In this paper, a facile solvothermal method assisted orthogonal experimental was applied to synthesis mesoporous Fe2O3/TiO2 heterostructured microsphere with the purpose of optimizing the preparation conditions. The as-prepared samples were characterized by TG, XRD, SEM, TEM, FT-IR, UV-vis DRS and N-2 adsorption/desorption. On the basis of the above analysis, it was found that the mesoporous Fe2O3/TiO2 heterostructured microsphere has high crystallinity, ordered morphology, strong optical absorption, large surface area and enhanced catalytic activity. Furthermore, it also confirmed that orthogonal experimental design method was very efficient to optimize the preparation conditions for the synthesis of mesoporous Fe2O3/TiO2. heterostructured microspheres. The experimental results show that the reaction temperature and molar ratio of Fe to Ti have the most influence on the photocatalytic performance. The optimized preparation conditions for the synthesis of Fe2O3/TiO2 microspheres are reaction temperature at 140 degrees C, the amount of glucose of 3.4 g and the Fe:Ti molar ratio of 0.005:0.01. What's more, a tentative formation mechanism of mesoporous Fe2O3/TiO2 microspheres and charge transfer mechanism are proposed. (C) 2014 Elsevier B.V. All rights reserved.