The electrochemical properties of nanocrystalline Zr0.35Ti0.65V0.85Cr0.26Ni1.30 alloy, which has the hexagonal C14 type structure, have been investigated. This material has been prepared using mechanical alloying (MA) followed by annealing. The amorphous phase forms directly from the starting mixture of the elements, without other phase formation. Heating the MA samples at 1070K for 0.5h resulted in the creation of ordered alloy. This alloy was used as negative electrode for Ni-MH x battery. The electrochemical results show very little difference between the nanocrystalline and polycrystalline powders, as compared with the substantial difference between these and the amorphous powder. In the annealed nanocrystalline Zr0.35Ti0.65V0.85Cr0.26Ni1.30 powders discharging capacities up to 150mAhg−1 (at 160mAg−1 discharging current) have been measured. The properties of nanocrystalline electrode were attributed to the structural characteristics of the compound caused by mechanical alloying.