879 resultados para Crystals--Thermal properties.


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ZnO thin films were prepared by the polymeric precursor method. The films were deposited on silicon substrates using the spin-coating technique, and were annealed at 330°C for 32h under pressure-assisted thermal annealing and under ambient pressure. Their structural and optical properties were characterized, and the phases formed were identified by X-ray diffraction. No secondary phase was detected. The ZnO thin films were also characterized by field-emission scanning electron microscopy, Fourier transform infrared spectroscopy, photoluminescence and ultraviolet emission intensity measurements. The effect of pressure on these thin films modifies the active defects that cause the recombination of deep level states located inside the band gap that emit yellow-green (575nm) and orange (645nm) photoluminescence. © 2012 John Wiley & Sons, Ltd.

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Glasses in the ternary system (70 - x)NaPO3-30WO 3-xBi2O3, with x = 0-30 mol %, were prepared by the conventional melt-quenching technique. X-ray diffraction (XRD) measurements were performed to confirm the noncrystalline nature of the samples. The influence of the Bi2O3 on the thermal, structural, and optical properties was investigated. Differential scanning calorimetry analysis showed that the glass transition temperature, Tg, increases from 405 to 440 C for 0 ≤ x ≤ 15 mol % and decreases to 417 C for x = 30 mol %. The thermal stability against devitrification decreases from 156 to 67 C with the increase of the Bi2O3 content. The structural modifications were studied by Raman scattering, showing a bismuth insertion into the phosphate chains by Bi-O-P linkage. Furthermore, up to 15 mol % of Bi 2O3 formation of BiO6 clusters is observed, associated with Bi-O-Bi linkage, resulting in a progressive break of the linear phosphate chains that leads to orthophosphate Q0 units. The linear refractive index, n0, was measured using the prism-coupler technique at 532, 633, and 1550 nm, whereas the nonlinear (NL) refractive index, n 2 was measured at 1064 nm using the Z-scan technique. Values of 1.58 ≤ n0 ≤ 1.88, n2 ≥ 10-15 cm 2/W and NL absorption coefficient, α2 ≤ 0.01 cm/GW, were determined. The linear and NL refractive indices increase with the increase of the Bi2O3 concentration. The large values of n0 and n2, as well as the very small α2, indicate that these materials have large potential for all-optical switching applications in the near-infrared. © 2012 American Chemical Society.

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Starch is arguably one of the most actively investigated biopolymer in the world. In this study, the native (untreated) cassava starch granules (Manihot esculenta, Crantz) were hydrolyzed by standard hydrochloric acid solution at different temperatures (30 °C and 50 °C) and the hydrolytic transformations were investigated by the following techniques: simultaneous thermogravimetry-differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), as well as non-contact atomic force microscopy (NC-AFM), X-ray diffraction (XRD) powder patterns, and rapid viscoamylographic analysis (RVA). After the treatment with hydrochloric acid at different temperatures, the thermal stability, a gradual loss of pasting properties (viscosity), alterations in the gelatinization enthalpy (ΔHgel), were observed. The use of NC-AFM and XRD allowed the observation of the surface morphology and topography of the starch granules and changes in crystallinity of the granules, respectively. © 2012 Elsevier B.V. All rights reserved.

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Lead molybdate (PbMoO4) crystals were synthesized by the co-precipitation method at room temperature and then processed in a conventional hydrothermal (CH) system at low temperature (70 °C for different times). These crystals were structurally characterized by X-ray diffraction (XRD), Rietveld refinement, micro-Raman (MR) and Fourier transformed infrared (FT-IR) spectroscopies. Field emission scanning electron microscopy images were employed to observe the shape and monitor the crystal growth process. The optical properties were investigated by ultraviolet-visible (UV-Vis) absorption and photoluminescence (PL) measurements. XRD patterns and MR spectra indicate that these crystals have a scheelite-type tetragonal structure. Rietveld refinement data possibilities the evaluation of distortions in the tetrahedral [MoO 4] clusters. MR and FT-IR spectra exhibited a high mode ν1(Ag) ascribed to symmetric stretching vibrations as well as a large absorption band with two modes ν3(Eu and Au) related to anti-symmetric stretching vibrations in [MoO 4] clusters. Growth mechanisms were proposed to explain the stages involved for the formation of octahedron-like PbMoO4 crystals. UV-Vis absorption spectra indicate a reduction in optical band gap with an increase in the CH processing time. PL properties of PbMoO4 crystals have been elucidated using a model based on distortions of tetrahedral [MoO4] clusters due to medium-range intrinsic defects and intermediary energy levels (deep and shallow holes) within the band gap. © 2012 Elsevier Ltd. All rights reserved.

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Lanthanide compounds of general formula [Ln2(2,5-tdc) 3(dmf)2(H2O)2] ·2dmf·H2O (Ln = Eu(III) (1), Tb(III) (2), Gd(III) (3) and Dy(III) (4), dmf = N,N′-dimethylformamide and 2,5-tdc2- = 2,5-thiophedicarboxylate anion) were synthesized and characterized by elemental analysis, X-ray powder diffraction patterns, thermogravimetric analysis and infrared spectroscopy. Phosphorescence data of Gd(III) complex showed that the triplet states (T1) of 2,5-tdc2- ligand have higher energy than the main emitting states of Eu(III), Tb(III) and Dy(III), indicating that 2,5-tdc2- ligand can act as intramolecular energy donor for these metal ions. An energy level diagram was used to establish the most relevant channels involved in the ligand-to-metal energy transfer. The high value of experimental intensity parameter Ω2 for the Eu(III) complex indicate that the europium ion is in a highly polarizable chemical environment. The emission quantum efficiency (η) of the 5D0 emitting level of Eu(III) was also determined. The complexes act as possible light conversion molecular devices (LCMDs). © 2013 Elsevier B.V. All rights reserved.

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In this article, the structural refinement, morphology and optical properties of barium strontium molybdate [(Ba1-x Sr x )MoO4 with x = 0, 0.25, 0.50, 0.75 and 1] crystals, synthesized by the co-precipitation (drop-by-drop) method, are reported. The crystals obtained were structurally characterized by X-ray diffraction (XRD), Rietveld refinement, and Fourier transform-Raman (FT-Raman) and Fourier transform-infrared (FT-IR) spectroscopies. The shapes of the crystals were observed by means of field-emission scanning electron microscopy (FE-SEM). The optical properties were investigated using ultraviolet-visible (UV-Vis) absorption spectroscopy and photoluminescence (PL) measurements. XRD patterns, Rietveld refinement, and FT-Raman and FT-IR spectra showed that all of the crystals are monophasic with a scheelite-type tetragonal structure. The refined lattice parameters and atomic positions were employed to model the [BaO8], [SrO8] and [MoO4] clusters in the tetragonal lattices. The FE-SEM images indicate that increased x content produces a decrease in the crystal size and modifications in the crystal shape. UV-Vis spectra indicated a decrease in the optical band gap with an increase in x in the (Ba1-x Sr x )MoO4 crystals. Finally, a decrease in the intensity of PL emission is apparent with an increase in x up to 0.75 in the (Ba1-x Sr x )MoO4 crystal lattice when excited by a wavelength of 350nm, probably associated with the degree of structural order-disorder. © 2013 International Union of Crystallography Printed in Singapore - all rights reserved.

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This study aimed to evaluate the effect of thermal treatment on the physical properties of juvenile and mature woods of Eucalyptus grandis. Boards were taken from 30-year-old E. grandis trees. The boards were thermally modified at 180 °C in the Laboratory of Wood Drying and Preservation at UNESP, Botucatu, Sao Paulo state, Brazil. The results showed that thermal modification caused: (1) decrease of 6.8% in the density at 0% equilibrium moisture content of mature wood; (2) significant decreases of 14.7% and 35.6% in the maximum volumetric swellings of juvenile and mature woods, respectively; (3) significant decreases of 13.7% and 21.3% in the equilibrium moisture content of juvenile and mature woods, respectively. The influence of thermal modification in juvenile wood was lower than in mature wood and caused greater uniformity in the physical variations between these types of wood in E. grandis.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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

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

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The main constituents of red mud produced in Aluminio city (S.P., Brazil) are iron, aluminum, and silicon oxides. It has been determined that the average particle diameter for this red mud is between 0.05 and 0.002 mm. It is observed that a decrease in the percentage of smaller particles occurs at temperatures greater than 400 degrees C. This observation corresponds with the thermal analysis and X-ray diffraction (XRD) data, which illustrate the phase transition of goethite to hematite. A 10% mass loss is observed in the thermal analysis patterns due to the hydroxide-oxide phase transitions of iron (primary phase transition) and aluminum (to a lesser extent). The disappearance and appearance of the different phases of iron and aluminum confirms the decomposition reactions proposed by the thermal analysis data. This Brazilian red mud has been classified as mesoporous at all temperatures except between 400 and 500 degrees C where the classification changes to micro/mesoporous.

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We report on the strong temperature-dependent thermal expansion, alpha(D), in CdS quantum dots (QDs) embedded in a glass template. We have performed a systematic study by using the temperature-dependent first-order Raman spectra, in CdS bulk and in dot samples, in order to assess the size dependence of alpha(D), and where the role of the compressive strain provoked by the glass host matrix on the dot response is discussed. We report the Gruneisen mode parameters and the anharmonic coupling constants for small CdS dots with mean radius R similar to 2.0 nm. We found that gamma parameters change, with respect to the bulk CdS, in a range between 20 and 50%, while the anharmonicity contribution from two-phonon decay channel becomes the most important process to the temperature-shift properties.

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Vanadium oxide nanotubes (NTs) were synthesized by the sol-gel method followed by a long-term hydrothermal treatment. The obtained nanotubes have a multiwall structure, and 70% of vanadium ions are in the V4+ state. This percentage was derived by evaluating three components of the magnetic susceptibility; namely, (i) the paramagnetic Curie-Weiss behavior, (ii) antiferromagnetic dimers, and (iii) magnetic trimers. The as-made NTs were annealed in situ in the cavity of the electron paramagnetic resonance (EPR) spectrometer. The line shape changes irreversibly at 390 K, and the EPR susceptibility presents an anomaly at 425 K. These changes are interpreted as a partial oxidation of the V4+ ions and consequently a decrease in the concentration of the magnetic species. The quantification of the V4+ ions of the annealed NTs reveals a diminution to 39% of V4+, a weakening of the Curie-Weiss and antiferromagnetic dimers contributions, and the suppression of magnetic trimers. Vibrational studies confirm the decrease of V4+ amount. (C) 2012 American Institute of Physics. [http://dx.doi.org/10.1063/1.4749417]

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Barium praseodymium tungstate (Ba1-xPr2x/3)WO4 crystals with (x = 0, 0.01, and 0.02) were prepared by the coprecipitation method. These crystals were structurally characterized by X-ray diffraction (XRD), Rietveld refinements, Fourier-transform Raman (FT-Raman) and Fourier-transform infrared (FT-IR) spectroscopies. The shape and size of these crystals were observed by field emission scanning electron microcopy (FE-SEM). Their optical properties were investigated by ultraviolet visible (UV-vis) absorption and photoluminescence (PL) measurements. Moreover, we have studied the photocatalytic (PC) activity of crystals for degradation of rhodamine B (RhB) dye. XRD patterns, Rietveld refinements data, FT-Raman and FT-IR spectroscopies indicate that all crystals exhibit a tetragonal structure without deleterious phases. FT-Raman spectra exhibited 13 Raman-active modes in a range from 50 to 1000 cm(-1), while FT-IR spectra have 8 infrared active modes in a range from 200 to 1050 cm(-1). FE-SEM images showed different shapes (bonbon-, spindle-, rice-and flake-like) as well as a reduction in the crystal size with an increase in Pr3+ ions. A possible growth process was proposed for these crystals. UV-vis absorption measurements revealed a decrease in optical band gap values with an increase of Pr3+ into the matrix. An intense green PL emission was noted for (Ba1-xPr2x/3)WO4 crystals (x = 0), while crystals with (x = 0.01 and 0.02) produced a reduction in the wide band PL emission and the narrow band PL emission which is related to f-f transitions from Pr3+ ions. High photocatalytic efficiency was verified for the bonbon-like BaWO4 crystals as a catalyst in the degradation of the RhB dye after 25 min under UV-light. Finally, we discuss possible mechanisms for PL and PC properties of these crystals.