In this work, we prepared two-dimensional hexagonal NiCo2O4 nanoplates@poly (3,4-ethylenedioxythiophene)/reduced graphene oxide (NiCo2O4@PEDOT/RGO) nanocomposite via hydrothermal method, in situ polymerization, and ultrasonic mixing, successively. The structures and properties of the composite were studied by Transmission electron microscope, Scanning electron microscopy, X-ray diffraction, Cyclic voltammograms, and Amperometric current-time method. Electrochemical studies show that the NiCo2O4@PEDOT/RGO nanocomposite has excellent H2O2 sensing performance. The sensor exhibits a wide linear detection range (0.388–44.156 mM), a low detection limit (0.031 μM, S/N = 3), and a high sensitivity (399.9434 mA mM−1 cm−2), and the response time is less than 3 s. The experimental result demonstrate that these excellent sensing properties are attributed to the NiCo2O4 simultaneous compositing with RGO and PEDOT, which enlarges the specific surface area, increases the active sites, and improves electroconductivity of the NiCo2O4. Especially, the electron transport and stability of the interface of NiCo2O4/RGO were improved via adding PEDOT. It also reveals that this sensor has high stability, outstanding reproducibility and good anti-interference. The results demonstrate that the nanocomposite is a potential electrode material for electrochemical biosensor.