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Site specific, high-resolution characterisation of porosity in graphite using FIB-SEM tomography
Journal of Nuclear Materials ( IF 3.1 ) Pub Date : 2018-09-04 , DOI: 10.1016/j.jnucmat.2018.08.047
José David Arregui-Mena , Philip D. Edmondson , Anne A. Campbell , Yutai Katoh

Graphite is used as a moderator of fast neutrons in some types of nuclear reactors and for other industrial applications. The influence of smaller pores on the mechanical and physical properties of graphite remains to be fully understood. In this work, focused ion beam-scanning electron microscopy (FIB-SEM) tomography was applied to characterise the porosity of AGX graphite – an electrode material. FIB-SEM tomography consists in alternating the ion milling and SEM imaging at an area of interest with the objective of creating a 3D reconstruction. Regions containing a filler and a mixture of filler and binder were selected as the areas of interest. Resolutions of a few nanometers were achieved in volumes up to 1400 μm3 for both regions. Typical porous structures were detected in the filler and binder regions such as thermal cracks, gas evolution porosity and lenticular pores. The resolution achieved with these experiments made possible detection of pores smaller than 150 nm in diameter, that is of the length scale of voids generated by neutron irradiation, and an improvement in spatial resolution of traditional x-ray tomography studies. The resolution achieved by FIB-SEM tomography may be essential for the study of the microstructure of graphite, providing complimentary data to x-ray tomography experiments.



中文翻译:

使用FIB-SEM断层成像技术对石墨中的孔隙进行特定位置的高分辨率表征

石墨在某些类型的核反应堆和其他工业应用中用作快中子的减速剂。较小的孔对石墨的机械和物理性能的影响仍有待充分了解。在这项工作中,使用聚焦离子束扫描电子显微镜(FIB-SEM)断层扫描来表征AGX石墨(一种电极材料)的孔隙率。FIB-SEM层析成像包括在感兴趣的区域交替进行离子铣削和SEM成像,目的是创建3D重建。选择包含填料以及填料和粘合剂的混合物的区域作为关注区域。几纳米的分辨率在体积内实现高达1400微米3这两个地区。在填充剂和粘合剂区域中检测到典型的多孔结构,例如热裂纹,气体逸出孔隙率和双凸透镜孔。通过这些实验获得的分辨率使检测直径小于150 nm的孔成为可能,这是中子辐照产生的空隙的长度尺度,并提高了传统X射线断层扫描研究的空间分辨率。通过FIB-SEM层析成像获得的分辨率对于研究石墨的微观结构可能是必不可少的,这为X射线层析成像实验提供了补充数据。

更新日期:2018-09-04
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