[en] Ternary nanocomposites made of γ-iron oxide and aluminum-doped zinc oxide (γ-Fe₂O₃/Al–ZnO NCs), with different metal oxides ratio (0%–100%) were prepared through a solvothermal sol–gel process. The synthesized materials were characterized by x-ray diffraction, UV–vis spectroscopy, photoluminescence (PL), scanning electron microscope and BET analysis. Characterization results demonstrated that the ternary γ-Fe₂O₃/Al–ZnO NCs are mainly constituted by γ-Fe₂O₃ and Al–ZnO individual phases, while structural and physical properties like surface area, pore size, optical band gap, PL and electrical conductivity were deeply affected by the composition of nanocomposite. The synthesized γ-Fe₂O₃/Al–ZnO NCs were employed to prepare conductometric gas sensors, then their sensing performances toward acetone were also investigated. Results revealed enhanced sensing performance of nanocomposites than both pure γ-Fe₂O₃ and Al–ZnO phases. In particular, the γ-Fe₂O₃(33%)/Al–ZnO based gas sensor showed the best sensing properties, like a high response of R _air/R _gas = 29, a short response time of 3 s, in addition to an improved selectivity toward acetone versus ethanol at an operating temperature of 200 °C. Overall, ternary γ-Fe₂O₃/Al–ZnO NCs appear to be promising for the development of conductometric acetone sensors. (paper)