In this work, a simple co-precipitation method for the preparation of Ag 2 SO 4 @BiOCl@Bi 25 FeO 40 (BFO) was developed. Ultraviolet-visible spectrophotometric analysis, X-ray diffraction patterns, Fourier transform infrared spectroscopy (FT-IR), and scanning field emission electron microscopy (FESEM) were performed to characterize the newly synthesized nanocomposite. In addition, the EDX method was used to determine the actual material quantities. The synthesized samples of Bi 25 FeO 40 and Ag 2 SO 4 Bi 25 FeO 40 showed high absorption in the visible region. Furthermore, the photocatalytic activity was significantly improved by the addition of Ag 2 SO 4 . The results showed photcatalytic efficiency was reached to about 99% with 0.01 g of Ag 2 SO 4 @BiOCl@Bi 25 FeO 40 in pH 4 under visible light. The isoelectric pH of the photocatalayst was obtained 5. Also, kinetic study showed a first order mechanism for photodegradation. Moreover, a mechanistic study was proposed for the newly synthesized heterostructures.