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NiTi alloy is produced by mechanical alloying(MA). It becomes amorphous after milling for enough time, such as 100 h in this paper. DSC measurement shows that the crystallization temperature is 676 K for the amorphous powder. Activation energy of crystallization is 199.98 kJ/mol for MA powder, which is lower than that of amorphous prepared by magnetron sputtering.Avrami parameter of crystallization is 1.07.