Synthesis and Characterization of Nanozirconia via Interaction of Zirconium (IV) with Oxamid under Solvothermal Conditions

Over the past two decades, various methods have been developed for the production of nanoparticles, which can be produced use of a variety of sol-gel, micro-plasma and hydrothermal methods with or without ultrasound [1]. Hydrothermal synthesis can be defined as a method of formation and growth of particles by chemical reactions and solubility changes of substances in a sealed heated aqueous solution above ambient conditions [2]. In this study, zirconia nanoparticles were synthesized from the zirconium(IV) oxynitrate in the presence of oxamide under hydrothermal condition and subsequent calcination of product. The product was characterized by TG-DTA, FT-IR, XRD and SEM analysis. Badylete was detected as the only phase of ZrO2 after hydrotreacting at 200ᵒC and is not changed after calcination at 600ᵒC. A gel, however, is formed under hydrotreating at 100ᵒC. A xerogel is formed upon drying of the gel, converting to a cubic nano-zirconia upon calcining at 600ᵒC. Crystallite size was calculated to be about 15-20 nm for the both phase (Sherrer formula). Particle size is observed to be about 20 nm in the SEM image. Results show that the hydrotreating temperature is a critical parameter of the formation of the crystalline phase.