Compared with the monometallic phosphides, bimetallic phosphides can further improve the catalytic performance for hydrogen evolution reaction (HER). As such, the rational design and facile synthesis of bimetallicbased phosphides with well-controlled architectures and compositions is of scientific and technological importance. In this work, Fe−Co Prussian blue analogue (PBA) nanocones (NCs) have been successfully fabricated via an intercalation reaction strategy by utilizing layer structured α-Co(OH) 2 NCs as self-sacrificing templates. After calcination and phosphorization process, Fe−Co PBA NCs can be converted to Fe-doped Co x P NCs without obvious shrinkage. Electrochemical tests show that Fe incorporation can effectively promote the electrocatalytic activities of Co x P. This simple and effective method will be of benefit for the development of other functional Co-based bimetallic compounds. Furthermore, this strategy can possibly be extended to fabricate a series of PBA materials with special structure and novel morphology, which can serve as a promising platform for diverse applications, especially in energy storage and conversion.

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High‐performance electrocatalysts with superior stability are critically important for their practical applications in the hydrogen evolution reaction (HER). Recently, some electrocatalysts with hollow and porous structures have attracted much attention because of their large surface‐to‐volume ratio and highly exposed active edge sites. In this study, the hierarchical Fe‐based glycolate hollow microspheres composed of nanosheet subunits are synthesized by the solvothermal method. The morphology and microstructure of Fe‐based glycolate hollow microspheres can be controlled by adjusting the amount of ethylenediamine. After phosphorizing in nitrogen, the Fe‐based glycolate can be converted into FeP with well‐retained structure. Furthermore, the hierarchical FeP hollow microspheres have been used as electrocatalysts for HER. Benefitting from its high surface area, the FeP hollow microspheres exhibited high catalytic activity toward HER with low onset overpotential, small Tafel slope, and good stability under acidic conditions. The excellent catalytic activity and long‐term stability suggest promising application potential of FeP hollow microspheres in electrocatalytic hydrogen evolution.

The Schematic illustration of the distribution of the electric field between two testing parallel-plates after the formation of chainlike structure in electrorheological fluids.

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