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首页> 外文期刊>Journal of Non-Crystalline Solids: A Journal Devoted to Oxide, Halide, Chalcogenide and Metallic Glasses, Amorphous Semiconductors, Non-Crystalline Films, Glass-Ceramics and Glassy Composites >Infrared attenuated total reflection spectroscopy studies of aprotic condensation of (EtO)(3)Si-R-Si(OEt)(3) and R-Si(OEt)(3) systems with carboxylic acids
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Infrared attenuated total reflection spectroscopy studies of aprotic condensation of (EtO)(3)Si-R-Si(OEt)(3) and R-Si(OEt)(3) systems with carboxylic acids

机译：（EtO）（3）Si-R-Si（OEt）（3）和R-Si（OEt）（3）与羧酸的质子惰性缩合的红外衰减全反射光谱研究

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摘要

Aprotic hydrolysis and condensation reactions of his end-capped trialkoxysilanes ((EtO)(3)Si-R-Si(OEt)(3)) linked via the organic chain R containing urea groups chemically bonded to a poly(propyleneglycol) (PPG) chain, in the presence of carboxylic acids, i.e. acetic-, chlorodifluoroacetic- and trifluoroacetic acids, were studied using infrared attenuated total reflection (IR ATR) spectroscopy. IR and Si-29 NMR spectral analysis revealed solvolysis reactions: the carboxylic acids interacted with ethoxysilane groups forming silyl esters leading to the formation of bridging Si-O-Si groups and carboxylic acid ester by-products. These results were compared with those obtained on simpler single capped methyltriethoxysilane (Me-Si(OEt)(3), MTEOS) condensed with trifluoroacetic acid. Gelation of (EtO)(3)Si-R-Si(OEt)(3) (catalyzed with acetic acid) encapsulated between a transparent conductive oxide (TCO) glass and a conductive and IR transparent silicon wafer was followed with the help of IR reflection-absorption spectroscopy. The results revealed that aprotic solvolysis of the hybrid precursor with acetic acid led to the formation of non-aqueous gels with low silanol content, confirming the advantages of aprotic solvolysis of organic-inorganic hybrids used as redox electrolytes in hybrid electrochromic (EC) and dye-sensitized photoelectrochemical (DSPEC) cells. Some comments regarding the accuracy of IR ATR spectral measurements compared to IR transmission spectra are also given. (c) 2005 Elsevier B.V. All rights reserved.
机译：他的封端三烷氧基硅烷（（EtO）（3）Si-R-Si（OEt）（3））的质子水解和缩合反应通过含有化学键合到聚丙二醇（PPG）上的脲基的有机链R连接在羧酸（即乙酸，氯二氟乙酸和三氟乙酸）存在下，使用红外衰减全反射（IR ATR）光谱研究了碳链。红外和Si-29 NMR光谱分析表明溶剂分解反应：羧酸与乙氧基硅烷基团相互作用形成甲硅烷基酯，从而导致桥接Si-O-Si基团和羧酸酯副产物。将这些结果与在用三氟乙酸缩合的更简单的单封端甲基三乙氧基硅烷（Me-Si（OEt）（3），MTEOS）上获得的结果进行了比较。借助红外跟踪封装在透明导电氧化物（TCO）玻璃与导电和IR透明硅片之间的（EtO）（3）Si-R-Si（OEt）（3）（用乙酸催化）的胶凝反射吸收光谱法。结果表明，杂质前体与乙酸的质子惰性溶剂化导致形成了低硅烷醇含量的非水凝胶，这证实了有机-无机杂化物的质子惰性溶剂解在混合电致变色（EC）和染料中用作氧化还原电解质的优势。敏化光电化学（DSPEC）细胞。还给出了一些与IR透射光谱相比IR ATR光谱测量准确性的评论。 （c）2005 Elsevier B.V.保留所有权利。

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