One-pot synthesis of monoclinic ZrO2 nanocrystals under subcritical hydrothermal conditions

• ZrO2 nanocrystals from a ZrO(NO3)2 precursor were synthesized by a one-pot hydrothermal method utilizing subcritical water.
• The reaction temperature and time strongly affected the crystalline phase of ZrO2 products.
• A single-phase monoclinic ZrO2 product was synthesized at 250 °C for the reaction time exceeded 12 h.
• The crystallite size of the single-phase monoclinic ZrO2 product was approximately 20 nm.
• The nanocrystals had chemisorbed water, terminated hydroxides, and nitro groups onto its surface.

This study reports a one-pot synthesis technique for the preparation of single-phase monoclinic zirconium oxide (ZrO2) nanocrystals. The products were synthesized from only zirconium oxynitrate (ZrO(NO3)2) as the precursor under hydrothermal conditions using subcritical water. The precursor was heat-treated in a batch-type reactor at a reaction temperature of 250 °C for 24 h to obtain pure monoclinic-structured ZrO2 nanocrystals. The crystallization temperature of the ZrO2 phase was also greater than 200 °C. However, the products of reactions conducted at 200 °C for 24 h were mixtures of the tetragonal and monoclinic structures. At a reaction temperature of 250 °C, the volume fraction of the monoclinic phase increased; however, the reaction time was also important. The heat-treatment was performed for more than 12 h in order to obtain single-phase monoclinic ZrO2 nanocrystals. The crystallite size of this product was approximately 20 nm, and water, hydroxide groups, and nitro groups were chemisorbed on its surface.

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