High-loading Pt/C catalysts play an important role in the practical application of metal–air batteries and fuel cells because of their superior activity, high conductivity, and commercial availability. It is well known that high loadings always lead to the agglomeration of Pt nanoparticles, resulting in a loss of catalytic activity and stability; thus, it still remains a challenge to prepare high-loading Pt/C catalysts with high dispersion and small particle sizes. Here, we introduce a surfactant-assisted microwave discharge method to prepare high-loading (>40 wt %) Pt/C electrocatalysts with ultrafine particle sizes (∼3.19 nm) and good dispersion. Benefitting from the high-temperature property and reducibility of carbon-induced-arc, the surfactant and Pt precursors undergo rapid decomposition, reduction, and carbonization, generating the structure of Pt@C on carbon black. The carbon derived from the surfactant can not only inhibit the agglomeration of Pt nanoparticles but also prevent the Pt core from toxication, ensuring high activity and stability of the high-loading Pt/C catalyst. When evaluated in the oxygen reduction reaction, the as-prepared Pt/C catalyst demonstrates a comparable activity and better methanol resistance to commercial Pt/C.

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