Continuous Hydrothermal Flow Synthesis and Characterization of ZrO₂ Nanoparticles Doped with CeO₂ in Supercritical Water

Abstract

A confined jet mixing reactor operated in continuous hydrothermal flow synthesis was investigated for the synthesis of CeO2-ZrO2 (CZ) nanoparticles. The obtained ultrafine powders were characterized using scanning electron microscopy–energy dispersive spectrometry (SEM-EDS), inductively coupled plasma–atomic emission spectroscopy (ICP-AES), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray diffraction analysis (XRD), transmission electron microscopy (TEM) coupled with selected area electron diffraction (SAED), a BET (Brunauer-Emmett-Teller)-specific surface area test and pore analysis, oxygen storage capacity (OSC) test, and a H2 temperature programmed reduction (H2-TPR) test. The XRD results show that all samples were composed of high-purity cubic CZ nanoparticles. High resolution transmission electron microscope (HR-TEM) analysis showed that CZ nanoparticles with uniform size and shape distributions were obtained in this investigation. The d-spacing values, determined based on the TEM-selected area electron diffraction (SAED) patterns, were in good agreements with the reference data. BET results showed that the prepared CZ samples had large specific surface areas. Pore volume and size distribution were obtained by pore analysis. Oxygen pulse adsorption technology was used to test the oxygen storage capacity of the sample. The redox capacity of the CZ material was determined by a H2 temperature-programmed reduction test.

Keywords

• continuous hydrothermal flow synthesis
• confined jet mixing reactor
• CeO₂-ZrO₂ nanoparticles
• XRD
• BET