Rational Synthesis of MOF‐Derived Selenium Vacancy‐Rich Hollow CoNiSe 2‐x Triangular Nanosheet Arrays on Carbon Cloth for Non‐Enzymatic Glucose Sensing

Rational structural and defect engineering of self‐supporting electrodes is highly desirable for developing high‐performance non‐enzymatic glucose sensors. Herein, selenium vacancy‐rich hollow CoNiSe 2‐ x triangular nanosheet arrays were directly constructed on carbon cloth through a MOF‐derived ion‐exchange strategy followed by solvothermal selenization and controlled NaBH 4 reduction. Compared with previously reported Co/Ni‐based selenide glucose sensors, CoNiSe 2‐x /CC combines hollow triangular nanosheets and selenium‐vacancy engineering in a binder‐free carbon‐cloth electrode. The hollow structure improves electrolyte access and exposes more electroactive surface, while selenium vacancies provide additional active sites for glucose oxidation. Benefiting from these synergistic advantages, the CoNiSe 2‐ x /CC electrode exhibits excellent electrocatalytic activity toward glucose, delivering an ultrawide linear range of 0.5–10,000 µM, a high sensitivity of 4919 µA mM –1 cm –2 , and a low detection limit of 0.34 µM. Moreover, the sensor demonstrates good selectivity, long‐term stability, repeatability, and reproducibility. Practical analysis in human serum further confirms its reliable applicability for real‐sample glucose detection. This work provides a facile strategy for designing vacancy‐rich hollow bimetallic selenide electrodes and highlights the potential of CoNiSe 2‐ x /CC for flexible non‐enzymatic glucose sensing.