Synthesis of nanozirconooligocarbosilanes |
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Authors: | P A Storozhenko G I Shcherbakova A M Tsirlin E K Florina E A Izmailova A A Savitskii M G Kuznetsova T M Kuznetsova I V Stolyarova G Yu Yurkov S P Gubin |
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Affiliation: | (1) State Research Institute of Chemistry and Technology of Organoelement Compounds, sh. Entuziastov 38, Moscow, 111123, Russia;(2) Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences, Leninskii pr. 31, Moscow, 119991, Russia |
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Abstract: | We describe the first chlorine-free synthesis of nanozirconooligocarbosilanes through thermal cocondensation of low-molecular oligocarbosilanes and zirconium tetrakis(diethylamide). The starting reagents, reaction intermediates, and final products have been characterized by 1H, 13C, and 29Si nuclear magnetic resonance, UV and IR spectroscopy, gel-permeation chromatography, thermogravimetry, transmission electron microscopy (TEM), and elemental analysis. The synthesized nanozirconooligocarbosilanes have been used to fabricate ceramic fibers and matrices through thermal and chemical processing. TEM results demonstrate that the particles of zirconium and products of its reactions with silicon, carbon, and nitrogen range in size from 10 to 20 nm in the oligomers and from 20 to 30 nm in the ceramics. |
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