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Open Access item Preparation of sol–gel hybrid materials from γ-methacryloxypropyltrimethoxysilane and tetramethyl orthosilicate: study of the hydrolysis and condensation reactions

Authors:El hadad, Amir A.
Carbonell, Diógenes
Barranco, Violeta
Jiménez-Morales, Antonia
Casal, Blanca
Galván Sierra, Juan Carlos
Keywords:Sol–gel, Silica, Organic–inorganic materials, Organopolysiloxane precursors, Si-29 and C-13 NMR, FTIR, Structural characterization
Issue Date:Sep-2011
Citation:Colloid & Polymer Science 289 (17-18) : 1875-1883 (2011)
Abstract:Organic–inorganic hybrid materials suitable for the development of sol–gel coatings for metallic surfaces were prepared by hydrolysis and condensation of γ- methacryloxypropyltrimethoxysilane (MAPTMS) and tetramethyl orthosilicate (TMOS). The hydrolysis of MAPTMS/ TMOS was carried out in an ethanol/water solution. The prehydrolysis stage of MAPTMS/TMOS system was monitored by Fourier transform infrared spectroscopy (FTIR) and liquid-state 29Si and 13C nuclear magnetic resonance (29Si and 13C NMR). FTIR analysis indicated that the hydrolysis of MAPTMS/TMOS was accomplished as far as the (SiOMe) band corresponding to unhydrolyzed silane disappeared. The concentration of the alkoxy groups and the extent of self-condensation of mono-, di-, and trisubstituted siloxanes (T species) in the sol were estimated by using liquid-state 29Si NMR spectroscopy. The hydrolysis of the prepared sol was also evaluated by liquid-state 13C NMR spectroscopy. The results indicated that under the adopted synthesis strategy conditions, the hydrolysis process requires 4 h to be completed.
Publisher version (URL):http://dx.doi.org/10.1007/s00396-011-2504-y
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