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A robust synthesis approach to develop CuO/ZnO nanocomposites using microwave-epoxide-assisted hydrothermal synthesis and their proficiency toward H2S gas-sensing application are reported. The low-cost metal salts (Cu and Zn) as precursors in aqueous media and epoxide (propylene oxide) as a proton scavenger/gelation agent are used for the formation of mixed metal hydroxides. The obtained sol was treated using the microwave hydrothermal process to yield the high-surface area (34.71 m2/g) CuO/ZnO nanocomposite. The developed nanocomposites (1.25-10 mol % Cu doping) showcase hexagonal ZnO and monoclinic CuO structures, with an average crystallite size in the range of 18-29 nm wrt Cu doping in the ZnO matrix. The optimized nanocomposite (2.5 mol % Cu doping) showed a lowest crystallite size of 21.64 nm, which reduced further to 18.06 nm upon graphene oxide addition. Morphological analyses (scanning electron microscopy and transmission electron microscopy) exhibited rounded grains along with copious channels typical for sol-gel-based materials . Elemental mapping displayed the good dispersion of Cu in the ZnO matrix. When these materials are employed as a gas sensor, they demonstrated high sensitivity and selectivity toward H2S gas in comparison with the reducing gases and volatile organic compounds under investigation. The systematic doping of Cu in the ZnO matrix exhibited an improved response from 76.66 to 94.28%, with reduction in operating temperature from 300 to 250 °C. The 2.5 mol % doped Cu in ZnO was found to impart a response of 23 s for 25 ppm of H2S. Gas-sensing properties are described using an interplay of epoxide-assisted sol-gel chemistry and structural and morphological properties of the developed material.