This paper aims to synthesize and describe BiFeO3/TiO2 nanocomposite with enhanced visible-light activity. At first, BiFeO3 nanoparticles were successfully synthesized by the thermal treatment method, and then titania nanoparticles were prepared by hydrolysis precipitation process. Composite nanoparticles were synthesized at different ratios of ferrite to titania. To characterize the nanocomposites’ structure, scanning electron microscopy, transmission electron microscopy, X-ray diffrac- tion, and Brunauer–Emmett–Teller analysis were applied. The UV–visible diffuse reflectance spectra showed that redshift in the absorption spectra of the nanocomposites was significantly related to the ratio of ferrite to titania. Moreover, the photo- catalytic activity of the nanocomposites was researched under visible light, discussing Congo red dye degradation. The best result was obtained by the BiFeO3/TiO2 (1:1), which the photocatalytic degradation efficiency reached 60% after 30 min of irradiation. PL spectroscopy was applied as a practical technique to examine the separation efficiency of the photogenerated carrier pairs. The accordance between PL and photocatalytic results showed vital role of the constructed heterojunction in the nanocomposites to prevent the charge carrier recombination. Also, the synthesized BiFeO3/TiO2 (1:1) nanocomposite showed a suitable reusability in the model pollutant treatment.