Quantitative chemical analysis on the nanoscale provides valuable information on materials and devices which can be used to guide further improvements to their performance. In particular, emerging families of technologically relevant composite materials such as organic–inorganic hybrid halide perovskites and metal‐organic frameworks stand to benefit greatly from such characterization. However, these nanocomposites are also vulnerable to damage induced by analytical probes such as electron, X‐ray, or neutron beams. Here the effect of electrons on a model hybrid halide perovskite is investigated, focusing on the acquisition parameters appropriate for energy‐dispersive X‐ray spectroscopy in a scanning transmission electron microscope (STEM‐EDX). The acquisition parameters are systematically varied to examine the relationship between electron dose, data quality, and beam damage. Five metrics are outlined to assess the quality of STEM‐EDX data and severity of beam damage, further validated by dark field STEM imaging. Loss of iodine through vacancy creation is found to be the primary manifestation of electron beam damage in the perovskite specimen, and iodine content is seen to decrease exponentially with electron dose. This work demonstrates data acquisition and analysis strategies that can be used for studying electron beam damage and for achieving reliable quantification for a broad range of beam‐sensitive materials.

中文翻译：

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光束敏感材料的纳米化学分析：钙钛矿太阳能电池上 STEM-EDX 的案例研究

纳米级的定量化学分析提供了有关材料和设备的宝贵信息，可用于指导进一步改进其性能。特别是，新兴的技术相关复合材料系列，如有机-无机杂化卤化物钙钛矿和金属-有机骨架，将从这种表征中受益匪浅。然而，这些纳米复合材料也容易受到分析探针（如电子、X 射线或中子束）引起的损伤。在这里，研究了电子对模型混合卤化物钙钛矿的影响，重点是扫描透射电子显微镜 (STEM-EDX) 中适合于能量色散 X 射线光谱的采集参数。系统地改变采集参数以检查电子剂量之间的关系，数据质量和光束损坏。概述了五个指标来评估 STEM-EDX 数据的质量和光束损伤的严重程度，并通过暗场 STEM 成像进一步验证。发现由于空位产生造成的碘损失是钙钛矿样品中电子束损伤的主要表现，并且可以看到碘含量随电子剂量呈指数下降。这项工作展示了数据采集和分析策略，可用于研究电子束损伤并实现对各种束敏感材料的可靠量化。发现由于空位产生造成的碘损失是钙钛矿样品中电子束损伤的主要表现，并且可以看到碘含量随电子剂量呈指数下降。这项工作展示了数据采集和分析策略，可用于研究电子束损伤并实现对各种束敏感材料的可靠量化。发现由于空位产生造成的碘损失是钙钛矿样品中电子束损伤的主要表现，并且可以看到碘含量随电子剂量呈指数下降。这项工作展示了数据采集和分析策略，可用于研究电子束损伤并实现对各种束敏感材料的可靠量化。