Hydrogen energy, as the most promising new energy for sustainable development, has aroused wide concern of researcher in the field of energy chemical industry. Among the many hydrogen generation approaches, electric water splitting for producing H2 is considered to be a simple and environmentally friendly method. Transition metal-based catalysts have become an important field in alkaline seawater electrolysis due to their high abundance and superior catalytic performance. Therefore, NiFeS (Ni3S2@FeS) was in-situ generated on nickel foam through a simple two-step hydrothermal approach in this paper. NiFeS/NF catalysts synthesized by three vulcanization reagents (Na2S·9H2O, CH3CSNH2, CH4N2S) were characterized and compared by a series of electrochemical tests. It is worth noting that for the first time, different vulcanization reagents were used to explore the activity of the same catalyst in seawater splitting and urea splitting. It was found that the NiFeS catalyst synthesized by Na2S·9H2O (Ni3S2@FeS-1/NF) had better oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) performance and good stability in alkaline seawater. The overpotential required for the OER with Ni3S2@FeS-1/NF electrode in alkaline seawater (1 M KOH + seawater electrolyte) is 290 mV at the 10 mA cm-2, and 92 mV for the hydrogen evolution reaction at the 10 mA cm-2. It is found that the NiFeS catalyst obtained by vulcanization of NiFe-LDH not only has high activity and conductivity, but also can effectively inhibit Cl- corrosion. Ni3S2@FeS-1/NF catalyst has a unique cluster rosette nanosheet array structure, which can present more catalytic reaction centres, accelerate the electron transfer rate and promote electrochemistry performance. The work proposes a novel way to explore the effect of different synthesis methods of the same composition on the performance of electrolytic seawater.