TiO₂/Fe₂O₃ nanocomposites with different morphologies were prepared by precipitation separation method combined with sol?gel method using Fe(NO₃)₃?9H₂O and tetrabutyl titanate as iron and titanium sources, and HF, HAc, NH₄F, NH₃?H₂O, H₂O₂ as morphology control agents, respectively. The structure and morphology of the TiO₂/Fe₂O₃ samples were characterized by X?ray powder diffraction (XRD) and field emission scanning electron microscope (FESEM), and the degradation performance of the TiO₂/Fe₂O₃ nanocomposites for methylene blue under UV?light irradiation condition was investigated. The results show that the NH₃?H₂O?TiO₂/Fe₂O₃ nanocomposites prepared with NH₃?H₂O as the morphology control agent have the best degradation effect on MB, with a degradation rate of 82.9%, which is approximately 1.00, 1.10, 1.14, 1.15, 1.56, 3.57, 12.95 times larger than that of HF?TiO₂/Fe₂O₃ (82.5%), H₂O₂?TiO₂/Fe₂O₃ (75.7%), NH₄F?TiO₂/Fe₂O₃ (72.9%), HAc?TiO₂/Fe₂O₃ (71.8%), TiO₂ (53.1%), Fe₂O₃ (23.1%) and blank (6.4%) samples, respectively. This is attributed to the synergistic effect of its large specific surface area, spindle morphology, highest crystallinity and suitable heterojunction structure.