| Summary: | Results of structural and morphological investigations of methylsilsesquioxane finely divided particles synthesized by hydrolytic co-condensation of in situ alkoxylated methyltrichlorosilane and tetrachlorous silicon are presented. The silica-type hydrophobe particles have been obtained using the abovementioned method with an output of 98.7–99.4 wt% of the load. These particles have been identified as crystalline formations with a lattice period of 5.5–8.0 nm and an interplane distance of 0.92–1.04 nm in the near order. We show that unlike for well-known crystalline methylsilsesquioxanes, introduction of chemically bonded SiO4/2 fragments to the material structure leads to the formation of 2–3 μm-sized spherical particles from the initial 10–15 nm particles; these particles are responsible for the spherical morphology of the surface. A method of extracting siloxane nanoparticles (2.5–280 nm) from the reaction products has been described, the behavior of particles in suspension has been studied and particle dimensional parameters have been determined using helium−neon 0.6328 nm laser correlation spectroscopy.
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