Utilizing a two-step method of mechanical and field activation, the heretofore-unachieved goal of incorporating Mg on the Si sub-lattice Of MoSi2 was successfully demonstrated. Mechanical activation was done through high-energy ball milling and field activation was achieved through the use of the spark plasma sintering (SPS) method. The incorporation of Mg was verified by a variety of techniques including XRD, SEM, and EDS. (C) 2004 Kluwer Academic Publishers.