Skip to main content
U.S. flag

An official website of the United States government

Official websites use .gov
A .gov website belongs to an official government organization in the United States.

Secure .gov websites use HTTPS
A lock ( ) or https:// means you’ve safely connected to the .gov website. Share sensitive information only on official, secure websites.

29Si NMR and SAXS investigation of the hybrid organic-inorganic glasses obtained by consolidation of the melting gels

Published

Author(s)

Andrei Jitianu, Sylvian Cadars, Fan Zhang, Gabriela Rodriguez, Quentin Picard, Mario Aparicio, Jadra Mosa, Lisa C. Klein

Abstract

This study is focused on structural characterization of hybrid glasses obtained by consolidation of melting gels. The melting gels were prepared in molar ratios of methyltriethoxysilane (MTES) and dimethyldiethoxysilane (DMDES) of 75%MTES-25%DMDES and 65%MTES-35%DMDES. Following consolidation, the hybrid glasses were characterized using Raman, 29Si and 13C Nuclear Magnetic Resonance (NMR) spectroscopies, synchrotron Small Angle X-Ray Scattering (SAXS) and scanning electron microscopy (SEM). Raman spectroscopy revealed the presence of Si-C bonds in the hybrid glasses and 8-membered ring structures in the Si-O-Si network. Qualitative NMR spectroscopy identified the main molecular species, while quantitative NMR data showed that the ratio of trimers (T) to dimers (D) varied between 4.6 and 3.8. Two-dimensional 29Si NMR data were used to identify two distinct types of T3 environments. SAXS data showed that the glasses are homogeneous across the nm to micrometer length scales. The scattering cross section was one thousand times lower than what is expected when phase separation occurs. The SEM images show a uniform surface without defects, in agreement with the SAXS results, which further supports that the hybrid glasses are nonporous.
Citation
Dalton Transactions
Volume
46

Keywords

hybrid organic-inorganic glass, structural characterization, NMR, small angle X-ray scattering

Citation

Jitianu, A. , Cadars, S. , Zhang, F. , Rodriguez, G. , Picard, Q. , Aparicio, M. , Mosa, J. and Klein, L. (2017), 29Si NMR and SAXS investigation of the hybrid organic-inorganic glasses obtained by consolidation of the melting gels, Dalton Transactions, [online], https://doi.org/10.1039/C6DT04394A (Accessed June 17, 2024)

Issues

If you have any questions about this publication or are having problems accessing it, please contact reflib@nist.gov.

Created March 14, 2017, Updated October 12, 2021