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As glucose (Glu) is an essential substance for metabolism as well as a symbol to diagnose diabetes, the demand of Glu sensors has increased significantly in recent decades. In this work, a hierarchical Ni-based electrochemical enzyme-free Glu sensor, namely, NiSe2/CNR (carbon nanorod), was engineered through a facile thermal treatment using dimethylglyoxime dinickel salt with selenium (Se) powder. The prepared NiSe2/CNR not only subtly introduces a hierarchical structure with rod-like carbon nanorods and rock-like NiSe2 nanoparticles, which are extremely helpful in offering a greater catalytic activity area and more catalytic active sites, but also incorporates the Se element to increase the inherent activity. The fabricated NiSe2/CNR exhibits distinguished performance for Glu detection in alkaline electrolytes with linear ranges of 0.5–411 μM and 411 μM to 6.311 mM, high sensitivities of 3636 μA mM–1 cm–2 at low concentrations, and 2121 μA mM–1 cm–2 at high concentrations, as well as a low detection limit of 380 nM (S/N = 3). It also possesses favorable reproducibility, stability, and long-term storage capacity. The practical feasibility of NiSe2/CNR was also validated by detecting Glu in human serum. Moreover, the prepared hierarchical NiSe2/CNR is of general interest for the construction of hierarchical Ni-based sensors.

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