Meng Xiaoxia, Bi Zhuanfang, Wang Xinru, Shang Guangyi
School of Physics, Beihang University, Beijing 100191, People's Republic of China.
Rev Sci Instrum. 2022 Jul 1;93(7):073707. doi: 10.1063/5.0096766.
The emergence of functional materials, especially energy materials made up of various structures with different properties, requires the development of complementary or integrated characterization technologies. The combination of atomic force microscopy and Raman spectroscopy (AFM-Raman) offers a powerful technique for the in situ characterization of physical properties (AFM) and chemical composition (Raman) of materials simultaneously. To further extend the potential application in the battery's field, we here present an electrochemical AFM-Raman (EC-AFM-Raman) in the reflection mode, developed by designing a novel structure including water-immersion objective lens-based optics for high-sensitivity Raman excitation/collection, optical level detection for AFM imaging in the solution, and a dual-cell for electrochemical reaction. EC-AFM imaging and Raman measurement can be realized simultaneously. Dynamic morphologic evolution and phase transition of the LiMnO particles during cyclic voltammetry measurement were successfully observed. This technique will provide the possibility of probing physicochemical phenomena of the battery materials and other surface/interface processes such as the formation of the solid electrolyte interphase layer.
功能材料的出现，尤其是由具有不同性质的各种结构组成的能量材料，需要开发互补或集成的表征技术。原子力显微镜与拉曼光谱相结合（AFM-Raman）提供了一种强大的技术，可同时对材料的物理性质（AFM）和化学成分（拉曼）进行原位表征。为了进一步扩展在电池领域的潜在应用，我们在此展示一种反射模式的电化学AFM-Raman（EC-AFM-Raman），它通过设计一种新颖的结构开发而成，该结构包括用于高灵敏度拉曼激发/收集的基于水浸物镜的光学器件、用于溶液中AFM成像的光学水平检测以及用于电化学反应的双电池。可以同时实现EC-AFM成像和拉曼测量。成功观察到循环伏安法测量过程中LiMnO颗粒的动态形态演变和相变。该技术将为探究电池材料的物理化学现象以及其他表面/界面过程（如固体电解质中间相层的形成）提供可能性。
