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.

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.