Abstract: In this work, natural ilmenite, which is low-cost and accessible to get, is being intensively utilized for raw material to prepare FeTiO₃ nanometer flower through the method of “the activation of mechanical ball mill+alkali leaching”, and TiO₂/FeTiO₃ nanometer particles are obtained through the process of “the activation of mechanical ball mill + alkali leaching + acid leaching”.First of all, the size of ilmenite is reduced by mechanical activation and its chemical properties become active.Then, FeTiO₃ nanoscale flower with three-dimensional petals are obtained by alkali leaching.The nanometer flowers are further pickled to achieve TiO₂/FeTiO₃ nanometer particles.By analyzing morphology and phase composition of FeTiO₃ nanoscale flower and TiO₂/FeTiO₃ nanometer particles found that FeTiO₃ nanoscale flower with a thickness of around 25 nm and a length between 200 nm and 400 nm is achieved by 1 mol/L NaOH for 2 h immersion.Subsequently, the nanometer flower is further immersed in 2 mol/L HCl for 8 h to obtain regular TiO₂/FeTiO₃ nanometer particles with a diameter of about 30 nm.In addition, the mechanisms of acid leaching and alkali leaching are analyzed, indicating the unstable liquid phase intermediates are formed in the two reactions, which can be explained by the mechanism of dissolution and precipitation generated by the hydrolysis of intermediates.Furthermore, the formation and hydrolysis of intermediates are related to the concentration of acid or alkali.