Mg76T12Fe12-xNix (x = 0, 4, 8, 12) alloys were prepared by mechanical alloying and the hydrogen storage properties were investigated C systematically. In Mg76Ti12Fe12 and Mg76Ti12Ni12Ti12 alloys, the main binary alloy phase is Fe2Ti and Mg2Ni, respectively. There are same binary alloy phase structures included Fe2Ti, Mg2Ni and NiTi in Mg(76)Ti(12)Fc(8)Ni(4) and Mg76Ti12Fe4Ni8 alloys. For Mg76Ti12Fe12-xNix (x = 0, 4, 8, 12) alloys, the hydrogen storage capacity is 2.88, 3.31, 3.12 and 2.24 wt%, respectively. The hysteresis between hydrogen absorption and desorption decreases gradually with increasing the amount of substitution Ni for Fe. Mg76Ti12Fe8Ni4 shows the highest hydrogen absorption and desorption rate among Mg76Ti12Fe12-xNix (x = 0, 4, 8, 12) alloys. Fe and Ni coexistence is favorable to improve hydrogen storage properties. For Mg76Ti12Fe8Ni4 alloy, the amorphous degree increase with the milling time, and the amorphous degree increase is unfavorable to improve hydrogen storage capacity. (C) 2006 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.