Carbon‐Embedded Fe‐Cu Composite Oxide Nanoparticles Derived From Spindle‐Shaped Bimetallic MOFs for Selective Oxidation of Methane

Achieving both high activity and selectivity in the direct oxidation of methane under mild conditions remains challenging. In this work, Fe‐Cu/C composites were prepared by pyrolysis of Fe‐Cu bimetallic MOF precursors and evaluated for methane oxidation with H 2 O 2 at 80°C. Among the catalysts, Fe 3 Cu 1 /C exhibited the highest C1 oxygenate productivity (6.38 mmol·g cat −1 ·h −1 ), with no detectable CO x under the standard analytical conditions and an apparent selectivity approaching 100% among quantified products that contain carbon. Structural characterization indicates Cu‐Fe composite oxide nanoparticles embedded in a carbon matrix. Control experiments show that catalyst composition affects productive H 2 O 2 utilization and detectable overoxidation relative to monometallic and atmosphere‐treated controls. 13 CH 4 labeling confirms that the quantified C1 oxygenates originate from methane. EPR data suggest radical species drive C‐H activation and oxygenation network without uniquely identifying radicals centered on carbon.