BackgroundWith the application of the scanning transmission electron microscopy (STEM) detector, transmitted electron images similar to transmission electron microscopy (TEM) can be obtained from scanning electron microscopy (SEM), which is referred to STEM-in-SEM imaging. Compared to TEM-energy dispersive spectroscopy (EDS), SEM-EDS is expected to be more efficient and reliable for chemical analysis of TEM specimens due to the larger sample space in SEM and the higher take-off angle of the SEM-EDS detector. Unfortunately, this advantage is not well applied to TEM specimens in practice, mainly because of fault signals generated from the commercial grid holders used in SEM and STEM-in-SEM. This study is designed to solve this problem by modifying the commercial holders and to test them through EDS analysis of apatite phases.FindingsWe first changed the way of assembling parts of the commercial multi-grid holder for SEM. This new assembly was capable of producing a thinner upper cover part, resulting in the reduction of the EDS fault signals generated from the holder. Furthermore, the thin upper part allowed us to get images in shorter working distances, that is, at higher magnifications. This design concept was also applied to the commercial single-grid holder for STEM-in-SEM, producing a new multi-grid holder to be used for loading multiple samples.ConclusionWe confirmed that the new holders produced reliable chemical data from apatite phases. In case of oxygen analysis, despite of low electron brightness from the tungsten source, 5 kV provided more stable acquisition and signal yields than 15 kV. We expect that these modified holders facilitate more efficient EDS analysis for multiple samples under the same analytical conditions in SEM and STEM-in-SEM.

中文翻译：

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用于 EDS 分析的 SEM 和 STEM-in-SEM 网格支架的开发及其在磷灰石相中的应用

背景随着扫描透射电子显微镜（STEM）探测器的应用，从扫描电子显微镜（SEM）中可以获得类似于透射电子显微镜（TEM）的透射电子图像，称为STEM-in-SEM成像。与 TEM-能量色散光谱 (EDS) 相比，由于 SEM 中更大的样品空间和 SEM-EDS 探测器的更高起飞角，预计 SEM-EDS 对 TEM 样品的化学分析更加有效和可靠。不幸的是，这一优势在实践中并没有很好地应用于 TEM 样品，主要是因为 SEM 和 STEM-in-SEM 中使用的商业网格支架产生的故障信号。本研究旨在通过修改商业持有人来解决这个问题，并通过磷灰石相的 EDS 分析对其进行测试。调查结果我们首先改变了用于 SEM 的商用多栅支架部件的组装方式。这种新组件能够生产更薄的上盖部件，从而减少了支架产生的 EDS 故障信号。此外，较薄的上部使我们能够在更短的工作距离（即更高的放大倍率）下获得图像。这一设计理念也应用于 STEM-in-SEM 的商业单网格支架，生产出一种新的多网格支架，用于加载多个样品。结论我们证实，新支架从磷灰石相中产生了可靠的化学数据。在氧气分析的情况下，尽管钨源的电子亮度较低，但 5 kV 提供了比 15 kV 更稳定的采集和信号产率。