Micro- and nanoparticles of NiSb2O6 were synthesized by the microwave-assisted colloidal method. Nickel nitrate, antimony chloride, ethylenediamine, and ethyl alcohol were used. The oxide was obtained at 600°C and was analyzed by X-ray diffraction (XRD) and Raman spectroscopy, showing a trirutile-type structure with cell parameters = 4.641 Å, = 9.223 Å, and a space group P42/mnm (136). Average crystal size was estimated at ~31.19 nm, according to the XRD-peaks. The microstructure was scrutinized by scanning electron microscopy (SEM), observing microrods measuring ~3.32 μm long and ~2.71 μm wide, and microspheres with an average diameter of ~8 μm; the size of the particles shaping the microspheres was measured in the range of ~0.22 to 1.8 μm. Transmission electron microscopy (TEM) revealed that nanoparticles were obtained with sizes in the range of 2 to 20 nm (~10.7 nm on average). Pellets made of oxide’s powders were tested in propane (C3H8) and carbon monoxide (CO) atmospheres at different concentrations and temperatures. The response of the material increased significantly as the temperature and the concentration of the test gases rose. These results show that NiSb2O6 may be a good candidate for gas sensing applications.
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