934 resultados para Differential scanning calorimeter (DSC)


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Chemorheology and corresponding models for an epoxy-terminated poly(phenylene ether ketone) (E-PEK) and 4,4'-diaminodiphenyl sulfone (DDS) system were investigated using a differential scanning calorimeter (DSC) and a cone-and-plate rheometer. For this system, the reported four-parameter chemorheological model and modified WLF chemorheological model can only be used in an isothermal or nonisothermal process, respectively. In order to predict the resin viscosity variation during a stepwise temperature cure cycle actually used, a new model based on the combination of the four-parameter model and the modified WLF model was developed. The combined model can predict the resin viscosity variation during a stepwise temperature cure cycle more accurately than the above two models. In order to simplify the establishment of this model, a new five-parameter chemorheological model was then developed. The parameters in this five-parameter model can be determined through very few rheology and DSC experiments. This model is practicable to describe the resin viscosity variation for isothermal, nonisothermal, or stepwise temperature cure cycles accurately. The five-parameter chemorheological model has also successfully been used in the E-PEK systems with two other curing agents, i.e., the diamine curing agent with the addition of a boron trifluride monoethylamine (BF3-MEA) accelerator and an anhydride curing agent (hexahydrophthalic acid anhydride). (C) 1997 John Wiley & Sons, Inc.

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Poly(ether diphenyl ether ketone) (PEDEK) synthesized by the nucleophilic route has the following chemical structure: [GRAPHICS] At some given temperatures for a given time isothermally crystallized PEDEK sample exhibits two endothermic peaks which are similar to PEEK and PEEKK The melting behavior of PEDEK crystallized from the glassy state is investigated through differential scanning calorimeter (DSC). We consider that the high-melting peak is related to the perfect crystals and the low-melting peak is associated with a few imperfect crystals. (C) 1997 John Wiley & Sons, Inc.

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Irradiated polyamide-1010 (PA1010) with and without heat treatment after gamma-ray irradiation was compared by wide angle x-ray diffraction (WAXD), differential scanning calorimeter (DSC) and the determination of gel fractions. The results indicate that post radiation effects due to post radiation crosslinking and scissions affect physical properties. Post radiation effects restrain the formation and perfection of the planes (010), and make the crystals imperfect. Post radiation effects change the crystalline structures of polyamide-1010.

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The heat capacity of nanostructured amorphous SiO2 (na-SiO2) has been measured by adiabatic calorimetric method over the temperature range 9-354 K. TG and differential scanning calorimeter (DSC) were also employed to determine the thermal stability. Glass transition temperature (T-g) for the two same grain sizes with different specific surface of naSiO(2) samples and one coarse-grained amorphous SiO2 (ca-SiO2) sample were determined to be 1377, 1397 and 1320 K, respectively. The low temperature experimental results show that there are significant heat capacity (C-P) enhancements among na-SiO2 samples and ca-SiO2. Entropy, enthalpy, Gibbs free energy and Debye temperature (theta (D)) were obtained based on the low temperature heat capacity measurement of na-SiO2. The Cp enhancements of na-SiO2 were discussed in terms of configurational and vibrational entropy. (C) 2001 Elsevier Science B.V. All rights reserved.

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Increasing amounts of plastic waste in the environment have become a problem of gigantic proportions. The case of linear low-density polyethylene (LLDPE) is especially significant as it is widely used for packaging and other applications. This synthetic polymer is normally not biodegradable until it is degraded into low molecular mass fragments that can be assimilated by microorganisms. Blends of nonbiodegradable polymers and biodegradable commercial polymers such as poly (vinyl alcohol) (PVA) can facilitate a reduction in the volume of plastic waste when they undergo partial degradation. Further, the remaining fragments stand a greater chance of undergoing biodegradation in a much shorter span of time. In this investigation, LLDPE was blended with different proportions of PVA (5–30%) in a torque rheometer. Mechanical, thermal, and biodegradation studies were carried out on the blends. The biodegradability of LLDPE/PVA blends has been studied in two environments: (1) in a culture medium containing Vibrio sp. and (2) soil environment, both over a period of 15 weeks. Blends exposed to culture medium degraded more than that exposed to soil environment. Changes in various properties of LLDPE/PVA blends before and after degradation were monitored using Fourier transform infrared spectroscopy, a differential scanning calorimeter (DSC) for crystallinity, and scanning electron microscope (SEM) for surface morphology among other things. Percentage crystallinity decreased as the PVA content increased and biodegradation resulted in an increase of crystallinity in LLDPE/PVA blends. The results prove that partial biodegradation of the blends has occurred holding promise for an eventual biodegradable product

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The aim of this work was to study the glass transition, the glass transition of the maximally freeze-concentrated fractions, the ice melting and the gelatinization phenomenon in dispersions of starch prepared using glycerol- water solutions. The starch concentration was maintained constant at 50 g cassava starch/100 g starch dispersions, but the concentration of the glycerol solutions was variable (C-g= 20, 40, 60, 80 and 100 mass/mass%). The phase transitions of these dispersions were studied by calorimetric methods, using a conventional differential scanning calorimeter (DSC) and a more sensitive equipment (micro-DSC). Apparently, in the glycerol diluted solutions (20 and 40%), the glycerol molecules interacted strongly with the glucose molecules of starch. While in the more concentrated glycerol domains (C-g> 40%), the behaviour was controlled by migration of water molecules from the starch granules, due to a hypertonic character of glycerol, which affected all phase transitions.

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The effect of the heat treatment on the corrosion behaviour of amorphous Al88Ni6La6 made by melt-spun has been investigated by electrochemical measurements. Heat treatment was carried out at 523 K and 673 K for 4 min and 15 min respectively. The evolution of the crystallization process after annealing was identified by differential scanning calorimeter (DSC) as well as X-ray diffraction. The XRD patterns show that the structure of samples heat-treated at higher temperature changes towards a crystal state. The results obtained from the polarization curves reveal that all Al88Ni6La6 alloys exhibit spontaneously passivated behaviour. Furthermore, it is noted that the partially crystallized alloy has the best corrosion resistance in comparison with as-spun amorphous and fully crystallized alloys, while the fully crystallized sample shows deterioration in the corrosion resistance.

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New plasticized polymer electrolytes were synthesized based on poly ethylene oxide (PEO), Poly (N,N-dimethylamino-ethyl-methacrylate) (PDMAEMA), LiN(CF3SO2)2 (LITFSI) as the salt and tetraethylene glycol dimethyl ether(tetraglyme) and EC + PC as plasticizers. The preparation and characterization of the polymer electrolytes were investigated as a function of temperature and various concentrations of LITFSI. Impedance spectroscopy and differential scanning calorimeter (DSC) were used to characterize the effects of various temperature, lithium salt concentration and two plasticizers on conductivity. The complex of PDMAEMA/PEO/LiTFSI/tetraglyme (S2) exhibits higher conductivity (4.74 × 10−4 S cm−1at 25 °C) than PDMAEMA/PEO/LiTFSI/EC + PC (S1).

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Solvent-free polymer electrolytes based on poly(vinyl alcohol) (PVA) and LiCF3SO3 have shown relatively high conductivities (10−8-10−4 S cm−1), with Arrhenius temperature dependence below the differential scanning calorimeter (DSC) glass transition temperature (343 K). This behaviour is in stark contrast to traditional polymer electrolytes in which the conductivity reflects VTF behaviour. 7Li nuclear magnetic resonance (NMR) spectroscopy has been employed to develop a better understanding of the conduction mechanism. Variable temperature NMR has indicated that, unlike traditional polymer electrolytes where the linewidth reaches a rigid lattice limit near Tg, the lithium linewidths show an exponential decrease with increasing temperature between 260 and 360 K. The rigid lattice limit appears to be below 260 K. Consequently, the mechanism for ion conduction appears to be decoupled from the main segmental motions of the PVA. Possible mechanisms include ion hopping, proton conduction or ionic motion assisted by secondary polymer relaxations.

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Wool fabrics, ultrasonically treated for different time durations, were analysed by Fourier transform infrared (FTIR), differential scanning calorimeter (DSC), and thermo-gravimetric analysis (TGA), in comparison with the wool without ultrasonic treatment. Fabric tensile and thermal properties were measured in addition to the fibre micro structure analysis. Wool protein chains in the macro fibrils were shown to be rearranged to a more regular and less flexible structure, as a result of the ultrasonically treated fabric. Prolonged ultrasonic treatment, however, significantly reduced both fabric tenacity and extensibility. Wool treated with ultrasonics was found to have less mass loss and a higher thermal degradation temperature than that of without ultrasonic treatment and prolonged treated. DSC analysis showed that while ultrasonic treatment has little effect on the fibre crystallinity, an appropriate treatment can provide wool with increased water absorption.

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The environmental impact caused by the disposal of non-biodegradable polymer packaging on the environment, as well as the high price and scarcity of oil, caused increase of searches in the area of biodegradable polymers from renewable resources were developed. The poly (lactic acid) (PLA) is a promising polymer in the market, with a large availability of raw material for the production of its monomer, as well as good processability. The aimed of this study was synthesis PLA by direct polycondesation of lactic acid, using the tool of experimental design (DOE) (central composite rotatable design (CCRD)) to optimize the conditions of synthesis. The polymer obtained was characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), viscosimetric analysis, differential scanning calorimeter (DSC) and size exclusion chromatography (SEC). The results confirmed the formation of a poly (lactic acid) semicrystalline in the syntheses performed. Through the central composite rotatable design was possible to optimize the crystallization temperature (Tc) and crystallinity degree (Xc). The crystallization temperature maximum was found for percentage of catalyst around the central point (0,3 (%W)) and values of time ranging from the central point (6h) to the upper level (+1) (8h). The crystallization temperature maximum was found for the total synthesis time of 4h (-1) and percentage of catalyst 0,1(W%) (-1). The results of size exclusion chromatography (SEC) showed higher molecular weights to 0,3 (W%) percent of catalyst and total time synthesis of 3,2h

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

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In this present work, barium ion was reacted with different ligands which are 5,7-dibromo, 5,7-dichloro, 7-iodo and 5-chloro-7-iodo-8-hydroxyquinoline, in acetone/ammonium hydroxide medium under constant stirring and the obtained compounds were as follows: (I) Ba[(C9H4ONBr2)(2)].1.5H(2)O; (II) Ba[(C9H4ONCl2)(OH)]. 1H(2)O; (III) Ba[(C9H5ONI)(2)]. 1H(2)O and (IV) Ba[(C9H4ONICl)(2)]. 5H(2)O, respectively. The compounds were characterized by elemental analysis, infrared absorption spectrum (IR), inductively coupled plasma spectrometry (ICP), simultaneous thermogravimetry-differential thermal analysis (TG-DTA) and differential scanning calorimeter (DSC).The final residue of the thermal decomposition was characterized as orthorhombic BaBr2 from (I); the intermediate residue, as a mixture of orthorhombic BaCO3 and BaCl2 and cubic BaO and the final residue, as a mixture of cubic and tetragonal BaO and orthorhombic BaCl2 (II); the intermediate residue, as orthorhombic BaCO3 and as a final residue, a mixture of cubic and tetragonal BaO from (III); and the intermediate residue, as a mixture of orthorhombic BaCO3 and BaCl2 and as a final residue, a mixture of cubic and tetragonal BaO and orthorhombic BaCl2 from (IV).

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