Thermal rearrangements during liquid–vapor phase pyrolysis polycondensation of polysilane to high-functional polycarbosilane: spectral and thermal studies
Abstract Thermally induced Kumada rearrangement of –Si–Si– linear chains in polysilanes to –Si–C– chain was conducted in the liquid–vapor phase, followed by isothermal treatments at 410, 460 °C and pressure of 15 kgf $ cm^{−2} $ leading to polycarbosilane(PCS) with higher silane (–Si–H) content in t...
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| Autor*in: |
Krishnan, G. Santhana [verfasserIn] |
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| Format: |
Artikel |
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| Sprache: |
Englisch |
| Erschienen: |
2021 |
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| Schlagwörter: |
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| Anmerkung: |
© Akadémiai Kiadó, Budapest, Hungary 2021 |
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| Übergeordnetes Werk: |
Enthalten in: Journal of thermal analysis and calorimetry - Springer International Publishing, 1998, 147(2021), 2 vom: 05. Jan., Seite 1251-1264 |
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| Übergeordnetes Werk: |
volume:147 ; year:2021 ; number:2 ; day:05 ; month:01 ; pages:1251-1264 |
| Links: |
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| DOI / URN: |
10.1007/s10973-020-10459-7 |
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| Katalog-ID: |
OLC2077777559 |
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| 520 | |a Abstract Thermally induced Kumada rearrangement of –Si–Si– linear chains in polysilanes to –Si–C– chain was conducted in the liquid–vapor phase, followed by isothermal treatments at 410, 460 °C and pressure of 15 kgf $ cm^{−2} $ leading to polycarbosilane(PCS) with higher silane (–Si–H) content in the range 0.46–0.58 mass%. Molecular and thermal changes during the oligomer to polymer transformation were investigated, applying spectral and thermal techniques. FTIR, Raman, and 1H, 13C, and 29Si-NMR analytical results established the chemical structural formula, –Si–Si–, –Si–C–, –Si–H bonding networks, and evolution of –Si–H functionality in as-synthesized polycarbosilane during the thermal transformations. FTIR and 29Si-NMR studies followed the increase in silane content (–Si–H). Raman data revealed the formation and disappearance of –Si–Si– functional group as the transformation progresses. Average molecular mass increased proportionally with polymerization reaction time. Thermogravimetric studies at 1400 °C confirmed a polymer to ceramic conversion (ceramic yield) of as-synthesized PCS increased with the increase in mass average molecular mass and found to be as high as 88% mass. The formation of a high purity green β-SiC powder on heat treatment at 1500 °C confirmed the high molecular polycarbosilane. | ||
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10.1007/s10973-020-10459-7 doi (DE-627)OLC2077777559 (DE-He213)s10973-020-10459-7-p DE-627 ger DE-627 rakwb eng 660 VZ Krishnan, G. Santhana verfasserin (orcid)0000-0001-9175-1907 aut Thermal rearrangements during liquid–vapor phase pyrolysis polycondensation of polysilane to high-functional polycarbosilane: spectral and thermal studies 2021 Text txt rdacontent ohne Hilfsmittel zu benutzen n rdamedia Band nc rdacarrier © Akadémiai Kiadó, Budapest, Hungary 2021 Abstract Thermally induced Kumada rearrangement of –Si–Si– linear chains in polysilanes to –Si–C– chain was conducted in the liquid–vapor phase, followed by isothermal treatments at 410, 460 °C and pressure of 15 kgf $ cm^{−2} $ leading to polycarbosilane(PCS) with higher silane (–Si–H) content in the range 0.46–0.58 mass%. Molecular and thermal changes during the oligomer to polymer transformation were investigated, applying spectral and thermal techniques. FTIR, Raman, and 1H, 13C, and 29Si-NMR analytical results established the chemical structural formula, –Si–Si–, –Si–C–, –Si–H bonding networks, and evolution of –Si–H functionality in as-synthesized polycarbosilane during the thermal transformations. FTIR and 29Si-NMR studies followed the increase in silane content (–Si–H). Raman data revealed the formation and disappearance of –Si–Si– functional group as the transformation progresses. Average molecular mass increased proportionally with polymerization reaction time. Thermogravimetric studies at 1400 °C confirmed a polymer to ceramic conversion (ceramic yield) of as-synthesized PCS increased with the increase in mass average molecular mass and found to be as high as 88% mass. The formation of a high purity green β-SiC powder on heat treatment at 1500 °C confirmed the high molecular polycarbosilane. Ceramic-yielding polymers High molecular mass Pressure pyrolysis polycondensation Solvent fractionation Naveen, S. aut Shahnawaz, M. aut Enthalten in Journal of thermal analysis and calorimetry Springer International Publishing, 1998 147(2021), 2 vom: 05. Jan., Seite 1251-1264 (DE-627)244148767 (DE-600)1429493-X (DE-576)066397693 1388-6150 nnns volume:147 year:2021 number:2 day:05 month:01 pages:1251-1264 https://doi.org/10.1007/s10973-020-10459-7 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_OLC SSG-OLC-TEC SSG-OLC-CHE SSG-OLC-PHA SSG-OLC-DE-84 AR 147 2021 2 05 01 1251-1264 |
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10.1007/s10973-020-10459-7 doi (DE-627)OLC2077777559 (DE-He213)s10973-020-10459-7-p DE-627 ger DE-627 rakwb eng 660 VZ Krishnan, G. Santhana verfasserin (orcid)0000-0001-9175-1907 aut Thermal rearrangements during liquid–vapor phase pyrolysis polycondensation of polysilane to high-functional polycarbosilane: spectral and thermal studies 2021 Text txt rdacontent ohne Hilfsmittel zu benutzen n rdamedia Band nc rdacarrier © Akadémiai Kiadó, Budapest, Hungary 2021 Abstract Thermally induced Kumada rearrangement of –Si–Si– linear chains in polysilanes to –Si–C– chain was conducted in the liquid–vapor phase, followed by isothermal treatments at 410, 460 °C and pressure of 15 kgf $ cm^{−2} $ leading to polycarbosilane(PCS) with higher silane (–Si–H) content in the range 0.46–0.58 mass%. Molecular and thermal changes during the oligomer to polymer transformation were investigated, applying spectral and thermal techniques. FTIR, Raman, and 1H, 13C, and 29Si-NMR analytical results established the chemical structural formula, –Si–Si–, –Si–C–, –Si–H bonding networks, and evolution of –Si–H functionality in as-synthesized polycarbosilane during the thermal transformations. FTIR and 29Si-NMR studies followed the increase in silane content (–Si–H). Raman data revealed the formation and disappearance of –Si–Si– functional group as the transformation progresses. Average molecular mass increased proportionally with polymerization reaction time. Thermogravimetric studies at 1400 °C confirmed a polymer to ceramic conversion (ceramic yield) of as-synthesized PCS increased with the increase in mass average molecular mass and found to be as high as 88% mass. The formation of a high purity green β-SiC powder on heat treatment at 1500 °C confirmed the high molecular polycarbosilane. Ceramic-yielding polymers High molecular mass Pressure pyrolysis polycondensation Solvent fractionation Naveen, S. aut Shahnawaz, M. aut Enthalten in Journal of thermal analysis and calorimetry Springer International Publishing, 1998 147(2021), 2 vom: 05. Jan., Seite 1251-1264 (DE-627)244148767 (DE-600)1429493-X (DE-576)066397693 1388-6150 nnns volume:147 year:2021 number:2 day:05 month:01 pages:1251-1264 https://doi.org/10.1007/s10973-020-10459-7 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_OLC SSG-OLC-TEC SSG-OLC-CHE SSG-OLC-PHA SSG-OLC-DE-84 AR 147 2021 2 05 01 1251-1264 |
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10.1007/s10973-020-10459-7 doi (DE-627)OLC2077777559 (DE-He213)s10973-020-10459-7-p DE-627 ger DE-627 rakwb eng 660 VZ Krishnan, G. Santhana verfasserin (orcid)0000-0001-9175-1907 aut Thermal rearrangements during liquid–vapor phase pyrolysis polycondensation of polysilane to high-functional polycarbosilane: spectral and thermal studies 2021 Text txt rdacontent ohne Hilfsmittel zu benutzen n rdamedia Band nc rdacarrier © Akadémiai Kiadó, Budapest, Hungary 2021 Abstract Thermally induced Kumada rearrangement of –Si–Si– linear chains in polysilanes to –Si–C– chain was conducted in the liquid–vapor phase, followed by isothermal treatments at 410, 460 °C and pressure of 15 kgf $ cm^{−2} $ leading to polycarbosilane(PCS) with higher silane (–Si–H) content in the range 0.46–0.58 mass%. Molecular and thermal changes during the oligomer to polymer transformation were investigated, applying spectral and thermal techniques. FTIR, Raman, and 1H, 13C, and 29Si-NMR analytical results established the chemical structural formula, –Si–Si–, –Si–C–, –Si–H bonding networks, and evolution of –Si–H functionality in as-synthesized polycarbosilane during the thermal transformations. FTIR and 29Si-NMR studies followed the increase in silane content (–Si–H). Raman data revealed the formation and disappearance of –Si–Si– functional group as the transformation progresses. Average molecular mass increased proportionally with polymerization reaction time. Thermogravimetric studies at 1400 °C confirmed a polymer to ceramic conversion (ceramic yield) of as-synthesized PCS increased with the increase in mass average molecular mass and found to be as high as 88% mass. The formation of a high purity green β-SiC powder on heat treatment at 1500 °C confirmed the high molecular polycarbosilane. Ceramic-yielding polymers High molecular mass Pressure pyrolysis polycondensation Solvent fractionation Naveen, S. aut Shahnawaz, M. aut Enthalten in Journal of thermal analysis and calorimetry Springer International Publishing, 1998 147(2021), 2 vom: 05. Jan., Seite 1251-1264 (DE-627)244148767 (DE-600)1429493-X (DE-576)066397693 1388-6150 nnns volume:147 year:2021 number:2 day:05 month:01 pages:1251-1264 https://doi.org/10.1007/s10973-020-10459-7 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_OLC SSG-OLC-TEC SSG-OLC-CHE SSG-OLC-PHA SSG-OLC-DE-84 AR 147 2021 2 05 01 1251-1264 |
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10.1007/s10973-020-10459-7 doi (DE-627)OLC2077777559 (DE-He213)s10973-020-10459-7-p DE-627 ger DE-627 rakwb eng 660 VZ Krishnan, G. Santhana verfasserin (orcid)0000-0001-9175-1907 aut Thermal rearrangements during liquid–vapor phase pyrolysis polycondensation of polysilane to high-functional polycarbosilane: spectral and thermal studies 2021 Text txt rdacontent ohne Hilfsmittel zu benutzen n rdamedia Band nc rdacarrier © Akadémiai Kiadó, Budapest, Hungary 2021 Abstract Thermally induced Kumada rearrangement of –Si–Si– linear chains in polysilanes to –Si–C– chain was conducted in the liquid–vapor phase, followed by isothermal treatments at 410, 460 °C and pressure of 15 kgf $ cm^{−2} $ leading to polycarbosilane(PCS) with higher silane (–Si–H) content in the range 0.46–0.58 mass%. Molecular and thermal changes during the oligomer to polymer transformation were investigated, applying spectral and thermal techniques. FTIR, Raman, and 1H, 13C, and 29Si-NMR analytical results established the chemical structural formula, –Si–Si–, –Si–C–, –Si–H bonding networks, and evolution of –Si–H functionality in as-synthesized polycarbosilane during the thermal transformations. FTIR and 29Si-NMR studies followed the increase in silane content (–Si–H). Raman data revealed the formation and disappearance of –Si–Si– functional group as the transformation progresses. Average molecular mass increased proportionally with polymerization reaction time. Thermogravimetric studies at 1400 °C confirmed a polymer to ceramic conversion (ceramic yield) of as-synthesized PCS increased with the increase in mass average molecular mass and found to be as high as 88% mass. The formation of a high purity green β-SiC powder on heat treatment at 1500 °C confirmed the high molecular polycarbosilane. Ceramic-yielding polymers High molecular mass Pressure pyrolysis polycondensation Solvent fractionation Naveen, S. aut Shahnawaz, M. aut Enthalten in Journal of thermal analysis and calorimetry Springer International Publishing, 1998 147(2021), 2 vom: 05. Jan., Seite 1251-1264 (DE-627)244148767 (DE-600)1429493-X (DE-576)066397693 1388-6150 nnns volume:147 year:2021 number:2 day:05 month:01 pages:1251-1264 https://doi.org/10.1007/s10973-020-10459-7 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_OLC SSG-OLC-TEC SSG-OLC-CHE SSG-OLC-PHA SSG-OLC-DE-84 AR 147 2021 2 05 01 1251-1264 |
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Thermal rearrangements during liquid–vapor phase pyrolysis polycondensation of polysilane to high-functional polycarbosilane: spectral and thermal studies |
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Thermal rearrangements during liquid–vapor phase pyrolysis polycondensation of polysilane to high-functional polycarbosilane: spectral and thermal studies |
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Krishnan, G. Santhana |
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Journal of thermal analysis and calorimetry |
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Krishnan, G. Santhana Naveen, S. Shahnawaz, M. |
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thermal rearrangements during liquid–vapor phase pyrolysis polycondensation of polysilane to high-functional polycarbosilane: spectral and thermal studies |
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Thermal rearrangements during liquid–vapor phase pyrolysis polycondensation of polysilane to high-functional polycarbosilane: spectral and thermal studies |
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Abstract Thermally induced Kumada rearrangement of –Si–Si– linear chains in polysilanes to –Si–C– chain was conducted in the liquid–vapor phase, followed by isothermal treatments at 410, 460 °C and pressure of 15 kgf $ cm^{−2} $ leading to polycarbosilane(PCS) with higher silane (–Si–H) content in the range 0.46–0.58 mass%. Molecular and thermal changes during the oligomer to polymer transformation were investigated, applying spectral and thermal techniques. FTIR, Raman, and 1H, 13C, and 29Si-NMR analytical results established the chemical structural formula, –Si–Si–, –Si–C–, –Si–H bonding networks, and evolution of –Si–H functionality in as-synthesized polycarbosilane during the thermal transformations. FTIR and 29Si-NMR studies followed the increase in silane content (–Si–H). Raman data revealed the formation and disappearance of –Si–Si– functional group as the transformation progresses. Average molecular mass increased proportionally with polymerization reaction time. Thermogravimetric studies at 1400 °C confirmed a polymer to ceramic conversion (ceramic yield) of as-synthesized PCS increased with the increase in mass average molecular mass and found to be as high as 88% mass. The formation of a high purity green β-SiC powder on heat treatment at 1500 °C confirmed the high molecular polycarbosilane. © Akadémiai Kiadó, Budapest, Hungary 2021 |
| abstractGer |
Abstract Thermally induced Kumada rearrangement of –Si–Si– linear chains in polysilanes to –Si–C– chain was conducted in the liquid–vapor phase, followed by isothermal treatments at 410, 460 °C and pressure of 15 kgf $ cm^{−2} $ leading to polycarbosilane(PCS) with higher silane (–Si–H) content in the range 0.46–0.58 mass%. Molecular and thermal changes during the oligomer to polymer transformation were investigated, applying spectral and thermal techniques. FTIR, Raman, and 1H, 13C, and 29Si-NMR analytical results established the chemical structural formula, –Si–Si–, –Si–C–, –Si–H bonding networks, and evolution of –Si–H functionality in as-synthesized polycarbosilane during the thermal transformations. FTIR and 29Si-NMR studies followed the increase in silane content (–Si–H). Raman data revealed the formation and disappearance of –Si–Si– functional group as the transformation progresses. Average molecular mass increased proportionally with polymerization reaction time. Thermogravimetric studies at 1400 °C confirmed a polymer to ceramic conversion (ceramic yield) of as-synthesized PCS increased with the increase in mass average molecular mass and found to be as high as 88% mass. The formation of a high purity green β-SiC powder on heat treatment at 1500 °C confirmed the high molecular polycarbosilane. © Akadémiai Kiadó, Budapest, Hungary 2021 |
| abstract_unstemmed |
Abstract Thermally induced Kumada rearrangement of –Si–Si– linear chains in polysilanes to –Si–C– chain was conducted in the liquid–vapor phase, followed by isothermal treatments at 410, 460 °C and pressure of 15 kgf $ cm^{−2} $ leading to polycarbosilane(PCS) with higher silane (–Si–H) content in the range 0.46–0.58 mass%. Molecular and thermal changes during the oligomer to polymer transformation were investigated, applying spectral and thermal techniques. FTIR, Raman, and 1H, 13C, and 29Si-NMR analytical results established the chemical structural formula, –Si–Si–, –Si–C–, –Si–H bonding networks, and evolution of –Si–H functionality in as-synthesized polycarbosilane during the thermal transformations. FTIR and 29Si-NMR studies followed the increase in silane content (–Si–H). Raman data revealed the formation and disappearance of –Si–Si– functional group as the transformation progresses. Average molecular mass increased proportionally with polymerization reaction time. Thermogravimetric studies at 1400 °C confirmed a polymer to ceramic conversion (ceramic yield) of as-synthesized PCS increased with the increase in mass average molecular mass and found to be as high as 88% mass. The formation of a high purity green β-SiC powder on heat treatment at 1500 °C confirmed the high molecular polycarbosilane. © Akadémiai Kiadó, Budapest, Hungary 2021 |
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Thermal rearrangements during liquid–vapor phase pyrolysis polycondensation of polysilane to high-functional polycarbosilane: spectral and thermal studies |
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