Simple and novel synthesis of zirconia whiskers from a phosphate flux

Abstract

High quality zirconia whiskers have been successfully prepared by molten salt method, using zirconium oxychloride (ZrOCl2·8H2O) and sodium phosphate tribasic dodecahydrate (Na3PO4·12H2O) as precursor and molten salt, respectively. The effects of types of molten salt and heat treatment temperature on the formation of zirconia whiskers were characterized by XRD, Raman, DTA-TG, FE-SEM, TEM, SAED and HR-TEM. When Na3PO4·12H2O is utilized as molten salt and the heat treatment temperature is 900 °C, the as-prepared zirconia whiskers with length ranging from 4 µm to 8 µm show an average aspect ratio of 25. The obtained ZrO2 whiskers with monoclinic structure are elongated along [010] direction and exhibit a smooth surface with no distinct defects. The XRD and Raman results reveal that the phase transformation from tetragonal zirconia to monoclinic zirconia occurs with the increased crystal size and the water quenching treatment can significantly reduce the content of sodium zirconium phosphate [Na9–4×Zrx(PO4)3] in the final product. The growth mechanism of zirconia whiskers is supposed to be a dissolution-precipitation process. Since the sodium zirconium phosphate [Na9–4×Zrx(PO4)3] effectively promotes the dissolution of zirconia in liquid molten salt, zirconia can grow into zirconia whiskers according to its anisotropy.