Bystromite (MgSb2O6) nanorods were prepared using a colloidal method in the presence of ethylenediamine, after a calcination step at 800 °C in static air. From X-ray powder diffraction analyses, a trirutile-type structure with lattice parameters a = 4.64 Å and c = 9.25 Å and space group P42/mnm was identified. Using scanning electron microscopy (SEM), microrods with sizes from 0.2 to 1.6 μm were observed. Transmission electron microscopy (TEM) analyses revealed that the nanorods had a length of ~86 nm and a diameter ~23.8 nm. The gas-sensing properties of these nanostructures were tested using pellets elaborated with powders of the MgSb2O6 oxide (calcined at 800 °C) at temperatures 23, 150, 200, 250 and 300 °C. The pellets were exposed to different concentrations of carbon monoxide (CO) and propane (C3H8) at these temperatures. The results showed that the MgSb2O6 nanorods possess excellent stability and high sensitivity in these atmospheres.
Experimental work on the synthesis of the CoSb 2 O 6 oxide and its CO 2 sensing properties is presented here. The oxide was synthesized by a microwave-assisted colloidal method in presence of ethylenediamine after calcination at 600 °C. This CoSb 2 O 6 oxide crystallized in a tetragonal structure with cell parameters = 4.6495 and = 9.2763 Å, and space group P4 2 /mnm. To prove its physical, chemical and sensing properties, the oxide was subjected to a series of tests: Raman spectroscopy, Scanning Electron Microscopy (SEM) and impedance (Z) measurements. Microstructures, like columns, bars and hollow hemispheres, were observed. For the CO 2 sensing test, a thick film of CoSb 2 O 6 was used, measuring the impedance variations on the presence of air/CO 2 flows (0.100 sccm/0.100 sccm) using AC (alternating current) signals in the frequency-range
OPEN ACCESSSensors 2014, 14 15803 0.1-100 kHz and low relative temperatures (250 and 300 °C). The CO 2 sensing results were quite good.
Mesoporous CoSb2O6nanoparticles, synthesized through a nonaqueous method (using cobalt nitrate, antimony trichloride, ethylenediamine, and ethanol as a solvent), were tested to establish their sensitivity to CO and C3H8atmospheres at relatively low temperatures. The precursor material was dried at 200°C and calcined at 600°C. X-ray diffraction and scanning electron microscopy were employed to verify the existence of crystal phases (P42/mnm) and the morphology of this trirutile-type CoSb2O6oxide. Pyramidal and cubic shaped crystals (average size: 41.1 nm), embedded in the material’s surface, were identified. Mesopores (average size: 6.5 nm) on the nanoparticles’ surface were observed by means of transmission electron microscopy. The best sensitivity of the CoSb2O6in a CO atmosphere was at the relatively low temperatures of 250 and 350°C, whereas, in a C3H8atmosphere, the sensitivity increased uniformly with temperature. These results encourage using the CoSb2O6nanoparticles as gas sensors.
Nanoparticles of manganese antimonate (MnSb2O6) were prepared using the microwave-assisted colloidal method for its potential application as a gas sensor. For the synthesis of the oxide, manganese nitrate, antimony chloride, ethylenediamine and ethyl alcohol (as a solvent) were used. The precursor material was calcined at 800 °C in air and analyzed by X-ray diffraction. The oxide crystallized into a hexagonal structure with spatial group P321 and cell parameters a = b = 8.8054 Å and c = 4.7229 Å. The microstructure of the material was analyzed by scanning electron microscopy (SEM), finding the growth of microrods with a size of around ~10.27 μm and some other particles with an average size of ~1.3 μm. Photoacoustic spectroscopy (PAS) studies showed that the optical energy band (Eg) of the oxide was of ~1.79 eV. Transmission electron microscopy (TEM) analyses indicated that the size of the nanoparticles was of ~29.5 nm on average. The surface area of the powders was estimated at 14.6 m2/g by the Brunauer–Emmett–Teller (BET) method. Pellets prepared from the nanoparticles were tested in carbon monoxide (CO) and propane (C3H8) atmospheres at different concentrations (0–500 ppm) and operating temperatures (100, 200 and 300 °C). The pellets were very sensitive to changes in gas concentration and temperature: the response of the material rose as the concentration and temperature increased. The results showed that the MnSb2O6 nanoparticles can be a good candidate to be used as a novel gas sensor.
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