Mg2Ni is a well-known hydrogen storage alloy. Most of the preparative methods for this alloy require high temperature processing of pure magnesium and nickel. The proposed method, studied in this work, involves the production of Mg2Ni alloy directly from NiO and MgCl2 in an electrochemical cell. This method can eliminate the difficulties that may arise, during handling due to the reactive nature of metallic components, especially Mg. XRD patterns of reduced samples indicated the partial formation of Mg2Ni. Experimental results also showed that sintering of NiO, which resulted in the decrease of porosities, adversely affects the formation of Mg-Ni intermetallic compounds. Such an observation was thought to be the result of higher molar volume of Mg2Ni as compared to that of NiO.