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SAXS and DSC studies on the structural characteristics of siliconized s-triazine glassy hybrid materials

机译:SAXS和DSC研究硅化三嗪玻璃化杂化材料的结构特征

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摘要

Three hybrid materials composed of planar s-triazine rings and polyhedral silica (SiO _2), phenylsilsesquioxane (PhSiO _(1.5)) and diphenylsiloxane (Ph _2SiO) building blocks were investigated by differential scanning calorimetry (DSC) and small angle X-ray scattering (SAXS) techniques. These measurements revealed that the geometrically dissimilar components were fully integrated into intact glassy hybrid structures. Their DSC thermograms showed that these hybrids are thermally stable below 350 °C with moderate glass transition temperatures (T _g) of 56-110°C consistent with the increasing structural connectivity of the silicone component. The SAXS data was analyzed to obtain different structural information using Porod, Guinier and Kratky approximations. The general features of each of the SAXS profiles of these hybrids are very similar to those of polyphenylsilsesquioxane (PPhSQ). The SAXS profiles reveal that these hybrids can be described as nano-scale primary particles that are self-organized in macromolecular ensembles to form extended unfolded textures of varying scattering lengths (91-168 ?). The obtained hybrid particles adopt either 3-D bulk fractals with open structures or 2-D surface fractals with dense cores. The short interfacial thickness (< 3 ?) and the low thermal fluctuation parameters strongly suggest that these particles are held together by substantial cohesion forces.
机译:通过差示扫描量热法(DSC)和小角度X射线散射研究了由平面s-三嗪环和多面体二氧化硅(SiO _2),苯基倍半硅氧烷(PhSiO _(1.5)和二苯基硅氧烷(Ph _2SiO)组成单元组成的三种杂化材料。 (SAXS)技术。这些测量结果表明,几何形状不同的组件已完全集成到完整的玻璃状混合结构中。他们的DSC热谱图显示,这些杂化物在350°C以下具有热稳定性,并且玻璃化转变温度(T _g)在56-110°C之间,这与硅氧烷组分的结构连通性不断提高是一致的。使用Porod,Guinier和Kratky近似分析SAXS数据以获得不同的结构信息。这些杂种的每个SAXS配置文件的一般特征与聚苯基倍半硅氧烷(PPhSQ)的特征非常相似。 SAXS谱图揭示了这些杂化体可以描述为纳米级的初级粒子,这些粒子在大分子集合体中自组织形成分散的散射长度(91-168?)的扩展展开结构。所获得的杂化颗粒采用具有开放结构的3-D本体分形或具有致密芯的2-D表面分形。界面厚度短(<3Ω)和低热波动参数强烈表明,这些颗粒通过相当大的内聚力保持在一起。

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