Abstract: Using titanium, aluminum and TiN powders with the molar ratio of 1∶1∶3 as raw materials, Ti4AlN3 powders were synthesized using general blender and high-energy ball milling with different rotation rates, and then were sintered at 1 100-1300 ℃ in vacuum. The phaes and morphology of products, the phase of mixed raw materials and the effect of sintering temperature on synthesis of Ti4AlN3 particles were studied and the suitable synthesis process for Ti4AlN3 particles was confirmed. The results show that the suitable synthesis process for Ti4AlN3 particles was ball milling at 400 r·min-1 for 3 h followed by sintering at 1 300 ℃ for 2 h.