62436-46-8Relevant articles and documents
Thermal Synthesis of Perchlorinated Oligosilanes: A Fresh Look at an Old Reaction
Neumeyer, Felix,Schweizer, Julia I.,Meyer, Lioba,Sturm, Alexander G.,Nadj, Andor,Holthausen, Max C.,Auner, Norbert
supporting information, p. 12399 - 12405 (2017/09/13)
A combined experimental and theoretical study of the high-temperature reaction of SiCl4 and elemental silicon is presented. The nature and reactivity of the product formed upon rapid cooling of the gaseous reaction mixture is investigated by comparison with the defined model compounds cyclo-Si5Cl10, n-Si5Cl12 and n-Si4Cl10. A DFT assessment provides mechanistic insight into the oligosilane formation. Experimental 29Si NMR investigations, supported by quantum-chemical 29Si NMR calculations, consistently show that the reaction product is composed of discrete molecular perchlorinated oligosilanes. Low-temperature chlorination is an unexpectedly selective means for the transformation of cyclosilanes to acyclic species by endocyclic Si?Si bond cleavage, and we provide a mechanistic rationalization for this observation. In contrast to the raw material, the product obtained after low-temperature chlorination represents an efficient source of neo-Si5Cl12 or the amine-stabilized disilene EtMe2N?SiCl2Si(SiCl3)2 through reaction with aliphatic amines.
POLYMERIZATION INHIBITOR FOR SILANE
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Paragraph 0041, (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.
Cyclopentasilane Si5H10: First single crystal X-ray structure of an oligosilane SixHy and thermal analysis with TG/MS
Schmidt, Dana,B?hme, Uwe,Seidel, Jürgen,Kroke, Edwin
, p. 92 - 95 (2013/10/08)
Cyclopentasilane Si5H10 (CPS) - a liquid silicon precursor - was crystallized in situ at - 100 C which allowed determination of the single crystal X-ray structure, showing short intermolecular distances below the sum of the v.d.Waals
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.
UV/Vis-Spectroscopic Investigations of Cyclosilanes
Stueger, Harald,Hengge, Edwin
, p. 873 - 888 (2007/10/02)
UV/Vis-spectra of Cyclosilanes (SiX2)n with X = Cl, Br, I, OMe and n = 4, 5, 6 are recorded and interpreted qualitatively.The spectra exhibit increasing influence of the substituents on the Si-Si-bond system within the rings in the order Cl OMe -> Br -> I.At the low energy side of the spectra weak absorption bands, possibly due to intramolecular charge transfer transitions, appear.The strong inductive effect of the electronegative substituents is documented by a marked increase of the first IP's compared to permethylcyclosilanes. - Keywords: Cyclopolysilanes; UV/vis-spectra
