Combustion synthesis, or self-propagating high temperature Synthesis (SHS) is a technique for producing ceramics, intermetallic, and composite materials. The advantage in the SHS process lies in its low cost, and, with high temperature deformation as a consideration, in the ability to form powders with very fine second phase particles or whiskers. At present, only a limited number of studies reported synthesis of MoSi2 composite powders reinforced by SiC particles [13], [14] and [15] and MoSi2/WSi2[11] by SHS process. There are two limits. Firstly, it is difficult for SiC whiskers to be evenly distributed in the reactant mixtures and the introduction of SiC whiskers to the MoSi2 matrix is a problem. Secondly, for the case of some systems, such as MoSi2–SiC and MoSi2–WSi2, ignition is impossible without additional activation. Primarily this is due to a thermodynamic limitation, i.e., a low reaction enthalpy and the resulting relatively low adiabatic combustion temperature of these systems.