Polymer ( IF 4.1 ) Pub Date : 2020-05-23 , DOI: 10.1016/j.polymer.2020.122589 Christopher K. Henry , Emil Sandoz-Rosado , Michael R. Roenbeck , Daniel J. Magagnosc , Giuseppe R. Palmese , Kenneth E. Strawhecker , Nicolas J. Alvarez
High performance ultra high molecular weight polyethylene (UHMWPE) fibers are primarily composed of extended chain (shish) and lamellae (kebab) crystalline domains. Characterization of these architectures commonly utilizes x-ray scattering techniques, which rely upon models to transform from inverse scattering space to real space. Scattering models for lamellae and straight chain crystalline domains were developed and intended for use in ideal scattering scenarios; ie. purely extended chain or purely lamellae. Simultaneous implementation of both models with real (non-ideal) fibers takes for granted the validity of either model in the presence of the other crystalline feature. In this work, we utilize atomic force microscopy (AFM) to directly couple real space stiffness measurements to the analysis of scattering data. The validity of scattering models is tested against real space image analysis and conclusions are drawn regarding the analysis of scattering data to quantify crystalline domain sizes. We find that the lamellae long spacing estimated from scattering data is consistent with real space image analysis. Whereas significant differences are observed for the analysis of lamellae diameter. The characteristic size of extended chain crystalline domains is measured via the streak analysis method on both SAXS 2D scattering data and the Fast Fourier Transform (FFT) of AFM stiffness maps. The streak analysis results in comparable length scales when applied to SAXS and FFT AFM images. A comparison of the streak analysis with novel filtered AFM images suggest that the streak analysis is capturing continuity of straight chain crystalline domains.
中文翻译:
直接测量聚乙烯纤维中晶域的大小,分布和取向
高性能超高分子量聚乙烯(UHMWPE)纤维主要由延伸链(shish)和薄片(kebab)晶域组成。这些体系结构的表征通常利用X射线散射技术,该技术依赖于模型从逆散射空间转换为真实空间。层状和直链晶域的散射模型已经开发出来,旨在用于理想的散射场景;即。纯延伸链或纯薄片。使用真实(非理想)纤维同时实现两个模型的前提是,在存在另一个晶体特征的情况下,两个模型的有效性都是理所当然的。在这项工作中,我们利用原子力显微镜(AFM)将实际空间刚度测量结果直接耦合到散射数据分析中。针对真实空间图像分析测试了散射模型的有效性,并得出了有关散射数据分析以量化晶畴尺寸的结论。我们发现从散射数据估计的薄片长间距与真实空间图像分析一致。然而观察到的薄片厚度分析存在显着差异。通过条纹分析方法,根据SAXS 2D散射数据和AFM刚度图的快速傅立叶变换(FFT),测量了延伸链晶域的特征尺寸。条纹分析应用于SAXS和FFT AFM图像时,可得到相当的长度比例。条纹分析与新型过滤后的AFM图像的比较表明,条纹分析正在捕获直链晶域的连续性。