Ultrasonic-hydrothermal and hydrothermal treatment was used for synthesis of nanocrystalline zirconia, titania, nickel and nickel-zinc ferrites powders from precipitated amorphous zirconyl, titanyl, binary nickel-iron and ternary nickel-zinc-iron hydroxides, respectively. Resulted nanopowders were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), nitrogen adsorption (BET), and magnetic susceptibility measurements. It was established that ultrasonically assisted hydrothermal treatment of amorphous zirconyl and titanyl gels results in significant rise of the rate of ZrO2 and TiO2 crystallization and promotes formation of thermodynamically stable monoclinic zirconia, but does not affect the microstructure and mean particles size of resulting nanopowders. Ultrasonic-hydrothermal processing of co-precipitated amorphous nickel, zinc and iron hydroxides favours formation of nanocrystalline ferrite powders with narrower particle size distribution.
Mesoporous nanosized TiO2 and Zn(x)Ti(1-x)O(2-x) solid solution having a Zn content below 10 mol % with a particles size between 13 and 17 nm are prepared by a template-free sol-gel method followed by high-temperature supercritical drying in 2-propanol. The structural, textural, and electronic properties of the obtained nanomaterials are methodically investigated by using XRD, SEM, TEM, ED, HREM, EDX, ICP-OES, N(2) adsorption-desorption, Raman spectroscopy, and diffuse reflectance UV-vis spectroscopy. It is shown that the proposed synthesis technique leads to the formation of a Zn(x)Ti(1-x)O(2-x) solid solution based on the anatase crystal structure rather than a two-phase sample. High-resolution electron microscopy and electron diffraction indicate that the distribution of zinc atoms over the anatase structure does not lead to a considerable deformation of the crystal structure.
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