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Optimization of Material Contrast for Efficient FIB‐SEM Tomography of Solid Oxide Fuel Cells
Fuel Cells ( IF 2.8 ) Pub Date : 2020-10-01 , DOI: 10.1002/fuce.202000080
M. Meffert 1 , F. Wankmüller 2 , H. Störmer 1 , A. Weber 2 , P. Lupetin 3 , E. Ivers‐Tiffée 2 , D. Gerthsen 1
Affiliation  

Focused ion beam (FIB) – scanning electron microscopy (SEM) serial sectioning tomography has become an important tool for three‐dimensional microstructure reconstruction of solid oxide fuel cells (SOFC) to obtain an understanding of fabrication‐related effects and SOFC performance. By sequential FIB milling and SEM imaging a stack of cross‐section images across all functional SOFC layers was generated covering a large volume of 3.5·10$^{4}$ μm$^{3}$. One crucial step is image segmentation where regions with different image intensities are assigned to different material phases within the SOFC. To analyze all relevant SOFC materials, it was up to now mandatory to acquire several images by scanning the same region with different imaging parameters because sufficient material contrast could otherwise not be achieved. In this work we obtained high‐contast SEM images from a single scan to reconstract all functional SOFC layers consisting of a Ni/Y$_{2}$O$_{3}$‐doped ZrO$_{2}$ (YDZ) cermet anode, YDZ electrolyte and (La,Sr)MnO$_{3}$/YDZ cathode. This was possible by using different, simultaneous read‐out detectors installed in a state‐of‐the‐art scanning electron microscope. In addition, we used a deterministic approach for the optimization of imaging parameters by employing Monte Carlo simulations rather than trial‐and‐error tests. We also studied the effect of detection geometry, detecting angle range and detector type.

中文翻译:

固体氧化物燃料电池高效 FIB-SEM 层析成像的材料对比度优化

聚焦离子束(FIB)-扫描电子显微镜(SEM)连续切片断层扫描已成为固体氧化物燃料电池(SOFC)三维微观结构重建的重要工具,以了解制造相关效应和SO​​FC性能。通过连续 FIB 铣削和 SEM 成像,生成了跨越所有功能性 SOFC 层的一系列横截面图像,覆盖了 3.5·10$^{4}$ μm$^{3}$ 的大体积。一个关键步骤是图像分割,其中将具有不同图像强度的区域分配给 SOFC 内的不同材料相。为了分析所有相关的 SOFC 材料,到目前为止,必须通过使用不同的成像参数扫描同一区域来获取多张图像,否则无法获得足够的材料对比度。在这项工作中,我们从单次扫描中获得了高对比度 SEM 图像,以重建由 Ni/Y$_{2}$O$_{3}$ 掺杂的 ZrO$_{2}$ (YDZ ) 金属陶瓷阳极、YDZ 电解质和 (La,Sr)MnO$_{3}$/YDZ 阴极。这可以通过使用安装在最先进的扫描电子显微镜中的不同的同步读出探测器来实现。此外,我们通过采用蒙特卡罗模拟而不是反复试验,使用确定性方法来优化成像参数。我们还研究了检测几何、检测角度范围和检测器类型的影响。安装在最先进的扫描电子显微镜中的同步读出探测器。此外,我们通过采用蒙特卡罗模拟而不是反复试验,使用确定性方法来优化成像参数。我们还研究了检测几何、检测角度范围和检测器类型的影响。安装在最先进的扫描电子显微镜中的同步读出探测器。此外,我们通过采用蒙特卡罗模拟而不是反复试验,使用确定性方法来优化成像参数。我们还研究了检测几何、检测角度范围和检测器类型的影响。
更新日期:2020-10-01
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