945 resultados para thermal and hydrothermal stability


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Supramolecular ionic networks based on highly delocalized dianions having (trifluoromethane-sulfonyl)imide, (propylsulfonyl)methanide and (cyano-propylsulfonyl)imide groups were developed and their physical properties were examined in detail. Most of the synthesized compounds were semi-crystalline possessing Tm values close to 100°C; however, amorphous networks were also obtained using aromatic asymmetric dianions. Rheological measurements in temperature sweep tests at a constant frequency confirmed two different behaviors: a fast melting close to the Tm for semi-crystalline materials and a thermoreversible network for liquid transition for the amorphous supramolecular ionic networks. It was found that the amorphous ionic networks showed significantly higher ionic conductivity (10-3 S cm-1 at 100°C) than the crystalline ionic networks (10-6 S cm-1) and previously reported amorphous citrate ionic networks (10-5 S cm-1). The supramolecular ionic networks containing hydrophobic (trifluoromethanesulfonyl)imide groups demonstrated improved water stability and higher thermal stability than the previously synthesized carboxylate ones. Noticeably, the obtained amorphous supramolecular ionic networks combine not only high ionic conductivity and thermal stability, but also self-healing properties into the same material.

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In the present work, electrospinnability as well as thermal, rheological, and morphological characteristics of low molecular weight hardwood organosolv lignin, as a potential precursor for carbon fiber, was investigated. Submicromter biobased fibers were electrospun from a wide range of polymer solutions with different ratios of organosolv lignin to polyacrylonitrile (PAN). Rheological studies were conducted by measuring viscosity, surface tension, and electrical conductivity of hybrid polymer solutions, and used to correlate electrospinning behavior of solutions with the morphology of the resultant electrospun composite fibers. Using scanning electron microscopy (SEM) images, the solutions that led to the formation of bead-free uniform fibers were found. Differential scanning calorimetry (DSC) analysis revealed that lignin-based fibers enjoy higher decomposition temperatures than that of pure PAN. Thermal stability of the lignin-based fibers was investigated by thermogravimetric analysis (TGA) indicating a high carbon yield of above 50% at 600 °C, which is highly crucial in the production of low-cost carbon fiber. It was also observed that organosolv lignin synergistically affects thermal decomposition of composite fibers. A significant lower activation energy was found for the pyrolysis of lignin-derived electrospun fibers compared to that of pure PAN.

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Cellulose nanowhiskers were prepared by sulfuric acid hydrolysis from coconut husk fibers which had previously been submitted to a delignification process. The effects of preparation conditions on the thermal and morphological behavior of the nanocrystals were investigated. Cellulose nanowhisker suspensions were characterized by Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), thermogravimetric analysis (TGA) and X-ray diffraction. Results showed that it was possible to obtain ultrathin cellulose nanowhiskers with diameters as low as 5 nm and aspect ratio of up to 60. A possible correlation between preparation conditions and particle size was not observed. Higher residual lignin content was found to increase thermal stability indicating that by controlling reaction conditions one can tailor the thermal properties of the nanowhiskers. Published by Elsevier Ltd.

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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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Synthesis, spectroscopic characterization and thermal analysis of the [Pd(dmba)(Cl)(iso)] (1), [Pd(dmba)(NCO)(iso)] (2), [Pd(dmba)(N(3))(iso)] (3) and [Pd(dmba)(Br)(iso)] (4) (dmba = N,N'-dimethylbenzylamine; iso = isonicotinamide) compounds are described in this work. The complexes were investigated by infrared spectroscopy (IR), differential thermal analysis (DTA) and thermogravimetry (TG) and the residues of the thermal decomposition were identified as Pd(o) by X-ray powder diffraction. The thermal stability order of the complexes varied as [Pd(dmba)(Cl)(iso)] (1) > [Pd(dmba)(Br)(iso)] (4) > [Pd(dmba)(NCO)(iso)] (2) > [Pd(dmba)(N(3))(iso)] (3).

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The dimeric compound [Pd(bzan)(mu-OOCCH3)](2) (1) (bzan=N-benzylideneaniline) reacts with KX, in methanol/acetone (2:1), affording the analogous dimeric pseudohalogen-bridged species [Pd(bzan)(mu-X)](2) [X=NCO(2), SCN(3), CN(4)]. The compounds were characterized by elemental analysis, infrared spectroscopy, NMR and thermogravimetric analysis. IR data for 2-4 showed bands typical of coordinated pseudohalogen ligands clearly indicating the occurrence of the exchange reaction. Their thermal behaviour was investigated and suggested that their stability is influenced by the bridging ligand. The thermal stability decreased in the order [Pd(bzan)(mu-CN)](2)>[Pd(bzan)(mu-SCN)](2)>[Pd(bzan)(mu-OOCCH3)](2)>[Pd(bzan)(mu-NCO)](2). X-ray results showed the formation of Pddegrees as final decomposition product.

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Synthesis, characterization, and thermal behavior of transition metal oxamates, M(NH(2)C(2)O(3))(2)center dot nH(2)O (M = Mn(II), Fe(II), Co(II), Ni(II), Cu(II), Zn(II)), as well as the thermal behavior of oxamic acid and its sodium salt (NaNH(2)C(2)O(3)) were investigated employing simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), experimental and theoretical infrared spectroscopy, TG-DSC coupled to FTIR, elemental analysis and complexometry. The results led to information about the composition, dehydration, thermal stability, thermal decomposition, as well as of the gaseous products evolved during the thermal decomposition of these compounds in dynamic air and N(2) atmospheres.

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Acrylic resins have been widely used due to their acceptable esthetics and desirable characteristics such as easy handling, good thermal conductivity, low permeability to oral fluids and color stability. Flexible resins were introduced on the market as an alternative to the use of conventional acrylic resins in the construction of complete and partial removable dentures. Although these resins present advantages in terms of esthetics and comfort, studies assessing chromatic and microhardness alterations of these materials are still scarce in the related literature. The aim of this study was to evaluate the chromatic and microhardness alterations of two commercial brands of flexible resins in comparison to the conventional resin Triplex when submitted to accelerated aging. The resins were manipulated according to manufacturers' instructions and inserted into a silicone matrix to obtain 21 specimens divided into 3 groups: Triplex, Ppflex and Valplast. Triplex presented the highest microhardness value (p < 0.05) for all the aging periods, which was significantly different from that of the other resins, followed by the values of Valplast and Ppflex. Comparison between the flexible resins (Ppflex and Valplast) revealed a statistically significant difference (p < 0.05) as regards color. The flexible resin Ppflex and the conventional resin Triplex presented no statistically significant difference (p < 0.05) as regards aging. The accelerated aging significantly increased the microhardness values of the resins, with the highest values being observed for Triplex. Valplast presented the greatest chromatic alteration after accelerated aging.

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Solid-state LnL3·1.25H2O compounds, where L is oxamate and Ln is light trivalent lanthanides, have been synthesized. Simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), experimental and theoretical infrared spectroscopy, TG-DSC coupled to FTIR, elemental analysis, complexometry, and X-ray powder diffractometry were used to characterize and to study the thermal behavior of these compounds. The results led to information about the composition, dehydration, thermal stability, thermal decomposition, and gaseous products evolved during the thermal decomposition of these compounds in dynamic air atmosphere. The dehydration occurs in a single step and through a slow process. The thermal decomposition of the anhydrous compounds occur in a single (Ce), two (Pr), and three (La, Nd to Gd) steps with the formation of the respective oxides, CeO2, Pr 6O11, and Ln2O3 (Ln = La, Nd to Gd). The theoretical and experimental spectroscopic study suggests that the carboxylate group and amide carbonyl group of oxamate are coordinate to the metals in a bidentate chelating mode. © 2012 Akadémiai Kiadó, Budapest, Hungary.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)