The aim of this study has been in-situe production of iron aluminide and tungsten carbide nanocomposite with mechano chemical-thermal synthesis. In this regard, the possibility of combustion synthesis of activated samples has been investigated. Three mixtures of raw materials were used to produce nanocomposites Fe 3 Al-WC. The first mixture is based on Fe, Al, C and W powder, the second one is based on Ferro tungsten, Al and C and the third one is the direct use of WC. 20 hours of milling the powder mixture of Al, Fe, C and W result i Fe3Al production, but even by 40 hours milling, WC was not formed and just lead to increase in lattice strain and decrease in grain size. Milling the mixture of ferro tungsten, aluminum, and carbon up to 40 hours only increase the lattice strain and decrease the grain size and no reaction takes place. 20 hours of milling the mixture of Fe, Al and WC produces Fe 3 Al. In addition, XRD tyupical peaks of Fe 3 Al and WC indicate that there is no by-product. Samples heated at temperatures of 700 and 1000°C for 5 minutes, combustion reaction was carried out and complex carbides of Fe-Al-WC were generated. These carbides constitute of tiny crystals that have been sintered in the form of clusters. Heat treatment of combustion synthesis samples at 1000°C for one hour, results in WC production and disintegration of the complex carbides. Microhardness as high as 612.4 HV was obtained for the produced composites. Keywords Nanocomposite, Iron Aluminide, Tungsten Carbide, Mechano chemical-Termal Synthesis