<p>The unregulated emission of dye-containing wastewater from industries into water bodies has been shown to cause significant environmental pollution, owing to the hazardous and non-degradable behavior of organic dyes. Therefore, photocatalytic degradation is an eco-friendly strategy to treat such pollutants. In this regard, the present research has developed the photocatalytically efficient CeO₂–ZnO nanocomposites through sonication-induced exfoliation method to improve charge transfer across interfaces. CeO₂ and ZnO nanoparticles were first produced by the hydrothermal method and then blended together in different proportions (60:40 and 80:20 wt%). These materials have been characterized for their crystal structure, chemical composition and morphology using techniques like Energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), High resolution transmission electron microscopy (HR-TEM) and Selected area electron diffraction (SAED). Photocatalytic activity was tested using MB dye degradation through UV light irradiation. The highest MB dye degradation rate among all samples studied reached about 92% in the CeO₂:ZnO (60 − 40) wt% nanocomposite sample due to better charge separation and higher number of reactive species generation. In addition, CeO₂-ZnO nanocomposites showed good stability and recyclability in successive cycles of experiments. The scavanger test is also performed for the identification of primary reactive species in the degradation process. Results obtained in this study suggest that CeO₂-ZnO nanocomposites can be promising materials for real-life wastewater remediation applications.</p>