This work shows a combined setup of Diffuse Reflectance FT-IR Spectroscopy (DRIFTS) and electrochemical characterization by AC and DC methods for in situ and operando investigations of surface species during CO2 electrolysis on metal oxide electrodes and their correlation with electrochemical activity. A high-temperature reaction chamber enables conducting DRIFTS and electrochemical experiments simultaneously at temperatures up to 1000 °C in both reductive and oxidative reaction atmospheres and under anodic and cathodic polarization conditions. A dedicated gas- and electrical feedthrough solution is presented, which is the key element required for recording electrochemical AC and DC characteristics using an electrochemical cell, which is simultaneously studied by DRIFTS experiments under realistic operation conditions. Selected results, obtained on a gadolinium doped ceria model solid oxide electrolysis cell upon different polarization states, demonstrate the basic functionality and capabilities of the setup and show how the simultaneous DRIFT-spectroscopic and electrochemical investigation of the surface and bulk chemistry on electrode materials leads to increased insight in the population of potential intermediates during CO2 electrolysis. With infrared spectroscopy and impedance spectroscopy as common and complementary spectroscopic methods in material science, the setup is considered to exhibit a huge potential in a wide field of fundamental and applied mechanistic research.

中文翻译：

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用于金属氧化物电极表面原位和操作机制研究的光谱电化学装置

这项工作展示了漫反射 FT-IR 光谱 (DRIFTS) 和通过 AC 和 DC 方法进行电化学表征的组合设置，用于在金属氧化物电极上的 CO2 电解过程中对表面物质进行原位和操作研究及其与电化学活性的相关性。高温反应室能够在高达 1000 °C 的温度下在还原和氧化反应气氛以及阳极和阴极极化条件下同时进行 DRIFTS 和电化学实验。提出了一种专用的气体和电气馈通解决方案，这是使用电化学电池记录电化学交流和直流特性所需的关键元素，同时在实际操作条件下通过 DRIFTS 实验进行研究。选定的结果，在不同极化状态下在掺钆二氧化铈模型固体氧化物电解池上获得的，展示了该装置的基本功能和能力，并展示了电极材料表面和本体化学的同步漂移光谱和电化学研究如何提高对CO2电解过程中潜在中间体的数量。随着红外光谱和阻抗光谱作为材料科学中常见和互补的光谱方法，该装置被认为在基础和应用力学研究的广泛领域中表现出巨大的潜力。展示了该装置的基本功能和能力，并展示了电极材料表面和本体化学的同步漂移光谱和电化学研究如何提高对 CO2 电解过程中潜在中间体群体的了解。随着红外光谱和阻抗光谱作为材料科学中常见和互补的光谱方法，该装置被认为在基础和应用力学研究的广泛领域中表现出巨大的潜力。展示了该装置的基本功能和能力，并展示了电极材料表面和本体化学的同步漂移光谱和电化学研究如何提高对 CO2 电解过程中潜在中间体群体的了解。随着红外光谱和阻抗光谱作为材料科学中常见和互补的光谱方法，该装置被认为在基础和应用力学研究的广泛领域中表现出巨大的潜力。