Synthesis and thermal behavior of sol-gel derived zirconium oxide

Reference	Presenter	Authors (Institution)	Abstract
17-017	Débora Guimarães da Silva	Silva, D.G.(Federal University of Minas Gerais); Paraguay, L.F.(Federal University of Minas Gerais); Vasconcelos, W.L.(Federal University of Minas Gerais);	Zirconium oxide is a multifunctional material being widely used in different applications such as catalysis, refractories and advanced ceramics. The great variety of applications that display the zirconia has increased the attention to investigate the factors controlling its structure including its thermal treatment. In this study the preliminary characterization of a mesoporous zirconium oxide submitted to different calcination temperatures for removal of organic compounds was described. Zirconia sols were synthesized via sol-gel process using zirconium n-propoxide as precursor, n-propanol as solvent, glacial acetic acid as a catalyst and inhibitor and deionized water for the hydrolysis. Subsequently, the sols were held under static condition at 60°C for completion of hydrolysis and condensation reactions. The zirconium hydroxide was obtained by drying gels at 100°C for 72 hours. Thermal analyses of the zirconium hydroxides were carried out by thermogravimetric analysis (TG) and differential scanning calorimetric analysis (DSC) in air atmosphere with a heating rate of 10°C/min from 30°C up to 900°C. The samples were calcined in air in a muffle furnace at 200°C, 300°C and 400°C with a heating rate of 1°C/min. Fourier transform-infrared spectroscopy (FT-IR) was employed for the identification of the chemical bonds present in the zirconia before and after the calcination at different temperatures. After calcined at 400°C, the specific surface area and pore size distribution were determined by nitrogen adsorption-desorption measurements using Brunauer-Emmet-Teller (BET) method and density functional theory (DFT). An X-ray diffractometer (DRX) was used to analyze the crystallographic phase of zirconia. The sample’s morphology was evaluated by scanning electron microscopy (SEM).
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