In‐Situ Growth of Cu₂S‐MoS₂ Bimetallic Electrocatalyst on Carbon Cloth for Hydrogen Evolution Reaction

Abstract Hydrogen evolution reaction (HER) is one of prospective methods to produce hydrogen energy, and the key technology of which lies in the preparation of electrocatalysts. Preparations of catalysts with high efficiency, low price and good stability are expected. In this work, a new polyoxometalate‐based copper‐organic framework, [{Cu^II(C₁₀N₆H₇)₄(H₂O)₂}H₆(PMo₁₂O₄₀)₂] ⋅ 12H₂O (1) [C₁₀N₆H₇: 3‐(1H‐pyrazol‐4‐yl)‐5‐(pyridin‐4‐yl)‐1,2,4‐triazole], was synthesized as an electrocatalyst precursor, and confirmed by infrared spectroscopy (IR), single‐crystal X‐ray diffraction (SXRD) and X‐ray powder diffraction (PXRD). A new electrocatalyst (Cu₂S‐MoS₂@CC‐1) was synthesized from 1, thiourea (TU) and carbon cloth (CC) by a one‐pot hydrothermal method. Due to the synergistic effects between Cu₂S and MoS₂, the Cu₂S‐MoS₂@CC‐1 catalyst exhibits high electrocatalytic HER activity and good stability in 0.5 M H₂SO₄. Namely, Cu₂S‐MoS₂@CC‐1 shows low overpotential of 150 mV@10 mA cm⁻² vs reversible hydrogen electrode (RHE) and small Tafel slope of 61 mV dec⁻¹, and remains good stability at least 94 h and over 1000 catalytic cycles. This method provides a promising strategy for development of non‐noble metal catalysts.