Synthesis of thermally stable, high surface area, nanocrystalline mesoporous tetragonal zirconium dioxide (ZrO2): Effects of different process parameters

Nanocrystalline mesoporous zirconium dioxide powder with high surface area and remarkable thermal stability was synthesized using ethylene diamine and zirconyl chloride octahydrate. Ethylene diamine used as precipitating agent also acted as a colloidal protecting agent. The material retained high surface area (193.1 m2/g) mesoporous structure even after calcination at 900 °C with the surface area of the as-prepared material exceeding 440 m2/g depending upon the preparation conditions. Effects of different process parameters such as digestion time, pH, precursor concentration and calcination temperature on structural properties of the material were studied. These preparation conditions significantly affected the structural stability, crystal size and the crystal phase of the final material. The material was characterized by nitrogen adsorption–desorption, X-ray diffraction, scanning electron microscopy, thermogravimetric and differential scanning calorimetry, energy dispersive X-ray spectroscopy and Fourier transform infrared spectroscopy. The final material has very high tetragonal phase stability even after calcination at 1000 °C temperature.

Nanocrystalline mesoporous tetragonal zirconia synthesized using ethylene diamine and zirconium oxychloride at different process parameters shows high surface area (193 m2/g) and remarkable thermal stability (stable even after calcination at 900 °C).Figure optionsDownload as PowerPoint slideHighlights
► Synthesis of stable, high surface area, nanocrystalline mesoporous tetragonal ZrO2.
► Studied effects of digestion time, pH, precursor concentration and calcination temperature.
► Identified the process parameters yielding the highest surface area and pore volume.
► The best operating conditions are 48 h digestion time, pH 11 and 0.045 M precursor.
► Preparation conditions have significant effects on structural and phase properties.