Synthesis of Zirconia Micro-Nanoflakes with Highly Exposed (001) Facets and Their Crystal Growth

This study reports a novel preparation method of zirconia micro-nanoflakes with high (001) facets that is generated through a hydrolysis reaction of the fluozirconic acid (H2ZrF6). Zirconia micro-nanoflakes synthesized at varied conditions were analyzed by the SEM, EDS, μ-XRD, and Raman spectroscopy to characterize the morphology and probe into the crystal growth mechanism. The synthesized zirconia crystals in the form of elliptical micro-nanoflakes or irregular nanoflakes generally display the highly exposed (001) facets with a thickness of 1–100 nm and a length of 0.1–2.0 μm. As the temperature and initial solution concentration increased, the particle sizes of the synthesized zirconia micro-nanoflakes became more uniform and the thicknesses of the (001) facets became larger, suggesting that the synthesized zirconia crystals grow along the (001) facets and mostly along the c-axis direction. This is confirmed by the data from the μ-XRD patterns. The results also demonstrate that an oriented attachment-based growth occurring in a fluorine-rich solution environment was involved in the aggregation and coarsening of zirconia micro-nanoflakes. Meanwhile, synthesized zirconia micro-nanoflakes also evolved from a mixture of monoclinic and tetragonal systems to a pure monoclinic system (i.e., baddeleyite) with the temperature increasing, suggesting a key role of temperature regarding zirconia’s growth.