The 3D graphene possesses fast electron transport mobility and high mechanical strengths owing to the combination of both intrinsic properties of 2D graphene and 3D microstructure. The microporous structure of 3D graphene provides excellent platform for combination with other nanostructures to form hybrid nanomaterials. These hybrid nanostructures have attracted a tremendous amount of interest in recent years due to their excellent surface-area-to-volume ratio, improved catalytic activity, high electron mobility and several functionalities that are superior to those of pure nanomaterials. In this study, hybrid zinc oxide (ZnO) nanorods with nickel oxide (NiO) nanosheets were grown on 3D graphene substrate via two step hydrothermal method and their structural characteristics analysed for application as biological sensing material. ZnO and NiO exhibited crystal lattice in preferred c-axis orientation with higher purities. Observations under field emission scanning electron microscopy revealed the growth of ZnO nanorods followed by the NiO nanosheets formation upon the second hydrothermal process. The obtained results showed significant growth of ZnO nanowire and NiO nanosheets via two step hydrothermal route. The created hybrid nanostructures of ZnO/NiO on 3D graphene demonstrate the optimized processing technique needed to generate novel advanced materials, which opens a new avenue for medical diagnostics. © 2019 Elsevier Ltd. All rights reserved.