Polymeric precursor method to the synthesis of XWO(4) (X = Ca and Sr) thin films-Structural, microstructural and spectroscopic investigations

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Pressure-induced electrical and structural anomalies in Pb1-xCaxTiO3 thin films grown at various oxygen pressures by chemical solution route

Lead calcium titanate (Pb1-xCaxTiO3 or PCT) thin films have been thermally treated under different oxygen pressures, 10, 40 and 80 bar, by using the so-called chemical solution deposition method. The structural, morphological, dielectric and ferroelectric properties were characterized by x-ray diffraction, FT-infrared and Raman spectroscopy, atomic force microscopy and polarization-electric-field hysteresis loop measurements. By annealing at a controlled pressure of around 10 and 40 bar, well-crystallized PCT thin films were successfully prepared. For the sample submitted to 80 bar, the x-ray diffraction, Fourier transformed-infrared and Raman data indicated deviation from the tetragonal symmetry. The most interesting feature in the Raman spectra is the occurrence of intense vibrational modes at frequencies of around 747 and 820 cm(-1), whose presence depends strongly on the amount of the pyrochlore phase. In addition, the Raman spectrum indicates the presence of symmetry-breaking disorder, which would be expected for an amorphous (disorder) and mixed pyrochlore-perovskite phase. During the high-pressure annealing process, the crystallinity and the grain size of the annealed film decreased. This process effectively suppressed both the dielectric and ferroelectric behaviour. Ferroelectric hysteresis loop measurements performed on these PCT films exhibited a clear decrease in the remanent polarization with increasing oxygen pressure.

Síntese hidrotérmica e caracterização estrutural de titanatos nanotubulares para aplicação na captura do dióxido de carbono

Nanostructured materials have been spreading successfully over past years due its size and unusual properties, resulting in an exponential growth of research activities devoted to nanoscience and nanotechnology, which has stimulated the search for different methods to control main properties of nanomaterials and make them suitable for applications with high added value. In the late 90 s an alternative and low cost method was proposed from alkaline hydrothermal synthesis of nanotubes. Based on this context, the objective of this work was to prepare different materials based on TiO2 anatase using hydrothermal synthesis method proposed by Kasuga and submit them to an acid wash treatment, in order to check the structural behavior of final samples. They were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), adsorption/desorption of N2, thermal analysis (TG/DTA) and various spectroscopic methods such as absorption spectroscopy in the infrared (FT-IR), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). All the information of characterizations confirmed the complete conversion of anatase TiO2 in nanotubes titanates (TTNT). Observing the influence of acid washing treatment in titanates structure, it was concluded that the nanotubes are formed during heat treatment, the sample which was not subjected to this process also achieved a complete phase transformation, as showed in crystallography and morphology results, however the surface area of them practically doubled after the acid washing. By spectroscopy was performed a discussion about chemical composition of these titanates, obtaining relevant results. Finally, it was observed that the products obtained in this work are potential materials for various applications in adsorption, catalysis and photocatalysis, showing great promise in CO2 capture

Hydrothermal syntheses of ETS-10 like vanadosilicates using chiral organic molecules. Part I

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Electron microprobe and Raman spectroscopic investigation of monazite from chromitites of Cedrolina (Goias State, Brazil)

Monazite from chromitites of Cedrolina (Goias State, Brazil) was investigated by electron microprobe and Raman spectroscopy. Monazite has been rarely encountered in chromitites. In Brazil, it was previously reported from chromitites of the Campo Formoso layered intrusion. Comparison between the two occurrences indicates similar morphology and textural characteristics, but remarkable differences in chemical composition. In both cases, monazite occurs as irregular grains (up to 200 mu m) preferentially located in the chlorite-serpentine matrix of the chromitite, more rarely included in chromite. However, the monazite from Cedrolina is characterized by higher Ce/La ratio, and Pr, Nd, Th contents, compared with the monazite from Campo Formoso. The obtained Raman spectra are very similar in the two cases, suggesting that the compositional variation of monazites and the spectral resolution of the Raman do not allow a conclusive chemical analysis with Raman spectra. Textural evidence indicates that, in both occurrences, monazite precipitation did not take place at high temperature, concomitantly with the host chromitite. In the Campo Formoso chromitites, precipitation of monazite has been related with percolation of hydrothermal, aqueous and acid fluids emanating from a granite batholith. on the contrary, the Cedrolina monazite probably formed during one of the metamorphic events that affected the area in which the host chromitite occurs.

Spectroscopic studies on glassy Ni(II) and Co(II) polyphosphate coacervates

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Vibrational spectra of pilocarpine hydrochloride crystals

Pilocarpine is a natural substance with potential application in the treatment of several diseases. In this work Fourier Transform (FT)-Raman spectrum and the Fourier Transform infra red (FT-IR) spectrum of pilocarpine hydrochloride C11H17N2O2+.Cl- were investigated at 300 K. Vibrational wavenumber and wave vector have been predicted using density functional theory (B3LYP) calculations with the 6-31 G(d,p) basis set. A comparison with experiment allowed us to assign most of the normal modes of the crystal.

Comparative vibrational spectra of pilosine and epiisopilosine crystals

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Influência da adição de níquel na síntese do SrSnO3

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Resistividade do filme depositado via sol-gel e estado de oxidação do dopante Ce na matriz SnO2

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Local Er(III) environment in luminescent titanosilicates prepared from microporous precursors

The local environment of Er3+ ions in microporous titanosilicate ETS-10 and in synthetic narsarsukite and glassy materials obtained by calcination of ETS-10 has been investigated by EXAFS, Raman and photoluminescence spectroscopies. Er L-III-edge EXAFS studies of Er3+-doped ETS-10 support the view that the exchanged Er3+ ions reside close to the (negatively charged) TiO6 octahedra. In ETS-10, Er3+ is partially bonded to framework oxygen atoms and hydration water molecules. The Er...Ti distance (3.3 Angstrom) is similar to the Na...Ti distances (3.15-3.20 Angstrom) reported previously for Na-ETS-10. Although the exact location of the ErO6 units within the host structure of Er3+-doped synthetic narsarsukite is still an open question, it is most likely that Er3+ substitutes Ti4+ rather than Na+ ions. EXAFS spectroscopy indicates that no significant clustering of erbium atoms occurs in the titanosilicate samples studied. Evidence for the insertion of Er3+ ions in the framework of narsarsukite has been obtained by Raman spectroscopy. This is indicated by the increasing full-width at half-maximum (FWHM) of the 775 cm(-1) peak and the increasing intensity of the anatase peaks as the erbium content increases. In addition, as the narsarsukite Er3+ content increases a band at ca. 515 cm(-1) firstly broadens and subsequently a new peak appears at ca. 507 cm(-1).Er3+-doped narsarsukite exhibits a characteristic local vibrational frequency, (h) over bar omega ca. 330 cm(-1), with an electron-phonon coupling, g ca. 0.2, which constitutes additional evidence for framework Er3+ insertion. The number of lines in the infrared emission spectrum of synthetic narsarsukite indicates the presence of two optically-active erbium centres with very similar local environments and an average I-4(13/2) lifetime of 7.8 +/- 0.2 ms.

Layer-by-layer hybrid films of polyaniline and vanadium oxide

Supramolecular structures of polyaniline (PANI) and vanadium oxide (V2O5) have been assembled via the electrostatic layer-by-layer (LBL) technique. The films were characterized by vibrational analyses which indicated that the interactions between the two components lead to different properties in the films when compared to sol-gel films. of the neat compounds. In particular, using surface enhanced Raman scattering we were able to probe LBL film properties that depend on which material comprises the topmost layer.

Temperature-dependent Raman spectra of K0.2Na0.8NbO3 ceramics

We performed temperature-dependent Raman scattering studies on K0.2Na0.8NbO3 ceramics and compared the results with those for NaNbO3. The wavenumbers associated with NbO6 vibrations suggest the existence of two phase transitions, as occurs with pure NaNbO3 ceramics. Although the disorder on the Na/K site does not change either the room temperature phase of K0.2Na0.8NbO3 or the sequence of phase transitions compared with NaNbO3, it changes the temperature of the lowest phase transition and strongly modifies the temperature of the antiferroelectric --> new phase II phase transition. Additionally, the linewidth analysis shows that the orientational mechanism is the dominant contribution to linewidth, although the anharmonic contribution is increased, when compared with NaNbO3, owing to the random distribution of potassium in the sodium niobate matrix. Copyright (C) 2004 John Wiley Sons, Ltd.

The investigation of alpha -> beta phase transition in poly(vinylidene fluoride) (PVDF)

The phase transition from the non-polar a-phase to the polar beta-phase of poly(vinylidene fluoride) (PVDF) has been investigated using micro-Raman spectroscopy, which is advantageous for being a non-destructive technique. Films of alpha-PVDF were subjected to stretching under controlled rates and at 80 degrees C, the transition to beta-PVDF being monitored by the decrease in the Raman band at 794 cm(-1) characteristic of the a-phase, with the concomitant increase in the 839 cm(-1) band characteristic of the beta-phase. Poling with negative corona discharge was found to affect the alpha-PVDF morphology improving the Raman bands related to this crystalline phase. This effect is minimized for films stretched to higher ratios. Significantly, corona-induced effects could not be observed with the other experimental techniques, viz. X-ray diffraction and infrared spectroscopy.

Micro-Raman analysis of cubic GaN layers grown by MBE on (001) GaAs substrate

Cubic GaN layers are grown by molecular beam epitaxy on (001) GaAs substrates. Optical micrographs of the GaN epilayers intentionally grown at Ga excess reveal the existence of surface irregularities such as bright rectangular structures, dark dots surrounded by rectangles and dark dots without rectangles. Micro-Raman spectroscopy is used to study the structural properties of these inclusions and of the epilayers in greater detail. We conclude that the observed irregularities are the result of a melting process due to the existence of a liquid Ga phase on the growing surface.