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In recent years, the catalyst efficiency of hydrogen evolution reaction (HER) has been extensively studied. However, the stability of catalysts at high current densities is still a challenge. Herein, layered Ni−Co−P was electrodeposited on carbon fiber paper (CFP) via cyclic voltammetry (CV). This low‐cost electrode exhibits high efficiency and excellent durability for HER in 1 M KOH. To achieve current densities of 10, 100, 500, and 1000 mA cm−2, Ni−Co−P/CFP required overpotentials of 49, 95, 170, and 295 mV, respectively. The layered structure allows the catalyst to fall off layer by layer. After the outer layer of catalyst falls off, the inner layer of catalyst will be exposed to continue working. After 300 h of HER at 1000 mA cm−2, Ni−Co−P/CFP still has a regular morphology and high efficiency. Our work shows that layered Ni−Co−P/CFP has excellent prospects for practical applications. [ABSTRACT FROM AUTHOR]

Developing cost‐effective and highly active hydrogen evolution reaction (HER) electrocatalysts is of pivotal importance in the roadmap of hydrogen economy. Increasing active sites and improving conductivity are two effective strategies to optimize the performance of electrocatalyst. In this paper, we report a highly active HER catalyst consisting of ultra‐small molybdenum carbide nanoparticles uniformly entrapped in mesoporous carbon microspheres (Mo2C@MCS) fabricated by in situ synthesis. In 1 M KOH, the catalyst exhibits an excellent HER performance with a pretty low overpotential (134 mV at current density of 10 mA cm−2) and a small Tafel slope (51 mV dec−1), which exceeded the currently reported un‐doped Mo2C catalyst. The excellent HER performance is attributed to the abundant active sites provided by the ultra‐small Mo2C nanoparticles as well as the superior conductivity originated from carbon matrix and the intimate contact between Mo2C nanoparticles and mesoporous carbon wall. [ABSTRACT FROM AUTHOR]