Rapid, High‐Temperature, In Situ Microwave Synthesis of Bulk Nanocatalysts

Carbon‐black‐supported nanoparticles (CNPs) have attracted considerable attention for their intriguing catalytic properties and promising applications. The traditional liquid synthesis of CNPs commonly involves demanding operation conditions and complex pre‐ or post‐treatments, which are time consuming and energy inefficient. Herein, a rapid, scalable, and universal strategy is reported to synthesize highly dispersed metal nanoparticles embedded in a carbon matrix via microwave irradiation of carbon black with preloaded precursors. By optimizing the amount of carbon black, the microwave absorption is dramatically improved while the thermal dissipation is effectively controlled, leading to a rapid temperature increase in carbon black, ramping to 1270 K in just 6 s. The whole synthesis process requires no capping agents or surfactants, nor tedious pre‐ or post‐treatments of carbon black, showing tremendous potential for mass production. As a proof of concept, the synthesis of ultrafine Ru nanoparticles (≈2.57 nm) uniformly embedded in carbon black using this microwave heating technique is demonstrated, which displays remarkable electrocatalytic performance when used as the cathode in a Li–O2 battery. This microwave heating method can be extended to the synthesis of other nanoparticles, thereby providing a general methodology for the mass production of carbon‐supported catalytic nanoparticles. A rapid, in situ high‐temperature microwave heating strategy is reported for the synthesis of carbon‐supported nanocatalysts. The temperature of this method reaches up to 1270 K in 6 s. The optimized loading amount of the carbon black is crucial to achieve the rapid high‐temperature heating.