In the present work is shown the results for solid interaction of a Cu-13.4Al-2Ni (wt%) elemental powders. Together with this mixture was placed tungsten carbide balls into a cylindrical vial under argon atmosphere. The weight ratio of the balls to powder was 20 to 1. A planetary ball mill (Fritsch Pulverizette 5) was used to perform MA at 250 rpm. The elemental powder was milled at 10min, 5 and 10 hours and a small amount of the powders were collected and analyzed via X-ray diffraction, using Cu Kα radiation (λ=0.15418 nm) and differential thermal analyses from 25 up to 450oC at a heating rate of 25oC min-1. The x-ray diffraction patterns showed that after 10h of milling the phase formation of the mechanical alloyed powders is composed of a Cu, full Cu(Al) solid solution and γAl9Cu4.