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Journal of Thermal Analysis and Calorimetry

, Volume 116, Issue 3, pp 1273–1278 | Cite as

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

  • C. A. Gracia-Fernández
  • S. Gómez-Barreiro
  • A. Álvarez-García
  • J. López-BeceiroEmail author
  • B. Álvarez-García
  • S. Zaragoza-Fernández
  • R. Artiaga
Article
  • 367 Downloads

Abstract

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.

Keywords

Poly-l-lactic acid DEA TMDSC Glass transition Enthalpic relaxation Crystallization 

Notes

Acknowledgements

This research has been partially supported by the Spanish Ministry of Science and Innovation, Grant MTM2011-22392 (ERDF included).

Supplementary material

10973_2013_3629_MOESM1_ESM.xls (478 kb)
Supplementary material 1 (XLS 477 kb)

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Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2014

Authors and Affiliations

  • C. A. Gracia-Fernández
    • 1
  • S. Gómez-Barreiro
    • 2
  • A. Álvarez-García
    • 3
  • J. López-Beceiro
    • 3
    Email author
  • B. Álvarez-García
    • 3
  • S. Zaragoza-Fernández
    • 3
  • R. Artiaga
    • 3
  1. 1.TA Instruments-Waters CromatografíaAlcobendasSpain
  2. 2.Department of Applied Physics, CESUGAUniversity College of DublinA CoruñaSpain
  3. 3.University of A CoruñaFerrolSpain

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