The thermoplastic Poly(ether ether ketone) , (PEEK), was used as a matrix in a high performance engineering composite. Ceramic reinforcing particles, consisting of either alumina or fly ash, were prepared using mechanical alloying (MA). MA offered an effective way to homogeneously mix the reinforcement and matrix material in different volume percentages. The resulting composite was then compression molded, mechanically tested, and analyzed using an Environmental Scanning Electron Microscope (ESEM). Results show that the PEEK matrix was significantly stiffened as well as strengthened by both the fly ash and the alumina. Electron micrographs show a large amount of porosity in samples with higher volume percent reinforcement.