Mesoporous Iron-doped MoS₂/CoMo₂S₄ Heterostructures through Organic–Metal Cooperative Interactions on Spherical Micelles for Electrochemical Water Splitting

Mesoporous metal sulfide hybrid (meso-MoS₂/CoMo₂S₄) materials via a soft-templating approach using diblock copolymer polystyrene-block-poly­(acrylic acid) micelles are reported. The formation of the meso-MoS₂/CoMo₂S₄ heterostructures is based on the sophisticated coassembly of dithiooxamide and metal precursors (i.e., Co²⁺, PMo₁₂), which are subsequently annealed in nitrogen atmosphere to generate the mesoporous material. Decomposing the polymer leaves behind mesopores throughout the spherical MoS₂/CoMo₂S₄ hybrid particles, generating numerous electrochemical active sites in a network of pores that enable faster charge transfer and mass/gas diffusion that enhance the electrocatalytic performance of MoS₂/CoMo₂S₄. Doping the spherical meso-MoS₂/CoMo₂S₄ heterostructures with iron improves the electronic properties of the hybrid meso-Fe-MoS₂/CoMo₂S₄ material and consequently results in its superior electrochemical activities for both hydrogen evolution reaction and oxygen evolution reaction.