| Summary: | This paper reports the first effective fabrication of a high-performance non-enzymatic glucose sensor based on activated carbon cloth (ACC) coated with reduced graphene oxide (RGO) decorated N-doped urchin-like nickel cobaltite (NiCo2O4) hollow microspheres. Hierarchically mesoporous N-doped NiCo2O4 hollow microspheres were synthesized using a facile solvothermal method, followed by thermal treatment in a nitrogen (N2) atmosphere. Subsequently, they were hydrothermally decorated with RGO nanoflakes. The resulting composite was dip-coated onto ACC, and its electrochemical and glucose sensing performances were investigated using electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and chronoamperometric measurements in a three-electrode system. The composite electrode sensor demonstrates admirable sensitivity (6122 μM mM−1 cm−2) with an ultralow detection limit (5 nM, S/N = 3), and it performs well within a substantial linear range (0.5–1.450 mM). Additionally, it exhibits good long-term response stability and outstanding anti-interference performance. These outstanding results can be attributed to the synergistic effects of the highly electrically conductive ACC with multiple channels, the enhanced catalytic activity of highly porous N-doped NiCo2O4 hollow microspheres, and the large electroactive sites provided by its well-developed hierarchical nanostructure and RGO nanoflakes. The findings highlight the enormous potential of the ACC/N-doped NiCo2O4@RGO electrode for non-enzymatic glucose sensing.
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