Mo-Ti3SiC2 layered material was prepared by spark plasma sintering. Mixed Ti, Si, graphite and Al powder with molar ratio of 3Ti:1Si:2C:0.2Al was put into a graphite mould and pressed with a pressure of about 0.5 MPa, then, Mo powder was put on top of the mixed powder. Experimental results showed that Mo-Ti3SiC2 layered material could be fabricated successfully by sintering the above powder mixture at 1300°C for 20 minutes under a pressure of 50 MPa in vacuum. The surface and interfaces of the layered composite were tight and clear without any observable crack. In order to study the thermal stability at elevated temperature, the fabricated Mo-Ti3SiC2 layered composite was heat treated at 800°C for 5, 10, 20 and 40 hours. After 40 hours of annealing, the intermediate layers formed between the Mo and Ti3SiC2 matrix grew thicker. The interfaces are clean and tight with no obvious formation of voids and new phases. The initial 10 hours of annealing is the fast growing period, after that, the growth rate slowed down significantly.