Federal State Research and Design Institute of Rare Metal Industry

P. A. Averichkin, Y. B. Andrusov, I. A. Denisov, Y. N. Parkhomenko, N. A. Smirnova

Chemical and Metallurgical Holding «Metal»

T. B. Klytchbaev

The results of structural and morphological investigations of methylsilsesquioxane finely divided particles synthesized by hydrolytical co−condensation of methyltrichlorosilane and tetrachlorous silicon alcocksilined «in situ» are presented. The silica−type hydrophobe particles were obtained using above mentioned method with the result of 98.7—99.4 % (mass) compared to load. These particles were identified as crystalline formations with lattice period of 5.5—8.0 nm and inter−planery distance 0.92—1.04 nm in near order. It is shown that in contrast to well−known crystalline methylsilsesquioxanes introduction of chemically bonded SiO_4/2 fragments in material structure leads to formation of 2—3 micrometer−size spherical particles from primarily existed 10—15 nm particles; these namely particles are responsible for spherical surface morphology. The method of extraction of siloxane nano−particles (2.5—280 nm) from products of reaction was described; the behavior of particles in suspension was studied and particle dimensional parameters were determined with the help of helium−neon 0.6328 nm laser correlation spectroscopy.

1. Andrianov, K. A. Polimery s neorganicheskimi glavnymi tsepyami makromolekul / K. A. Andrianov − M. : Izd. AN SSSR, 1962. − 360 s.
2. Andrianov, K. A. O gidroliticheskoy polikondensatsii metiltrikhlorsilana / K. A. Andrianov, T. V. Vasil'eva, B. I. D'yachenko // Izv. AN SSSR. ser. Khimiya. − 1973. − T. 1. − S. 76—79.
3. Vasil'eva, T. V. O produktakh gidroliticheskoy polikondensatsii metiltrikhlorsilana / T. V. Vasil'eva, K. A. Andrianov, N. M. Katashuk // Vysokomolekulyarnye soedineniya. − 1976. − T. 17, № 6. − S. 1270—1275.
4. Andrianov, K. A. / K. A. Andrianov, T. V. Vasil'eva, B. I. D'yachenko // Izv. AN SSSR. ser. Khimiya. − 1977. − № 2. − S. 420—422.
5. Andrianov, K. A. Gidroliticheskaya polikondensatsiya chetyrekhkhloristogo kremniya v smesi s organokhlorsilanami razlichnoy funktsional'nosti / K. A. Andrianov, T. V. Vasil'eva, B. I. D'yachenko // Zhurnal obshchey khimii. − 1973. − T. 43. − S. 2458—2462.
6. Vasil'eva, T. V. Gidroliticheskaya polikondensatsiya chetyrekhkhloristogo kremniya v smesi s organokhlorsilanami / T. V. Vasil'eva, K. A. Andrianov, B. I. D'yachenko // Tam zhe. − 1973. − T. 43. − S. 768—771.

7. Andrianov, K. A. O gidroliticheskoy polikondensatsii organokhlorsilanov s chetyrekhkhloristym kremniem ili kremnevymi kislotami pri vysokikh funktsional'nostyakh smesey / K. A. Andrianov, N. M. Petrovnina, T. V. Vasil'eva // Tam zhe. − 1973. − T. 48, vyp. 12. − S. 2454—2458.
8. Larsson, K. // Ark. kemi. − 1960. − N 16. − P. 203—206.
9. Barry, A. J. Cristalline organosilsesqioxanes / A. J. Barry, W. H. Daudt, J. J. Domicone, J. M. Gilkey // J. Amer. Chem. Soc. − 1955. − V. 77. − P. 4248—4252.
10. Averichkin, P. A. Izgotovlenie podlozhek na osnove CdZnTe s ispol'zovaniem poliedricheskikh metilsilseskvioksanov / P. A. Averichkin, Yu. B. Andrusov, M. B. Grishechkin, I. A. Denisov, N. A. Smirnova // Izv. vuzov. Materialy elektron. tekhniki. − 2011. − № 1. − S. 12—15.
11. Averichkin, P. A. Gidroliticheskaya polikondensatsiya alkoksilirovannykh (in situ) organokhlorsilanov nepreryvnym sposobom / P. A. Averichkin, E. A. Chernyshev // Tez. dokl. «I Kremniyorganicheskiy mikrosimpozium». − M., 1994. − S. 22—23.
12. Pat. RF № 2444539. Sposob polucheniya poliedricheskikh organosilseskvioksanov / P. A. Averichkin, Yu. B. Andrusov, I. A. Denisov, V. A. Kal'nov, Yu. N. Parkhomenko, N. A. Smirnova // (Zayavl. 05.10. 2010 g.; Opubl. 10.03.2012 g.; Byull. № 7.
13. Koptyug, V. A. IK−spektry kislorodsoderzhashchikh kremniyorganicheskikh soedineniy. − Novosibirsk; 1986. − 182 s.
14. Svergun, D. I. Rentgenovskoe i neytronnoe malouglovoe rasseyanie / D. I. Svergun, L. A. Feygin. − M. : Nauka, 1986. − 230 s.
15. Lebedev, A. D. Primenenie lazernoy korrelyatsionnoy spektroskopii dlya izucheniya EF biologicheskikh ob"ektov v rastvorakh. Instrumental'nye metody v fiziologii i biofizike / A. D. Lebedev, A. V. Lomakin, V. A. Noskin. − L. : Nauka, 1987. − S. 90—95.
16. Kaszuba, M. / M. Kaszuba, D. McKnight, M. Connah, F. McNeil // J. Nanopart Res. − 2007. − V. 1. − P. 34—41.
17. Volchek, B. E. / B. E. Volchek, A. P. Purkina, N. N. Nikitin // Vysokomol. soed. − 1976. − T. 8A. − S. 1203—1207.
18. Voronkov, M. G. Siloksanovaya svyaz' / M. G. Voronkov, V. P. Mileshkevich, Yu. A. Yuzhelevskiy. − Novosibirsk : Nauka, 1976. − 413 s.