Wang Wenbin, Qi Junlei, Wu Zongxiao, Zhai Wei, Pan Yanghang, Bao Kai, Zhai Li, Wu Jingkun, Ke Chengxuan, Wang Lingzhi, Ding Mengning, He Qiyuan
Department of Materials Science and Engineering, City University of Hong Kong, Kowloon, Hong Kong, China.
Department of Chemistry, City University of Hong Kong, Kowloon, Hong Kong, China.
Nat Protoc. 2023 Oct;18(10):2891-2926. doi: 10.1038/s41596-023-00866-z. Epub 2023 Aug 18.
On-chip electrocatalytic microdevices (OCEMs) are an emerging electrochemical platform specialized for investigating nanocatalysts at the microscopic level. The OCEM platform allows high-precision electrochemical measurements at the individual nanomaterial level and, more importantly, offers unique perspectives inaccessible with conventional electrochemical methods. This protocol describes the critical concepts, experimental standardization, operational principles and data analysis of OCEMs. Specifically, standard protocols for the measurement of the electrocatalytic hydrogen evolution reaction of individual 2D nanosheets are introduced with data validation, interpretation and benchmarking. A series of factors (e.g., the exposed area of material, the choice of passivation layer and current leakage) that could have effects on the accuracy and reliability of measurement are discussed. In addition, as an example of the high adaptability of OCEMs, the protocol for in situ electrical transport measurement is detailed. We believe that this protocol will promote the general adoption of the OCEM platform and inspire further development in the near future. This protocol requires essential knowledge in chemical synthesis, device fabrication and electrochemistry.
片上电催化微器件（OCEMs）是一种新兴的电化学平台，专门用于在微观层面研究纳米催化剂。OCEM平台允许在单个纳米材料层面进行高精度电化学测量，更重要的是，提供了传统电化学方法无法获得的独特视角。本方案描述了OCEMs的关键概念、实验标准化、操作原理和数据分析。具体而言，介绍了用于测量单个二维纳米片电催化析氢反应的标准方案，并进行了数据验证、解释和基准测试。讨论了一系列可能影响测量准确性和可靠性的因素（例如材料的暴露面积、钝化层的选择和电流泄漏）。此外，作为OCEMs高适应性的一个例子，详细介绍了原位电输运测量方案。我们相信，本方案将促进OCEM平台的广泛应用，并在不久的将来激发进一步的发展。本方案需要化学合成、器件制造和电化学方面的基础知识。
