Paulo T. C. Freire

Temperature- and Pressure-Induced Phase Transitions in the Metal Formate Framework of [ND4][Zn(DCOO)3] and [NH4][Zn(HCOO)3]

Vibrational properties and the temperature-induced phase transition mechanism have been studied in [NH4][Zn(HCOO)3] and [ND4][Zn(DCOO)3] metal organic frameworks by variable-temperature dielectric, IR, and Raman measurements. DFT calculations allowed proposing the detailed assignment of vibrational modes to respective motions of atoms in the unit cell. Temperature-dependent studies reveal a very weak isotopic effect on the phase transition temperature and confirm that ordering of ammonium cations plays a major role in the mechanism of the phase transition. We also present high-pressure Raman scattering studies on [ND4][Zn(DCOO)3]. The results indicate the rigidity of the formate ions and strong compressibility of the ZnO6 octahedra. They also reveal the onset of a pressure-induced phase transition at about 1.1 GPa. This transition has strong first-order character, and it is associated with a large distortion of the metal formate framework. Our data indicate the presence of at least two nonequivalent formate ions in the high-pressure structure with very different C-D bonds. The decompression experiment shows that the transition is reversible.

Phonons in ferroelectric Bi2WO6: Raman and infrared spectra and lattice dynamics

Bi2WO6 ferroelectric single crystal was investigated by micro-Raman scattering and infrared spectroscopies. Symmetry of modes was established and the mode assignment was proposed.

Polarized Raman and Infrared Spectra of Taurine Crystals

Polarized Raman and infrared absorption spectra of taurine crystals were measured at room temperature and an assignment of normal modes was made. The usefulness of these assignments comes from the fact that some modes are related to important vibrations indicating the crystal form and stability of structure under different external conditions such as temperature and pressure.

Piezoelectric coefficients of l-arginine hydrochloride monohydrate obtained by X-ray multiple diffraction using synchrotron radiation

In this paper, a very useful development to improve the application of a method based on the multiple-diffraction technique to determine the piezoelectric coefficients of crystals is described. The idea is to choose any specific crystallographic direction (plane) through the secondary peaks in the Renninger scan instead of those directions related to the electric field by the piezoelectric tensor. For a set of multiple-diffraction planes, it is possible to obtain an equation system based on the ordinary peak position for each H secondary plane that appears in the Renninger scan. This useful development was successfully applied to the amino acid L-arginine hydrochloride monohydrate in order to provide the d 21 , d 22 , d 23 and d 25 piezoelectric coefficients by applying the electric field along the [010] crystallographic direction.

Raman evidence for pressure-induced formation of diamondene

Despite the advanced stage of diamond thin-film technology, with applications ranging from superconductivity to biosensing, the realization of a stable and atomically thick two-dimensional diamond material, named here as diamondene, is still forthcoming. Adding to the outstanding properties of its bulk and thin-film counterparts, diamondene is predicted to be a ferromagnetic semiconductor with spin polarized bands. Here, we provide spectroscopic evidence for the formation of diamondene by performing Raman spectroscopy of double-layer graphene under high pressure. The results are explained in terms of a breakdown in the Kohn anomaly associated with the finite size of the remaining graphene sites surrounded by the diamondene matrix. Ab initio calculations and molecular dynamics simulations are employed to clarify the mechanism of diamondene formation, which requires two or more layers of graphene subjected to high pressures in the presence of specific chemical groups such as hydroxyl groups or hydrogens.The synthesis of two-dimensional diamond is the ultimate goal of diamond thin-film technology. Here, the authors perform Raman spectroscopy of bilayer graphene under pressure, and obtain spectroscopic evidence of formation of diamondene, an atomically thin form of diamond.

Taninos hidrolisáveis em Bixa orellana L.

The aqueous material found in the fruits of Bixa Orellana L. was collected, dried, and characterized using several experimental techniques, namely phytochemical analysis in order to identify the biologically active constituents, Fourier transform infrared (FT-IR) spectroscopy for vibrational analysis, and X-ray powder diffraction in order to identify the presence of crystalline phases in the sample. The results showed that the aqueous material possesses high concentrations of hydrolyzable tannin. This result justifies the anti-inflammatory activity of this substance reported in other studies.

Raman and Neutron Scattering Study of Partially Deuterated L‐Alanine: Evidence of a Solid‐Solid Phase Transition

Raman and neutron experiments using specific isotope labeling were combined in order to study the dynamics and structure of L-alanine. Inelastic neutron and Raman scattering data of C(2)H(4)(ND(2))CO(2)D are discussed in relation to the doubling of the lattice parameter a observed by means of neutron powder diffraction in C(2)D(4) (NH(2))CO(2)H. The major changes accompanying the phase transition are found in the vibrational frequencies involving the torsional vibration tau(CO(2)(-)), which is clearly affected by the hydrogen bonds between the protons of the ammonium group and the oxygen atoms of the carboxylate group. At lower temperatures the rearrangement of identifiable hydrogen bonds induces changes in the bending vibration delta(ND(3)), confirming some orientational disorder.

Spectroscopic analysis and X-ray diffraction of trunk fossils from the Parnaíba Basin, Northeast Brazil.

The Parnaiba Sedimentary Basin is of the Paleozoic age and is located in Northeast Brazil, covering the states of Piauí, Maranhão and Tocantins and a small part of Ceará and Pará. In this work we applied several chemical analytical techniques to characterize trunk fossils found in the Parnaíba Sedimentary Basin, collected from four different sites, and discuss their fossilization process. We performed a study of the trunk fossils through X-ray diffraction, energy dispersive spectroscopy, infrared and Raman spectroscopy. The analysis allow us to identify the different compositions which are present in the trunk fossils: kaolinite (Al2Si2O5(OH)4), hematite (Fe2O3) and quartz (SiO2). Based in these results we were able to identify that the main fossilization mechanism of the trunk fossil was silicification. Furthermore, through Raman spectroscopy, we have observed the presence of carbonaceous materials in the Permian fossils, as evidenced by the D and G Raman bands. The relative intensities and bandwidths of the D and G bands indicated that the carbon has a low crystallinity. Thus, most of trunk fossils analyzed were permineralized and not petrified, because there is the presence of carbon that characterizes the partial decomposition of the organic matter in some trunks.

Caracterização espectroscópica de peixe do período cretáceo (Bacia do Araripe)

The study of fossils has made considerable progress over the last years as a result of the use of new experimental techniques. This paper describes the chemical composition of a fossilized fish of the Cretaceous period, from a 100 million-year-old, material originated from the Araripe Basin (northeastern Brazil). The chemical composition of the fossilized fish was analyzed by means of X-ray powder diffraction and Fourier transform infrared spectroscopy (FT-IR). The spectroscopic study has proven that the main substances found in the fossilized fish are CaCO3 and Ca5(PO4)3(OH). A tentative mechanism to explain the fossilization process is also given.

Synthesis of cubic Y zeolite using a pulsed microwave heating system

Cubic Y zeolite were successfully synthesized using microwave heating for 18 - 25 min, whereas 10 - 50 h are required by hydrothermal heating technique depending upon the lattice Si/Al ratio. To this end, we used a commercial microwave oven modified in order to provide pulsed microwave pumping on the synthesis mixtures. The obtained samples were analyzed by X-ray diffraction, BET surface area and infrared spectroscopy measurements. As a result, we verify that Y zeolite samples obtained from hydrogels containing low aluminum contents, present a good degree of crystallinity and then can be suitable for using in adsorption and catalysis experiments.