<p>Industrial development has led to water and environmental pollution, and semiconductor photocatalysis is being explored as a solution. However, current photocatalysts can be expensive, complex, and hazardous to synthesize. This research is driven by the development of a simple and economical approach of sol-gel for the synthesis of zirconium dioxide (ZrO₂)/ titanium dioxide (TiO₂) composites, aimed at enhancing their photocatalytic performance. The synthesized samples were characterized thoroughly. Electron microscope images displayed a porous worm-like morphology for the synthesized composites. The structural analysis confirmed that the composite samples contained ZrO₂/TiO₂ with TiO₂ had grown solely in the anatase phase. The mechanisms of electron-hole recombination and separation of charge carriers were discussed using photoluminescence (PL). The catalytic properties of the prepared samples were studied by methylene blue (MB) under ultraviolet light at a wavelength of 360 nm. By adding 25 mg of TiO₂ in 50 mg ZrO₂ (sample ZT3), the degradation rate of MB dye reached 63% in 80 min. This result demonstrated a notable improvement in the degradation rate, featuring a 50% improvement over the performance of intrinsic TiO₂. The obtained results have significant implications for the development of efficient and sustainable photocatalysts for environmental protection.</p>