Formation of borosilicate glasses from silicon alkoxides and metaborate esters in dry non-aqueous solvents |
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Authors: | Michael A. Beckett Martin P. Rugen-Hankey K. Sukumar Varma |
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Affiliation: | (1) Department of Chemistry, University of Wales, Bangor, Gwynedd, LL57 2UW, UK;(2) Pilkington Building Products R and D, European Technical Centre, Lathom, Lancashire, L40 5UF, UK |
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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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Keywords: | Borosilicate glass Metaborate esters NMR (29Si, 11B) |
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