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Si NMR, TGA and ATR-IR. Results showed an unusually high condensation yield of approximately 90% and two distinct silsesquioxane structures. No traces of the remaining isocyanate groups were found. Advanced morphological characterization of the ternary O-I hybrids was performed using a combination of electron microscopy and X-ray scattering techniques such as SEM, TEM, ESI-TEM, WAXS and temperature-dependent SAXS. Results showed the occurrence of spherical nanoparticles, associated with polysilsesquioxane, and ordered network grains, associated with PCL and/or PEG chains cross-linked by silsesquioxane cages. As a consequence, a four-phased nanostructured morphology was proposed. In this model, PCL and PEG are undistinguishable, while polysilsesquioxane nanoparticles are uniformly distributed throughout a homogeneous cross-linked matrix, which shows gel-like behavior. Moreover, a mobile phase made up of unbound polymer chains occurs at the grain interface.
Silva et al. (Mon,) studied this question.