Mg-Ti-H alloys were synthesized by high energy ball milling from equi molar mixtures of MgH2 + TiH2, MgH2 + Ti and Mg + T1H2 in the presence of 10 wt.% Pd. X-ray diffraction analyses combined with Rietveld refinement revealed that after 60 h of milling, all as-milled Mg-Ti-H alloys are made of two face-centered-cubic (fcc) phases, with lattice parameters similar to 4.47 and similar to 4.25 angstrom, in different proportions depending on the composition of the initial mixture. The Mg-Ti-H alloys displayed a similar electrochemical behavior, i.e. their hydrogen discharge capacity was highest during the first cycle and then decreased rapidly with cycling. The maximum discharge capacities of the 60 h-milled MgH2 + TiH2, MgH2 + Ti and Mg + TiH2 materials were 300,443 and 454 mAh g(-1), respectively. No apparent correlation could be established between the maximum discharge capacity of the Mg-Ti-H materials and the two fcc phase proportion. (C) 2010 Elsevier B.V. All rights reserved.