The focus of this research is on (a) the use of mechanical alloying (MA) to produce nanostructured titanium silicide (Ti5Si3) powder and (b) use of equal channel angular extrusion (ECAE) for powder consolidation to preserve the fine scale structure achieved via mechanical alloying. MA is a high-intensity ball milling process that can be used to produce nanocrystalline and amorphous powders. A 23 factorial design is applied to optimize the process and study the effect of MA parameters (milling time, milling speed, ball-to-powder ratio) on the grain size of powder. ECAE is a process that produces intense and uniform plastic deformation caused by simple shear of the material. A 4 2 factorial design was used to study the effect of ECAE parameters (number of extrusions, billet orientation, temperature) on the properties of the final product. The final product possesses a grain size of less than 20 nanometers.