In this research, for the first time, Fe-TiC nano-crystalline composite was produced via simultaneous reduction of iron and titanium oxides by petrocoke. Powder mixture of Fe2O3/TiO2/petrocoke was mechanically activated in a high-energy ball mill at different times. X-ray diffraction method (XRD) and Scanning Electron Microscopy (SEM) were used to characterize the milled powders. The results showed that new phases were not formed during milling, even after 20 h of milling. However, crystallite size and lattice strain of hematite were remarkably decreased and increased, respectively. Thermogravimetry and Differential Thermal Analysis (TG-DTA) were done on 0, 10 and 20 h mechanically activated powders. These experiments showed a substantial decrease in reduction temperature of iron and titanium oxides as a result of mechanical activation. Then, the powders were cold compacted and sintered at 1200 degrees C in argon atmosphere for 1 h. XRD results of 20 h milled samples demonstrated that, in this condition, iron oxide was completely reduced to nano-crystalline iron and titanium dioxide was reduced to nano-crystalline titanium carbide and Fe-TiC nano-crystalline composite was successfully formed. (C) 2014 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.