Study of morphology, phase composition, optical properties, and thermal stability of hydrothermal zirconium dioxide synthesized at low temperatures

Abstract

Oxide nanoparticles exhibit unique features such as high surface area, enhanced catalytic activity, and tunable optical and electrical properties, making them valuable to various industry applications as well as for the development of new research projects. Nowadays, ZrO2 nanoparticles are widely used as catalysts and precursors in ceramic technology. Hydrothermal synthesis with metal salts is one of the most common methods for producing stable tetragonal-phase zirconium dioxide nanoparticles. However, hydrothermal synthesis requires relatively high process temperatures (160–200 °C) and the use of advanced heat-resistant autoclaves capable of maintaining high pressure. This paper investigates how different precursors (ZrOCl₂·8H₂O and ZrO(NO₃)₂·2H₂O) and synthesis temperatures (110–160 °C) affect the phase composition, optical properties, size, and shape of ZrO₂ nanoparticles produced by hydrothermal synthesis without calcination. In addition, the effect of temperature exposure in the range of 100–1000 °C on the phase stability of the synthesized nanoparticles was studied. X-ray diffraction and Raman spectroscopy techniques were used to determine the structure and phase composition, while the optical properties were examined through the analysis of transmission and absorption spectra in the visible and UV ranges. It was found that the obtained particles at synthesis temperatures of 110–130 °C have predominantly cubic c-ZrO2 phase, which changes to monoclinic phase when heated above 500 °C. Analysis of visible and UV spectroscopy data reveals that the experimental samples have pronounced absorption in the middle UV range (200–260 nm) and have an energy band gap Eg varying from 4.8 to 5.1 eV. The hydrothermal powders synthesized in this study can be used as absorbers in the mid-UV range and as reinforcing additives in the preparation of technical ceramics.