The purpose of this study was to produce Fe3Al/TiC-SiC nanocomposite by mechanical alloying of the FeSiTiO3, Al and C powder mixture. The phases made of the samples were characterized by XRD. The morphological evolution was analyzed during mechanical alloying by FESEM. The particle size of the 30 h milled powder was determined by TEM. The results showed that ball milling led to the formation of SiC after 10 h. Increasing of milling time to 20 h caused TiCx and Fe3Al were formed with remained TiO2 phase. After 30 h milling, all peaks of TiO2 phase eliminated and Fe3Al/TiC-SiC nanocomposite was formed. The XRD investigation of the powders after annealing showed that no new phases were formed. TEM image confirmed that average particle size of syntehsized powder after 30 h milling was 60 nm.