Effect of mechanical activation on carbothermic reduction kinetics and mechanism of ilmenite concentrate containing self-reducing mixture has been investigated using a combination of thermogravimetry and X-ray diffraction. Thermogravimetric comparative study of mechanically activated and non-activated ilmenite concentrate containing self-reducing mixtures with C/O molar ratio of 1.5 was conducted non-isothermally. The samples were heated up to 1573 K at three different heating rates (10, 15, and 20 K min⁻¹) under controlled atmosphere. The reduction mechanism of mechanically activated mixture was followed by X-ray diffraction analysis of arrested samples at different reduction extents. In addition, reaction kinetics was further investigated and corresponding kinetic parameters were estimated using isoconversional (model-free) and model-fitting (Coats–Redfern) methods.