Ni-Ti system is an interesting binary system having different intermetallic compounds. NiTi is the one of them having commercial importance because of its shape memory and superelastic characteristics. In this study, effect of mechanical alloying was studied against milling time to observe powder state changes and phase formations. 35Ni-65Ti, 45Ni-55Ti and 50Ni-50Ti compositions in Ni-Ti binary system were selected, It was possible to obtain different intermetallic compounds in Ni-Ti binary system by mechanical alloying of initial Ni-Ti powders. It is also observed that, particle size and distribution measurements, XRD phase analysis, density measurements and morphological evaluation of the mechanical alloyed powders can be used for the determination of optimum conditions for obtaining desired level of alloying and final product.