Uniform Pt76Co24 myriapods with abundant active sites were prepared by a one-pot solvothermal method, which exhibited excellent catalytic performances for ORR and HER in acid media.

Three‐dimensional (3D) hollow nanoframes with high surface‐to‐volume ratio and abundant accessible active sites are a type of promising catalysts, albeit with the challenging synthesis by a one‐step solvothermal method. In this research, uniform bimetallic PtCu alloyed hollow cubic nanoframes (HCNFs) were synthesized with high yield by a simple, template‐free, one‐step co‐reduction approach, where cetyltrimethylammonium chloride (CTAC), Cl−/O2, ethanolamine, and oleylamine served as the structure director, oxidative etchant, reducing agent, and co‐reductant, respectively. The architectures were characterized by a series of characterization techniques. Combined with the 3D hollow structures, PtCu HCNFs exhibited enlarged specific/mass activities, boosted catalytic activity, and improved durability for the oxygen reduction reaction (ORR) and glycerol oxidation reaction (GOR) compared with Pt nanocubes (Pt NCs), commercial Pt/C (20 wt %), and Pt black catalysts in alkaline solutions. This work provides guidelines for the rational design and synthesis of frame‐like nanocatalysts with superior catalytic activity and stability.

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