Porous carbon has been extensively employed as a support for phosphide and sulfi de nanoparticles to develop effi cient

and low-cost oxygen evolution reaction (OER) catalysts, owing to its superior electrical conductivity. This paper utilizes

a cation exchange process in which the cations in the cation exchange resin (CER) are readily replaced by transition metal

ions. Moreover, utilizing the inherent carbon-rich and sulfur-rich characteristics of CER, carbonization and phosphidation

treatments were performed. The study successfully synthesizes a novel bimetallic phosphide-sulfi de nanoparticle embedded

in S-doped three-dimensional porous carbon electrocatalyst, NiCoPS@SC. The electrocatalyst exhibits exceptional catalytic

performance in the OER: a low overpotential (329 mV) at 10 mA cm −2 current density, a Tafel slope of 87.0 mV dec −1 , and

a charge transfer resistance (2.47 Ω). The improved activity of NiCoPS@SC is attributed to the distinctive three-dimensional

porous structure of the carbon nanomaterials and excellent electrical conductivity, which signifi cantly increase the specifi c

surface area (228.82 m 2 g −1 ) and the density of active sites. Furthermore, the synergistic interaction between transition

metal phosphide and sulfi de nanoparticles, in conjunction with the strong integration with carbon nanostructures, improves

interfacial interactions. This reduces metal particle agglomeration and erosion, thus enhancing catalytic performance while

ensuring the structural stability and durability of the electrocatalyst. This three-dimensional porous transition bimetallic

phosphide-sulfi de carbon nanostructure off ers a novel approach for developing practical transition metal OER catalysts.