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Melting Peaks (melting + peak)
Selected AbstractsEffects of silver nanoparticles on the dynamic crystallization and physical properties of syndiotactic polypropyleneJOURNAL OF APPLIED POLYMER SCIENCE, Issue 5 2008Dong Wook Chae Abstract The effects of silver (Ag) nanoparticles on the physical properties of syndiotactic PP (sPP) were investigated concentrating on the isothermal melt crystallization behavior under shear. sPP with 5 wt % Ag nanoparticles presented higher crystallization temperature (Tc) and heat of crystallization (,Hc) than pure sPP. At 90°C, the Ag nanoparticles had little effect on the induction time of crystallization but a little increased the half-time (t1/2) for the crystallization. At 100°C, however, the induction time was decreased with increasing the Ag content and the t1/2 was decreased up to the Ag content of 0.5 wt %. DSC melting endotherms exhibited double melting peaks when crystallized at 90°C under shear but a single melting peak when crystallized at 100°C. The WAXD patterns exhibited that the presence of Ag nanoparticles did not produce any change in the crystal structure of sPP. The tensile strength of sPP is little changed up to the Ag content of 0.1 wt % but it was decreased with further addition. In addition, the introduction of less than 0.1 wt % Ag increased the elongation at break, but further addition decreased it abruptly. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008 [source] Isothermal crystallization kinetics and melting behaviors of nanocomposites of poly(trimethylene terephthalate) filled with nano-CaCO3JOURNAL OF APPLIED POLYMER SCIENCE, Issue 3 2007Mingtao Run Abstract The isothermal crystallization and subsequent melting behavior of poly(trimethylene terephthalate) (PTT) composites filled with nano-CaCO3 were investigated at designated temperatures with differential scanning calorimetry. The Avrami equation was used to fit the isothermal crystallization. The Avrami exponents were determined to be 2,3 for the neat PTT and PTT/CaCO3 composites. The particles of nano-CaCO3, acting as nucleating agents in the composites, accelerated the crystallization rate, with the half-time of crystallization decreasing or the growth rate constant (involving both nucleation and growth rate parameters) increasing. The crystallization activation energy calculated from the Arrhenius formula was reduced as the nano-CaCO3 content increased from 0 to 2%, and this suggested that nano-CaCO3 made the molecular chains of PTT easier to crystallize during the isothermal crystallization process. Subsequent melting scans of the isothermally crystallized composites exhibited triple or double melting endotherms: the greater the content was of nano-CaCO3, the lower the temperature was of the melting peak. The degree of crystallization deduced from the melt enthalpy of composites with the proper concentration of nano-CaCO3 was higher than that of pure PTT, but it was lower when the nano-CaCO3 concentration was more than 2%. The transmission electron microscopy pictures suggested that the dispersion state of nano-CaCO3 particles in the polymer matrix was even when its concentration was no more than 2%, whereas some agglomeration occurred when its concentration was 4%. Polarized microscopy pictures showed that much smaller or less perfect crystals formed in the composites because of the interaction between the molecular chains and nano-CaCO3 particles. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007 [source] Thermal and mechanical properties of uncrosslinked and chemically crosslinked polyethylene/ethylene vinyl acetate copolymer blendsJOURNAL OF APPLIED POLYMER SCIENCE, Issue 5 2007H. A. Khonakdar Abstract Uncrosslinked and chemically crosslinked binary blends of low- and high-density polyethylene (PE), with ethylene vinyl acetate copolymer (EVA), were prepared by a melt-mixing process using 0,3 wt % tert -butyl cumyl peroxide (BCUP). The uncrosslinked blends revealed two distinct unchanged melting peaks corresponding to the individual components of the blends, but with a reduced overall degree of crystallinity. The crosslinking further reduced crystallinity, but enhanced compatibility between EVA and polyethylene, with LDPE being more compatible than HDPE. Blended with 20 wt % EVA, the EVA melting peak was almost disappeared after the addition of BCUP, and only the corresponding PE melting point was observed at a lowered temperature. But blended with 40% EVA, two peaks still existed with a slight shift toward lower temperatures. Changes of mechanical properties with blending ratio, crosslinking, and temperature had been dominated by the extent of crystallinity, crosslinking degree, and morphology of the blend. A good correlation was observed between elongation-at-break and morphological properties. The blends with higher level of compatibility showed less deviation from the additive rule of mixtures. The deviation became more pronounced for HDPE/EVA blends in the phase inversion region, while an opposite trend was observed for LDPE/EVA blends with co-continuous morphology. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 3261,3270, 2007 [source] Ultrasound-compacted indomethacin/polyvinylpyrrolidone systems: Effect of compaction process on particle morphology and dissolution behaviorJOURNAL OF PHARMACEUTICAL SCIENCES, Issue 8 2002Adamo Fini Abstract Indomethacin (IMC)/polyvinylpyrrolidone systems were prepared under different technological conditions, using co-evaporation, kneading, traditional, and ultrasound (US) compaction. The materials thus obtained were milled and sieved and the powders were analyzed by using scanning electron microscopy to evaluate the morphology of the final particles and the fractal dimension of the particle contour. In the case of US-treated particles, scanning electron micrographs suggest that IMC could have partially covered the excipient granule surface, which appears lustrous and smooth, whereas after co-evaporation, the particles display a stratified structure. The external color of the granules, the hot stage microscopy examination, and the absence of the melting peak of the drug in thermograms supports the idea that IMC converts into an amorphous form under US discharge. Each technological treatment performed on the binary mixtures increases the dissolution rate of the drug, with respect to the pure drug and the physical mixture, but to a lesser extent than US compaction. US compaction and co-evaporation produce comparable results in improving the release of the drug. Polyvinylpyrrolidone offers better results than ,-cyclodextrin in promoting the dissolution of IMC, when both systems are compacted under US. © 2002 Wiley-Liss Inc. and the American Pharmaceutical Association J Pharm Sci 91:1880,1890, 2002 [source] Structure, Morphology and Properties of a Novel Molecular Composite by In-Situ Blending of Anionic Polyamide 6 with a Polyamide Copolymer Containing Rigid SegmentsMACROMOLECULAR MATERIALS & ENGINEERING, Issue 2 2007Xiaochun Wang Abstract Molten caprolactam, in which a polyamide copolymer (HPN) containing rigid segments was dissolved, was polymerized by means of anionic ROP to in produce polyamide (PA, nylon) 6 blends with HPN in situ. A novel molecular composite was achieved in which toughness and strength were simultaneously improved, as well as modulus, compared to virgin PA6. In view of the interchange reaction between PA6 and PA1212 (and PA66) in blends fabricated in the same way, it was deduced that a similar reaction between PA6 and HPN took place during the blending and led to copolymerization between the two components. The formation of copolymers was verified by their single glass transition and single melting peak, measured through DMA and DSC, respectively. DSC analysis also showed that the occurrence of the interchange reaction inhibited the crystallization and suppressed the melting point of PA6. Analysis by FT-IR spectroscopy indicated that the difference in the distance between the amide groups for PA6 and HPN induced a decrease in the amount and strength of hydrogen bonding. Moreover, characterization by POM and XRD revealed that the spherulite size of the PA6 crystals decreased dramatically and the amount of , crystal increased slightly with the majority of crystallites being , crystals. Furthermore, it was found through the observation of the morphology by SEM that no phase separation existed in the composites. On the basis of detailed analysis and a comparison between the in situ PA6/PA66 and PA6/HPN blends, it is believed that the combination of markedly decreasing spherulite size and similar segmental mobility resulted in the simultaneous improvement of mechanical properties for the in situ PA6/HPN blends. [source] Anisotropy in the electrical behavior of immiscible polypropylene/nylon/carbon black blends processed slightly below the melting temperature of the nylonPOLYMER ENGINEERING & SCIENCE, Issue 9 2006J. Zoldan Carbon black (CB) containing polypropylene/nylon (PP/Ny) blends, processed slightly below the melting temperature (Tm) of the dispersed Ny phase, leads to formation of fibrillar Ny phase and electrically anisotropic systems. CB containing PP/Ny blends were compounded (twin screw extruder) and processed (injection molding) slightly below the Tm of dispersed Ny phase at different blending sequences. To establish structure,property relationships scanning electron microscopy, high resolution scanning electron microscopy, differential scanning calorimeter were used and electrical properties were also studied. Addition of CB to binary PP/Ny blends, processed below the Ny Tm, altered the Ny fibrillation process forming an irregular continuous phase, containing the CB particles, rather than the fibrils formed in the PP/Ny blends. Yet, upon changing the processing sequence, i.e., compounding PP and CB and then adding Ny in the injection molding stage, Ny fibrils were attained, maintaining phase continuity, oriented in the flow direction and CB particles preferentially located on their surfaces. Blends exhibiting a fibrillar Ny network covered by CB particles exhibited electrical anisotropy. The Ny fibrils exhibited an additional higher crystalline melting peak and molecular orientation. The composites are conductive in the Ny fibril direction, while insulating in the perpendicular direction. Once the CB is located within both, the Ny and the PP matrix the electrical behavior is isotropic. POLYM. ENG. SCI., 46:1250,1262, 2006. © 2006 Society of Plastics Engineers [source] Formation and behaviour of low-temperature melting peak of quenched and annealed isotactic polypropylenePOLYMER INTERNATIONAL, Issue 2 2002ke Dudi Abstract The process of low-melting point (LMP) ,-phase formation in a quenched and annealed isotactic polypropylene (iPP) was studied by means of differential scanning calorimetry. The influence of preparation conditions (quenching and annealing temperatures, annealing times and sample thickness), together with the measurement parameters (heating and cooling rates), on the iPP melting behaviour are analysed. The results reveal a constant yield of LMP crystals over a wide range of quenching temperatures. This study also suggests that the LMP ,-crystals originate from the crystallization of polymer portions, which are somewhere between the amorphous and the smectic phase on the macromolecular scale of order. © 2001 Society of Chemical Industry [source] Crystallization Kinetics of the (Zr58Ni13.6Cu18Al10.4)Nb1 Bulk Metallic Glass,ADVANCED ENGINEERING MATERIALS, Issue 8 2006D. Qiao The differential thermal analysis (DTA) curve of the (Zr58Ni13.6Cu18Al10.4)Nb1 bulk metallic glass (BMG) shows that there are two exothermic crystallization peaks and two endothermic melting peaks. The BMG has been completely crystallized in the first crystallization peak. X-ray shows that the quenched BMG only includes the glass single phase. The BMG heated to 823 K (between the first and the second crystallization peak) has the precipitation of the cubic NiZr2. The BMG heated to 1003 K (after the second crystallization peak) has the cubic NiZr2, bct NiZr2, and bct CuZr2. HRTEM shows that there are some nano-crystalline phases for the quenched BMG. [source] Crystallization effects on autoclave foaming of polycarbonate using supercritical carbon dioxideADVANCES IN POLYMER TECHNOLOGY, Issue 4 2006L. Mascia Abstract In this study, the conditions leading to the formation of cells and to the onset of crystallization of polycarbonate were examined with the use of supercritical carbon dioxide for the production of foams from preforms. Small plaques cut from extruded sheets were treated with supercritical carbon dioxide in an autoclave at temperatures varying from 60 to 200°C and from 4.5 to 30 MPa pressure. Visual observations and stereoscan electron microscopy examination revealed that penetration of supercritical carbon dioxide takes place via the advancing layer mechanism and that, for the particular grade of polycarbonate used in this study, the nucleation of the cells can take place at temperatures as low as 60°C. It requires, however, long treatment times and high pressures, and the growth of foam cells is severely restricted. Nucleation and growth of cells occurred much more readily at somewhat higher temperatures. With treatments at around 80°C, the onset of crystallization started to impose considerable hindrance to the formation of uniform and evenly distributed cells. This becomes increasingly evident at higher temperatures, between 100 and 180°C, owing to the formation of large spherulitic crystalline domains. A very effective nucleation and growth mechanism for the formation of cells was obtained, on the other hand, with treatments at 200°C due to the absence of crystallization phenomena. The degree of crystallinity increased with increasing treatment temperature, and the resulting morphology gave rise to two broad melting peaks. These are displaced to higher temperatures and become closer, merging into one peak with a low-temperature shoulder. These events were monitored by thermal analysis and wide-angle X-ray diffraction examinations. © 2007 Wiley Periodicals, Inc. Adv Polym Techn 25:225,235, 2006; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/adv.20075 [source] Effects of silver nanoparticles on the dynamic crystallization and physical properties of syndiotactic polypropyleneJOURNAL OF APPLIED POLYMER SCIENCE, Issue 5 2008Dong Wook Chae Abstract The effects of silver (Ag) nanoparticles on the physical properties of syndiotactic PP (sPP) were investigated concentrating on the isothermal melt crystallization behavior under shear. sPP with 5 wt % Ag nanoparticles presented higher crystallization temperature (Tc) and heat of crystallization (,Hc) than pure sPP. At 90°C, the Ag nanoparticles had little effect on the induction time of crystallization but a little increased the half-time (t1/2) for the crystallization. At 100°C, however, the induction time was decreased with increasing the Ag content and the t1/2 was decreased up to the Ag content of 0.5 wt %. DSC melting endotherms exhibited double melting peaks when crystallized at 90°C under shear but a single melting peak when crystallized at 100°C. The WAXD patterns exhibited that the presence of Ag nanoparticles did not produce any change in the crystal structure of sPP. The tensile strength of sPP is little changed up to the Ag content of 0.1 wt % but it was decreased with further addition. In addition, the introduction of less than 0.1 wt % Ag increased the elongation at break, but further addition decreased it abruptly. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008 [source] Double-Grafted Cylindrical Brushes: Synthesis and Characterization of Poly(lauryl methacrylate) BrushesMACROMOLECULAR CHEMISTRY AND PHYSICS, Issue 15 2007Youyong Xu Abstract Double-grafted cylindrical brushes with poly(lauryl methacrylate) (PLMA) as the side chains were synthesized using the grafting-from strategy via atom transfer radical polymerization (ATRP). The polyinitiator poly[2-(2-bromoisobutyryloxy)ethyl methacrylate] (PBIEM) with ,=,240 and 1,500 served as the backbone. The PLMA side chains of the brushes carry long alkyl chains. GPC and 1H NMR measurements confirmed the successful formation of the PLMA cylindrical brushes. The side chains were cleaved from the cylindrical brushes by transesterification. GPC and 1H NMR results indicate that the initiating efficiency of the bromoester groups on the backbone for the bulky monomer was in the range of 0.34,,,f,,,0.67. Static and dynamic light scattering show that the ratio of the radius of gyration to the hydrodynamic radius, Rg/Rh, is in the range of 1.2,1.3, indicating that the LMA cylindrical brushes are semiflexible in solution. Atomic force microscopy (AFM) measurements show that short PLMA brushes exhibit a spherical morphology while the long brushes exhibit a worm-like structure. DSC displayed melting peaks at around ,30,°C, indicating the alkyl side chains of the PLMA chains in the double-grafted cylindrical brushes are crystallizable. [source] DGEBA monomer as a solvent for syndiotactic polystyreneMACROMOLECULAR SYMPOSIA, Issue 1 2003Jaap Schut Abstract Syndiotactic polystyrene (sPS) has to be processed at high temperatures (i.e. >290°C due to its melting point of 270°C), which approaches its degradation temperature. We aim to facilitate the processing of sPS by lowering its melt temperature and viscosity with a curable epoxy/amine model system as reactive solvent, which will result in a thermoplastic-thermoset polymer blend. As a first step we therefore investigated the melting behaviour of sPS in epoxy monomer, established its phase diagram, and investigated the crystalline form of sPS in these mixtures. DGEBA epoxy monomer is found to be a solvent for syndiotactic polystyrene at temperatures above 220°C. The DGEBA-sPS phase diagram was established by means of DSC, on the basis of crystallization and melting peaks. The form of the curve in the phase diagram indicates that DGEBA is a poor solvent for sPS. In WAXS studies of blends only the , crystalline form was detected, not the , form, thus no sPS-DGEBA polymer-solvent compounds (clathrates) were detected. However, DGEBA can still serve as a monomer for improved processing as it depresses the crystallization temperature by 20 to 60 K upon addition of 20 to 90 wt% DGEBA respectively, while a 16 to 45 K melting peak depression can be observed by adding 20 to 90 wt% DGEBA. [source] Nanocomposites of silver nanoparticle and dinonylnaphthalene disulfonic acid-doped thermoreversible polyaniline gelPOLYMER ENGINEERING & SCIENCE, Issue 3 2010Ashesh Garai Silver/polyaniline-dinonylnaphthalene disulfonic acid (PANI-DNNDSA) gel nanocomposites are prepared from the reduction of silver salt by polyaniline in formic acid medium. Scanning electron micrographs (SEM) indicate the presence of three-dimensional fibrillar network structure and the silver nanoparticles remain dispersed within the PANI-DNNDSA fibrillar network. Differential scanning calorimetric (DSC) study shows reversible first-order phase transition characterizing the composite to behave as a thermoreversible gel. Transmission electron micrographs (TEM) show a decrease of nanoparticle size with increasing AgNO3 concentration. Wide angle X-ray scattering (WAXS) patterns show lamellar structure in the gel as well as in the gel metal nanocomposites (GMNCs) and the two melting peaks in the DSC patterns correspond to the melting of monolayer and bilayer crystals produced from the interdigitation of DNNDSA tails anchored from PANI chains within the PANI lamella. The above melting points are greater in the GMNCs than that of pure gel indicating the formation of complex melting thermogram with crystallites produced from the anchored surfactants tails at the surface of Ag nanoparticles. The GMNCs show a higher thermal stability than that of pure PANI-DNNDSA gel. PANI-DNNDSA gel has an emission peak at 354 nm but fluorescence quenching occurs in the GMNCs and the emission peak becomes red shifted. Also in the UV,vis spectra the , band-polaron band transition peak shows a red shift and the DC conductivity increases with increasing Ag nanoparticle concentration in the GMNCs. The current (I),voltage (V) characteristic curves indicate Ohmic nature of conductivity of the gel and the current at the same voltage increases appreciably with increasing Ag nanoparticle concentration. These GMNCs are easily processible due to its thermoreversible nature. So, an easily processible, thermally stable and highly conducting DNNDSA-doped PANI-Ag gel nanocomposite with interesting photoluminescent property has been successfully developed suitable for optoelectronic applications. POLYM. ENG. SCI., 2010. © 2009 Society of Plastics Engineers [source] Solid-state structure and formation of organized molecular films of methacrylate copolymers containing fluorinated and hydrogenated side-chainsPOLYMER ENGINEERING & SCIENCE, Issue 4 2007Atsuhiro Fujimori Surface morphology of monolayers related to solid-state structure for methacrylate comb copolymers having fluorocarbon and hydrocarbon side-chains was investigated by X-ray diffraction (XRD), differential scanning calorimetry, and atomic force microscopy (AFM). From the XRD profiles, two kinds of short spacing peaks were confirmed at 5.0 and 4.2 Å, which assigned the sub-cells for both side-chains. Furthermore, two kinds of endothermic peaks, which corresponded to melting peaks of the both side-chain crystals, appeared in the thermograms. From the AFM observation, it was found that there were hydrogenated domains at a few hundred nanometer diameter in their monolayers, whereas corresponding acrylate copolymer monolayers form the phase-separated structure at 10,30 nm order scales. POLYM. ENG. SCI., 47:354,364, 2007. © 2007 Society of Plastics Engineers. [source] Vapor-induced crystallization behavior of bisphenol-A polycarbonatePOLYMER ENGINEERING & SCIENCE, Issue 6 2006Zhongyong Fan The effects of exposure time and vapor pressure on the crystallization behaviors of bisphenol-A polycarbonate (BAPC) films were investigated at 25°C by using differential scanning calorimetry (DSC). Double melting peaks were observed for various BAPC samples after vapor-induced crystallization. The low temperature melting peak shifted to higher temperature and became sharper with increasing exposure time, and could be assigned to defective crystals with smaller crystal size. Crystallinity and average crystal dimension normal to (020) were calculated from wide-angle X-ray diffraction spectra. A good agreement was obtained between crystallinity values obtained from WAXD and those from DSC. The morphology of crystallized samples after various exposure time periods was examined by means of polarized optical microscopy. Nucleation occurred at the initial stage of vapor-induced crystallization. Poor crystals become perfect through segment reorganization with increasing exposure time, and spherulites' growth was observed. The average diameter of spherulites increased from 2 ,m for 1 h, to 7 and 16 ,m after 3 and 56 h, respectively. POLYM. ENG. SCI., 46:729,734, 2006. © 2006 Society of Plastics Engineers [source] Control of orientation for carbazole group in comb copolymers arranged by method of organized molecular filmsPOLYMERS FOR ADVANCED TECHNOLOGIES, Issue 5 2007Hiroko Hoshizawa Abstract We investigated the molecular orientation of organized molecular films with regard to solid-state structures for newly synthesized comb copolymers with N -vinylcarbazole (NVCz) by in-plane and out-of plane X-ray diffraction (XRD), differential scanning calorimetry (DSC), and atomic force microscopy (AFM). In the bulk state, hydrogenated and fluorinated comb copolymers form side-chain crystals for a two-dimensional lattice spacing of 4.2 and 5.0,Å, respectively. The findings suggest that the carbazole rings in the main-chain are arranged in opposition to each other. From the results of the DSC measurement, sharp-shaped melting peaks appear on the relatively lower temperature side of the thermograms. This result supports the formation of side-chain crystals in the synthesized comb copolymers. These monolayers of the copolymers on the water surface were extremely condensed, except for the fluorocarbon:NVCz,=,1:1 copolymer. From the in-plane XRD measurement of multilayers on solids, the changes in the two-dimensional lattice structure of fluorinated comb copolymer films containing NVCz units, as opposed to their bulk state, were confirmed. It seems that these structural changes are caused by the stronger ,,, interaction between the carbazole rings rather than the van der Waals interaction between fluorocarbons. Copyright © 2007 John Wiley & Sons, Ltd. [source] |