Ti3SiC2 + SiC and TiC + SiC were deposited on graphite substrate at 1300–1600 8C by chemical vapor deposition with TiCl4, SiCl4, C3H8, H2 as reactive gases. Process parameters such as temperature, pressure, concentration of C3H8 were varied to study their effects on the phases and microstructure of the deposited layers. The results show that binary phases of Ti3SiC2 + SiC are formed at temperature less than 1400 8C. For temperature above 1500 8C, TiC + SiC phases are formed. Increase of the process pressure causes the disappearance of Ti3SiC2 and the formation of TiC. The surface morphology of Ti3SiC2 shows a plate-like structure. The hardness of Ti3SiC2 + SiC and TiC + SiC is HV4251 and HV4612 respectively for a load of 10 g.