| Summary: | ZnO/Fe<sub>2</sub>O<sub>3</sub> nanocomposites with different concentration and thickness of the Fe<sub>2</sub>O<sub>3</sub> layer were obtained by two-stage aerosol vapor deposition (AACVD). It was shown that the ZnO particles have a wurtzite structure with an average size of 51–66 nm, and the iron oxide particles on the ZnO surface have a hematite structure and an average size of 23–28 nm. According to EDX data, the iron content in the films was found to be 1.3–5.8 at.%. The optical properties of the obtained films were studied, and the optical band gap was found to be 3.16–3.26 eV. Gas-sensitive properties at 150–300 °C were studied using a wide group of analyte gases: CO, NH<sub>3</sub>, H<sub>2</sub>, CH<sub>4</sub>, C<sub>6</sub>H<sub>6</sub>, ethanol, acetone, and NO<sub>2</sub>. A high response to 100 ppm acetone and ethanol at 225–300 °C and a high and selective response to 300–2000 ppb NO<sub>2</sub> at 175 °C were established. The effect of humidity on the magnitude and shape of the signal obtained upon NO<sub>2</sub> detection was studied.
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