Synthesis and Properties of Branched Hydrogenated Nonasilanes and Decasilanes

Viktor Christopoulos, Markus Rotzinger, Maik Gerwig, Jürgen Seidel, Edwin Kroke, Michael Holthausen, Odo Wunnicke, Ana Torvisco, Roland Fischer, Michael Haas, Harald Stueger

Research output: Contribution to journalArticleResearchpeer-review

Abstract

Branched higher silicon hydrides Si nH2 n+2 with n > 6 were recently found to be excellent precursors for the liquid phase deposition of silicon films. Herein we report the gram-scale synthesis of the novel nona- and decasilanes (H3Si)3Si(SiH2) nSi(SiH3)3 (2: n = 1, 5: n = 2) from (H3Si)3SiLi and Cl(SiPh2) nCl by a combined salt elimination/dephenylation/hydrogenation approach. Structure elucidation of the target molecules was performed by NMR spectroscopy and X-ray crystallography. 2 and 5 are nonpyrophoric and exhibit a bathochromically shifted UV absorption compared to neopentasilane and the structurally related octasilane (H3Si)3SiSi(SiH3)3. TG-MS analysis elucidated increased decomposition temperatures and decreased ceramic yields for branched hydrosilanes relative to cyclopentasilane. Otherwise, very similar thermal properties were observed for hydrosilane oligomers with linear and branched structures.

Original languageEnglish
Pages (from-to)8820-8828
Number of pages9
JournalInorganic chemistry
Volume58
Issue number13
DOIs
Publication statusPublished - 1 Jul 2019

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X ray crystallography
Silicon
silicon films
Silanes
oligomers
Oligomers
Nuclear magnetic resonance spectroscopy
Hydrogenation
hydrogenation
crystallography
hydrides
elimination
liquid phases
Thermodynamic properties
thermodynamic properties
Salts
ceramics
salts
Decomposition
decomposition

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Synthesis and Properties of Branched Hydrogenated Nonasilanes and Decasilanes. / Christopoulos, Viktor; Rotzinger, Markus; Gerwig, Maik; Seidel, Jürgen; Kroke, Edwin; Holthausen, Michael; Wunnicke, Odo; Torvisco, Ana; Fischer, Roland; Haas, Michael; Stueger, Harald.

In: Inorganic chemistry, Vol. 58, No. 13, 01.07.2019, p. 8820-8828.

Research output: Contribution to journalArticleResearchpeer-review

Christopoulos, Viktor ; Rotzinger, Markus ; Gerwig, Maik ; Seidel, Jürgen ; Kroke, Edwin ; Holthausen, Michael ; Wunnicke, Odo ; Torvisco, Ana ; Fischer, Roland ; Haas, Michael ; Stueger, Harald. / Synthesis and Properties of Branched Hydrogenated Nonasilanes and Decasilanes. In: Inorganic chemistry. 2019 ; Vol. 58, No. 13. pp. 8820-8828.
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AU - Christopoulos, Viktor

AU - Rotzinger, Markus

AU - Gerwig, Maik

AU - Seidel, Jürgen

AU - Kroke, Edwin

AU - Holthausen, Michael

AU - Wunnicke, Odo

AU - Torvisco, Ana

AU - Fischer, Roland

AU - Haas, Michael

AU - Stueger, Harald

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N2 - Branched higher silicon hydrides Si nH2 n+2 with n > 6 were recently found to be excellent precursors for the liquid phase deposition of silicon films. Herein we report the gram-scale synthesis of the novel nona- and decasilanes (H3Si)3Si(SiH2) nSi(SiH3)3 (2: n = 1, 5: n = 2) from (H3Si)3SiLi and Cl(SiPh2) nCl by a combined salt elimination/dephenylation/hydrogenation approach. Structure elucidation of the target molecules was performed by NMR spectroscopy and X-ray crystallography. 2 and 5 are nonpyrophoric and exhibit a bathochromically shifted UV absorption compared to neopentasilane and the structurally related octasilane (H3Si)3SiSi(SiH3)3. TG-MS analysis elucidated increased decomposition temperatures and decreased ceramic yields for branched hydrosilanes relative to cyclopentasilane. Otherwise, very similar thermal properties were observed for hydrosilane oligomers with linear and branched structures.

AB - Branched higher silicon hydrides Si nH2 n+2 with n > 6 were recently found to be excellent precursors for the liquid phase deposition of silicon films. Herein we report the gram-scale synthesis of the novel nona- and decasilanes (H3Si)3Si(SiH2) nSi(SiH3)3 (2: n = 1, 5: n = 2) from (H3Si)3SiLi and Cl(SiPh2) nCl by a combined salt elimination/dephenylation/hydrogenation approach. Structure elucidation of the target molecules was performed by NMR spectroscopy and X-ray crystallography. 2 and 5 are nonpyrophoric and exhibit a bathochromically shifted UV absorption compared to neopentasilane and the structurally related octasilane (H3Si)3SiSi(SiH3)3. TG-MS analysis elucidated increased decomposition temperatures and decreased ceramic yields for branched hydrosilanes relative to cyclopentasilane. Otherwise, very similar thermal properties were observed for hydrosilane oligomers with linear and branched structures.

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