We showed that the exposure of a pressed mixture of MgH 2 and Ni powders to a hydrogen atmosphere at 450 °C leads to the direct formation of Mg 2 NiH 4 . No pre-milling was used. The reaction was carried out at a hydrogen pressure exceeding the equilibrium over MgH 2 and Mg 2 NiH 4 . The pressure invariability during the synthesis evidences the absence of a separate stage of magnesium hydride decomposition and stabilization of the synthesized hydride. The amount of Mg 2 NiH 4 was determined by the XRD and TDS methods. SEM with EDX microanalysis was used to examine the morphology of the reaction products. The influence of the exposure time and the synthesis temperature on the reaction yield was studied.