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TMDSC phase angle for a better nanocomposite interphase identification

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Abstract

The present study suggests a new approach, based on the utilization of temperature modulated differential scanning calorimetry (TMDSC) technique, for identifying and characterizing the organic–inorganic interphase of two materials: an epoxy–fumed silica nanocomposite and a thermoplastic polyurethane (TPU)–multiwalled nanotube (MWNT) composite. The approach used here makes use of TMDSC data and basically consists of using the phase angle or the derivative of the reversing heat flow instead of the reversing heat flow curve itself. In the case of epoxy–fumed silica composites, two glass transition regions were identified. The glass transition temperature (T g) of the composite was observed to vary as a consequence of the filler content. This study shows that the T g variation is due to the formation of an organic–inorganic interphase, with its own glass transition temperature, which is different from the epoxy matrix T g. In the case of TPU–MWNT composites, two relaxations and an additional first order transition were observed: the first relaxation corresponds to the hard segment, the second is related to an interaction between filler and matrix and the third process may be connected to the partial melting of the hard segment. The addition of 0.5 wt% MWNT causes a small reduction in T g of the TPU. A major nanotube addition, 10 wt%, induces the appearance of a new relaxation that may be associated with the existence of an interface. In general, a better separation between the matrix and interphase glass transitions was obtained by the TMDSC phase angle signal.

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Acknowledgements

This research has been partially supported by the Spanish Ministry of Science and Innovation, Grant MTM2008-00166 (ERDF included) and Grant MTM2011-22393. The authors thank Senén Paz for constructive comments and the referees for their valuable suggestions.

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Authors and Affiliations

  1. Higher Polytechnic School, University of A Coruña, Campus de Esteiro, 15403, Ferrol, Spain

    Javier Tarrío-Saavedra, Jorge López-Beceiro, Salvador Naya & Ramón Artiaga

  2. Thermal Analysis, Rheology and Microcalorimetry Applications, TA Instruments-Waters Cromatografía, S.A. Avda. Europa, 21 Parque Empresarial La Moraleja, 28108, Alcobendas, Madrid, Spain

    Carlos Gracia-Fernández

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  1. Javier Tarrío-Saavedra
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  2. Carlos Gracia-Fernández
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  3. Jorge López-Beceiro
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  4. Salvador Naya
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  5. Ramón Artiaga
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Correspondence to Javier Tarrío-Saavedra.

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Tarrío-Saavedra, J., Gracia-Fernández, C., López-Beceiro, J. et al. TMDSC phase angle for a better nanocomposite interphase identification. J Therm Anal Calorim 109, 1277–1284 (2012). https://doi.org/10.1007/s10973-012-2568-z

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