The Ni-Mo system processed through mechanical alloying (MA) technique has been widely investigated. For the composition Mo-47 at % Ni partially amorphous phase was obtained after 36 h milling time. Fe contamination was detected in the samples milled in a stainless steel container. Longer milling times have an important effect in the crystallization temperature. The peak temperature was shifted to lower temperatures as increases the milling time. Milling device, milling container, Fe and oxygen have an important effect in the rate of amorphization and in the activation energy (Q) for crystallization. Q values for samples milled under air atmosphere are lower than those observed in samples milled in argon atmosphere.