A detailed understanding of the processes taking place during the in situ synthesis of metal/polymer nanocomposites is crucial to manipulate the shape and size of nanoparticles (NPs) with a high level of control. In this paper, we report an in-depth time-resolved analysis of the particle formation process in silver/epoxy nanocomposites obtained through a visible-light-assisted in situ synthesis. The selected epoxy monomer was based on diglycidyl ether of bisphenol A, which undergoes relatively slow cationic ring-opening polymerization. This feature allowed us to access a full description of the formation process of silver NPs before this was arrested by the curing of the epoxy matrix. In situ time-resolved small-angle X-ray scattering investigation was carried out to follow the evolution of the number and size of the silver NPs as a function of irradiation time, whereas rheological experiments combined with near-infrared and ultraviolet–visible spectroscopies were performed to interpret how changes in the rheological properties of the matrix affect the nucleation and growth of particles. The analysis of the obtained results allowed us to propose consistent mechanisms for the formation of metal/polymer nanocomposites obtained by light-assisted one-pot synthesis. Finally, the effect of a thermal postcuring treatment of the epoxy matrix on the particle size in the nanocomposite was investigated.

中文翻译：

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通过可见光辅助原位合成获得的银/环氧纳米复合材料中颗粒形成的机理

对金属/聚合物纳米复合材料原位合成过程中发生的过程的详细了解，对于以高水平的控制来操纵纳米颗粒（NP）的形状和尺寸至关重要。在本文中，我们报告了通过可见光辅助原位合成获得的银/环氧树脂纳米复合材料中颗粒形成过程的深入时间分辨分析。选择的环氧单体基于双酚A的二缩水甘油醚，其经历相对缓慢的阳离子开环聚合。此功能使我们能够获得对银纳米颗粒形成过程的完整描述，然后再通过环氧基质的固化将其阻止。进行了原位时间分辨的小角X射线散射研究，以追踪银纳米颗粒的数量和大小随照射时间的变化，而流变学实验与近红外和紫外可见分光光度法相结合为了解释基质流变特性的变化如何影响颗粒的形核和生长而进行的研究。对获得的结果的分析使我们能够提出一致的机制，以形成通过光辅助一锅法合成获得的金属/聚合物纳米复合材料。最后，研究了环氧树脂基体的热后固化处理对纳米复合材料粒径的影响。而流变学实验结合近红外和紫外可见光谱学进行了解释，以解释基体流变性质的变化如何影响颗粒的形核和生长。对获得的结果的分析使我们能够提出一致的机制，以形成通过光辅助一锅法合成获得的金属/聚合物纳米复合材料。最后，研究了环氧树脂基体的热后固化处理对纳米复合材料粒径的影响。而流变学实验结合近红外和紫外可见光谱学进行了解释，以解释基体流变性质的变化如何影响颗粒的形核和生长。对获得的结果的分析使我们能够提出一致的机制，以形成通过光辅助一锅法合成获得的金属/聚合物纳米复合材料。最后，研究了环氧树脂基体的热后固化处理对纳米复合材料粒径的影响。