This paper presents some resulted investigation about amorphization phenomena of mixture powders Ni-Ti (atomic ratio 50 percent Ni : 50 percent Ti) by mechanical alloying while preparing powders for SHS reaction. The XRD results showed that the amorphization phenomena started from 15h and completed at upper 25h, and did not appear the peaks of Ni, Ti and NixTi1-x. The SEM results showed that, particles size of mixture powders Ni + Ti decreased clearly from 10-100um to under 2um. The DSC result showed that the temperature required complete recrystallization process about 1000°C in range time upper 4h. The product of heat treatment process of amorphous Ni-Ti were mainly NiTi phase, and Ni3Ti and NiTi2.