Topological Conversion of Nickel Foams to Monolithic Single‐Atom Catalysts

Abstract Single‐atom catalysts have emerged as a promising class of catalysts due to their tailored coordination environments on the support, which can improve a variety of catalytic reactions, making them a highly desirable research subject in materials science with significant potential for industrial applications. However, traditional synthesis methods mainly obtain low‐yield powder catalysts without macroscopic mechanical strength, and also require tedious procedures, limiting their practicability. Here, monolithic carbon fibers are prepared with single atomic Ni sites directly from bulk metal. The synchronous support growth and metal diffusion realizes the effective atomization of nickel foam, and the innovative strategy of topological growth within a confined space results in robust and tough monolith. The application of this single‐atom‐monolith is demonstrated as a free‐standing electrode for highly efficient electrochemical CO 2 reduction. The proposed synthesis strategy allows feasible preparation of functional single‐atom catalysts for potential industrial applications with advantages of using low‐cost raw materials, enabling large‐scale production, and providing processable, moldable monolithic materials.