▎ 摘　　要

Nowadays, given the booming demand of blood sugar control from the soaring number of diabetes patients and the insufficient stability of costly enzyme-based glucose sensors in clinic, the development of enzyme-free sensors has been drawing tremendous attraction. Herein, we fabricated a unique structure of Ni/NiO hybrid nanoparticles with mixed-valence states encapsulated in and cross-linked by nitrogen-doped graphene via a facile NiMOF-annealing approach and developed its notable feature in efficiently non-enzymatic glucose sensing. The microstructure and valence states, proved vital to the electrochemical activity and sensing performance, were simultaneously regulated by the annealing temperature. The optimized sample obtained at 400 degrees C displays the superior activation behavior and best glucose sensing performance, offering a high sensitivity of 3.2518 mA mM(-1) cm(-2), a wide linear range (0.001-3.568 mM), a low detection limit (0.032 mu M, S/N = 3) as well as excellent selectivity, good reproducibility, long-term stability, and satisfactory applicability in real sample. By further investigation of the electrochemical kinetics mechanism, the synergistic effect of multivalent system and well-organized microstructure was proved beneficial for charge transfer, activation of reaction sites, and elimination of electrode polarization as well, thus providing a promising strategy in designing non-enzymatic biosensor platform for glucose detection in actual diagnosis.