Investigation of hydrolysis and condensation in organically modified sol-gel systems: {sup 29}Si NMR and the INEPT sequence

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The spectral editing properties of the {sup 29}Si NMR INEPT heteronuclear transfer experiment have been utilized for the identification and characterization of hydrolysis and initial condensation products in methyltrimethoxysilane (MTMS) sol-gel materials. {sup 29}Si NMR assignments in MTMS are complicated by a small spectral dispersion ({approximately} 0.5 ppm) and two different {sup 29}Si-{sup 1}H J couplings. By using analytical expressions for the INEPT signal response with multiple heteronuclear J couplings, unambiguous spectral assignments can be made. For this organomethoxysilane the rate of hydrolysis was found to be very rapid and significantly faster than either the water or alcohol producing condensation ... continued below

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12 p.

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Alam, T.M.; Assink, R.A. & Loy, D.A. June 1, 1996.

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  • Sandia National Laboratories
    Publisher Info: Sandia National Labs., Albuquerque, NM (United States)
    Place of Publication: Albuquerque, New Mexico

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Description

The spectral editing properties of the {sup 29}Si NMR INEPT heteronuclear transfer experiment have been utilized for the identification and characterization of hydrolysis and initial condensation products in methyltrimethoxysilane (MTMS) sol-gel materials. {sup 29}Si NMR assignments in MTMS are complicated by a small spectral dispersion ({approximately} 0.5 ppm) and two different {sup 29}Si-{sup 1}H J couplings. By using analytical expressions for the INEPT signal response with multiple heteronuclear J couplings, unambiguous spectral assignments can be made. For this organomethoxysilane the rate of hydrolysis was found to be very rapid and significantly faster than either the water or alcohol producing condensation reactions. The hydrolysis species of both the MTMS monomer and its initial T{sup 1} condensation products follow statistical distributions that can be directly related to the extent of the hydrolysis reactions. The role of the statistical distribution of hydrolysis products on the production and synthetic control of organically modified sol-gels is discussed.

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12 p.

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OSTI as DE96010991

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  • Spring meeting of the Materials Research Society (MRS), San Francisco, CA (United States), 8-12 Apr 1996

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  • Other: DE96010991
  • Report No.: SAND--96-1308C
  • Report No.: CONF-960401--32
  • Grant Number: AC04-94AL85000
  • Office of Scientific & Technical Information Report Number: 244536
  • Archival Resource Key: ark:/67531/metadc669923

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  • June 1, 1996

Added to The UNT Digital Library

  • June 29, 2015, 9:42 p.m.

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  • April 14, 2016, 4:14 p.m.

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Alam, T.M.; Assink, R.A. & Loy, D.A. Investigation of hydrolysis and condensation in organically modified sol-gel systems: {sup 29}Si NMR and the INEPT sequence, article, June 1, 1996; Albuquerque, New Mexico. (digital.library.unt.edu/ark:/67531/metadc669923/: accessed October 21, 2017), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.