Xuehang Wu

Nanocrystalline ZrO2 preparation and kinetics research of phase transition

The precursor of nanocrystalline ZrO2 was synthesized by solid-state reaction at low heat using ZrOCl2·8H2O, and Na2CO3·10H2O as raw materials. The nanocrystalline ZrO2 was obtained by calcining the precursor. The precursor and its calcined products were characterized using TG/DTA, FT-IR, XRD, and SEM. The results showed that the precursor dried at 353 K was a zirconyl carbonate compound. When the precursor was calcined at 673 K for 150 min, highly crystallization ZrO2 with tetragonal structure (space group P42/nmc (137)) was obtained with a crystallite size of 24 nm. However, when the precursor was calcined at 1023 K for 150 min, highly crystallization ZrO2 with monoclinic structure (space group P21/c(14)) was obtained with a crystallite size of 20 nm. The mechanism and kinetics of the thermal process of the precursor were studied using DTA and XRD techniques. Based on the Kissinger and Arrhenius equation, the values of the activation energies associated with the thermal process of the precursor were determined to be 26.80 and 566.73 kJ·mol−1 for the first and third steps, respectively. The mechanism of ZrO2 phase transition from tetragonal to monoclinic structure is the random nucleation and growth of nuclei reaction.