A 76.5wt%Mg - 23.5wt%Ni (Mg-23.5Ni) sample was prepared by reactive mechanical grinding (RMG) and its hydriding and dehydriding properties were then investigated. Activation of the Mg-23.5Ni sample was completed only after two hydriding (under 12 bar H2) - dehydriding (under 1.0 bar H2) cycles at 593K. The reactive mechanical grinding of Mg with Ni is considered to facilitate nucleation and shorten diffusion distances of hydrogen atoms. After hydriding - dehydriding cycling, the Mg-23.5Ni sample contained Mg2Ni phase.