Barium antimonate (BaSb2O6) powders were prepared using a microwave-assisted wet chemistry process. The powders were calcined at 800 °C and their crystallinity was studied by X-ray diffraction, finding a hexagonal crystal structure with cell parameters a = 5.303 Å and c = 5.758 Å, and a P-31m (162) space group. Material’s morphology and particle size were analyzed by field-emission scanning and transmission electron microscopy, finding that nano-plates (~ 70 nm) and other apparently shapeless particles (~ 70 nm) were produced. By means of X-Ray Photoelectron Spectroscopy, it was found that the Ba 3d had a doublet (Ba 3d5/2 and Ba 3d3/2) with binding energies at 779.69 and 794.97 eV, respectively, which was associated with the Ba2+ oxidation state. The Sb 3d spectrum presented a doublet (Sb 3d5/2 and Sb 3d3/2) at 530.44 and 539.79 eV, while the O 1 s at 530.30 eV overlapped the Sb 3d5/2 peak. Photoacoustic Spectroscopy measurements of the oxide showed a band gap of 3.43 eV. Pellets manufactured with BaSb2O6’s powders calcined at 800 °C were tested in CO (1–300 ppm) and C3H8 (1–500 ppm) atmospheres at different operating temperatures (100, 200 and 300 °C). The pellets exhibited an excellent response, showing a high sensitivity as concentrations and temperature increased. Furthermore, the results indicated that the BaSb2O6 is highly selective to CO atmospheres. In particular, the good response of the pellets suggests that this oxide can be applied as a potential sensor for toxic gases.
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