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Recently, molybdenum (Mo)-based catalysts have been proved to be effective NRR catalysts due to the high affinity of nitrogen to Mo. The design of a heterostructure and the introduction of defects, such as vacancies and heteroatom doping, are effective means to regulate the microstructure of catalysts and further improve their electrocatalytic N2 into NH3 performance. In this paper, VS-Fe-doped 1T/2H mixed-phase MoS2/C (VS means sulfur vacancies) heterostructure sphere-like nanoflowers with rich sulfur vacancies are prepared through a pectin-assisted hydrothermal reaction, followed by calcination and treatment with NaBH4 solution. VS-Fe-MoS2/C exhibits good electrocatalytic NRR performance with a high ammonia yield rate of 17.8 ± 0.7 μg h–1 mg–1 at −0.5 V versus reversible hydrogen electrode (vs RHE) and a Faraday efficiency (FE) of 9.2% at −0.3 V (vs RHE) under ambient conditions. Introducing sulfur vacancies, iron doping, and preparing 2H-phase MoS2 have greatly improved the performance of electrocatalytic nitrogen reduction to ammonia.

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