933 resultados para in surfo crystallization
Resumo:
Nonisothermal and isothermal crystallization kinetics of an aromatic thermoplastic polyimide derived from 3,3',4,4'-oxydiphthalic dianhydride and 4,4'-oxydianiline have been investigated by means of differential scanning calorimetry (DSC) and wide-angle X-ray diffraction. The results for nonisothermal crystallization study showed that a weak melting peak appeared during the first heating process, whereas no crystallization peak appeared in the DSC curve during the subsequent cooling process. On the other hand, the study for the isothermal crystallization in the temperature range of 260-330 degrees C showed that a new exothermic peak appeared at lower temperature for the samples crystallized for 100 min at 300 degrees C.
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Protein electrochemistry affords a direct method to study the biological electron transfer processes. However, supplying a biocompatible environment to maintain the native state of protein is all-important and challengeable. Here, we chose vaterite, one of the crystalline polymorphs of calcium carbonate, with highly porous nature and large specific surface area, which was doped with phospholipids, as the matrix to immobilize horseradish peroxidase (HRP). The integrity of HRP was kept during the simple immobilization procedure. By virtue of this organic/inorganic complex matrix, the direct electrochemistry of HRP was realized, and the activity of HRP for catalyzing reduction of O-2 and H2O2 was preserved.
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The morphology of a H-shaped block copolymer (poly(ethylene glycol) backbone and polystyrene branches (PS)(2)PEG(PS)(2)) in a thin film has been investigated. A peculiar square lamella that has a phase-separated microdomain at its surface is obtained after spin coating. The experimental temperature plays a critical role in the lamellar formation. The copolymer first self-assembles into square lamellar micelles with an incomplete crystalline core due to the crystallizability of PEG.
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We demonstrate a strikingly novel morphology of high-density polyethylene (HDPE) crystal obtained upon melt crystallization of spin-coated thin film. This crystal gives windmill-like morphology which contains a number of petals. A detailed inspection on this morphology reveals that each petal is actually composed of terrace-stacked PE lamellae, in which the polymer chains within crystallographic a-c planes adopt similar to 45 degrees tilting around b-axis. The surrounding domains associated with a petal of the windmill composed of twisted lamellar overgrowths with an identical orientation of their long axis, which is the crystallographic b-axis shared by the petal and its corresponding twisted lamellar overgrowths.
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The multiphase morphology of high impact polypropylene (hiPP), which is a reactor blend of polypropylene (PP) with ethylene-propylene copolymer, was investigated by transmission electron microscopy, selected area electron diffraction, atomic force microscopy, and field-emission scanning electron microscopy techniques in conjunction with an analysis of the hiPP composition and chain structure based on solvent fractionation, C-13-NMR, and differential scanning calorimetry measurements.
Resumo:
Banded spherulite patterns are simulated in three dimensions by means of a Coupled Logistic map lattice model. The patterns obtained by numerical calculation are consistent with those in experiments. The simulation results also indicate that the hand spacing is decreased with the increase of parameter mu in the Logistic map and increased with the increase of the coupling parameter e for cube lattices, and increased with the increase of the thickness of the lattice for polymer film, which is quite similar to the results in some experiments. Spiral pattern in three dimensions is also shown in this paper, which helps us understand the form of banded spherulite in polymers.
Resumo:
The substantial crystallization suppression of poly(3-hexylthiophene) (P3HT) in the untreated P3HT:C60 composite film prepared from o-dichlorobenzene (ODCB) solution has been revealed. Besides, the effective conjugation length of P3HT in this composite has been nearly maintained to that in the solution. The different crystallization behaviors of P3HT in its composites with C60 and [6,6]-phenyl C-61 butyric acid methyl ester (PCBM) are mainly attributed to the relative solubility of C60 and PCBM with respect to P3HT in ODCB. The solution to overcome this disadvantage of chain conformation and crystallinity of P3HT in the composite with C60 is thus proposed and finalized by resorting to the addition of low volatile solvent with much higher solubility of C60 than P3HT into the main solvent used, so as P3HT can crystallize before C60 forms crystallites in the solution. The feasibility of this approach has been proven by the improved efficiency of devices based on composites of P3HT and the low cost C60 without resorting to post-treatments.
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Syndiotactic polystyrene (sPS) nanorods with different diameters have been prepared by using anodic aluminum oxide templates, and the orientation of the sPS crystals in the nanorods has been investigated by FT-IR spectroscopy. It is found that the c axis of the beta' crystals preferentially oriented perpendicular to the axis of the nanorod, and the degree of orientation is lower as the diameter of the nanorod decreases. This unexpected result is attributed to nuclei formed at the surface of the nanopores and their subsequent growth, in addition to the preferential growth compatible with the pore direction by the nuclei formed in the bulk film and in the nanorods.
Resumo:
Enhancing the stability of plasticized poly(L-lactic acid) (PLLA) with poly (ethylene glycol) (PEG) is necessary for its practical application. In this study, plasticized PLLA (PLLA/PEG 80/20 wt/wt) was crosslinked under I-ray (Co-60) in the presence of triallyl isocyanurate (TALC) as crosslinking agent. FTIR analysis revealed that PLLA, PEG, and TALC formed a cocrosslinking structure. Crystallization behavior and mechanical properties of the crosslinked plasticized PLLA were investigated by differential scanning calorimetry (DSC), wide-angle X-ray diffraction (WAXD), scanning electron microscopy (SEM), and tensile tests. Experimental results indicated that the crystallization behaviors of both PEG and PLLA in the blends were restrained after irradiation. The melting peak of PEG in the crystallized samples disappeared at a low irradiation doses about 10 kGy. Although PLLA still owned the behavior of crystallize, its cold crystallization temperature and glass transition temperature shifted to higher temperature. Mechanical properties of the plasticized PLLA were strengthened through crosslinking. Both yield strength and elastic modulus of the samples increased after crosslinking.
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A notable amount of PP beta-crystal (30%, by X-ray diffraction pattern) has been found in the PP samples as polymerized at normal static isothermal crystallization conditions without using any extra nucleating agents. Existence of catalyst residues in the sample is decisive, which slows down the crystallization rate facilitating the formation of beta-form spherulites. Comparatively, high molecular weight PP favors the formation of beta-form spherulites, deducting from no beta-crystal detected in the degraded samples. Finally, high isotacticity is also required for obtaining qualitative beta-form spherulites, demonstrated by increased beta-crystal content after removal of weak crystalline fraction of the sample.
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Rhythmic growth of ring-banded spherulites in blends of liquid crystalline methoxy-poly(aryl ether ketone) (M-PAEK) and poly(aryl ether ether ketone) (PEEK) has been investigated by means of differential scanning calorimetry (DSC), polarized light microscopy (PLM), and scanning electron microscopy (SEM) techniques. The measurements reveal that the formation of the rhythmically grown ring-banded spherulites in the M-PAEK/PEEK blends is strongly dependent on the blend composition. In the M.-PAEK-rich blends, upon cooling, an unusual ring-banded spherulite is formed, which is ascribed to structural discontinuity caused by a rhythmic radial growth. For the 50:50 M-PAEK/PEEK blend, ring-banded spherulites and individual PEEK spherulites coexist in the system. In the blends with PEEK as the predominant component, M-PAEK is rejected into the boundary of PEEK spherulites. The cooling rate and crystallization temperature have great effect on the phase behavior, especially the ring-banded spherulite formation in the blends. In addition, the effects of M-PAEK phase transition rate and phase separation rate on banded spherulite formation is discussed.
Resumo:
Syndiotactic 1,2-polybutadiene/organoclay nanocomposites were prepared and characterized by thermogravimetry analysis (TGA), X-ray diffraction (XRD), polarized optical microscopy (POM), and differential scanning calorimetry (DSC), respectively. The XRD shows that exfoliated nanocomposites are formed dominantly at lower clay concentrations (less than 2%), at higher clay contents intercalated nanocomposites dominate. At the same time, the XRD indicates that the crystal structures of sPB formed in the sPB/organoclay nanocomposites do not vary, only the relative intensity of the peaks corresponding to (0 1 0) and (2 0 0)/(1 1 0) crystal planes, respectively, varies. The DSC and POM indicate that organoclay layers can improve cooling crystallization temperature, crystallization rate and reducing the spherulite sizes of sPB. TGA shows that under argon flow the nanocomposites exhibit slight decrease of thermal stability, while under oxygen flow the resistance of oxidation and thermal stability of sPB/organoclay nanocomposites were significantly improved relative to pristine sPB. The primary and secondary crystallization for pristine sPB and sPB/organoclay (2%) nanocomposites were analyzed and compared based on different approaches.
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Nanocomposites based on poly(iminosebacoyl imino-decamethylene) (PA1010) and multiwall carbon nanotubes (MWNTs) were successfully prepared by melt blending technique. environmental scanning electron microscope micrographs of the fracture surfaces showed that not only is there an evenly dispersion of MWNTs throughout the PA1010 matrix but also a strongly interfacial adhesion with the matrix. The combined effect of more defects on MWNTs and low temperature buckling fracture is mainly responsible for the broken tubes. Differential scanning calorimeter results showed that the MWNTs acted as a nucleation agent and increased the crystallization rate and decreased crystallite size. In the linear region, rheological measurements showed a distinct change in the frequency dependence of storage modulus, loss modulus, and complex viscosity particularly at low frequencies. We conclude that the rheological percolation threshold might occur when the content of MWNTs is over 2 wt% in the composites.