In this work, molybdenum disulfide/reduced graphene oxide (MoS2/rGO) nanosheets are prepared by the hydrothermal process, and then iron-nickel (FeNi) transition bimetallic hybrids are monotonously distributed on the ultrathin MoS2/rGO substrate using a simple ethylene – glycol reduction process. Transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) analysis displays the uniformity and distribution of FeNi nanoparticles onto the surface of catalyst's support, respectively. X-ray photoelectron spectroscopy (XPS) analysis demonstrates the presence of all the constituent elements of the nanocomposite. The excellent catalytic performance of the nanocomposite for oxygen reduction reaction (ORR) in alkaline conditions, which is due to the cooperative effect between FeNi transition bimetallic alloys and the MoS2/rGO substrate, is recognized by its high current density (6.10 mA cm−2), half-wave potential (0.895 V vs. RHE), and onset potential (0.988 V vs. RHE). Meanwhile, the electrode made by the nanocomposite also exhibits superior durability (94.6%) and methanol endurance (100%) with respect to Pt/C (53.8% and 87.91%). Finally, the results obtained from the Koutechy-Levich (K-L) plots of the nanocomposite are related to the 4-electron conveyance procedure. The synergetic effects of the excellent conductivity and high aspect ratio of rGO, as well as high catalytic activity and role of susbtrate-like such as MoS2, along with the use of the FeNi transition bimetallic hybrid, can make FeNi–MoS2/rGO as a suitable candidate for high performance electrocatalytic applications.
