Silicon Carbide Precursor: Structure Analysis and Thermal Behavior from Polymer Cross-Linking to Pyrolyzed Ceramics
The Silres H62C methyl-phenyl-vinyl-hydrogen polysiloxane is a promising candidate as a SiC precursor for 3D printing based on photopolymerization reaction. An in-depth nuclear magnetic resonance spectroscopy analysis allowed us to determine its structure and quantify its functional groups. The poly...
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| Format: | Article |
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MDPI AG
2022-11-01
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| Series: | Ceramics |
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| Online Access: | https://www.mdpi.com/2571-6131/5/4/76 |
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| author | Sébastien Vry Marilyne Roumanie Pierre-Alain Bayle Sébastien Rolère Guillaume Bernard-Granger |
| author_facet | Sébastien Vry Marilyne Roumanie Pierre-Alain Bayle Sébastien Rolère Guillaume Bernard-Granger |
| author_sort | Sébastien Vry |
| collection | DOAJ |
| description | The Silres H62C methyl-phenyl-vinyl-hydrogen polysiloxane is a promising candidate as a SiC precursor for 3D printing based on photopolymerization reaction. An in-depth nuclear magnetic resonance spectroscopy analysis allowed us to determine its structure and quantify its functional groups. The polysiloxane was found to have a highly branched ladder-like structure, with 21.9, 31.4 and 46.7% of mono-, di- and tri-functional silicon atoms. The polysiloxane cross-links from 180 °C using hydrosilylation between silyl groups (8.4% of the total functional groups) and vinyl groups (12.0%) and contains a non-negligible ethoxy content (2.4%), allowing cross-linking through a hydrolyze/condensation mechanism. After converting the polymer into ceramic and thus releasing mainly hydrogen and methane, the ceramic yield was 72.5%. An X-ray diffraction analysis on the cross-linked and pyrolyzed polysiloxane showed that the ceramic is amorphous at temperatures up to 1200 °C and starts to crystallize from 1200 °C, leading into 3C-SiC carbon-rich ceramic at 1700 °C in an argon atmosphere. |
| first_indexed | 2024-03-09T17:12:26Z |
| format | Article |
| id | doaj.art-76c259bc30a34e90a4ce4d3e92dc44a0 |
| institution | Directory Open Access Journal |
| issn | 2571-6131 |
| language | English |
| last_indexed | 2024-03-09T17:12:26Z |
| publishDate | 2022-11-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Ceramics |
| spelling | doaj.art-76c259bc30a34e90a4ce4d3e92dc44a02023-11-24T13:57:02ZengMDPI AGCeramics2571-61312022-11-01541066108310.3390/ceramics5040076Silicon Carbide Precursor: Structure Analysis and Thermal Behavior from Polymer Cross-Linking to Pyrolyzed CeramicsSébastien Vry0Marilyne Roumanie1Pierre-Alain Bayle2Sébastien Rolère3Guillaume Bernard-Granger4CEA, LITEN, DTNM, Université Grenoble Alpes, 38000 Grenoble, FranceCEA, LITEN, DTNM, Université Grenoble Alpes, 38000 Grenoble, FranceCEA, IRIG, MEM, Université Grenoble Alpes, 38000 Grenoble, FranceCEA, LITEN, DTNM, Université Grenoble Alpes, 38000 Grenoble, FranceCEA, DES, ISEC, DMRC, SPTC, LSEM, Université Montpellier, 30207 Marcoule, FranceThe Silres H62C methyl-phenyl-vinyl-hydrogen polysiloxane is a promising candidate as a SiC precursor for 3D printing based on photopolymerization reaction. An in-depth nuclear magnetic resonance spectroscopy analysis allowed us to determine its structure and quantify its functional groups. The polysiloxane was found to have a highly branched ladder-like structure, with 21.9, 31.4 and 46.7% of mono-, di- and tri-functional silicon atoms. The polysiloxane cross-links from 180 °C using hydrosilylation between silyl groups (8.4% of the total functional groups) and vinyl groups (12.0%) and contains a non-negligible ethoxy content (2.4%), allowing cross-linking through a hydrolyze/condensation mechanism. After converting the polymer into ceramic and thus releasing mainly hydrogen and methane, the ceramic yield was 72.5%. An X-ray diffraction analysis on the cross-linked and pyrolyzed polysiloxane showed that the ceramic is amorphous at temperatures up to 1200 °C and starts to crystallize from 1200 °C, leading into 3C-SiC carbon-rich ceramic at 1700 °C in an argon atmosphere.https://www.mdpi.com/2571-6131/5/4/76polymer-derived ceramicsSiCpolysiloxaneNMR characterization |
| spellingShingle | Sébastien Vry Marilyne Roumanie Pierre-Alain Bayle Sébastien Rolère Guillaume Bernard-Granger Silicon Carbide Precursor: Structure Analysis and Thermal Behavior from Polymer Cross-Linking to Pyrolyzed Ceramics Ceramics polymer-derived ceramics SiC polysiloxane NMR characterization |
| title | Silicon Carbide Precursor: Structure Analysis and Thermal Behavior from Polymer Cross-Linking to Pyrolyzed Ceramics |
| title_full | Silicon Carbide Precursor: Structure Analysis and Thermal Behavior from Polymer Cross-Linking to Pyrolyzed Ceramics |
| title_fullStr | Silicon Carbide Precursor: Structure Analysis and Thermal Behavior from Polymer Cross-Linking to Pyrolyzed Ceramics |
| title_full_unstemmed | Silicon Carbide Precursor: Structure Analysis and Thermal Behavior from Polymer Cross-Linking to Pyrolyzed Ceramics |
| title_short | Silicon Carbide Precursor: Structure Analysis and Thermal Behavior from Polymer Cross-Linking to Pyrolyzed Ceramics |
| title_sort | silicon carbide precursor structure analysis and thermal behavior from polymer cross linking to pyrolyzed ceramics |
| topic | polymer-derived ceramics SiC polysiloxane NMR characterization |
| url | https://www.mdpi.com/2571-6131/5/4/76 |
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