Gas sensors based on the multi-sensor platform MSP 632, with thin nanocomposite films based on tin dioxide with a low content of zinc oxide (0.5–5 mol.%), were synthesized using a solid-phase low-temperature pyrolysis technique. The resulting gas-sensitive ZnO-SnO₂ films were comprehensively studied by atomic force microscopy, Kelvin probe force microscopy, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, scanning transmission electron microscopy, energy dispersive X-ray spectrometry, and X-ray photoelectron spectroscopy. The obtained films are up to 200 nm thick and consist of ZnO-SnO₂ nanocomposites, with ZnO and SnO₂ crystallite sizes of 4–30 nm. Measurements of ZnO-SnO₂ films containing 0.5 mol.% ZnO showed the existence of large values of surface potential, up to 1800 mV, leading to the formation of a strong surface electric field with a strength of up to 2 × 10⁷ V/cm. The presence of a strong surface electric field leads to the best gas-sensitive properties: the sensor’s responsivity is between two and nine times higher than that of sensors based on ZnO-SnO₂ films of other compositions. A study of characteristics sensitive to NO₂ (0.1–50 ppm) showed that gas sensors based on the ZnO-SnO₂ film demonstrated a high sensitivity to NO₂ with a concentration of 0.1 ppm at an operating temperature of 200 °C.

Thin TiO₂–SnO₂ nanocomposite films with high gas sensitivity to NO₂ were synthesized by oxidative pyrolysis and comprehensively studied. The composite structure and quantitative composition of the obtained film nanomaterials have been confirmed by X-ray photoelectron spectroscopy, high-resolution transmission electron microscopy, and energy dispersive X-ray spectroscopy, which causes the presence of n-n heterojunctions and provides improved gas-sensitive properties. The sensor based on the 3TiO₂–97SnO₂ film has the maximum responses, which is explained by the existence of a strong surface electric field formed by large surface potentials in the region of TiO₂–SnO₂ heterojunctions detected by the Kelvin probe force microscopy method. Exposure to low-intensity radiation (no higher than 0.2 mW/cm², radiation wavelength—400 nm) leads to a 30% increase in the sensor response relative to 7.7 ppm NO₂ at an operating temperature of 200 °C and a humidity of 60% RH. At room temperature (20 °C), under humidity conditions, the response is 1.8 when exposed to 0.2 ppm NO₂ and 85 when exposed to 7.7 ppm. The lower sensitivity limit is 0.2 ppm NO₂. The temporal stability of the proposed sensors has been experimentally confirmed.