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.

从根本上了解与能源设备（例如，可充电电池、燃料电池和电解槽）相关的复杂电化学反应已引起全世界的关注。原位液体细胞透射电子显微镜 (TEM) 提供了直接观察和分析液体样品的机会，无需冷冻或干燥，这为在纳米尺度上实时可视化这些复杂的电化学反应打开了一扇门。这项技术成功的关键在于设计和制造具有薄而坚固的成像窗口的电化学液体电池。该协议描述了我们为制造这种电化学液体电池（~110 小时）而建立的技术的详细程序。此外，还介绍了使用纳米制造电化学液体电池对电化学反应进行原位 TEM 观察的协议（2 小时）。我们还展示并分析了与捕获的电化学反应相关的实验结果。我们相信，该协议将阐明制造高质量 TEM 液体电池的策略，以高分辨率探测动态电化学反应，提供强大的研究工具。该协议需要进入配备有专门的纳米加工装置和 TEM 表征设备的洁净室。我们相信，该协议将阐明制造高质量 TEM 液体电池的策略，以高分辨率探测动态电化学反应，提供强大的研究工具。该协议需要进入配备有专门的纳米加工装置和 TEM 表征设备的洁净室。我们相信，该协议将阐明制造高质量 TEM 液体电池的策略，以高分辨率探测动态电化学反应，提供强大的研究工具。该协议需要进入配备有专门的纳米加工装置和 TEM 表征设备的洁净室。