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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Colloid & polymer science 276 (1998), S. 289-296 
    ISSN: 1435-1536
    Keywords: Key words Semicrystalline polymer ; PEEK ; TMDSC ; DMA ; melting ; crystallization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract  Temperature-modulated DSC (TMDSC) and dynamic-mechanical analysis (DMA) allows the study of degree of crystallinity changes of polymers. From the comparison of the two methods using the same temperature–time program, one expects additional information about the processes occurring in the melting region. A first description of temperature-modulated DMA is given. The effect of reversible melting during every period of temperature modulation has been observed in the melting region of PEEK. The number of molecules which undergo reversible melting for a given quasi-isotherm decreases with time. At 600 K the fraction of the material involved in this process during one modulation cycle is between 0.35% and 0.25%, but has a non-zero value at infinity. The kinetics of this decrease indicates that the process of the structural changes is most likely related to the melt. It can be explained considering an entanglement of the disentangled melt surrounding the just molten crystals. The results are in agreement with the four-state scheme for polymer crystallization and melting proposed by Strobl.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 60 (2000), S. 807-820 
    ISSN: 1572-8943
    Keywords: calorimetry ; crystallization ; PCL ; PEEK ; PEN ; PET ; polymer ; temperature modulation ; TMDMA ; TMDSC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Quasi-isothermal temperature modulated DSC and DMA measurements (TMDSC and TMDMA, respectively) were performed to determine heat capacity and shear modulus as a function of time during crystallization. Non-reversible and reversible phenomena in the crystallization region of polymers can be observed. The combination of TMDSC and TMDMA yields new information about local processes at the surface of polymer crystals, like reversible melting. Reversible melting can be observed in complex heat capacity and in the amplitude of shear modulus in response to temperature perturbation. The fraction of material involved in reversible melting, which is established during main crystallization, keeps constant during secondary crystallization for PCL PET and PEEK. This shows that also after long crystallization times the surfaces of the individual polymer crystallites are in equilibrium with the surrounding melt. Simply speaking, polymer crystals are ‘living crystals’.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 61 (2000), S. 649-659 
    ISSN: 1572-8943
    Keywords: complex heat capacity ; non-linearity ; non-linear thermal response ; non-stationarity ; reversing heat capacity ; TMDSC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract To treat data from temperature modulated differential scanning calorimetry (TMDSC) in terms of complex or reversing heat capacity firstly one should pay attention that the response is linear and stationary because this is a prerequisite for data evaluation. The reason for non-linear and non-stationary thermal response is discussed and its influence on complex (reversing) heat capacity determination is shown. The criterion for linear and stationary response is proposed. This allows to choose correct experimental conditions for any complex heat capacity measurement. In the case when these conditions can not be fulfilled because of experimental restrictions one can estimate the influence of non-linearity and non-stationarity on measured value of complex or reversing heat capacity.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 59 (2000), S. 279-288 
    ISSN: 1572-8943
    Keywords: AC calorimetry ; crystallization ; PCL ; polymer ; temperature modulation ; TMDSC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: 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.
    Type of Medium: Electronic Resource
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