MoSi2 is one of the few intermetallics to have potential for further systems. However, the use of MoSi2 has been hindered due to the brittle nature of the material at low temperatures, inadequate creep resistance at high temperatures, accelerated (pest) oxidation at temperatures between 450~ 550°C. In this investigation Mo(Al,Si2)/Ti3SiC2 composites has been prepared by reaction hot-pressing from Mo, Si, SiC, Ti, Al powder mixture under different temperatures. XRD results show that the main products are Mo(Si,Al)2 and Ti3SiC2. Part of TiC and SiC also appeared at low treating temperature. With the treating temperature increasing SiC disappeared. No evidence show lattice change of Mo(Si,Al)2. It must be the results of sufficient Al added. The electrical conductivity properties were also investigated. Samples treating under different temperatures showed different changes. Samples under high treating temperature showed a near linear change ranging from 27~800°C and Samples under low treating temperature showed a nonlinear change.