Spark plasma sintering (SPS) is a newly developed technique for multiple-phase material preparation. In this article, a Laves phase related BCC solid solution V-Ti-Cr alloy was prepared by SPS method, and its microstructure and hydrogen storage properties were investigated and compared with those of the alloy prepared by arc melting method. The results indicated that the alloy prepared by SPS method possessed not only excellent activation and kinetics properties, but also a much larger hydrogen storage capacity. The maximum hydrogen storage capacity was determined to be 2.89 mass%, which is about 24% higher than that of the arc melting alloy, and the hydrogen desorption ratio was improved from 35% for the arc melting alloy to 60% for the SPS alloy. This was due to the absence of Laves formation elements in the BCC solid solution and the formation of the interface phase between the Laves phase and the BCC solid solution during the SPS process, which fully optimized the hydrogen storage property of the Laves phase related BCC solid solution alloy. (c) 2009 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved