In this work, bismuth sulfide (Bi₂S₃) thin films were deposited by a chemical bath deposition (CBD) technique (called soft chemistry), while titanium dioxide (TiO₂) nanoparticles were synthesized by sol–gel and zinc oxide (ZnO) nanoparticles were extracted from alkaline batteries. The resulting nanoparticles were then deposited on the Bi₂S₃ thin films by spin coating at 1000 rpm for 60 s each layer to create heterojunctions of Bi₂S₃/ZnO and Bi₂S₃/TiO₂. These materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDX). The optical and contact angle analyses were undertaken by UV–Vis spectroscopy and a contact microscopy angle meter, respectively. The calculated band gap values were found to be between 1.9 eV and 2.45 eV. The Bi₂S₃ presented an orthorhombic structure, the TiO₂ nanoparticles presented an anatase structure, and the ZnO nanoparticles presented a wurtzite hexagonal crystal structure. Furthermore, heterogeneous solar photocatalysis was performed using the Bi₂S₃, Bi₂S₃/ZnO, and Bi₂S₃/TiO₂ thin film combinations, which resulted in the degradation of Congo red increasing from 8.89% to 30.80% after a 30 min exposure to sunlight.