289-22-5Relevant articles and documents
POLYMERIZATION INHIBITOR FOR SILANE
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Paragraph 0042, (2017/06/02)
To provide a silane polymerization inhibitor in order to enable a cyclic silane to be present in a monomer state without a polymer being formed, even if heating by way of distillation is performed, said silane polymerization inhibitor enabling the cyclic silane to be purified further than when heated and distilled. To use the polymerization inhibitor to obtain a highly pure cyclic silane, particularly a highly pure cyclopentasilane. To apply, to a substrate, as a coating-type polysilane composition, a composition including polysilane obtained by polymerizing the cyclic silane, and bake the composition to subsequently provide an excellent silicon thin film exhibiting high electrical conductivity. This silane polymerization inhibitor includes a secondary or tertiary aromatic amine. The silane is a cyclic silane. The silane is a cyclopentasilane. The aromatic amine is a secondary aromatic amine. The aromatic group is a phenyl group or a naphthyl group. 0.01-10 mol% of the polymerization inhibitor is included per mole of the silane. In the polymerization inhibitor, the boiling point of the aromatic amine is at least 196 DEG C.
Partial halogenation of cyclic and branched perhydropentasilanes
Stueger, Harald,Mitterfellner, Thomas,Fischer, Roland,Walkner, Christoph,Patz, Matthias,Wieber, Stephan
, p. 6173 - 6179 (2012/07/14)
The perhydropentasilanes (H3Si)4Si and Si 5H10 were chlorinated with SnCl4 to give chlorohydropentasilanes without destruction of the Si-Si backbone. Tetrachloroneopentasilane (ClH2Si)4Si (2) was prepared in high yield from (H3Si)4Si and 3.5 equiv of SnCl 4, while Si5H10 and an equimolar amount of SnCl4 afforded a mixture of ～60% of ClSi5H9 (1) with polychlorinated cyclopentasilanes and unreacted starting material, which could not be separated by distillation. The selective monochlorination of Si5H10 was achieved starting from MesSi5Cl 9 (3; Mes = 2,4,6-trimethylphenyl) or TBDMP-Si5Cl 9 (4; TBDMP = 4-tert-butyl-2,6-dimethylphenyl). 3 or 4 was successfully hydrogenated with LiAlH4 to give MesSi5H 9 (6) or TBDMP-Si5H9 (7), which finally gave 1 along with aryl-H and Si5H10 after treatment with an excess of liquid anhydrous HCl. All compounds were characterized by standard spectroscopic techniques. For Si-H derivatives, the coupled 29Si NMR spectra were analyzed in detail to obtain an unequivocal structural assignment. The molecular structures of 2-4 were further confirmed by X-ray crystallography.
Inorganic Bi(cyclopentasilanyls): Synthesis and Spectroscopic Characterization
Stueger, Harald,Lassacher, Paul,Hengge, Edwin
, (2008/10/08)
Nonachloro- or nonabromocyclopentasilane, which are accessible from nonaphenylcyclopentasilane with HX/AlX3 (X=Cl, Br), easily can be converted to the bicyclic oligosilanes bi(nonachlorocyclopentasilanyl) (7) and bi(nonabromocyclopentasilanyl) (8) upon treatment with (t-Bu)2Hg. The phenylderivative bi(nonaphenylcycopentasilanyl) (6) can be synthesized from bromononaphenylcyclopentasilanyl) with naphthyllithium. The reaction of 6with HX/AlX3 again affords 7 or 8. When 7 or 8 are reacted with LiAlH4, about 15% of cyclopentasilane are obtained along with the expected prod uct bi(cyclopentasilanyl), what demonstrates the remarkable sensitivity of the central Si-Si bond in 7 and 8 towards nucleophilic attack. A smaller binding energy of the central Si-Si bond in 7 and 9, however, cannotbe deduced from mass spectroscopic studies.
