni particles to generate the intermetallic Ni 5 Zr. The pure Ni 5 Zr alloy can be prepared by direct electrochemical reduction of mixed 5NiO-ZrO 2 pellets when the cell voltage of 3.2 V is applied. The reduction rate increases with higher content of NiO in a NiO-ZrO 2 mixture pellet. However, the quality of formed Ni 5 Zr intermetallic compound particle seems unaffected under different preparation conditions.