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Fullerene-modified polyamide 6 by in situ anionic polymerization in the presence of PCBM

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Abstract

Activated anionic ring-opening polymerization of ε-caprolactam (ECL) was carried out for the first time in the presence of [6,6]-phenyl-C61-butyric acid methyl ester (PCBM) to prepare polyamide 6 (PA6)-based composites comprising up to 3 wt% of this fullerene derivative. This in situ polymerization process produced high molecular weight composites containing 52–80 % of gel fraction at PCBM concentration ≥0.5 wt%. Spectral, thermo-mechanical, synchrotron X-ray, and scanning electron microscopy data were used to elucidate the structure and morphology of the PA6/PCBM composites. A mechanism of the chemical structure evolution was proposed starting with incipient complexation between ECL and PCBM, via subsequent chemical linking of ECL moieties on the C60 spheroid and final formation of star-burst and cross-linked morphologies. PCBM amounts of 0.1 wt% and more decreased the volume resistivity from 1012 Ω cm (neat PA6) to 109–107 Ω cm, thus opening the way for new applications of anionic PA6.

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Acknowledgements

This work was supported by FCT (Fundação para a Ciência e Tecnologia—Portugal) through the program Strategic Project LA 25 2013–2014 and by the European Regional Development Fund (FEDER) through COMPETE, project EXPL/CTM-POL/0933/2012. N. Dencheva is grateful to the FCT for supporting her research by the postdoctoral award SFRH/BPD/45252/2008, co-financed by QREN–POPH program of the European Union. The financial support of HASYLAB at DESY (Grant No. II-07-011 EC) is also gratefully acknowledged. The authors wish to thank Mauricio Malheiro for his technical assistance in the DMTA and UV-Vis experiments.

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Authors and Affiliations

  1. Institute for Polymers and Composites/I3N, University of Minho, 4800-058, Guimarães, Portugal

    Nadya Dencheva, Hugo Gaspar, Gabriel Bernardo & Zlatan Denchev

  2. CENIMAT/I3N, New University of Lisbon, 2829-516, Caparica, Portugal

    Sergej Filonovich

  3. Electrical and Computer Engineering, University of New Mexico, Albuquerque, NM, 87106, USA

    Olga Lavrova & Tito Busani

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  1. Nadya Dencheva
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  2. Hugo Gaspar
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  6. Gabriel Bernardo
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  7. Zlatan Denchev
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Correspondence to Zlatan Denchev.

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Dencheva, N., Gaspar, H., Filonovich, S. et al. Fullerene-modified polyamide 6 by in situ anionic polymerization in the presence of PCBM. J Mater Sci 49, 4751–4764 (2014). https://doi.org/10.1007/s10853-014-8174-7

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