The carbothermic reduction and nitridation process of titanomagnetite concentrates with the help of mechanical activation were investigated by particle size analysis, thermodynamic calculation, thermogravimetric analysis, X-ray diffraction analysis, scanning electron microscopy, and energydispersive spectroscopy analysis. The thermogravimetric and X-ray diffraction results indicated that either the reduction of iron oxide or the reduction and nitridation of M3O5 to TiN could be promoted significantly with the increase in activation time. The results obtained from scanning electron microscopy and energy-dispersive spectroscopy showed that, when samples were not activated, chunks of and thin M3O5 were derived from the reduction of ilmenite and titanomagnetite. They were severely sintered with impurities to form a dense structure. As a result, M3O5 was difficult to be converted to TiN, especially chunks of M3O5. However, when samples were activated, the sintering degrees of the impurity and M3O5 were mitigated, and the particle size of the iron as a medium for delivering C to M3O5 was decreased in the roasted product. This condition enhanced the diffusion of C to the surface of M3O5. Meanwhile, the bulk of ilmenite was broken in the activation process, which prevented the formation of chunks of M3O5. Thus, the conversion of M3O5 to TiN was promoted.