Ti 3 SiC 2 +SiC and TiC+SiC were deposited on graphite substrate at 1300–1600°C by chemical vapor deposition with TiCl 4 , SiCl 4 , C 3 H 8 , H 2 as reactive gases. Process parameters such as temperature, pressure, concentration of C 3 H 8 were varied to study their effects on the phases and microstructure of the deposited layers. The results show that binary phases of Ti 3 SiC 2 +SiC are formed at temperature less than 1400°C. For temperature above 1500°C, TiC+SiC phases are formed. Increase of the process pressure causes the disappearance of Ti 3 SiC 2 and the formation of TiC. The surface morphology of Ti 3 SiC 2 shows a plate-like structure. The hardness of Ti 3 SiC 2 +SiC and TiC+SiC is HV4251 and HV4612 respectively for a load of 10g.