Low temperature synthesis of monodisperse nanoscaled ZrO2 with a large specific surface area

Thermal decomposition of Zr(C(2)O(4))(2)·4H(2)O within an autoclave or in a conventional tube furnace at temperatures below 380 °C resulted in nano- and micron-sized ZrO(2), respectively. Reactions under autogenic pressure yielded monodisperse monoclinic (m) and tetragonal (t) ZrO(2) nanoparticles with an average diameter of ~8 nm and interconnected t-ZrO(2) nanoparticles with diameters of ~4 nm, depending on the synthesis temperature. Samples were characterised by X-ray diffraction (XRD), small angle X-ray scattering (SAXS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) associated with energy dispersive X-ray spectroscopy (EDS), Raman microspectroscopy and photoluminescence spectroscopy (PL). Nanostructured zirconia materials exhibited high specific areas of 276-385 m(2) g(-1) which make them promising candidates as catalysts and catalyst supports. Co-existence of m- and t-ZrO(2) nanoparticles with diameters of 6-9 nm, i.e. above the critical particle size of 6 nm for the formation of t-ZrO(2), demonstrated that the particle size is not the only factor for stabilisation of the t-ZrO(2) modification at room temperature.