Experimental investigation and simulation of SEM image intensity behaviors for developing thickness-controlled S/TEM lamella preparation via FIB-SEM.

Jun Uzuhashi, Yuanzhao Yao, Tadakatsu Ohkubo, Takashi Sekiguchi
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Abstract

High-quality thin lamellae are essential for state-of-the-art scanning transmission electron microscopy (S/TEM) analyses. While the preparation of S/TEM lamellae using focused ion beam (FIB) scanning electron microscopy has been established since the early twenty-first century, two critical factors have only recently been addressed: precise control over lamella thickness and a systematic understanding of FIB-induced damage. This study conducts an experimental investigation and simulation to explore how the intensities of backscattered and secondary electrons (BSEs and SEs, respectively) depend on lamella thickness for semiconductor (Si), insulator (Al2O3), and metallic (stainless-steel) materials. The BSE intensity shows a simple linear relationship with the lamella thickness for all materials below a certain thickness, whereas the relationship between the SE intensity and thickness is more complex. In conclusion, the BSE intensity is a reliable indicator for accurately determining lamella thickness across various materials during FIB thinning processing, while the SE intensity lacks consistency due to material and detector variability. This insight enables the integration of real-time thickness control into S/TEM lamella preparation, significantly enhancing lamella quality and reproducibility. These findings pave the way for more efficient, automated processes in high-quality S/TEM analysis, making the preparation method more reliable for a range of applications.

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FIB-SEM制备厚度可控S/TEM薄片的SEM图像强度行为的实验研究与模拟。
高质量的薄薄片是最先进的扫描透射电子显微镜(S/TEM)分析必不可少的。虽然自21世纪初以来,利用聚焦离子束(FIB)扫描电子显微镜(SEM)制备S/TEM片层已经建立起来,但两个关键因素直到最近才得到解决:精确控制片层厚度和对FIB诱导损伤的系统理解。本研究进行了实验研究和模拟,以探讨半导体(Si)、绝缘体(Al2O3)和金属(不锈钢)材料的背散射和二次电子(分别为bse和SEs)的强度如何依赖于片层厚度。在一定厚度以下的材料中,BSE强度与片层厚度呈简单的线性关系,而SE强度与片层厚度之间的关系则更为复杂。综上所述,在FIB减薄过程中,BSE强度是准确确定各种材料薄片厚度的可靠指标,而SE强度由于材料和探测器的可变性而缺乏一致性。这种洞察力使实时厚度控制集成到S/TEM薄片制备中,显着提高了薄片质量和再现性。这些发现为高质量S/TEM分析中更高效、自动化的过程铺平了道路,使制备方法在一系列应用中更加可靠。
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