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Formation of borosilicate glasses from silicon alkoxides and metaborate esters in dry non-aqueous solvents

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Abstract

The reaction of metaborate esters (RO)3B3O3 [R = Me, Et, ClCH2CH2–, Cl3CCH2–, ClCH2CH2CH2–, (ClCH2)2CH–] with Si(OR)4 (R = Me, Et), either neat or in dry propan-2-one or dry THF at room temperature, led to gels which when dried and heated in air for 20 mins at 600°C afforded borosilicate glasses in high ceramic yields. The dried gels and glasses were characterized by elemental analysis, TGA, IR, and powder XRD, and solid-state MAS 29Si and 11B NMR. The gelling reaction was investigated by solution 11B and 29Si NMR. These NMR studies indicated B–O–Si reaction intermediates and a mechanism involving alkoxy exchange and various condensation/elimination reactions of the borosilicate esters have been proposed.

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Authors and Affiliations

  1. Department of Chemistry, University of Wales, Bangor, Gwynedd, LL57 2UW, UK

    Michael A. Beckett & Martin P. Rugen-Hankey

  2. Pilkington Building Products R and D, European Technical Centre, Lathom, Lancashire, L40 5UF, UK

    K. Sukumar Varma

Authors
  1. Michael A. Beckett
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  2. Martin P. Rugen-Hankey
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  3. K. Sukumar Varma
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Correspondence to Michael A. Beckett.

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Beckett, M.A., Rugen-Hankey, M.P. & Varma, K.S. Formation of borosilicate glasses from silicon alkoxides and metaborate esters in dry non-aqueous solvents. J Sol-Gel Sci Technol 39, 95–101 (2006). https://doi.org/10.1007/s10971-006-8972-8

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  • DOI: https://doi.org/10.1007/s10971-006-8972-8

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