A Mg-23.5wt%Ni-5wt%Cu alloy was synthesized by the gravity casting method in a large quantity (7.5 kg). From this alloy, Mg-23.5wt%Ni-xwt%Cu (x = 2.5, 5 and 7.5) samples for hydrogen storage were prepared by melt spinning and crystallization heat treatment. The samples were ground under H 2 in order to obtain a fine powder. These alloys contained crystalline Mg and Mg 2 Ni phases. The Mg-23.5Ni-2.5Cu alloy had the highest hydriding and dehydriding rates after activation among these alloys. The dehydriding curve under 1.0 bar H 2 at 573 K exhibits two stages; the dehydriding rate is high for about 2.5 min (the decomposition of Mg 2 Ni hydride and Mg hydride in small particles), and then it becomes lower (the decomposition of Mg hydride).