Abstract: As a layered ternary machinable cermet, Ti₃SiC₂ has been widely used as the strengthening phase of metal composite materials due to its many excellent performance. Using Ti/Si/C/Al as the composition of raw materials, Ti₃SiC₂ material was prepared by prediffusion treatment and vacuum pressureless sintering process. XRD and SEM were applied to determine the phases and microstructure of the synthesized products. The effects of prediffusion treatment on raw material powder and the effects of sintering temperature on preparation of Ti₃SiC₂ were explored. The results show that the chemical component is refined and its activity also increases by prediffusion, which encourages the formation and reduces the formation temperature of Ti₃SiC₂ phase in the sintering stage. By analyzing the morphology of Ti₃SiC₂ powder, the layered structure, in which, the thickness of the single layer is only about 50 nm, can be found.