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Detecting Carbon in Carbon: Exploiting Differential Charging to Obtain Information on the Chemical Identity and Spatial Location of Carbon Nanotube Aggregates in Composites by Imaging X-ray Photoelectron Spectroscopy

机译:检测碳中的碳:利用差分充电通过X射线光电子能谱获得复合材料中碳纳米管聚集体的化学识别和空间位置信息

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摘要

To better assess risks associated with nano-enabled products including multiwalled carbon nanotubes (MWCNT) within polymer matrices, it is important to understand how MWCNT are dispersed throughout the composite. The current study presents a method which employs imaging X-ray photoelectron spectroscopy (XPS) to chemically detect spatially segregated MWCNT rich regions at an epoxy composites surface by exploiting differential charging. MWCNT do not charge due to high conductivity and have previously been shown to energetically separate from their insulating surroundings when characterized by XPS. XPS in imaging mode revealed that these conductive regions were spatially separated due to micrometer-scale MWCNT aggregation and poor dispersion during the formation of the composite. Three MWCNT concentrations were studied; (1, 4 and 5) % by mass MWCNT within an epoxy matrix. Images acquired in periodic energy intervals were processed using custom algorithms designed to efficiently extract spectra from regions of interest. As a result, chemical and electrical information on aggregate and non-aggregate portions of the composite was extracted. Raman imaging and scanning electron microscopy were employed as orthogonal techniques for validating this XPS-based methodology. Results demonstrate that XPS imaging of differentially charging MWCNT composite samples is an effective means for assessing dispersion quality.
机译:为了更好地评估与纳米基质产品(包括聚合物基质中的多壁碳纳米管(MWCNT))相关的风险,了解MWCNT如何分散在整个复合材料中非常重要。当前的研究提出了一种方法,该方法利用成像X射线光电子能谱(XPS)通过利用差分电荷化学检测环氧复合材料表面的空间隔离的MWCNT富集区域。 MWCNT由于具有高电导率而不会充电,并且以前已被证明在通过XPS表征时会与其绝缘环境发生能量分离。 XPS成像模式显示,由于微米级MWCNT聚集和复合材料形成过程中的分散性差,这些导电区域在空间上分开。研究了三种MWCNT浓度;环氧基质中MWCNT的质量为(1、4和5)%。使用自定义算法处理以周期性能量间隔获取的图像,该自定义算法旨在有效地从目标区域提取光谱。结果,提取了关于复合材料的聚集和非聚集部分的化学和电学信息。拉曼成像和扫描电子显微镜被用作正交技术来验证这种基于XPS的方法。结果表明,对带电荷的MWCNT复合样品进行XPS成像是评估分散质量的有效手段。

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