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Novel Sulfur‐Containing Cross‐Linking Agent for Si‐Based Preceramic Polymers
Macromolecular Chemistry and Physics ( IF 2.5 ) Pub Date : 2019-12-12 , DOI: 10.1002/macp.201900380 Poroshat Taheri 1 , Apparao Bokka 1 , Parham Asgari 1 , Junha Jeon 1 , John C. Lang 1 , Renzo Campostrini 2 , Gian Domenico Sorarù 2 , Peter Kroll 1
Macromolecular Chemistry and Physics ( IF 2.5 ) Pub Date : 2019-12-12 , DOI: 10.1002/macp.201900380 Poroshat Taheri 1 , Apparao Bokka 1 , Parham Asgari 1 , Junha Jeon 1 , John C. Lang 1 , Renzo Campostrini 2 , Gian Domenico Sorarù 2 , Peter Kroll 1
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Cross‐linking polymethylhydrosiloxane (PMHS) with divinylthiophene (DVT) via hydrosilylation in highly dilute conditions and subsequent supercritical drying in CO2 yield a polymeric aerogel containing aromatic sulfur integrally and uniformly distributed throughout the monolith. Fourier‐transform infrared (FT‐IR) spectroscopy indicates almost complete consumption of vinyl groups and SiH bonds in the product. Both FT‐IR and Raman spectroscopic analyses support loss of conjugation of vinyl groups with the retained double bonds of the thiophene ring. Scanning electron microscopy (SEM) indicates a condensed colloidal structure with characteristic particulate diameters of about 165 nm. SEM coupled with energy dispersive X‐ray spectroscopy elemental mapping shows that sulfur is distributed homogeneously in the polymeric aerogel. Porosimetry of the mesoporous aerogel indicates the effective average pore diameters are about 12 nm. Thermogravimetric analysis (TGA) establishes greater thermal stability of the PMHS‐DVT product than either of the pure unreacted components. TGA coupled with mass spectrometric (TG‐MS) identification of the volatiles released during pyrolysis shows that sulfur is driven from the cross‐linked polymer as thiophene and its derivatives. Recorded mass spectra support the hypothesis that cross‐linking DVT bridges between PMHS chains in the polymeric aerogel, and that this results in a more thermally stable monolith.
中文翻译：
用于硅基陶瓷的新型含硫交联剂
在高度稀释的条件下，通过氢化硅烷化作用使聚甲基氢硅氧烷（PMHS）与二乙烯基噻吩（DVT）交联，然后在CO 2中进行超临界干燥，得到的聚合物气凝胶整体整体均匀地分布了芳香族硫。傅立叶变换红外（FT-IR）光谱表明乙烯基和Si几乎完全消耗产品中的H键。FT-IR和拉曼光谱分析均支持乙烯基与噻吩环保留的双键的共轭损失。扫描电子显微镜（SEM）表明具有特征颗粒直径为约165nm的浓缩胶体结构。SEM结合能量色散X射线光谱仪的元素图谱显示，硫在聚合物气凝胶中均匀分布。中孔气凝胶的孔隙率测定表明有效平均孔径为约12nm。热重分析（TGA）建立的PMHS-DVT产品的热稳定性高于任何未反应的纯组分。TGA结合质谱（TG-MS）对热解过程中释放的挥发物的鉴定表明，硫以噻吩及其衍生物形式从交联聚合物中驱出。记录的质谱支持以下假设：聚合物气凝胶中PMHS链之间的DVT桥交联，这导致了更热稳定的整体结构。
更新日期：2019-12-12
中文翻译：
用于硅基陶瓷的新型含硫交联剂
在高度稀释的条件下，通过氢化硅烷化作用使聚甲基氢硅氧烷（PMHS）与二乙烯基噻吩（DVT）交联，然后在CO 2中进行超临界干燥，得到的聚合物气凝胶整体整体均匀地分布了芳香族硫。傅立叶变换红外（FT-IR）光谱表明乙烯基和Si几乎完全消耗产品中的H键。FT-IR和拉曼光谱分析均支持乙烯基与噻吩环保留的双键的共轭损失。扫描电子显微镜（SEM）表明具有特征颗粒直径为约165nm的浓缩胶体结构。SEM结合能量色散X射线光谱仪的元素图谱显示，硫在聚合物气凝胶中均匀分布。中孔气凝胶的孔隙率测定表明有效平均孔径为约12nm。热重分析（TGA）建立的PMHS-DVT产品的热稳定性高于任何未反应的纯组分。TGA结合质谱（TG-MS）对热解过程中释放的挥发物的鉴定表明，硫以噻吩及其衍生物形式从交联聚合物中驱出。记录的质谱支持以下假设：聚合物气凝胶中PMHS链之间的DVT桥交联，这导致了更热稳定的整体结构。
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