The synthesis of the Fe2O3–CuO–CuFe2O4 nanocomposite was effectively achieved through the sol–gel technique, utilizing ethanol as a reactive fuel. Investigation of the nanocomposite’s structure via X-ray Diffraction confirmed the coexistence of Fe2O3, CuO, and CuFe2O4 phases within the material. The Scherrer equation was applied to determine an average crystallite size ranging from 60 to 95 nm. UV–visible spectroscopy studies suggested the material possesses an approximate energy bandgap of 4 eV. Scanning Electron Microscopy provided insights into the nanocomposite’s surface morphology, which exhibited a porous and heterogeneous aggregation of particles in various sizes and shapes. When tested for antibacterial efficacy, the nanocomposite exhibited activity against gram-positive S. aureus with a maximum zone of inhibition (ZOI) measuring 9 mm at the highest concentration, whereas no inhibitory effect was detected against gram-negative E.coli.