▎ 摘　　要

The 3D NiO hollow sphere/reduced graphene oxide (rGO) composite was synthesized according to the coordinating etching and precipitating process by using Cu2O nanosphere/graphene oxide (GO) composite as template. The morphology, structure, and composition of the materials were characterized by SEM, TEM, HRTEM, XPS, and Raman spectra, and the electrochemical properties were studied by cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and amperometry. Moreover, the electrochemical activity of the composite materials with different morphologies were also investigated, which indicating a better combination of the NiO hollow sphere and the rGO. Used as glucose sensing material, the 3D NiO hollow sphere/rGO composite modified electrode exhibits high sensitivity of similar to 2.04 mA mM(-1) cm(-2), quick response time of less than 5 s, good stability, selectivity, and reproducibility. Its application for the detection of glucose in human blood serum sample shows acceptable recovery and R. S. D. values. The outstanding glucose sensing performance should be attributed to the unique 3D hierarchical porous superstructure of the composite, especially for its enhanced electron-transfer kinetic properties.