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Abstract  

Secondary crystallization of PEA, occurring during DSC scan and performed after isothermal primary crystallization has been investigated. The high temperature exotherm peak has been attributed to the crystallization of amorphous fraction included between crystallites formed at the primary crystallization. The temperature position of the highest rate of the secondary crystallization depended on the temperature of the isothermal primary crystallization.

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Abstract  

The crystallinity of poly(ethyleneterephthalate) has been determined by differential scanning calorimetry and by density. The results obtained by calorimetry show that the increment in the crystallinity due to the heatsetting treatment is produced by the increase of the crystallinity corresponding to the premelting endothermic peak.

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Abstract  

We report the results of an investigation by differential scanning calorimetry (DSC) of two mobility controlled processes in the amorphous phas e of semicrystalline PEEK — enthalpy relaxation below the glass transition (T g) and secondary crystallization aboveT g. Both result in the observation of an endothermic peak just above the annealing temperature in the DSC scan of the polymer — the enthalpy recovery peak and the low temperature melting peak, respectively. There is a striking similarity in the time and temperature dependence of the endothermic peak for these two processes. These results are reminiscent of those obtained from small strain creep studies of “physical aging” of semicrystalline PEEK below and aboveT g.

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calorimetry (DSC) technique. Unusual fourfold melting endotherms were observed. A new and comprehensive explanation on the origin of the complex multiple melting behavior particularly the origin of the secondary crystallization, which is different from

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lower temperature. So that secondary crystallization appears obvious at cooling rate 40 K min −1 and little at cooling rate 2.5 K min −1 , which suggests that the secondary crystallization of P4MP1 was the re-arrangement of loose packed chains during

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Abstract  

A crystallization kinetics analysis of several polypropylene-polyethylene (PP-PE), PP-rich copolymers was made by means of differential scanning calorimetry. The crystallization was studied via calorimetric measurements at different cooling rates. Several additives were added to the base material. Some test samples were subjected to artificial ageing processes. A modified isoconversional method was used to describe the crystallization process under non-isothermal conditions. The value of the Avrami parameter was determined for primary and secondary crystallization.

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Abstract  

The crystallisation kinetics, melting behaviour and morphology, of bacterial poly(3-hydoxybutyrate) (PHB) have been investigated by using differential scanning calorimetry (DSC), step-scan DSC (SDSC), wide angle X-ray diffraction (WAXRD) and hot stage polarised optical microscopy (HSPOM). DSC imparted isothermal crystallisation thermal history. The subsequent melting behaviour revealed that all PHB materials experienced secondary crystallisation during heating and the extent of secondary crystallisation varied depending on the crystallisation temperature. PHB samples were found to exhibit double melting behaviour due to melting of SDSC scan-induced secondary crystals, while considerable secondary crystallisation or annealing took place under the modulated heating conditions. The overall melting behaviour was rationalised in terms of recrystallisation and/or annealing of crystals. Interestingly, the PHB materials analysed by SDSC showed a broad exotherm before the melting peak in the non-reversing curve and a multiple melting peak reversing curve, verifying that the melting-recrystallisation and remelting process was operative. HSOM studies supported the conclusions from DSC that the radial growth rate of the PHB spherulites was significantly varied upon the crystallisation conditions. One form of crystals was shown by WAXRD from isothermally crystallised PHB.

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Abstract  

Quasi-isothermal temperature modulated DSC (TMDSC) were performed during crystallization to determine heat capacity as function of time and frequency. Non-reversible and reversible phenomena in the crystallization region of polymers were distinguished. TMDSC yields new information about the dynamics of local processes at the surface of polymer crystals, like reversible melting. The fraction of material involved in reversible melting, which is established during main crystallization, keeps constant during secondary crystallization for polycaprolactone (PCL). This shows that also after long crystallization times the surfaces of the individual crystallites are in equilibrium with the surrounding melt. Simply speaking, polymer crystals are living crystals. A strong frequency dependence of complex heat capacity can be observed during and after crystallization of polymers.

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Abstract  

The melting and crystallisation behaviour of poly(m-xylene adipamide) (MXD6) are investigated by using the conventional DSC, X-ray diffraction and polarised light microscopy. Triple, double or single melting endotherms are obtained in subsequent heating scan for the samples after isothermal crystallisation from the melt state at different temperatures. The lowest melting peak can be ascribed to the melting of secondary crystals. The melting of primary crystals causes the medium melting peak and the highest melting peak is attributed to the melting of recrystallised species formed during heating. Following the Hoffman–Weeks theory, the equilibrium melting temperature is equal to 250C and the equilibrium melting enthalpy ΔH m 0 to 175 J g–1. Then, using the Lauritzen–Hoffmann theory of secondary crystallisation, the analyse of the spherulitic growth shows that the temperature of transition between the growing regimes II and III is equal to 176C. Finally the Gibbs-Thomson relationship allows the determination of the distribution function of crystalline lamellae.

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