Research by this working group's takes as a principal aim the study and manufacture of bulk metal glass based copper (Cu-Ni-Zr) by mechanical alloying. First, the characterization of the milled pure copper, Cu-Ni and Cu-Zr binary alloys and Cu-Ni-Zr ternary alloys in the same conditions of high energy millings. In this work, the microstructural change of Nickel to be subjected to high energy milling is presented. For this purpose a SPEX 8000D mill with the following conditions of milling: argon, stearic acid, BPR = 10:1, with milling time from 1 to 60 hours, 1 h of effective milling followed by a rest period of 0,5 h. Subsequent to the milling samples were analyzed by ray-X diffraction, transmission electron microscopy and atomic absorption spectroscopy, obtaining the crystallite size, lattice parameters and Fe contamination. The results show that nickel when subjected to mechanical milling reaches a crystallite size of about 10 nm which is asymptotic from 5 h; the lattice parameter increases with increasing milling time, possibly due to increased interfacial component together with the incorporation of Fe, due to the high percentage contamination at 60 h.