Thermal characterization of poly-l-lactide by dielectric analysis and modulated DSC

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• 作者：C. A. Gracia-Fernández (1)
  S. Gómez-Barreiro (2)
  A. álvarez-García (3)
  J. López-Beceiro (3)
  B. álvarez-García (3)
  S. Zaragoza-Fernández (3)
  R. Artiaga (3)
  
• 关键词：Poly ; l ; lactic acid ; DEA ; TMDSC ; Glass transition ; Enthalpic relaxation ; Crystallization
• 刊名：Journal of Thermal Analysis and Calorimetry
• 出版年：2014
• 出版时间：June 2014
• 年：2014
• 卷：116
• 期：3
• 页码：1273-1278
• 全文大小：
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• 作者单位：C. A. Gracia-Fernández (1)
  S. Gómez-Barreiro (2)
  A. álvarez-García (3)
  J. López-Beceiro (3)
  B. álvarez-García (3)
  S. Zaragoza-Fernández (3)
  R. Artiaga (3)
  
  1. TA Instruments-Waters Cromatografía, 20108, Alcobendas, Madrid, Spain
  2. Department of Applied Physics, CESUGA, University College of Dublin, Feáns 152, 15190, A Coru?a, Spain
  3. University of A Coru?a, EPS Avda. Mendizábal s/n, 15403, Ferrol, Spain
  
• ISSN：1572-8943

文摘

Dielectric analysis (DEA) is a very sensitive technique, which allows for detection of small structural changes at the low scale. An advantage of DEA, with respect to other modulated techniques, is the possibility of using a wider frequency range. Molecular relaxations of the order of only a few nanometers are not observed by any other thermoanalytic method. Nevertheless, these small relaxations involve dipole changes that can be observed by DEA. Thus, this technique is used here, in combination with temperature-modulated differential scanning calorimetry (TMDSC) to obtain insightful information about the thermal transitions of poly-l-lactic acid (PLLA), one of the stereo-isomers of polylactide. Its complex thermal behavior is the subject of ongoing debate, with several overlapping crystallization and melting processes. The combined use of TMDSC and DEA provides a better insight of three important transitions of this polymer: the alpha relaxation, the enthalpic relaxation, and the cold crystallization. The dependences of the enthalpy relaxation on the dynamic glass transition relaxation and on the glass transition as a thermal event are evaluated. On the other hand, it will be shown how the cold crystallization can be identified by TMDSC, and DEA helps us understand the effect of crystallization on the dipole movements. The shape of the dielectric permittivity curve at low frequencies is compared to that of the reversing heat capacity to check whether both signals are sensitive or not to the same events. It is also verified how the experimental results of alpha relaxation of PLLA follow an Arrhenius or a Vogel trend.