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

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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.

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Acknowledgments

This work has been supported by the Ministry of Science and Innovation of Spain (Projects MAT2006-04486 and MAT2009-13530) and the Regional Community of Madrid (Project 2009/MAT-1585). AA El hadad acknowledges a predoctoral contract JAE financed by CSIC, and VB acknowledges a Ramon y Cajal researcher contract financed by CSIC-MICINN.

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Authors and Affiliations

  1. Centro Nacional de Investigaciones Metalúrgicas (CSIC), Madrid, Spain

    Amir A. El hadad, Blanca Casal & Juan Carlos Galván

  2. Departamento de Ciencia e Ingeniería de Materiales e Ingeniería Química, Universidad Carlos III de Madrid, Madrid, Spain

    Diogenes Carbonell & Antonia Jiménez-Morales

  3. Instituto de Ciencia de Materiales de Madrid (CSIC), Madrid, Spain

    Violeta Barranco

Authors
  1. Amir A. El hadad
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  2. Diogenes Carbonell
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  3. Violeta Barranco
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  4. Antonia Jiménez-Morales
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  5. Blanca Casal
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  6. Juan Carlos Galván
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Corresponding author

Correspondence to Juan Carlos Galván.

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El hadad, A.A., Carbonell, D., Barranco, V. et al. Preparation of sol–gel hybrid materials from γ-methacryloxypropyltrimethoxysilane and tetramethyl orthosilicate: study of the hydrolysis and condensation reactions. Colloid Polym Sci 289, 1875–1883 (2011). https://doi.org/10.1007/s00396-011-2504-y

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  • DOI: https://doi.org/10.1007/s00396-011-2504-y

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