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Revealing the three-dimensional filler structure in a rubber matrix based on fluorescein modified layered double hydroxides

机译：基于荧光素改性的层状双氢氧化物在橡胶基质中显示三维填料结构

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摘要

To gain insight into nonlinear viscoelastic behavior, e.g. the Payne effect, and in situ visualize the filler structure in a rubber matrix under strain, a methodology was developed to detect and track structural evolution based on fluorescent labeling. As a model system, layered double hydroxides (LDHs) with different lateral sizes (nanosheets and microsheets) were labeled with fluorescein (FLU) and then uniformly introduced into the rubber matrix through solution blending. The strain-induced deformation and destruction of the three-dimensional LDH filler structure were directly observed for the first time through laser scanning confocal microscopy (LSCM). The contributions of the breakdown of the filler network, strain softening of the glassy layer and macromolecular disentanglement to the Payne effect were qualitatively determined and analyzed in detail based on the structural information probed via LSCM together with transmission electron microscopy, rheometry and modulated differential scanning calorimetry. The primary mechanism for the Payne effect in this system was then proposed and the macromolecular disentanglement in the rubber matrix played a key role. Furthermore, the enhanced Payne effect with increasing LDH content was ascribed to the strain amplification effect induced by the filler network for the LDH nanosheet filled system and the chain sliding on orientated LDHs for microsheet filled compounds, respectively.
机译：为了深入了解非线性粘弹性行为，例如 Payne效应和原位可视化应变下橡胶基质中的填料结构，开发了一种检测和跟踪结构的方法荧光标记的进化。作为模型系统，使用荧光素（FLU）标记具有不同横向尺寸（纳米片和微片）的层状双氢氧化物（LDH），然后通过溶液共混将其均匀引入橡胶基质中。通过激光扫描共聚焦显微镜（LSCM）首次直接观察到了应变诱导的三维LDH填料结构的变形和破坏。基于通过探测的结构信息以及透射电子显微镜，定性分析了填料网络的破坏，玻璃层的应变软化和高分子解缠对Payne效应的贡献。 ，流变仪和调制差示扫描量热仪。然后提出了该系统中Payne效应的主要机理，并且橡胶基质中的高分子解缠起了关键作用。此外，随着LDH含量的增加，Payne效应增强，这归因于LDH纳米片填充系统的填充剂网络和微片片填充化合物的定向LDH上链滑动所引起的应变放大效应。

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