Ultrasound‐Assisted Growth and Electrodeposition Syntheses of Trimetallic Phosphides: Engineering Heterogeneous Interfaces for Superior Alkaline Hydrogen Evolution

Transition metal phosphides (TMPs), recognized as economical electrocatalysts with superior performance, demonstrate exceptional electrocatalytic performance in water electrolysis systems. Researchers demonstrate that optimizing their catalytic activity can be achieved through dual approaches: atomic‐level compositional modification via heteroatom incorporation and precision engineering of nanoscale architectures. Herein, we employ an ultrasound method to directly grow 2D metal organic phosphates on nickel foam (NF) and then decompose the phosphate at high temperatures to obtain NiCo‐P/NF. Subsequently, FeP is electrodeposited on the nickel foam substrate through cyclic voltammetry, synthesizing a trimetal phosphide nanosheet catalyst, namely, NiCoP‐FeP/NF. Electrochemical measurements results display that the overpotential for HER is 110 mV at 10 mA cm −2 , and the Tafel slope is 21 mV dec −1 in 1M KOH electrolyte. SEM results demonstrate that the abundant heterogeneous interfaces in NiCoP‐FeP/NF generate and expose highly active catalytic sites, resulting in outstanding hydrogen evolution reaction (HER) performance. Moreover, the incorporation of iron (Fe) markedly enhances charge transport properties within the catalyst, boosting its overall electrochemical activity. This research provides an innovative approach to achieving high‐efficiency and economical catalysts tailored for sustainable hydrogen generation via water electrolysis.