Abstract: Uniform hierarchical nickel hydroxide microspheres were successfully synthesized via a microwave-assisted hydrothermal process. The composition and morphology of the composites were determined with X-ray diffraction(XRD), scanning electron microscopy(SEM), and transmission electron microscopy(TEM). The nickel hydroxide microspheres had an average diameter of 1.6 μm and a flower-like structure, which meant a large specific surface area. Furthermore, the nickel hydroxide modified glassy carbon electrode was built and utilized for the detection of uric acid (UA) in a 0.1 mol/L NaOH, where it indicated excellent electrocatalytic activity. This biosensor exhibited a wide linear range from 0.1 mmol/L to 1.5 mmol/L with a high sensitivity of 475.71 μA ·L/(mmol ·cm²)and a low detection limit of 1.8 μmol/L. It was found in an electrochemical test that the Ni(OH)₂ microspheres-modified electrode had good selectivity. All the results demonstrated that the Ni(OH)₂ microspheres possessed significant potential for application to the development of non-enzymatic sensors for UA detection.