AB₂type Laves phase alloys are attractive anode materials for Ni/MH secondary batteries because of their large hydrogen storage capacity in KOH electrolyte. However, they have a disadvantage of requiring many charge-discharge cycles for activation. When the mechanical alloying was performed with elemental powders in Zr-Cr system, the mechanically alloyed powders were composed of a microscopic mixture of starting elements. The milled powders could be transformed into the ZrCr₂type Laves phase of C14(hcp) by the heat-treatment for 3 hours at 900℃ The heat-treated powders had nano-sized grains of less than 100 ㎚. The hydrogen solubility and the maximum discharge capacity of the milled electrode were less than those of the arc-melted one. However, the discharge capacity of the heat-treated electrode was increased and the activation behavior was improved owing to the nano-sized microstructure.