Determination of the equilibrium enthalpy of melting of two-phase semi-crystalline polymers by fast scanning calorimetry

Clément Fosse, Aurélie Bourdet, Estève Ernault, Antonella Esposito*, Nicolas Delpouve, Laurent Delbreilh, Shanmugam Thiyagarajan, Rutger J.I. Knoop, Eric Dargent

*Corresponding author for this work

Research output: Contribution to journalArticleAcademicpeer-review

Abstract

The equilibrium enthalpy of melting ΔHm 0 [J·g−1] is an extrapolated thermodynamic quantity attributed to crystallizable macromolecules and widely used to characterize polymers in their semi-crystalline state, for it allows estimating the degree of crystallinity by direct comparison with the enthalpy of melting obtained from differential scanning calorimetry. ΔHm 0 is typically obtained by cross-comparing the results obtained by at least two techniques. This work proposes a simplified experimental protocol to determine ΔHm 0 by the use of Fast Scanning Calorimetry (FSC). This approach applies to any crystallizable polymer for which a specific microstructure can be obtained (i.e. a two-phase semi-crystalline microstructure with a negligible amount of rigid amorphous fraction) and that can also be quenched to its fully amorphous state. Such a two-phase microstructure can be obtained on nanoscale samples through an annealing process performed in situ on the FSC sensor at crystallization temperatures as close as possible to the melting temperature. The enthalpy of melting is then evaluated from the two-phase model for different crystallization times (i.e. different crystallinities) and the ΔHm 0 is obtained by extrapolating the data to the 100% crystalline state. This procedure was applied on samples whose ΔHm 0 values are already available in the literature, but also on more recent biobased polyesters whose thermal properties are still under investigations.

Original languageEnglish
Pages (from-to)67-78
Number of pages12
JournalThermochimica Acta
Volume677
DOIs
Publication statusPublished - 1 Jul 2019

Keywords

  • Enthalpy of melting
  • Fast scanning calorimetry
  • PBF
  • PEF
  • Rigid amorphous fraction

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    Fosse, C., Bourdet, A., Ernault, E., Esposito, A., Delpouve, N., Delbreilh, L., ... Dargent, E. (2019). Determination of the equilibrium enthalpy of melting of two-phase semi-crystalline polymers by fast scanning calorimetry. Thermochimica Acta, 677, 67-78. https://doi.org/10.1016/j.tca.2019.03.035