Phase Engineering of MoS 2 for High‐Performance Anion Exchange Membrane Water and Glucose Electrolyzer

ABSTRACT Water electrolysis for green hydrogen production is hindered by the high energy consumption of the oxygen evolution reaction (OER). Replacing OER with the glucose oxidation reaction (GOR) using a phase‐engineered MoS 2 ‐based electrocatalyst offers a promising route to lower the overall cell voltage while simultaneously valorizing biomass. Herein, Fe and P co‐doping induces a 2H‐to‐1T phase transition in MoS 2 , generating abundant sulfur vacancies and metallic conductivity. At high glucose coverage, electron transfer shifts from Fe to Mo sites, enabling selective GOR over OER. The Fe, P‐MoS 2 catalyst delivers ultralow overpotentials of 98 mV for HER and 260 mV for OER, along with a low operating voltage of 1.30 V (vs. RHE) for GOR at 10 mA cm −2 . In a full anion‐exchange membrane glucose electrolyzer (AEMGE), the Fe, P‐MoS 2 ||Fe, P‐MoS 2 configuration achieves cell voltages of 1.74 and 2.00 V at 0.5 and 1.0 A cm −2 , respectively, substantially lower than the corresponding water electrolyzer (2.16 and 2.56 V), with excellent stability over 50 h. DFT calculations reveal that Fe/P co‐doping synergistically enhances charge carrier mobility and optimizes adsorption energies for glucose activation and intermediate conversion. This work highlights efficient hydrogen production alongside biomass upgrading with reduced energy consumption.