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High‐efficiency and low‐cost catalysts for oxygen evolution reaction (OER) are critical for electrochemical water splitting to generate hydrogen, which is a clean fuel for sustainable energy conversion and storage. Among the emerging OER catalysts, transition metal dichalcogenides have exhibited superior activity compared to commercial standards such as RuO₂, but inferior stability due to uncontrolled restructuring with OER. In this study, we create bimetallic sulfide catalysts by adapting the atomic ratio of Ni and Co in Co_xNi_1‐xS_yelectrocatalysts to investigate the intricate restructuring processes. Surface‐sensitive X‐ray photoelectron spectroscopy and bulk‐sensitive X‐ray absorption spectroscopy confirmed the favorable restructuring of transition metal sulfide material following OER processes. Our results indicate that a small amount of Ni substitution can reshape the Co local electronic structure, which regulates the restructuring process to optimize the balance between OER activity and stability. This work represents a significant advancement in the development of efficient and noble metal‐free OER electrocatalysts through a doping‐regulated restructuring approach.

The electrochemical carbon dioxide reduction reaction (CO₂RR) is a promising approach for reducing atmospheric carbon dioxide (CO₂) emissions, allowing harmful CO₂to be converted into more valuable carbon‐based products. On one hand, single carbon (C₁) products have been obtained with high efficiency and show great promise for industrial CO₂capture. However, multi‐carbon (C₂₊) products possess high market value and have demonstrated significant promise as potential products for CO₂RR. Due to CO₂RR's multiple pathways with similar equilibrium potentials, the extended reaction mechanisms necessary to form C₂₊products continue to reduce the overall selectivity of CO₂‐to‐C₂₊electroconversion. Meanwhile, CO₂RR as a whole faces many challenges relating to system optimization, owing to an intolerance for low surface pH, systemic stability and utilization issues, and a competing side reaction in the form of the H₂evolution reaction (HER). Ethylene (C₂H₄) remains incredibly valuable within the chemical industry; however, the current established method for producing ethylene (steam cracking) contributes to the emission of CO₂into the atmosphere. Thus, strategies to significantly increase the efficiency of this technology are essential. This review will discuss the vital factors influencing CO₂RR in forming C₂H₄products and summarize the recent advancements in ethylene electrosynthesis.