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Unraveling the Dynamic Structural Evolution of Phthalocyanine Catalysts during CO₂ Electroreduction
Jianing Mao, Bingbao Mei*, Ji Li, Shuai Yang, Fanfei Sun, Siyu Lu, Wei Chen, Fei Song* and Zheng Jiang*

Phthalocyanine catalysts have well-defined active site structures that allow reaction-based mechanism exploration. In this regard, the actual behaviors of metal ions in the phthalocyanine catalysts have aroused considerable attention. Operando high-energy resolution fluorescence detected X-ray absorption (HERFD-XANES) can be employed in the practical situation of electrocatalysis to realize the interfacial interaction between metal ions and the reactants, offering a unique insight into the active site geometry and structural evolution during CO₂ reduction. In this work, the CO₂RR to CO dominates over the HER with Faradaic efficiency reaching the maximum value of 89% at 0.85 V versus RHE. The results demonstrate the atomically dispersed, low-valent Ni(I) centres with high intrinsic CO₂ reduction activity.