Thin nanocomposite films composed of ZnO and SnO₂ at 0.5–5 mol.% concentrations were synthesized by a new solid-phase low-temperature pyrolysis under the developed protocols. This hetero-oxide material was thoroughly studied by X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES) techniques to be compared with electrical and gas-sensing properties. We have found that the films have a poly-nanocrystal structure of ZnO and SnO₂ crystals with characteristic grain sizes at 10–15 nm range. When comparing the chemiresistive response of the films with varied tin dioxide content, the sample of Sn:Zn optimum ratio taken as 1:99 yields 1.5-fold improvement upon to 5–50 ppm NO₂ exposure at 200 °C. We argue that these remarkable changes have matured from both a reducing the intergrain potential barrier down to 0.58 eV and increasing the concentration of anionic vacancies at this rational composite. The results demonstrate that solid-phase low-temperature pyrolysis is a powerful technique for adjusting the functional gas-sensing properties of hetero-oxide film via modifying the ratio of the oxide components.

Thin nanocrystalline transparent Al-doped ZnO (1–10 at.% Al) films were synthesized by solid-phase pyrolysis at 700 °C. Synthesized Al-doped ZnO films were investigated by X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM, TEM). All obtained materials were crystallized into the wurtzite structure, which was confirmed by XRD. The material crystallinity decreases with the introduction of aluminum. SEM and TEM showed that the films are continuous and have a uniform distribution of nanoparticles with an average size of 15–20 nm. TEM confirmed the production of Al-doped ZnO films. The transmittance of Al-doped ZnO films in the range of 400–1000 nm is more than 94%. The introduction of 1% Al into ZnO leads to a narrowing of the band gap compared to ZnO to a minimum value of 3.26 eV and a sharp decrease in the response time to the radiation exposure with a wavelength of 400 nm. An increase in aluminum concentration leads to a slight increase in the band gap, which is associated with the Burstein–Moss effect. The minimum response time (8 s) was shown for film containing 10% Al, which is explained by the shortest average lifetime of charge carriers (4 s).

Thin nanocomposite films based on zinc oxide (ZnO) added with cobalt oxide (Co₃O₄) were synthesized by solid-phase pyrolysis. According to XRD, the films consist of a ZnO wurtzite phase and a cubic structure of Co₃O₄ spinel. The crystallite sizes in the films increased from 18 nm to 24 nm with growing annealing temperature and Co₃O₄ concentration. Optical and X-ray photoelectron spectroscopy data revealed that enhancing the Co₃O₄ concentration leads to a change in the optical absorption spectrum and the appearance of allowed transitions in the material. Electrophysical measurements showed that Co₃O₄-ZnO films have a resistivity up to 3 × 10⁴ Ohm∙cm and a semiconductor conductivity close to intrinsic. With advancing the Co₃O₄ concentration, the mobility of the charge carriers was found to increase by almost four times. The photosensors based on the 10Co-90Zn film exhibited a maximum normalized photoresponse when exposed to radiation with wavelengths of 400 nm and 660 nm. It was found that the same film has a minimum response time of ca. 26.2 ms upon exposure to radiation of 660 nm wavelength. The photosensors based on the 3Co-97Zn film have a minimum response time of ca. 58.3 ms versus the radiation of 400 nm wavelength. Thus, the Co₃O₄ content was found to be an effective impurity to tune the photosensitivity of radiation sensors based on Co₃O₄-ZnO films in the wavelength range of 400–660 nm.

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.