The TiO2/NiFe2O4 (TN) composite nanoparticles with different mass ratios of NiFe2O4 to TiO2 were prepared via sol-gel method. X-ray diffraction was used to characterize the phase structure of TN. The results indicated that adulterating a smidgen of NiFe2O4 into the TiO2 (about 0.1%) can promote the phase transformation of TiO2, however, when the doping amount of NiFe2O4 surpasses 1%, the introduction of NiFe2O4 can inhibit the growth of TiO2 crystal grain and reduce the size of TiO2 crystal grain. The degradation experiment of methyl orange solution under UV illumination (253.7 nm) showed that the content of NiFe2O4 in the TN was higher, the photocatalytic activity of TN was worse, and the 0.1% TiO2/NiFe2O4 calcined at 400 °C presented the best photocatalytic activity.
