Spark plasma sintering (SPS) is a newly developed material preparation technology and is very suitable for the multi-component and/or dissimilar materials preparation. In this paper, Mg-V(77.8)Zr(7.4)Ti(7.4)Ni(7.4), Mg-V(38)Zr(25)Ti(15)Ni(22) and mg-ZrMn(2) composites were synthesized by SPS method and their hydrogen storage properties were evaluated. The results showed that with the addition of the second alloys, the hydrogen desorption temperature of pure Mg decreased apparently, with the reversible hydrogen storage capacity increased from nearly 0 of pure Mg to near 95% of its total absorption at 573 K. The hydrogen ab/desorption kinetics were also greatly improved, with the hydrogen absorption mechanism changed from surface reaction of pure Mg to three-dimension diffusion of the composite. TEM observation indicated that a thin transition zone of nanocrystalline Mg was produced at the sintering interface during SPS, which may be responsible for the improvement of hydrogen storage properties of these Mg-based composites. (c) 2010 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.