Effects of Solvent on the Phase Composition and Microstructure of ZrSiO₄ Film

Abstract

Zirconium silicate thin film was prepared via a novel non-hydrolytic sol-gel (NHSG) process at low temperature using zirconium tetrachloride (ZrCl4) and tetraethoxysilane (TEOS) as precursors. The phase composition and the microstructure of samples were characterized by X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM), respectively. The results demonstrate that pure ZrSiO4 film can be synthesized by using ethanol and isopropanol as solvent rather than dimethyl formamide (DMF) and dimethyl nylon acid (DBE) which cause impurity ZrO2. However, only ethanol can achieved smooth and dense ZrSiO4 film. The viscosity results suggest that the sol with ethanol has great stability. With a pulling rate of 1.0 mm s-1, a high quality ZrSiO4 film was prepared after drying at 50 oC for 2 h and calcination at 850 °C with a heating rate of 1.0 °C min-1.