Abstract: In this paper a new route to the preparation of LaNi₅by chemical synthetic method is presented.Lanthanum Nickel oxalate was first prepared by coprecipitation reactions from aqueous solutions,and the oxalate formed after dehydration was reduced by CaH₂at 950℃ to give LaNi₅.The reaction was studied in detail and the lattice parameters ofLaNi₅were found a₀=5.003Å and c₀=3.987Å.The LaNi₅thus prepared shows excellent absorption ability for hydrogen and the hydride formed has the composition corresponding to LaNi₅H_6.1The method seems to have general utility for chemical preparation of some transition metal alloys and intermetallic compounds.