This study investigates the photocatalytic degradation of organic Methyl Blue (MB) using a ZnO-Fe2O3 composite prepared via the sol-gel technique. FTIR analysis elucidates the substantial impact of Fe2O3 addition, as evidenced by shifts in the ZnO absorption bands, notably observed at 631 cm-1 and 919.74 cm-1 peaks. X-ray diffraction (XRD) corroborates heightened crystallinity due to interactions between ZnO and Fe2O3. SEM analysis unveils a highly aggregated structure, showcasing promising capabilities for efficient dye degradation and environmental applications. Photoluminescence (PL) spectra exhibit an intensified peak at 377 nm, indicative of efficient charge separation and electron transfer, offering potential in optoelectronic applications. The composite's distinctive refractive index (n) of 2.33, extinction coefficient (k) of 2.12, optical electronegativity (∆X*) of 0.75, and dielectric constants (εr of 0.40 and εi of 9.92) underscore its versatile bonding and broad application prospects. Evaluating the photocatalytic activity (PCA) reveals that among all samples, the nanocomposite ZnO-Fe2O3 synthesized at 500°C exhibits superior performance, showcasing heightened degradation of MB dye under 90 minutes of sunlight irradiation.