Abstract: The paper has described the preparation of Ni_xMo_100-x. (X=80, 70, 62, 55, and 40)alloy using mechanical alloying process and studied the change of powder structure during the process of ball milling by using X-ray diffraction. The results have shown that in case of X ≥ 70 the nickel solid solution was obtained, while in case of X ≤ 62 a partial amorphous alloy was obtained. The crystallizing behaviour of partial amorphous alloy Ni₆₂Mo₃₈ has been analysed through DSC differential thermal analysis and the possibility of forming complete amorphous alloy from the alloy system has been theoretically discussed.