Department of Materials Science and Engineering, City University of Hong Kong, Kowloon, Hong Kong, China.
State Key Lab of Physical Chemistry of Solid Surfaces, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, China.
Nat Protoc. 2023 Feb;18(2):555-578. doi: 10.1038/s41596-022-00762-y. Epub 2022 Nov 4.
Fundamentally understanding the complex electrochemical reactions that are associated with energy devices (e.g., rechargeable batteries, fuel cells and electrolyzers) has attracted worldwide attention. In situ liquid cell transmission electron microscopy (TEM) offers opportunities to directly observe and analyze in-liquid specimens without the need for freezing or drying, which opens up a door for visualizing these complex electrochemical reactions at the nano scale in real time. The key to the success of this technique lies in the design and fabrication of electrochemical liquid cells with thin but strong imaging windows. This protocol describes the detailed procedures of our established technique for the fabrication of such electrochemical liquid cells (~110 h). In addition, the protocol for the in situ TEM observation of electrochemical reactions by using the nanofabricated electrochemical liquid cell is also presented (2 h). We also show and analyze experimental results relating to the electrochemical reactions captured. We believe that this protocol will shed light on strategies for fabricating high-quality TEM liquid cells for probing dynamic electrochemical reactions in high resolution, providing a powerful research tool. This protocol requires access to a clean room equipped with specialized nanofabrication setups as well as TEM characterization equipment.
深入理解与能源设备（如可充电电池、燃料电池和电解槽）相关的复杂电化学反应引起了全球关注。原位液体池透射电子显微镜（TEM）提供了在无需冷冻或干燥的情况下直接观察和分析液体样品的机会，为在纳米尺度上实时可视化这些复杂的电化学反应开辟了一扇大门。该技术的关键在于设计和制造具有薄但坚固成像窗的电化学液体池。本方案描述了我们用于制造这种电化学液体池的既定技术的详细步骤（~110 小时）。此外，还介绍了使用纳米制造电化学液体池原位 TEM 观察电化学反应的方案（2 小时）。我们还展示和分析了所捕获的与电化学反应相关的实验结果。我们相信，该方案将为制造高质量 TEM 液体池以高分辨率探测动态电化学反应提供策略，提供强大的研究工具。该方案需要进入配备有专用纳米制造设备和 TEM 表征设备的洁净室。
