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Influence of Heat Treatment Temperature on the Microstructure Evolution of Poly(vinylborosiloxane) Derived Ceramics

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Abstract

Polycondensation of boric acid and vinyltriethoxysilane in 1:2, 1:1.5 and 1:1 mole ratio in diglyme at 83–87 °C for 3 h using hydrochloric acid as catalyst afforded vinylfunctionalized borosiloxane oligomers soluble in the reaction medium. Complete removal of ethanol, the by-product, and diglyme rendered the oligomers intractable due to the advancement of polycondensation. They were characterized by FTIR and TGA and converted to ceramics by heat treatment at 900 °C, 1500 °C and 1650 °C in argon atmosphere. The ceramics obtained were characterized by IR, Raman, 13C-and 29Si-solid state NMR spectroscopy and XRD. These studies infer the formation of SiOC/SiBOC glass on pyrolysis of these oligomers at 900 °C and onset of formation of β-SiC at 1500 °C. On further heat treatment at 1650 °C, complete conversion of the ceramic to a mixture of α and β-SiC was observed along with the presence of diamond like carbon phases.

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Author notes

  1. B. Swaminathan

    Present address: R&D Center, Udaipur Minerals Development Syndicate Private Limited, 4th Floor, Golcha Trade Center, MI Road, Jaipur, 302001, India

  2. S. Packirisamy

    Present address: Advanced Polymeric Materials Laboratory, Department of Chemistry and Biochemistry, School of Basic Sciences and Research, Sharda University, 32-34 Knowledge Park 3, Greater Noida, 201 306, India

Authors and Affiliations

  1. Ceramic Matrix Products Division, Analytical, Spectroscopy and Ceramics Group, PCM Entity, Vikram Sarabhai Space Centre, Thiruvananthapuram, 695 022, India

    Deepa Devapal, K. J. Sreejith, B. Swaminathan & S. Packirisamy

  2. Analytical and Spectroscopy Division, Analytical, Spectroscopy and Ceramics Group, PCM Entity, Vikram Sarabhai Space Centre, Thiruvananthapuram, 695 022, India

    Srinivas Chinthalapalli & S. Bhuvaneswari

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  1. Deepa Devapal
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Devapal, D., Sreejith, K.J., Swaminathan, B. et al. Influence of Heat Treatment Temperature on the Microstructure Evolution of Poly(vinylborosiloxane) Derived Ceramics. J Inorg Organomet Polym 30, 2224–2233 (2020). https://doi.org/10.1007/s10904-020-01457-1

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