In this work, flame-spray-made SnO2 nanoparticles are systematically studied by doping with 0.1-2 wt % nickel (Ni) and loading with 0.1-5 wt % electrolytically exfoliated graphene for acetone-sensing applications. The sensing films (∼12-18 μm in thickness) were prepared by a spin-coating technique on Au/Al2O3 substrates and evaluated for acetone-sensing performances at operating temperatures ranging from 150 to 350 °C in dry air. Characterizations by X-ray diffraction, transmission/scanning electron microscopy, Brunauer-Emmett-Teller analysis, X-ray photoelectron spectroscopy and Raman spectroscopy demonstrated that Ni-doped SnO2 nanostructures had a spheriodal morphology with a polycrystalline tetragonal SnO2 phase, and Ni was confirmed to form a solid solution with SnO2 lattice while graphene in the sensing film after annealing and testing still retained its high-quality nonoxidized form. Gas-sensing results showed that SnO2 sensing film with 0.1 wt % Ni-doping concentration exhibited an optimal response of 54.2 and a short response time of ∼13 s toward 200 ppm acetone at an optimal operating temperature of 350 °C. The additional loading of graphene at 5 wt % into 0.1 wt % Ni-doped SnO2 led to a drastic response enhancement to 169.7 with a very short response time of ∼5.4 s at 200 ppm acetone and 350 °C. The superior gas sensing performances of Ni-doped SnO2 nanoparticles loaded with graphene may be attributed to the large specific surface area of the composite structure, specifically the high interaction rate between acetone vapor and graphene-Ni-doped SnO2 nanoparticles interfaces and high electronic conductivity of graphene. Therefore, the 5 wt % graphene loaded 0.1 wt % Ni-doped SnO2 sensor is a promising candidate for fast, sensitive and selective detection of acetone.
In this work, flame-spray-made undoped SnO2 nanoparticles were loaded with 0.1-5 wt % electrolytically exfoliated graphene and systematically studied for NO2 sensing at low working temperatures. Characterizations by X-ray diffraction, transmission/scanning electron microscopy, and Raman and X-ray photoelectron spectroscopy indicated that high-quality multilayer graphene sheets with low oxygen content were widely distributed within spheriodal nanoparticles having polycrystalline tetragonal SnO2 phase. The 10-20 μm thick sensing films fabricated by spin coating on Au/Al2O3 substrates were tested toward NO2 at operating temperatures ranging from 25 to 350 °C in dry air. Gas-sensing results showed that the optimal graphene loading level of 0.5 wt % provided an ultrahigh response of 26,342 toward 5 ppm of NO2 with a short response time of 13 s and good recovery stabilization at a low optimal operating temperature of 150 °C. In addition, the optimal sensor also displayed high sensor response and relatively short response time of 171 and 7 min toward 5 ppm of NO2 at room temperature (25 °C). Furthermore, the sensors displayed very high NO2 selectivity against H2S, NH3, C2H5OH, H2, and H2O. Detailed mechanisms for the drastic NO2 response enhancement by graphene were proposed on the basis of the formation of graphene-undoped SnO2 ohmic metal-semiconductor junctions and accessible interfaces of graphene-SnO2 nanoparticles. Therefore, the electrolytically exfoliated graphene-loaded FSP-made SnO2 sensor is a highly promising candidate for fast, sensitive, and selective detection of NO2 at low operating temperatures.
ZnO nanoparticles were produced by flame spray pyrolysis (FSP) using zinc naphthenate as a precursor dissolved in toluene/acetonitrile (80/20 vol%). The particle properties were analyzed by XRD, BET, and HR-TEM. The sensing films were produced by mixing the particles into an organic paste composed of terpineol and ethyl cellulose as a vehicle binder and were fabricated by doctor-blade technique with various thicknesses (5, 10, 15 µm). The morphology of the sensing films was analyzed by SEM and EDS analyses. The gas sensing characteristics to ethanol (25-250 ppm) were evaluated as a function of film thickness at 400°C in dry air. The relationship between thickness and ethanol sensing characteristics of ZnO thick film on Al 2 O 3 substrate interdigitated with Au electrodes were investigated. The effects of film thickness, as well as the cracking phenomenon, though, many cracks were observed for thicker sensing films. Crack widths increased with increasing film thickness. The film thickness, cracking and ethanol concentration have significant effect on the sensing characteristics. The sensing characteristics with various thicknesses were compared, showing the tendency of the sensitivity to ethanol decreased with increasing film thickness and response time. The relationship between gas sensing properties and film thickness was discussed on the basis of diffusively and reactivity of the gases inside the oxide films. The thinnest sensing film (5 µm) showed the highest sensitivity and the fastest response time (within seconds).
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