
The concept of high-temperature electrochemistry has broad ranging applications in multiple fields; however, researchers yet remain to conduct real-time observations to gain in-depth understanding of the evolution in such systems. The primary limits include harsh reaction conditions and multiphysics fields. In a new report now published in Science Advances, Handong Jiao and a team of scientists in advanced structure technology and metallurgy in Beijing, China, addressed the challenge by developing a high-temperature electrolysis facility. The facility allowed in-situ X-ray computer microtomography (µCT) for non-destructive and quantitative three-dimensional (3D) imaging. The µCT further probed the dynamic evolution of 3D morphology and components of electrodes in 4D. The team visualized the 4D process using reconstructed images to monitor the efficiency of the process, and explore dynamic mechanisms to provide real-time optimization. The 4D analysis platform provided in-depth combinations of traditional electrochemistry with digital twin methods to extract data and facilitate multiscale visualization.
The experiments
High temperature electrochemistry has many applications across metallurgy, nuclear, chemical production and energy industries. The process can facilitate the molten salt/oxide electrolysis to extract and purify metal, with a prominent role in large-scale stationary energy storage transformation. The process of experimentally examining the evolution of internal dynamics in such systems remains challenging due to limited development of the method. To monitor the dynamic evolution under harsh temperature and electrochemical systems, Li et al. developed a specific high-temperature electrochemical facility with built in X-ray microtomography (µCT) for quantitative 3D imaging, including the morphology and components of electrodes within such systems under extreme conditions. The team verified the apparatus via classical electrorefining experiments of titanium in molten salt. They then performed a 4D study on the electrode structures and chemical components through time. The results combined high temperature electrochemistry with mathematical simulations to quantitatively design and optimize high-temperature electrochemistry.

4D facility of high-temperature electrochemistry in the lab
The homemade in situ 4D characterization apparatus for high temperature electrochemistry contained a quartz tube electrolysis cell fixed vertically to the rotation