From Earth‐Abundant Mineral Sources to High‐Efficiency Dual‐Atom Catalysts: A Chloride‐Guided One‐Pot Synthesis Approach

Abstract While atomically dispersed catalysts (ADCs) exhibit exceptional catalytic performance, their scalable synthesis remains challenging due to metal aggregation tendencies. Traditional preparation methods relying on precursor optimization and multi‐step protocols often fail to ensure atomic dispersion. In this work, a groundbreaking chloride‐mediated diffusion strategy is introduced to synthesize carbon‐supported ADCs, with the strategically designed Fe‐Mg hetero‐diatomic pair catalyst as a pioneering demonstration. This approach enables the spontaneous conversion of diverse metal precursors—including earth‐abundant unprocessed mineral ores into volatile metal chlorides under HCl, which subsequently diffuse and atomically anchor on nitrogen‐doped carbon supports. The Fe‐Mg dual‐atom catalyst, featuring synergistic metal coordination, exhibits remarkable CO 2 electroreduction activity, underscoring the method's capacity to create heteronuclear active sites. This strategy bypasses precursor limitations and complex procedures, offering a universal, viable pathway to scalable ADC fabrication, with the Fe‐Mg system exemplifying its transformative potential for designing advanced multi‐atomic catalysts.