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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Sol–gel analogous aminolysis–ammonolysis of chlorosilanes to chlorine-free Si/(C)/N–materials
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Sol–gel analogous aminolysis–ammonolysis of chlorosilanes to chlorine-free Si/(C)/N–materials

机译：溶胶-凝胶类似的氨解-氯硅烷氨解成无氯的Si /（C）/ N-材料

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摘要

Large amounts of chlorosilanes, especially SiCl4 and CH3SiCl3, are produced as side-products of the industrial fabrication of solar or electronic grade silicon and the M¨uller–Rochow process. It was a goal of the present study to transform these compounds into useful chlorine-free precursors for Si/(C)/N ceramics via a sol–gel analogous liquid processing route. Chlorine substitution of the chlorosilanes (mixtures) with diethylamine did not yield chlorine-free products, complete reactions are only possible with lithium diethylamide. However, aminolyses with n-propylamine were successful. Transamination with ammonia was not possible with diethylaminosilanes but was with n-propylaminosilanes in various solvents. This result was attributed to steric reasons and polar interactions of the N–H groups. Colourless solid or liquid polysilazanes were obtained, depending on the silane (mixture) and the solvent. Transamination reactions of CH3Si(NH-n-Pr)3 in chloroform reproducibly yielded a cage-like oligosilazane of the composition (CH3)9Si9(NH)12N. Single crystal X-ray structure analysis revealed a seven-cyclic cluster containing four six- and three ten-membered silazane rings. This unique silazane cage as well as the other aminosilanes and the silazanes were comprehensively characterised using multi-nuclear solid state and solution NMR, elemental analyses and thermal gravimetry (TGA).
机译：大量的氯硅烷，特别是SiCl4和CH3SiCl3，是太阳能或电子级硅的工业生产和穆勒-罗霍工艺的副产品。本研究的目标是通过溶胶-凝胶类似的液体加工路线将这些化合物转变为适用于Si /（C）/ N陶瓷的无氯前体。用二乙胺对氯硅烷（混合物）进行氯取代不能得到不含氯的产物，只有与二乙胺化锂才能完全反应。然而，用正丙胺进行的氨解是成功的。用二乙基氨基硅烷不可能用氨进行氨基转移，但是在各种溶剂中用正丙基氨基硅烷则不能。该结果归因于空间原因和N–H组的极性相互作用。根据硅烷（混合物）和溶剂，获得无色固体或液体聚硅氮烷。 CH3Si（NH-n-Pr）3在氯仿中的氨基转移反应可重复生成笼形的低聚硅氮烷，其组成为（CH3）9Si9（NH）12N。单晶X射线结构分析显示一个七环簇，其中包含四个六元和三个十元硅氮烷环。使用多核固态和溶液NMR，元素分析和热重分析（TGA），对这种独特的硅氮烷笼以及其他氨基硅烷和硅氮烷进行了全面表征。

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