Preparation and characterization of zirconium carbide nano powder by hydrothermal and carbothermal reduction methods

Abstract

A hydrothermal method was employed to synthesize the precursor of nano-zirconium carbide, which was subsequently heat treated at high temperatures under vacuum to obtain finely dispersed nanometer-sized zirconium carbide powder through a carbothermic reduction reaction. Scanning Electron Microscopy (SEM) was utilized to examine the microstructure of the precursors obtained under different hydrothermal conditions and carbon contents. The effects of different heat treatment temperatures on the microstructure of the products were analyzed. Transmission Electron Microscopy (TEM) confirmed the boundary coating structure of the hydrothermal precursor and provided insights into the phase structure of the nanometer-sized zirconium carbide. The reaction mechanism and temperature involved in the carbothermic reaction process were determined through calculations. Furthermore, the energy, phase and microstructure of the reaction were investigated using Thermogravimetric Analysis (TG-DSC) and X-ray Diffraction (XRD) at different temperatures. The obtained results revealed that the zirconium carbide precursor was synthesized via the hydrothermal method exhibited a core-shell structure with a boundary coating, which not only ensured uniform contact between C and ZrO2 particles but also facilitated the formation of zirconium carbide. The results show that the most suitable process parameters are Zr/C 1: 7, 240 °C and 24 h. The thermodynamic calculation results show that ZrO2 combines with carbon to form CO and ZrC when the temperature reaches 1656.56 °C. As the temperature rises, CO reacts with ZrO2 to form ZrC and CO2. TG-DSC shows that the carbothermal reduction reaction starts at 1100 °C and reaches its peak at 1418 °C. XRD analysis confirms that when the temperature reached 1450 °C ZrC appeared. At 1600 °C, the phase transition of ZrC is basically completed. TEM images showed that the synthesized zirconium carbide particles were about 30 nm.