Crystallization and ring-banded spherulite morphology of poly(ethylene oxide)-block-poly(epsilon-caprolactone) diblock copolymer

The crystallization behavior of crystalline-crystalline diblock copolymer containing poly(ethylene oxide) (PEO) and poly(epsilon-caprolactone) (PCL), in which the weight fraction of PCL is 0.815, has been studied via differential scanning calorimeter (DSC), wide-angle X-ray diffraction (WAXD), and polarized optical microscopy (POM). DSC and WAXD indicated that both PEO and PCL blocks crystallize in the block copolymer. POM revealed a ring-banded spherulite morphology or the PEO-b-PCL diblock copolymer.

Fractionated crystallization of dispersed PA6 phase of PP/PP-g-MAH/PA6 blends

Fractionated crystallization behavior of dispersed PA6 phase in PP/PA6 blends compatibilized with PP-g-MAH was investigated by scanning electron microscopy (SEM), differential scanning calorimeter (DSC), polarized light microscopy (PLM), and wide-angle X-ray diffraction (WAXD) in this work. The lack of usual active heterogeneities in the dispersed droplet was the key factor for the fractionated crystallization of PA6. The crystals formed with less efficient nuclei might contain more defects in the crystal structures than those crystallized with the usual active nuclei. The lower the crystallization temperature, the lesser the perfection of the crystals and the lower crystallinity would be. The fractionated crystallization of PP droplets encapsulated by PA6 domains was also observed. The effect of existing PP-g-MAH-g-PA6 copolymer located at the interface on the fractionated crystallization could not be detected in this work.

Synthesis and characterization of blue-light-emitting poly(aryl ether)s containing oligofluorenes in the main chain

A series of blue light-emitting poly(aryl ether)s (PAEs) containing ter- or pentafluorenes in the main chain have been synthesized via nucleophilic substitution polycondensation reaction. The energy levels of the polymers were tuned by introducing hole-transporting triaryamine groups in the side chains and/or incorporating electron-transporting oxadiazole segments in the main chain. The optical properties of the polymers are dominantly determined by the well-defined oligofluorene segments, and therefore all polymers show high photoluminescence quantum yield. Differential scanning calorimeter (DSC) characterizations indicate that they are vitrified polymers with high glass transition temperature (up to 156 degrees C). The polymers comprising pentafluorenes exhibit electroluminescent properties equal to or better than fully conjugated fluorene homopolymers. With the device structure of ITO/PEDOT:PSS/polymer/Ca/Al, an external quantum efficiency of 1.4% along with Commission Internationale de L'Eclairage (CIE) coordinates of (0.17, 0.09) has

Microstructures and properties of melt-spun and as-cast Mg-20Gd binary alloy

Mg-20Gd(%, mass fraction) samples were prepared using melt-spinning and copper mold casting techniques. Microstructures and properties of the Mg-20Gd were investigated. Results show that the melt-spun ribbon is mainly composed of supersaturated alpha-Mg solid solution phase and the as-east ingot mainly contains alpha-Mg solid solution and Mg5Gd phase. The differential scanning calorimeter (DSC) curve of the ribbon exhibits a small exothermic peak in the temperature range from 630 to 680 K, which indicates that the ribbon contains a metastable phase (amorphous). Tensile strength at room temperature of the melt-spun ribbon and as-cast specimen are 308 and 254 MPa, respectively. The elongations of the two samples are less than 2%. The fracture surfaces demonstrate that the fracture mode of the as-cast Mg-20Gd is a typical cleavage fracture and that of the melt-spun sample is a combination of brittle fracture and ductile fracture.

Melting behaviors, isothermal and non-isothermal crystallization kinetics of nylon 1212

Isothermal crystallization, subsequent melting behavior and non-isothermal crystallization of nylon 1212 samples have been investigated in the temperature range of 160-171 degreesC using a differential scanning calorimeter (DSC). Subsequent DSC scans of isothermally crystallized samples exhibited three melting endotherms. The commonly used Avrami equation and that modified by Jeziorny were used, respectively, to fit the primary stage of isothermal and non-isothermal crystallizations of nylon 1212. The Avrami exponent n was evaluated, and was found to be in the range of 1.56-2.03 for isothermal crystallization, and of 2.38-3.05 for non-isothermal crystallization. The activation energies (DeltaE) were determined to be 284.5 KJ/mol and 102.63 KJ/mol, respectively, for the isothermal and non-isothermal crystallization processes by the Arrhenius' and the Kissinger's methods.

Multiple melting behavior of isotactic polypropylene and poly(propylene-co-ethylene) after stepwise isothermal crystallization

The multiple melting behavior of several commercial resins of isotactic polypropylene (iPP) and random copolymer, poly(propylene-co-ethylene) (PPE), after stepwise isothermal crystallization (SIC) were studied by differential scanning calorimeter and wide-angle X-ray diffraction (WAXD). For iPP samples, three typical melting endotherms appeared after SIC process when heating rate was lower than 10 degreesC/min. The WAXD experiments proved that only alpha-form crystal was formed during SIC process and no transition from alpha1- to alpha2-form occurred during heating process. Heating rate dependence for each endotherm was discussed and it was concluded that there were only,two major crystals with different thermal stability. For the PPE sample, more melting endotherms appeared after stepwise isothermal crystallization. The introduction of ethylene comonomer in isotactic propylene backbone further decreased the regularity of molecular chain, and the short isotactic propylene sequences could crystallize into gamma-form crystal having a low melting temperature whereas the long sequences crystallized into alpha-form crystal having high melting temperature.

Effect of nucleating agents on the crystallization of poly(3-hydroxybutyrate-co-3-hydroxyvalerate)

The effect of nucleating agents on the crystallization behavior of poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) was studied. A differential scanning calorimeter was used to monitor the energy of the crystallization process from the melt and melting behavior. During the crystallization process from the melt, nucleating agent led to an increase in crystallization temperature (T-c) of PHBV compared with that for plain PHBV (without nucleating agent). The melting temperature of PHBV changed little with addition of nucleating agent. However, the areas of two melting peaks changed considerably with added nucleating agent. During isothermal crystallization, dependence of the relative degree of crystallization on time was described by the Avrami equation. The addition of nucleating agent caused an increase in the overall crystallization rate of PHBV, but did not influence the mechanism of nucleation and growth of the PHB crystals. The equilibrium melting temperature of PHBV was determined as 187degreesC. Analysis of kinetic data according to nucleation theories showed that the increase in crystallization rate of PHBV in the composite is due to the decrease in surface energy of the extremity surface.

Preparation, characterization, and crystallization of naphthalene-labeled polypropylene

Naphthalene-labeled polypropylene (PP) was prepared by melt reaction of maleic anhydride-grafted-polypropylene (PP-g-MA) with 1-aminonaphthalene in a Barabender mixer chamber. The structure of the product was analyzed with fourier transform infrared (FT-IR), ultraviolet (UV) and fluorescence. The results showed that naphthyl groups grafted onto the PP molecular chains through the imide bonds formed between MA and 1-aminonaphthalene. The content of the chromophores was 1.8 X 10(-4) mol g(-1) measured by elemental analysis. Isothermal crystallization behavior was studied by differential scanning calorimeter (DSC). Labeled PP had a higher crystallization rate than PP-g-MA. Wide-angle X-Ray diffraction (WAXD) analysis revealed that labeled PP had higher crystallinity than PP-g-MA.

Influence of annealing on structure of Nylon 11

Differential scanning calorimeter (DSC), wide-angle X-ray diffraction (WAXD), small-angle X-ray scattering (SAXS), and density techniques have been used to investigate the structural parameters of the solid state of Nylon 11 annealed at different temperatures. The equilibrium heat of fusion Delta H-m(0) and equilibrium melting temperature T-m(0) were estimated to be 189.05 J g(-1) and 202.85 degrees C respectively by using the Hoffman-Weeks approach. The degree of crystallinity (W-c,W-x) ranged approximately 24-42% was calculated by WAXD and compared with those by calorimetry (W-c,W-h) and density (W-c,W-d) measurements. The radius of gyration R-g, crystalline thickness L-c, noncrystalline thickness L-a, long period L, semiaxes of the particles (a, b), electron-density difference between the crystalline and noncrystalline regions eta(c) - eta(a), and the invariant Q increased with increasing annealing temperature. The analysis of the SAXS data was based upon the particle characteristic function and the one-dimensional electron-density correlation function. An interphase region existed between the crystalline and noncrystalline region with a clear dimension of about 2 nm for semicrystalline Nylon 11. Instead of the traditional two-phase model, a three-phase model has been proposed to explain these results by means of SAXS.

Confined crystallization behavior of PEO in silica networks

Poly(ethylene oxide) (PEO) and silica (SiO2) organic-inorganic hybrid materials have been synthesized by sol-gel approach. The crystallization behavior of PEO in silica networks has been investigated by differential scanning calorimeter (DSC) and scanning electron micrograph (SEM). The degree of PEO crystallinity in PEO/SiO2 hybrid networks reduces with the increase of SiO2. PEO is in amorphous state when the concentration of PEO is lower than 50 wt% in the hybrid materials. The melting points of PEO in the networks are lower than that of pure PEG, but the melting point of PEO in the networks almost has the same melting point. WAXD and SEM results show that the crystalline behavior of PEO in PEO/SiO2 hybrid system is sternly confined. (C) 1999 Elsevier Science Ltd. All rights reserved.

Effect of nucleating agent on the isothermal crystallization kinetics of PHBV

The crystallization behavior of PHBV, poly(beta -hydroxybutyrate-co-beta -hydrxyvalerate), with nucleating agents under isothermal conditions was investigated. A differential scanning calorimeter was used to monitor the crystallization process from the melt. During isothermal crystallization, the dependence of relative degree of crystallinity on time was described by the Avrami equation. It has been shown that the addition of BN and Tale causes a considerable increase in the overall crystallization rate of PHBV but does not influence the Avrami exponent n, mechanism of nucleation and spherulite growth mode of PHBV. A little of nucleating agent will increase the crystallization rate and decrease the fold surface free energy sigma (e), remarkably. The effect of BN is more significant than that of Talc.

Confined crystallization behavior of PEO in organic networks

Poly (ethylene oxide) (PEO) and poly (trimethopropane trimethacrylate) (PTMPTMA) interpenetrate networks have been synthesized. The confined crystallization behavior of PEO in the PTMTYTMA networks has been investigated by a differential scanning calorimeter and scanning electron microscope. The degree of PEO crystallinity in PEO/PTMPTMA interpenetrate networks reduces with the increase of PTMPTMA. PEO is in an amorphous state when the concentration of PEO is lower than 50% in the interpenetrate networks system. The melting points of crystalline PEO in the networks are lower than that of pure PEG, and the melting point of PEO in the networks is higher and increases with the increase of PEO in the interpenetrate networks. Wide-angle X-ray diffraction results show that the PEO crystallite size perpendicular to the (120) plane is not affected as much as PEO in silica networks. (C) 2001 Elsevier Science Ltd. All rights reserved.

Size-affected crystallization of trans-1,4-polybutadiene

By using different catalyst systems, two trans-1,4-polybutadiene (TPBD) samples with different tr trans-content and molecular weight were synthesized. The phase transition of two samples from monoclinic form to hexagonal phase was revealed by differential calorimeter scanning and X-ray, respectively. The small-angle X-ray scattering measurements showed the remarkable discrepancy of phase transition and melting point between the two samples was attributed to the different lamellar thickness of crystals: The crystals with different crystalline morphology and lamellar thickness were developed by casting different concentration TPBD solutions. Transmission electron microscopy morphology observations proved that annealing the specimen at the temperature above the phase transition point for different times resulted in the different lamellae thickening of monoclinic form. It means that annealing the TPBD in its hexagonal phase will also slightly favor the increase of both the phase transition temperature and melting point of hexagonal phase. (C) 2001 Elsevier Science Ltd. All rights reserved.

Miscibility and crystallization of PHB PMA blends

The miscibility, crystallization behavior and morphological structure of PHB/PMA blends have been studied by the differential scanning calorimeter (DSC) and polarized optical microscopy (POM). The chemical repeat units of the two components of the blend are isomers. The results indicate that PHB and PMA are miscible in the melt. The addition of PMA into PHB results in a depression in the spherulite growth rate of PHB. With increasing PMA content in the blends, the texture of PHB spherulite becomes more open.

Studies on uniaxially drawn poly(vinylidene fluoride) films

Poly(vinylidene fluoride) (PVDF), under certain conditions, shows a crystal transition between the alpha (TGT (G) over bar) and beta (TTT) forms, where T, G, and (G) over bar, respectively, denote trans, gauche, and minus gauche. We investigated the mechanism of this crystal transition by FT-TR and X-ray diffraction, which yielded consistent results. We also carried out differential scanning calorimeter experiments.