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通过“经典”和阳离子前沿聚合制备的环氧基热固性材料的微观结构研究。

Microstructural study of epoxy-based thermosets prepared by "classical" and cationic frontal polymerization.

作者信息

Švajdlenková Helena, Kleinová Angela, Šauša Ondrej, Rusnák Jaroslav, Dung Tran Anh, Koch Thomas, Knaack Patrick

机构信息

Department of Synthesis and Characterization of Polymers, Polymer Institute of SAS Dúbravská cesta 9 Bratislava 845 41 Slovakia

Institute of Applied Synthetic Chemistry, TU Wien Getreidemarkt 9/163 MC 1060 Vienna Austria

出版信息

RSC Adv. 2020 Nov 11;10(67):41098-41109. doi: 10.1039/d0ra08298h. eCollection 2020 Nov 9.

Abstract

A microstructural study of bisphenol-A diglycidyl ether (BADGE), prepared both "classical" and novel photo- and thermally-induced cationic frontal polymerization, can help to understand the relationships between the microstructure of epoxides and their material properties, as well as the propagation of frontal polymerization waves. Microstructural PALS characteristics, such as the -positronium lifetime ( ), lifetime distribution, and void fraction, were investigated in relation to the extension of H bonds obtained from ATR/FTIR and the bulk density. The thermal profiles of differently-induced RICFP revealed that photo-triggered propagation is twice as fast as thermally-induced RICFP, with a comparable maximal reaction temperature (∼283 °C) and heat conductivity. Both RICFP-based samples, induced by UV light and heat, showed a lower , narrower lifetime distributions, and a reduced void fraction, in comparison to the "classical" cured anhydride-based epoxy sample. These may be the main factors which result in better material properties. In addition, both their radial and angular profiles of free volume fraction confirmed experimentally the rotational movement of the propagating frontal waves and their influence on the microstructural inhomogeneities, and the final material properties.

摘要

对双酚 A 二缩水甘油醚(BADGE)进行微观结构研究,该研究采用了“经典”方法以及新型的光致和热致阳离子前沿聚合方法,这有助于理解环氧化合物的微观结构与其材料性能之间的关系,以及前沿聚合波的传播情况。研究了微观结构的正电子湮没寿命谱(PALS)特征,如正电子素寿命( )、寿命分布和空隙率,并将其与通过衰减全反射傅里叶变换红外光谱(ATR/FTIR)得到的氢键扩展情况以及堆积密度相关联。不同引发方式的快速原位阳离子前沿聚合(RICFP)的热曲线表明,光引发的传播速度是热引发的RICFP的两倍,具有相当的最高反应温度(约283°C)和热导率。与“经典”固化酸酐基环氧树脂样品相比,基于紫外光和热引发的RICFP的样品均表现出更低的 、更窄的寿命分布和更低的空隙率。这些可能是导致更好材料性能的主要因素。此外,它们自由体积分数的径向和角向分布通过实验证实了传播前沿波的旋转运动及其对微观结构不均匀性和最终材料性能的影响。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/0737/9057714/6c26cd90d3b1/d0ra08298h-f1.jpg

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