Hydrothermal synthesis and characterization of nanorods of various titanates and titanium dioxide.

The formation process of titania based nanorods during hydrothermal synthesis starting from an amorphous TiO2.nH2O gel has been investigated. Sodium tri-titanate (Na2Ti3O7) particles with a rodlike morphology were prepared by a simple hydrothermal process in the presence of a concentrated NaOH aqueous solution. The ion exchange reaction of the synthesized Na2Ti3O7 nanorods with HCl under ultrasonic treatment promotes a complete sodium substitution and the formation of H2Ti3O7 nanorods. Low-temperature annealing of the as-produced nanorods of Na2Ti3O7 and H2Ti3O7 leads to a loss of the layered crystal structure and the formation of nanorods of condensed framework phases-sodium hexa-titanate (Na2Ti6O13) and metastable TiO2-B phases, respectively. These transformations proceed without a significant change in particle morphology. The nanostructures were investigated by scanning electron microscopy (SEM), powder X-ray diffraction (XRD), the Brunauer-Emmett-Teller (BET) method, thermogravimetric analysis (TGA), and Raman spectroscopy. The structural defects of the synthesized nanorods were investigated by high-resolution electron microscopy. The presence of planar defects can be attributed to the exfoliation of the zigzag ribbon layers into two-dimensional titanates as well as to the condensation of the layers of TiO6 octahedra into three-dimensional frameworks.

Ultrasonically assisted hydrothermal synthesis of nanocrystalline ZrO2, TiO2, NiFe2O4 and Ni0.5Zn0.5Fe2O4 powders.

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.

Structural, textural, and electronic properties of a nanosized mesoporous ZnxTi1-xO2-) solid solution prepared by a supercritical drying route.

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.