Abstract
Octa(aminophenyl)-T8-polyhedral silsesquioxane, 1, can serve as a cross-linking agent for organic polymeric resins. Amino functional groups of 1 can form chemical bonds or hydrogen-bonds to appropriate matrix polymers or resins. Various resole phenolic resin/1 nanocomposites (0, 1, 3, 6, and 12 wt% 1) were prepared. Hydrogen bonding between phenolic hydroxyls and the amino groups of 1 in these nanocomposites were investigated by FT-IR. The aggregation morphologies of 1 within these samples were examined using SEM, TEM, and Wide Angle X-ray Diffraction (WAXD) studies. Small quasispherical nanometer-sized POSS particles which were further aggregated into clusters, like individual grapes in a bunch, formed into phase-separated domains as large as 400 nm in diameter as the loading of 1 increased. These particles exhibited a broad 2θ = 5.8° WAXD peak indicating the presence of some crystalline order within the nanoparticles of 1 making up the aggregates. This corresponds to an average crystalline plane lattice distance of 17.5 A. However, extraction of the finely powdered nanocomposites by refluxing THF failed to remove 1 indicating the vast majority of 1 must be chemically bound. Thus, the aggregates must have resin within their structure. The storage modulus (E') in both the glassy and rubbery regions, thermal stability, and glass transition temperature of the composites were improved by 1 wt% 1. However, at high loadings of 1, these properties gradually decreased. Surface extractions by THF removed only a portion of the 1 in the surface regions based on X-EDS analyses for Si, suggesting that a portion of 1 might chemically bond into the phenolic resin matrix during the cure. As the loading of 1 increased, the content of 1 at specific surface locations gradually tends to increase and confirmed excellent dispersion of 1 in the micron size-scale at all locations.
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