context: All the electrochemical measurements were carried out on a CHI 660E electrochemical workstation with a standard three-electrode system in 0.5 M aqueous urea solution, and 1 M KOH solution with or without 0.5 M urea at room temperature. A mercury oxide electrode (Hg/HgO), platinum electrode (Pt), and the prepared materials were used as the reference electrode, the counter electrode, and the working electrode, respectively. The mass loading of the catalysts on the nickel foam is 1.5 mg cm−2. And the amount of commercial Pt/C and IrO2 on NF is the same as the loading of MoP@NiCo-LDH/NF-20. The two-electrode electrolyser uses a 007-2H exchangeable membrane electrolytic cell (50 mL) with Nafion 117 as the diaphragm. The synthesized catalysts were used as the cathode and anode electrodes with a distance of 5 cm between the two electrodes. During the test, the anode was connected to the working electrode and the cathode was connected to the counter and reference electrodes. Current densities were calculated based on the geometric area. All potential values were measured on an Hg/HgO electrode and converted to reversible hydrogen potential (RHE) according to the following equation: E (V vs. RHE) = E (V vs. Hg/HgO) + 0.059pH + 0.098 V.