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In this paper,TiAl alloy powders were prepared successfully by high-energy ball milling and diffusion reaction in vacuum at low temperature.The titanium powder,aluminum powder,and titanium hydride powder were used as raw materials.The samples were characterized by scanning electron microscopy (SEM),X-ray diffraction (XRD),field-emission scanning electron microscopy (FESEM),and differential thermal analysis (DTA).The results show that the alloy powders with the main intermetallic compounds of TiAl are obtained using Ti-Al powders and TiH2-Al powders after heated for 2 h at 500 ℃,3 h at 600 ℃,and 3 h at 750 ℃,respectively.The average grain sizes of alloy powder are about 45 and 20 μm with irregular shape,respectively.The prepared TiAl alloy powders are relatively pure,and the average quality content of oxygen in the alloy powders is 0.33 wt％.The forming process of alloy powder contains both the diffusion reaction of Ti and Al,which gives priority to the diffusion reaction of aluminum.