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Three-dimensional NiCo2O4 is a kind of superior sensing material owing to its high electron transfer capability, large available surface area and numbers of active sites. In this work, NiCo2O4 of the three-dimensional chestnut-like structure were easily achieved through a one step hydrothermal process. Afterwards, the morphology and structure were characterized by scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS). Based on the three-dimensional porous chestnut-like NiCo2O4, an electrochemical sensor for hydrazine (N2H4) detection is fabricated. This electrochemical platform can realize good selectivity, excellent stability, high sensitivity (∼2154.4 μA mM-1 cm-2), and low detection limit (0.3 μM), as well as a wide linear range from 1 μM to 1096 μM. The synergistic effect of nickel-cobalt in such mixed transition metal oxides which Co in Co3O4 is partially replaced by Ni are beneficial for enhancing sensing properties. This study proves that three-dimensional porous chestnut-like NiCo2O4 is electrochemically active for catalytic performance which is particular and promising material for good application in the practical detection of N2H4.