Structure and Characterization of Sol-gel and Aerogel Materials and Oxidation Products from the Reaction of (CH3O)4Si and C16H33Si(OCH3)3
Abstract
Reactions of (CH3O)4Si and C16H33Si(OCH3)3 at various mole ratios were performed in methanol using base and acid catalysis. Sol-gel materials were formed that have low surface areas (approx. 10 sq m/g). Subsequent supercritical drying using CO2 at 40 deg. C produced materials that are very different than traditional aerogels, with surface areas around the same values as the corresponding sol-gels, as well as no detectable meso-pore features. In some cases the aerogels even melted upon heating. Spectroscopic characterization, using IR, Si-29 and C-13 NMR revealed normal Si-O substitution as well as incorporation of the carbon chain into the Si framework. Heating of the stable forms of the materials in air at different temperatures yielded, depending upon oxidation conditions, several materials with much higher surface areas, typical of aerogels. Pore size distribution measurements revealed meso-pore features with a narrow distribution around 35A. Spectroscopic characterization revealed the disappearance of the R-Si substitution and the appearance of an oxidized intermediate. This paper will describe the chemistry and characterization of these unusual sol-gels, aerogels, and oxidation products, as well as potential applications.
Document Details
- Document Type
- Technical Report
- Publication Date
- Jan 01, 2003
- Accession Number
- ADP014281
Entities
People
- John G. Reynolds
- Thomas M. Tillotson
Organizations
- Lawrence Livermore National Laboratory