Core Viewpoint - The article discusses the development of novel characterization techniques in spectroscopy, particularly focusing on in-situ electrochemical Raman spectroscopy, circular dichroism spectroscopy combined with electrochemistry, laser-induced fluorescence spectroscopy, and miniaturized quantum yield testing systems. These advancements aim to study the relationship between the spectra and catalytic activity of various photo/electrocatalytic material interfaces, enhancing the understanding of catalytic materials' surface and interface activities [1][2][3]. Group 1: Research Background and Overall Approach - The conventional spectroscopic techniques are no longer sufficient to meet the increasing demands of research, prompting the development of new characterization techniques [3]. - The research team established in-situ spectral-electrocatalytic testing techniques to investigate surface reconstruction phenomena of catalytic materials, deepening the understanding of their catalytic activities [3]. Group 2: Achievements and Innovations - **Achievement 1**: The construction of an in-situ photochemical reaction attachment for laser confocal Raman spectroscopy, which allows real-time detection and analysis, providing strong support for mechanistic studies in reaction processes [4][5]. - **Achievement 2**: Development of a circular dichroism spectroscopy in-situ measurement electrochemical device, which aids in overcoming the limitations of conventional static detection methods [11][12][16]. - **Achievement 3**: The construction of a laser-induced fluorescence spectroscopy detection module, which is crucial for understanding charge separation and transfer processes in semiconductor photocatalytic materials [18][21][22]. Group 3: Representative Cases - A representative case involved modifying monolayer black phosphorus with hydroxyl and fluorine functional groups to enhance stability and catalytic activity in photocatalytic CO2 reduction [6][9]. - Another case demonstrated the use of Raman-electrochemical coupling to analyze the structural changes in nickel hydroxide catalysts under different potential windows, revealing significant differences in spectral responses [10][14]. Group 4: System Integration and Application - The project team integrated three main devices: laser confocal Raman spectrometer, transient steady-state fluorescence testing system, and circular dichroism spectrometer, establishing a series of in-situ analysis characterization modules [35]. - Over the past three years, the team supported the publication of 445 SCI papers in the field of photocatalysis, contributing to the development of various disciplines such as physics, chemistry, and materials science [37]. Group 5: Conclusion - The research team has established innovative characterization techniques that significantly enhance the understanding of the relationship between spectra and catalytic activity in photo/electrocatalytic materials, leading to original and leading-edge results recognized by peers [36].