FeAl-TiB2 composites have been combustion synthesized from mixtures of Fe, Al, Ti and B powders. When the powder mixture was heated in vacuum to approximately 900 K, an abrupt increase in temperature was observed, indicating that the combustion synthesis reactions occurred in the powder mixture. X-ray diffraction analyses revealed that the combustion-synthesized sample consisted of only FeAl and TiB2. Metallographic investigations using a scanning electron microscope revealed that fine TiB2 particles were dispersed in FeAl matrix phase. As the volume fraction of the TiB2 particles increased from 0.3 to 0.8 by controlling the powder mixture composition, the average TiB2 particle size increased to 1 to 7 μm and the average Vickers hardness of the composites increased from 800 to 1600. This method has been applied to the fabrication of some other ceramic particle dispersed metal matrix composites such as Fe-TiC and FeAl-TiC systems.