Fabrication and analysis of the structural phase transition of ZrO₂ nanoparticles using modified facile sol–gel route

ABSTRACT

The synthesis of zirconia nanoparticles is achieved through a modified facile sol–gel route. The as-prepared gel is analyzed thermally using TGA and DTA techniques to spot the crystallization process of zirconia nanoparticles. The prepared gel is then annealed at different temperatures and the structure was found to change between tetragonal and monoclinic crystal systems. The first stable tetragonal phase is achieved after annealing for 2 h at 400°C. The annealed powders between 600°C and 800°C demonstrate mixed tetragonal/monoclinic phases. Annealing at 1000°C and higher temperatures up to 1200°C resulted in pure monoclinic phase. Cubic phase was not detected within the annealing temperature range in this study. The elemental analysis of the annealed powder confirmed the formation of zirconia nanoparticles with the chemical formula ZrO₂. The FTIR spectra of the annealed samples introduced a variation in the vibrational bands especially around the phase transition temperature. HR-TEM images reported the formation of nano-zirconia crystals with apparently large particle sizes. The optical energy gap of zirconia nanoparticles is investigated and determined.

KEYWORDS:

• ZrO₂ nanoparticles
• sol–gel synthesis
• EDAX
• HR-TEM
• optical energy gap

ORCID

A. Abu El-Fadl http://orcid.org/0000-0003-2413-5965

Additional information

Funding

The authors gratefully acknowledge the financial support unit at the Faculty of Science, Assiut University for the financial support.