227 resultados para Crystallization and thermal analysis


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Lanthanum, zirconate (La2Zr2O7, LZ) coatings were prepared under four different deposition conditions by electron beam-physical vapor deposition (EB-PVD). The composition, crystal structure, surface and cross-sectional morphology, cyclic oxidation behavior of these coatings were studied. Elemental analysis indicates that the coating composition has partially deviated from the stoichiometry of pyrochlore, and the existence of excess La2O3 is also observed. The deviation could be reduced by properly controlling the electron beam current or by changing the ingot composition.

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The measured results of thermal analysis depend on experimental conditions. The international and national organizations have constituted a series of methods to characterize the physical and chemical properties for substances. The applications to physical transition, chemical reaction, and characteristic parameters of substances are given in the article as examples.

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Plasticized poly(L-lactide)-silica nanocomposite materials have been successfully synthesized by sol-gel process. The resultant nanocomposites were characterized by infrared spectra (IR), X-ray diffraction (XRD), thermogravimetry (TG), Tensile testing and scanning electron microscope (SEM). IR measurements show that vibration of C-O-C group is confined by silica network. Also the crystallization of poly (L-lactide) is partly confined by silica network. The presence of even small amount of silica largely improves the tensile strength of the samples, TGA results reveal that the thermal stability of samples is improved with silica loading.

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In this paper, melt blends of poly(propylene carbonate) (PPC) with poly(butylene succinate) (PBS) were characterized by dynamic mechanical analysis (DMA), differential scanning calorimetry (DSC), tensile testing, wide-angle X-ray diffraction (WAXD), polarized optical microscopy and thermogravimetric analysis (TGA). The results indicated that the glass transition temperature of PPC in the 90/10 PPC/PBS blend was decreased by about 11 K comparing with that of pure PPC. The presence of 10% PBS was partially miscible with PPC. The 90/10 PPC/PBS blend had better impact and tensile strength than those of the other PPC/PBS blends. The glass transition temperature of PPC in the 80/20, 70/30, and 60/40 PPC/PBS blends was improved by about 4.9 K, 4.2 K, and 13 K comparing with that of pure PPC, respectively; which indicated the immiscibility between PPC and PBS. The DSC results indicated that the crystallization of PBS became more difficult when the PPC content increased. The matrix of PPC hindered the crystallization process of PBS. While the content of PBS was above 20%, significant crystallization-induced phase separation was observed by polarized optical microscopy. It was found from the WAXD analysis that the crystal structure of PBS did not change, and the degree of crystallinity increased with increasing PBS content in the PPC/PBS blends.

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Notch Izod impact strength of poly(propylene) (PP)/glass bead blends was studied as a function of temperature. The results indicated that the toughness for various blends could undergo a brittle-ductile transition (BDT) with increasing temperature. The BDT temperature (T-BD) decreased with increasing glass bead content. Introducing the interparticle distance (ID) concept into the study, it was found that the critical interparticle distance (IDc) reduced with increasing test temperature correspondingly. The static tensile tests showed that the Young's modulus of the blends decreased slightly first and thereafter increased with increasing glass bead content. However, the yield stress decreased considerably with the increase in glass bead content. Dynamic mechanical analysis (DMA) measurements revealed that the heat-deflection temperature of the PP could be much improved by the incorporation of glass beads. Moreover, the glass transition temperature (T-g) increased obviously with increasing glass beads content. Differential scanning calorimetry (DSC) results implied that the addition of glass beads could change the crystallinity as well as the melting temperature of the PP slightly.

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The mechanical and thermal properties of glass bead-filled nylon-6 were studied by dynamic mechanical analysis (DMA), tensile testing, Izod impact, thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC) tests. DMA results showed that the incorporation of glass beads could lead to a substantial increase of the glass-transition temperature (T-g) of the blend, indicating that there existed strong interaction between glass beads and the nylon-6 matrix. Results of further calculation revealed that the average interaction between glass beads and the nylon-6 matrix deceased with increasing glass bead content as a result of the coalescence of glass beads. This conclusion was supported by SEM observations. Impact testing revealed that the notch Izod impact strength of nylon-6/glass bead blends substantially decreased with increasing glass bead content. Moreover, static tensile measurements implied that the Young's modulus of the nylon-6/glass bead blends increased considerably, whereas the tensile strength clearly decreased with increasing glass bead content.

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A novel 3D supramolecular assembly constructed from decavanadate and caffeine building blocks, (NH4)(2)(C8H10N4O2)(4)[H4V10O28].2H(2)O (1), has been synthesized in aqueous solution and characterized by elemental analysis, IR, H-1 NMR, V-51 NMR, TG-DTA, and single crystal X-Ray diffraction. The compound 1 crystallizes in monoclinic system, space group P2(1)/n, a = 15.801(1) Angstrom, b = 12.914(1) Angstrom, c = 15.913(2) Angstrom, beta = 113.55degrees, V = 2976.4 (5) Angstrom(3), Z = 2, R = 0.0498 with 6818 reflections. Water molecules, ammonium ions, and caffeine act as "cement" linking the polyanions into 1D chain along the c-axis by hydrogen bonding. In compound 1, extensive hydrogen-bond contacts and strong pi-pi interactions lead to an ordered 3D supramolecular framework. TG-DTA curves indicate that the weight loss of the complex can be divided into three stages.

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The crystallization and melting behavior of poly(beta-hydroxybutyrate-co-beta-hydroxyvalerate) (PHBV) and a 30/70 (w/w) PHBV/poly(propylene carbonate) (PPC) blend was investigated with differential scanning calorimetry (DSC) and Fourier transform infrared (FTIR). The transesterification reaction between PHBV and PPC was detected in the melt-blending process. The interaction between the two macromolecules was confirmed by means of FTIR analysis. During the crystallization process from the melt, the crystallization temperature of the PHBV/PPC blend decreased about 8 degreesC, the melting temperature was depressed by 4 degreesC, and the degree of crystallinity of PHBV in the blend decreased about 9.4%; this was calculated through a comparison of the DSC heating traces for the blend and pure PHBV. These results indicated that imperfect crystals of formed, crystallization was inhibited, and the crystallization ability of PHBV was weakened in the blend. The equilibrium melting temperatures of PHBV and the 30/70 PHBV/PPC blend isothermally crystallized were 187.1 and 179 degreesC, respectively.

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Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) was irradiated by Co-60 gamma-rays (doses of 50, 100 and 200kGy) under vacuum. The thermal analysis of control and irradiated PHBV, under vacuum was carried out by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The tensile properties of control and irradiated PHBV were examined by using an Instron tensile testing machine. In the thermal degradation of control and irradiated PHBV, a one-step weight loss was observed. The derivative thermogravimetric curves of control and irradiated PHBV confirmed only one weight-loss step change. The onset degradation temperature (T-o) and the temperature of maximum weight-loss rate (T-p) of control and irradiated PHBV were in line with the heating rate (degreesC min(-1)). T-o and T-p of PHBV decreased with increasing radiation dose at the same heating rate. The DSC results showed that Co-60 gamma-radiation significantly affected the thermal properties of PHBV. With increasing radiation dose, the melting temperature (T-m) of PHBV shifted to a lower value, due to the decrease in crystal size. The tensile strength and fracture strain of the irradiated PHBV decreased, hence indicating an increased brittleness.

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The effects of three triblock copolymers of poly [styrene-b-(ethylene-co-butylene)-b-styrene] (SEBS) of different molecular weight (MW) on the morphology, tensile strength and thermal behavior of isotactic polypropylene/syndiotactic polystyrene (iPP/sPS, 80/20) blend are investigated. Morphology observation shows that both the medium MW and the lower MW SEBS are more effective than the higher MW SEBS in compatibilizing the blends. Tensile tests revels both the medium and low MW compatibilizer lead to a significant improvement in tensile strength, while the higher MW compatibilizer is efficient in increasing the elongation at break of the blends. The localization of compatibilizers in the blends is observed by mean of SEM and the correlation between the distribution of the compatibilizers and mechanical properties of the blends is evaluated. The mechanical properties of the iPP/sPS blends depend on not only the interfacial activity of the compatibilizers but also the distribution of the compatibilizer in the blend. Addition of the compatibilizers to the blend causes a remarkable decrease in the magnitude of the crystallization peak of sPS at its usual T-c. Vicat softening points demonstrate that the heat resistance of iPP/sPS blend is much higher than that of the pure iPP.

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Intermolecular hydrogen bonds, miscibility, crystallization and thermal stability of the blends of biodegradable poly(3-hydroxybutyrate) (PHB), poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) [P(3HB-3HHx)] with 4,4-dihydroxydiphenylpropane (DOH2) were investigated by FTIR, C-13 Solid state NMR, DSC, WAXD and TGA. Intermolecular hydrogen bonds were found in both blend systems, which resulted from the carbonyl groups in the amorphous phase of both polyesters and the hydroxyl groups of DOH2. The intermolecular interaction between P(3HB-3HHx) and DOH2 is weaker than that between PHB and DOH2 owing to the steric hindrance of longer 3HHx side chains. Because of the effect of the hydrogen bonds, the chain mobility of both PHB and P(3HB-3HHx) components was limited after blending with DOH2 molecules. Single glass transition temperature depending on the composition was observed in all blends, indicating that those blends were miscible in the melt. The addition of DOH2 suppressed the crystallization of PHB and P(3HB-3HHx) components. Moreover, the crystallinity of PHB and P(3HB-3HHx) components also decreased with increasing DOH2 content in the blends.

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Supported nickel catalyst (Ni-Cat) was used as a catalyst to improve the flame retarclancy of intumescent flame-retardants (IFR) systems based on ammonium polyphosphate and pentaerythritol (PETOL) in polypropylene (PP) matrix. Limited oxygen index (LOI), UL-94 rating, and thermogravimetric analysis were used to characterize the flame retardancy and thermal stability of the PP systems, and field emission scanning electron microscopy (FE-SEM) and Fourier transformed infrared spectroscopy (FTIR) were used to analyze the microstructure and composition of the chars formed during measuring LOI value and after combustion at 800 degrees C. The catalytic effect of NiCat was shown in an increase of LOI, a change in the char microstructure, and improvement of the thermal stability in the PP systems, which result from the synergistic effect of Ni-Cat and IFR. The results from FE-SEM and FTIR spectra of the char can explain how this synergistic effect happened.

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Nonisothermal crystallization and melting behavior of poly(3-hydroxybutyrate) (PHB) and maleated PHB were investigated by differential scanning calorimetry using various cooling rates. The results show that the crystallization behavior of maleated PHB from the melt greatly depends on cooling rates and its degree of grafting. With the increase in cooling rate, the crystallization process for PHB and maleated PHB begins at lower temperature. For maleated PHB, the introduction of maleic anhydride group hinders its crystallization, causing crystallization and nucleation rates to decrease, and crystallite size distribution becomes wider. The Avrami analysis, modified by Jeziorny, was used to describe the nonisothermal crystallization of PHB and maleated PHB. Double melting peaks for maleated PHB were observed, which was caused by recrystallization during the heating process.

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This paper studies the radiation properties of the immiscible blend of nylon1010 and HIPS. The gel fraction increased with increasing radiation dose. The network was found mostly in nylon1010, the networks were also found in both nylon1010 and HIPS when the dose reaches 0.85 MGy or more. We used the Charleby-Pinner equation and the modified Zhang-Sun-Qian equation to simulate the relationship with the dose and the sol fraction. The latter equation fits well with these polymer blends and the relationship used by it showed better linearity than the one by the Charleby-Pinner equation. We also studied the conditions of formation of the network by the mathematical expectation theorem for the binary system. Thermal properties of polymer blend were observed by DSC curves. The crystallization temperature decreases with increasing dose because the cross-linking reaction inhibited the crystallization procession and destroyed the crystals. The melting temperature also reduced with increasing radiation dose. The dual melting peak gradually shifted to single peak and the high melting peak disappeared at high radiation dose. However, the radiation-induced crystallization was observed by the heat of fusion increasing at low radiation dose. On the other hand, the crystal will be damaged by radiation. A similar conclusion may be drawn by the DSC traces when the polymer blends were crystallized. When the radiation dose increases, the heat of fusion reduces dramatically and so does the heat of crystallization. (C) 1999 Elsevier Science Ltd. All rights reserved.

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The crystallization and melting behavior of mellocene-catalized branched and linear polyethylenes of low molecular weight was studied. It was found that the crystalline lattice of branched polyethylene is larger than that of linear polyethylene because of the existence of branched chains. The melting behavior of branched polyethylene is similar to that of linear polyethylene since the branched chains can not enter the lattice. However, the crystalline behavior of low molecular weight branched polyethylene is the same as that of high molecular weight linear polyethylene, but different with that of low molecular weigh linear polyethylene. Kinetics theory analysis evidenced that the transition temperature of growth regime of the branched polyethylene is about 20 degreesC lower than that of linear polyethylene with the same molecular weight. It may be attributed to the existence of short branched chains.