Abstract: Aligned with the “101 Plan” teaching reform objectives for chemical measurement experiments, an innovative instrumental analysis experiment utilizing electrochemical in situRaman spectroscopy was designed and developed. Based on the green ammonia synthesis from electrocatalytic nitrate reduction, this study aims to track the real-time dynamic evolution of active sites and key intermediates on the catalyst surface through the advanced in situ Raman spectroscopy technology, to accurately identify the true catalytic active sites and infer the possible reaction pathways. This experiment has established a comprehensive experimental teaching system that integrates “reaction-characterization-mechanism”, focusing on helping students master knowledge, enhance abilities, and cultivate comprehensive qualities. This experiment fully demonstrates frontier science’s reliance and need for advanced characterization techniques, filling the gap in the interdisciplinary course of “in situ characterization-electrocatalytic reaction”. It can serve as a typical example of experimental teaching reform in new engineering disciplines under the “double helix of scientific research and teaching” model.

Key words: In situ Raman spectroscopy, Electrocatalysis, Nitrate reduction reaction, Ammonia synthesis, Innovative experimental teaching