A reasonable design of excellent bifunctional catalyst is an effective strategy for large-scale hydrogen production. In this study, a two-stage electrodeposition method was used to prepare a crystalline-amorphous structure cobalt molybdenum phosphide layered particles with different sizes on a nickel foam (NF) substrate. Electron rearrangement at the Co/CoMoP₂@CoMoO₄ heterogeneous interface can reduce the reaction energy barrier for HER and OER, and accelerate the catalytic reaction kinetics. The doping of Mo can promote the synergistic effect between Co and Mo, thereby optimizing the Gibbs free energy of hydrogen adsorption/desorption. This layered arrangement of different size particles greatly improves the active area of the catalyst. In alkaline solution, achieving a current density of 10 mA cm⁻² only required overpotentials of 40 mV for HER and 278 mV for OER, respectively. The cell voltage required for the CoMo-P/NF||CoMo-P/NF electrolytic cell is only 1.53 V at 10 mA cm⁻². This study provides a reference for the rapid, efficient, and environmentally friendly preparation of high-activity water splitting catalysts with large surface areas.

合理设计优良的双功能催化剂是大规模制氢的有效策略。本研究采用两阶段电沉积方法在泡沫镍（NF）基底上制备了不同尺寸的晶非晶结构磷化钴钼层状颗粒。 Co/CoMoP ₂ @CoMoO ₄异质界面的电子重排可以降低HER和OER的反应能垒，加速催化反应动力学。 Mo的掺杂可以促进Co和Mo之间的协同效应，从而优化氢吸附/脱附的吉布斯自由能。这种不同尺寸颗粒的层状排列极大地提高了催化剂的活性面积。在碱性溶液中，实现10 mA cm ^-2的电流密度仅需要HER 40 mV 和OER 278 mV 的过电势。 CoMo-P/NF||CoMo-P/NF电解池所需的电池电压在10 mA cm ^-2下仅为1.53 V。该研究为快速、高效、环境友好地制备高活性大比表面积水分解催化剂提供参考。