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Image Analysis Optimization for Quantifying Nanoparticle Dispersions in Polymer-based Nanocontposites Using Transmission Electron Microscopy (TEM)

机译:图像分析优化,用于使用透射电子显微镜(TEM)量化聚合物基纳米复合材料中的纳米颗粒分散体

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When comparing large numbers of TEM micrographs of insoluble additives in polymer-based nanocomposite systems, the ability to determine or estimate the dispersion quality (i.e. uniformity of size and/or spatial distribution) is often difficult. The objective of this study was to develop a method to quantify dispersions observed in TEM micrographs that enables both a numerical "ranking" to be assigned to individual dispersions as well as tabulation a multitude of images acquired over time. Several methods were reviewed and applied to a set of TEM dispersion images of an insoluble additive in polystyrene. Projected area diameter, particle area, and Euclidean distance between particle centroids were chosen from all the particle size distribution and spatial distribution parameters present in the literature, but none successfully yielded a quantitative indicator of dispersion quality for the micrographs. In contrast, generating cumulative volume percent curves for each sample appeared to be a preferred method of quantifying and comparing dispersions in TEM micrographs. The volume diameter values obtained by this method can be used for "ranking" and tabulation of dispersion quality and account for both "good" additive dispersions (i.e. those with small domains of a narrow size range around 1 μm or less) and "bad" additive dispersions (i.e. those with non-uniform domains ranging in size by several microns or more). As a result, the numerical values generated by this method can be used to quantitatively determine correlations between the dispersion quality of nanoparticles in polymer-based nanocomposite materials and various macroscale physical and/or performance properties of such materials. This method's precision was statistically determined to decrease with increasing particle size and be heavily dependent on representative sampling.
机译:当比较基于聚合物的纳米复合系统中不溶性添加剂的大量TEM显微照片时,确定或估计分散质量(即尺寸和/或空间分布的均匀性)的能力通常很困难。这项研究的目的是开发一种量化在TEM显微照片中观察到的色散的方法,该方法既可以将数字“等级”分配给各个色散,也可以将随时间推移采集的大量图像制成表格。综述了几种方法,并将其应用于聚苯乙烯中不溶性添加剂的TEM分散图像。从文献中存在的所有粒度分布和空间分布参数中,选择了投影面积直径,颗粒面积和质心之间的欧式距离,但没有一个能成功地为显微照片提供定量的分散质量指标。相反,为每个样品生成累积体积百分比曲线似乎是定量和比较TEM显微照片中分散度的首选方法。通过此方法获得的体积直径值可用于分散质量的“分级”和制表,并同时考虑“良好”的添加剂分散(即那些具有在1μm或更小的窄尺寸范围内的小区域的添加剂)和“不良”分散剂添加剂分散体(即具有大小不等的微米范围的不均匀区域的分散体)。结果,通过该方法产生的数值可用于定量确定基于聚合物的纳米复合材料中的纳米颗粒的分散质量与这种材料的各种宏观物理和/或性能之间的相关性。统计上确定了该方法的精度会随着粒度的增加而降低,并且在很大程度上取决于代表性的采样。

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