en Research Paper Research Paper In this research, two different carbonaceous materials (Graphite:G and Petrocoke:P) were separately compared in terms of the carbothermic reduction of hematite and anatase in order to synthesize Fe-TiC nanocrystalline composite by mechanically activated sintering method. Powders were activated in a planetary high-energy ball mill under argon atmosphere for 0, 2, 5, 10,and 20 h. Then, the activated powders were analyzed by XRD and SEM to investigate phase constituents and microstructure of the mixtures. Results proved that Fe 2 O 3 and TiO 2 were not reduced by carbonaceous materials even after 20h of milling. SEM investigations showed that G-mixture was more homogenous than P-mixture after 20h of milling, meaning that graphite-anatase-hematite was mixed satisfactorily. Thermogravimetry analysis was done on 0 and 20h milled powders. TG and DTG curves showed that mechanical activation led to almost 300°C decrease in the reduction temperature of hematite and anatase in both mixtures. In the next step, the powders were sintered in a tube furnace under argon atmosphere. In the G-mixture, anatase was reduced to titanium carbide at 1100°C but, in the P-mixture, temperature of 1200°C was essential for completely reducing anatase to titanium carbide.Results of phase identification of the sintered powders showed that anano-crystalline ironbased composite with titanium carbide, as the reinforcement was successfully synthesized after 20 h high-energy milling of the initial powders and subsequent sintering occurred at 1200˚C for 1h Mechanical Activation, Heat Treatment, Fe-TiC, Nano-crystalline Composite, Petrocoke, Graphite. 56 70 http://ijmse.iust.ac.ir/browse.php?a_code=A-10-127-86&slc_lang=en&sid=1 S. Niksirat 180031947532846003183 180031947532846003183 No School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, Tehran, Iran. SH. Raygan shraygan@ut.ac.ir 180031947532846003184 180031947532846003184 Yes School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, Tehran, Iran. S. Moradi Ghiassabadi 180031947532846003185 180031947532846003185 No School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, Tehran, Iran.