Titanium nitride (TiN) is prepared from ilmenite (FeTiO3) powders by microwave-assisted carbothermic reduction–nitridation in air atmosphere followed by acid leaching treatment. The thermal analysis of the reduction–nitridation of FeTiO3 powders is conducted by thermogravimetry/differential scanning calorimeter. The phase transition sequence of microwave carbothermal synthesis of TiN–Fe composite is: FeTiO3 → Fe + TiO2 → Fe + TiN. There is no any other oxygen-deficient titanium oxides detected. Particularly, FeTiO3 can be transformed into TiN–Fe composite completely at 900°C for 60 min by microwave heating. The increase in both the reaction temperature and dwelling time is in favour of the transformation of FeTiO3. The product morphologies are spherical about 2–5 μm in size. Then TiN is obtained with the removal of Fe and their oxides from TiN–Fe composite by acid leaching treatment. This method not only reduces the reaction temperature significantly through microwave heating but also can simplify the operation process effectively.
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