Using 4-D X-ray computer microtomography to observe high-temperature electrochemistry

Schematics and photographs of 4D imaging apparatus for high-temperature electrochemistry. (A) 3D scheme of the assembled 4D characterization facility for high-temperature electrochemistry. (B) Schematic of the facility in transmission mode for x-ray μ-CT. (C) Photograph of the 4D studying facility. (D) Photograph of the high-temperature electrolysis cell through a peephole of the facility. (E) 3D reconstructed image of the experimental electrolysis cell at high temperature. Credit: Science Advances, DOI: 10.1126/sciadv.abm5678

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 /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.

Using 4-D X-ray computer microtomography to observe high-temperature electrochemistry
4D imaging and analysis of Ti electrorefining in the molten salt medium. (A and B) 3D reconstructed images of the Ti anode and Ni cathode at different electrolysis time ranges. Current density, 0.3 A cm−2 (A) and 0.6 A cm−2 (B). (C and D) The change of the dissolution mass of Ti anode and the Ti deposition mass on the Ni cathode at different electrolysis stages. The insets are current efficiencies of Ti anode and Ni cathode at different electrolysis stages. (E) The competitive mechanism of possible reactions at electrodes. Credit: Science Advances, DOI: 10.1126/sciadv.abm5678

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

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