Soo, Joshua ZheyanRiaz, AsimZhang, DoudouJagadish, ChennupatiTan, Hark HoeKaruturi, Siva2025-05-302025-05-300897-4756ORCID:/0000-0003-2119-0256/work/171154210ORCID:/0000-0002-7816-537X/work/171155282ORCID:/0000-0003-1528-9479/work/171155967ORCID:/0000-0003-4903-2444/work/187269292http://www.scopus.com/inward/record.url?scp=85190737681&partnerID=8YFLogxKhttps://hdl.handle.net/1885/733755259In pursuit of efficient water-splitting technologies, the development of high-performing electrocatalysts is crucial, particularly for the hydrogen evolution reaction (HER). In addition, it is paramount to adopt cost-effective approaches that leverage earth-abundant metals, together with scalable synthesis methods. In this study, we introduce a synthesis approach that combines a facile solution corrosion technique with plasma modification, thereby enhancing the hydrogen evolution activity of NiMo alloys. The inclusion of NH3 plasma modification plays a dual role by concurrently reducing and nitriding as-synthesized NiMo hydroxide. The treatment results in a significant reduction in the HER overpotential to 95 mV at 10 mA/cm2 compared to its initial overpotential. This improvement is attributed to enhanced kinetics due to substantial reductions in charge transfer resistance and an increased double-layer capacitance. Furthermore, the catalyst demonstrates excellent stability of close to 120 h, thereby highlighting the potential of this synthesis method for large-area synthesis of HER electrocatalysts.The authors would like to acknowledge the financial support from the Australian Government through the Australian Renewable Energy Agency (ARENA). The authors would also like to acknowledge the technical support and the fabrication facilities provided by the Australian National Fabrication Facility (ANFF), ACT Node. This work is also made possible with the technical support from Dr. Bin Gong from the Mark Wainright Analytical Centre, UNSW, and Dr. Lachlan Smillie from the University of Wollongong.10enPublisher Copyright: © 2024 American Chemical Society.2024-05-1410.1021/acs.chemmater.3c0297885190737681