Synthesis and characterization of superfine pure tetragonal nanocrystalline sulfated zirconia powder by a non-alkoxide sol-gel route

摘要

Nanocrystalline sulfated zirconia powder was prepared by a non-alkoxide sol-gel route using acidic condition (pH 1-2). The samples had superfine crystallites and pure tetragonal phase at 700 °C. Zr(acac)4 was used as jirconium precursor due to a better retention of sulfate species and H2SO4 0.5 M was used as sulfating agent. Fourier transform infrared (FT-IR) spectra have shown Zr-O-Zr and sulfate bonds. Crystal phase and crystallite size have been determined by X-ray Diffraction (XRD) analysis. Besides, the morphology of the samples has been investigated by field emission scanning electron microscope (FE-SEM) and transmission electron microscope (TEM). The optical properties of the samples have been analyzed using photoluminescence (PL) spectroscopy, too. All the analyses consistently have shown fairly uniform nanoparticles (calcined at 600 and 700 °C) with very small size and pure tetragonal phase with crystallite size between 5 and 10 nm.