Nanocrystalline cobalt oxide Co₃O₄ has been prepared by precipitation and subsequent thermal decomposition of a carbonate precursor, and has been characterized in detail using XRD, transmission electron microscopy, and FTIR spectroscopy. The sensory characteristics of the material towards carbon monoxide in the concentration range 6.7–20 ppm have been examined in both dry and humid air. A sensor signal is achieved in dry air at sufficiently low temperatures T = 80–120 °C, but the increase in relative humidity results in the disappearance of sensor signal in this temperature range. At temperatures above 200 °C the inversion of the sensor signal in dry air was observed. In the temperature interval 180–200 °C the sensor signal toward CO is nearly the same at 0, 20 and 60% r.h. The obtained results are discussed in relation with the specific features of the adsorption of CO, oxygen, and water molecules on the surface of Co₃O₄. The independence of the sensor signal from the air humidity combined with a sufficiently short response time at a moderate operating temperature makes Co₃O₄ a very promising material for CO detection in conditions of variable humidity.

Improvement of sensitivity, lower detection limits, stability and reproducibility of semiconductor metal oxide gas sensor characteristics are required for their application in the fields of ecological monitoring, industrial safety, public security, express medical diagnostics, etc. Facile and scalable single step flame spray pyrolysis (FSP) synthesis of bimetal AuPd sensitized nanocrystalline SnO₂ is reported. The materials chemical composition, structure and morphology has been studied by XRD, XPS, HAADFSTEM, BET, ICP-MS techniques. Thermo-programmed reduction with hydrogen (TPR-H₂) has been used for materials chemical reactivity characterization. Superior gas sensor response of bimetallic modified SnO₂ towards wide concentration range of reducing (CO, CH₄, C₃H₈, H₂S, NH₃) and oxidizing (NO₂) gases compared to pure and monometallic modified SnO₂ is reported for dry and humid gas detection conditions. The combination of facilitated oxygen molecule spillover on gold particles and electronic effect of Fermi level control by reoxidizing Pd-PdO clusters on SnO₂ surface is proposed to give rise to the observed enhanced gas sensor performance.

To obtain a nanocrystalline SnO₂ matrix and mono- and bimetallic nanocomposites SnO₂/Pd, SnO₂/Pt, and SnO₂/PtPd, a flame spray pyrolysis with subsequent impregnation was used. The materials were characterized using X-ray diffraction (XRD), a single-point BET method, transmission electron microscopy (TEM), and high angle annular dark field scanning transmission electron microscopy (HAADF-STEM) with energy dispersive X-ray (EDX) mapping. The electronic state of the metals in mono- and bimetallic clusters was determined using X-ray photoelectron spectroscopy (XPS). The active surface sites were investigated using the Fourier Transform infrared spectroscopy (FTIR) and thermo-programmed reduction with hydrogen (TPR-H₂) methods. The sensor response of blank SnO₂ and nanocomposites had a carbon monoxide (CO) level of 6.7 ppm and was determined in the temperature range 60–300 °C in dry (Relative Humidity (RH) = 0%) and humid (RH = 20%) air. The sensor properties of the mono- and bimetallic nanocomposites were analyzed on the basis of information on the electronic state, the distribution of modifiers in SnO₂ matrix, and active surface centers. For SnO₂/PtPd, the combined effect of the modifiers on the electrophysical properties of SnO₂ explained the inversion of sensor response from n- to p-types observed in dry conditions.