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Synthesis and thermal analysis of silicon-containing bis-phthalonitrile resin with enhanced solubility

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Abstract

Silicon-containing bis-phthalonitrile (SiPN) resin has been synthesized via multi-step synthetic route and characterized through spectroscopic (1H, 13C NMR and FT-IR) and thermal methods. The curing behaviour of the resin has been studied using differential scanning calorimetry (DSC). The uncured resin showed melting peak at 421 K with curing onset at 477 K and curing exotherm peak appeared at 519 K and curing end-set at 573 K. The processing and the curing windows of resin were observed to be 62 K and 72 K respectively. The DSC analysis of cured resin showed no glass transition temperature up-to 623 K. The thermal stability of crosslinked resin was assessed via thermo-gravimetric analyser (TGA). The TGA analysis of cured resin displayed ~ 5% decomposition at 730 K and char yield of 68% at 1073 K under nitrogen atmosphere with limiting oxygen index (LOI) value of 44.7, calculated via empirical method using (Krevelen’s equation). The resin showed 0.12% moisture absorption of when immersed in water for 48 h.

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Acknowledgements

The authors would like to acknowledge Director, DMSRDE Kanpur for providing financial and technical support to accomplish the work. Authors acknowledge the support offered by Mr. Pankaj Sharma for contact angle measurement of samples.

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Authors and Affiliations

  1. Defence Materials and Stores Research and Development Establishment (DMSRDE), G.T. Road, Kanpur, 208013, India

    J. K. Bansiwal, Ajit Shankar Singh & D. S. Bag

  2. Defence Institute of Advanced Technology (DIAT), Pune, 411025, India

    T. U. Patro

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  2. Ajit Shankar Singh
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  4. D. S. Bag
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Contributions

All authors have contributed to the study conception and design. Material preparation was done Mr. Jeetendra Kumar Banshiwal and Dr. Ajit Shankar Singh. Data collection and analysis were performed by Mr. Jeetendra Kumar Banshiwal, T.U. Patro, Dr. Ajit Shankar Singh and D. S. Bag The first draft of the manuscript was written by Dr. Ajit Shankar Singh and all authors commented on previous versions of the manuscript. All authors read and approved the final manuscript.

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Correspondence to Ajit Shankar Singh.

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Bansiwal, J.K., Singh, A.S., Patro, T.U. et al. Synthesis and thermal analysis of silicon-containing bis-phthalonitrile resin with enhanced solubility. J Therm Anal Calorim 148, 383–392 (2023). https://doi.org/10.1007/s10973-022-11853-z

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  • DOI: https://doi.org/10.1007/s10973-022-11853-z

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