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Well-organized substrate materials have got a considerable significance in the progress of energy-efficient pseudocapacitor electrodes. Herein, functionalized three-dimensional (3D) carbon nanocoils on nickel foam (CNCs/NF), have been used as a...

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High fabrication cost, chemical instability, and complex immobilization of enzyme molecules are critical issues of enzyme‐based glucose sensors. Designing state‐of‐the‐art, binder‐free, and non‐enzymatic glucose sensing probes plays an imperative role to cope with the aforementioned issues. 3D carbonaceous nanomaterials coated with transition metal vanadates (TMVs) are a favorable biomimetic platform for glucose quantification. Peculiar hierarchical structure, enhanced conductivity, synergistic interaction, multiple oxidation states, and high catalytic activity would make such composite a potential contender for non‐enzymatic glucose sensing. Herein, 3D helical‐shaped carbon nanocoils (CNCs) are grown on nickel foam (NF) via chemical vapor deposition method to prepare a robust CNCs/NF scaffold. Then, a hydrothermal route is followed to grow interconnected free‐standing Ni3V2O8 nanosheets (NSs) on CNCs/NF scaffold. This novel and binder‐free Ni3V2O8 NSs/CNCs/NF hierarchical composite possesses superior electrochemical active area (ECSA) and exceptional electrochemical efficacy. Amperometric analysis exhibits extremely prompt detection time (0.1 s), elevated sensitivity (5214 µA mM−1 cm−2), and low detection limit (0.04 µM). Developed sensor demonstrates appreciable recoveries (93.3 to 103.3%) regarding glucose concentration in human serum. The appealing analytical results show that deployment of a 3D helical‐shaped hierarchical smart scaffold can be an effective strategy for developing efficient and advanced non‐enzymatic glucose sensors.