The increasing prevalence of organic pollutants in water sources necessitates the development of efficient and cost-effective photocatalysts for their degradation. ZnO nanoparticles (NPs) have been widely studied for their photocatalytic properties; however, their application is hindered by low photocatalytic efficiency and high recombination rates of photogenerated carriers. This manuscript explores the enhanced photocatalytic performance of intercalated ZnO/SiO₂ nanocomposites (NCs), synthesized through a combination of co-precipitation and Stöber methods, as a solution to these challenges. A comprehensive analysis of the structural, optical elemental and Morphological properties of both ZnO NPs and ZnO/SiO₂ NCs was conducted using various characterization techniques, including X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), UV–Vis spectrometry and Brunauer-Emmett-Teller (BET) analysis. Through, XRD analysis, the calculated crystallite sizes of ZnO NPs and ZnO/SiO₂ NCs were found to be 36 nm and 39 nm respectively. TEM images illustrated that the ZnO NPs and ZnO/SiO₂ NCs have crystallized in elongated spherical morphology. XPS and FTIR analyses provided the signature band details the presence of Cu and Si in their Zn²⁺ and Si⁴⁺ oxidation states. The optical bandgap energies were calculated to be 3.38 eV for ZnO NPs and 3.22 eV for ZnO/SiO₂ NCs. The enhanced photocatalytic efficiency of the ZnO/SiO₂ NCs achieved an impressive degradation rate of 92 % for Rhodamine B (RhB), compared to a relatively lower rate of 81 % for pure ZnO NPs for the degradation of RhB under visible light due to its lower bandgap, high surface area, and lower electron-hole recombination rate. BET surface area measurements revealed that ZnO nanoparticles have a surface area of 11.234 m²/g, while ZnO/SiO₂ NCs show 57.118 m²/g, highlighting SiO₂'s enhancement. The NCs demonstrated exceptional reusability for degradation, sustaining high efficiency across multiple cycles. Its ability to scavenge superoxide radicals highlighted the effectiveness of the ZnO/SiO₂ NCs in environmental remediation, especially for wastewater treatment.