Many modern energy devices rely on solid–liquid interfaces, highly reactive materials, or both, for their operation and performance. The difficulty of characterizing such materials means these devices often lack high-resolution characterization in an unaltered state. Here, we demonstrate how cryogenic sample preparation and transfer can extend the capabilities of FIB/SEM techniques to solid–liquid interfaces and reactive materials common to energy devices by preserving their integrity through all stages of preparation and characterization. We additionally show how cryo-FIB/SEM paired with energy dispersive X-ray spectroscopy enables nanoscale elemental mapping of cross-sections produced in these materials and discuss strategies to achieve optimal results. Finally, we consider current limitations of the technique and propose future developments that could enhance its capabilities. Our results illustrate that cryo-FIB/SEM will be a useful technique for fields where solid–liquid interfaces or reactive materials play an important role and could, thus far, not be characterized at high resolution.

中文翻译：

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通过Cryo-FIB / SEM实现的能量装置中完整的固液界面和活性材料的纳米尺度元素映射

许多现代能源设备的运行和性能都依赖于固液界面，高反应性材料或两者兼而有之。表征此类材料的困难意味着这些设备在未更改的状态下通常缺乏高分辨率的表征。在这里，我们演示了低温样品的制备和转移如何通过在制备和表征的所有阶段保持完整性，将FIB / SEM技术的功能扩展到能量设备常用的固液界面和反应性材料。我们还展示了冷冻FIB / SEM与能量色散X射线光谱技术配对如何使这些材料中产生的横截面的纳米级元素映射成为可能，并讨论了实现最佳结果的策略。最后，我们考虑了该技术的当前局限性，并提出了可以增强其功能的未来发展。我们的研究结果表明，对于固液界面或反应性材料起着重要作用并且迄今为止可能无法以高分辨率表征的领域，cryo-FIB / SEM将是一种有用的技术。