Synthesis and characterization of ZnO nano and micro structures grown by low temperature spray pyrolysis and vapor transport.

In this work we present a systematic study of ZnO micro and nanostructures grown by spray pyrolysis (SP) and by physical vapour transport (PVT) on glass and c-sapphire substrates at low temperatures. Optimised growth conditions have allowed to obtain homogeneous ZnO nanolayers composed of quasi-spherical nanoparticles in the range 2 to 8 nm by spray pyrolysis, while by PVT the selected growth conditions allow to produce a wide variety of morphologies (tripods, grains, arrows and wires) of nano and microsize dimension. Grazing incidence X-ray diffraction, field emission scanning electron microscopy (FE-SEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED) and energy dispersive X-ray spectroscopy (EDX) were used as characterization techniques in the investigation of structural, morphological and compositional nature of these nanostructures in relation with the growth method.

Temperature dependent polarized Raman spectra of nonaaqualanthanoid (Pr) single crystal.

Polarized Raman spectral changes with respect to temperature were investigated for Pr(BrO3)3.9H2O single crystals. FTIR spectra of hydrated and deuterated analogues were also recorded and analysed. Temperature dependent Raman spectral variation have been explained with the help of the thermograms recorded for the crystal. Factor group analysis could propose the appearance of BrO3 ions at sites corresponding to C3v (4) and D3h (2). Analysis of the vibrational bands at room temperature confirms a distorted C3v symmetry for the BrO3 ion in the crystal. From the vibrations of water molecules, hydrogen bonds of varying strengths have also been identified in the crystal. The appearance upsilon1 mode of BrO3- anion at lower wavenumber region is attributed to the attachment of hydrogen atoms to the BrO3- anion. At high temperatures, structural rearrangement is taking place for both H2O molecule and BrO3 ions leading to the loss of water molecules and structural reorientation of bromate ions causing phase transition of the crystal at the temperature of 447 K.

Raman and FTIR spectra of [Cu(H2O)6](BrO3)2 and [Al(H2O)6](BrO3)3 x 3H2O.

Raman and FTIR spectra of [Cu(H2O)6](BrO3)2 and [Al(H2O)6](BrO3)3 x 3H2O are recorded and analyzed. The observed bands are assigned on the basis of BrO3- and H2O vibrations. Additional bands obtained in the region of v3 and v1 modes in [Cu(H2O)6](BrO3)2 are due to the lifting of degeneracy of v3 modes, since the BrO3- ion occupies a site of lower symmetry. The appearance v1 mode of BrO3- anion at a lower wavenumber (771 cm(-1)) is attributed to the attachment of hydrogen to the BrO3- anion. The presence of three inequivalent bromate groups in the [Al(H2O)6](BrO3)3 x 3H2O structure is confirmed. The lifting of degeneracy of v4 mode indicates that the symmetry of BrO3- anion is lowered in the above crystal from C3v to C1. The appearance of additional bands in the stretching and bonding mode regions of water indicates the presence of hydrogen bonds of different strengths in both the crystals. Temperature dependent Raman spectra of single crystal [Cu(H2O)6](BrO3)2 are recorded in the range 77-523 K for various temperatures. A small structural rearrangement takes place in BrO3- ion in the crystal at 391 K. Hydrogen bounds in the crystal are rearranging themselves leading to the loss of one water molecule at 485 K. This is preceded by the reorientation of BrO3- ions causing a phase transition at 447 K. Changes in intensities and wavenumbers of the bands and the narrowing down of the bands at 77 K are attributed to the settling down of protons into ordered positions in the crystal.