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The Multilevel Structure of Sulfonated Syndiotactic-Polystyrene Model Polyelectrolyte Membranes Resolved by Extended Q-Range Contrast Variation SANS

机译:扩展Q范围对比度变化SANS解析的磺化间同立构聚苯乙烯模型聚电解质膜的多级结构

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摘要

Membranes based on sulfonated synditoactic polystyrene (s-sPS) were thoroughly characterized by contrast variation small-angle neutron scattering (SANS) over a wide Q-range in dry and hydrated states. Following special sulfonation and treatment procedures, s-sPS is an attractive material for fuel cells and energy storage applications. The film samples were prepared by solid-state sulfonation, resulting in uniform sulfonation of only the amorphous phase while preserving the crystallinity of the membrane. Fullerenes, which improve the resistance to oxidation decomposition, were incorporated in the membranes. The fullerenes seem to be chiefly located in the amorphous regions of the samples, and do not influence the formation and evolution of the morphologies in the polymer films, as no significant differences were observed in the SANS patterns compared to the fullerenes-free s-sPS membranes, which were investigated in a previous study. The use of uniaxially deformed film samples, and neutron contrast variation allowed for the identification and characterization of different structural levels with sizes between nm and μm, which form and evolve in both the dry and hydrated states. The scattering length density of the crystalline regions was varied using the guest exchange procedure between different toluene isotopologues incorporated into the sPS lattice, while the variation of the scattering properties of the hydrated amorphous regions was achieved using different H O/D O mixtures. Due to the deformation of the films, the scattering characteristics of different structures can be distinguished on specific detection sectors and at different detection distances after the sample, depending on their size and orientation.
机译:通过在干燥和水合状态下在宽Q范围内的对比度变化小角中子散射(SANS),彻底表征了基于磺化间规聚苯乙烯(s-sPS)的膜。遵循特殊的磺化和处理程序,s-sPS是用于燃料电池和能量存储应用的有吸引力的材料。通过固态磺化制备膜样品,导致仅非晶相均匀磺化,同时保持膜的结晶度。膜中加入了富勒烯,可提高抗氧化分解性。富勒烯似乎主要位于样品的无定形区域中,并且不影响聚合物膜中形态的形成和演变,因为与无富勒烯的s-sPS相比,在SANS模式中未观察到显着差异。膜,在先前的研究中进行了研究。使用单轴变形的薄膜样品和中子对比度变化,可以识别和表征尺寸在nm和μm之间的不同结构水平,这些结构水平在干燥和水合状态下均会形成和演化。使用结合到sPS晶格中的不同甲苯同位素之间的客体交换程序,可改变晶体区域的散射长度密度,而使用不同的H O / D O混合物可实现水合非晶区​​域散射特性的变化。由于薄膜的变形,根据样品的大小和方向,可以在特定的检测扇区和样品之后的不同检测距离处区分不同结构的散射特性。

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