This paper presents the synthesis of a novel corn-stalk-like MnO₂/CoNi oxide composite using an in situ epitaxial attachment growth strategy, in which CoNi oxide nanosheets are anchored onto MnO₂ nanowires. The one-dimensional MnO₂ nanowires, with their large specific surface area, serve as a support to enhance the electronic conductivity of the CoNi oxides. Hexamethylenetetramine (HMTA) is employed as an alkaline linking agent, playing a key role in shaping the CoNi oxide nanosheets and ensuring their successful growth on the MnO₂ nanowires. The MnO₂/CoNi oxide composite-based electrochemical sensor exhibits excellent synergistic and interfacial effects, promoting electron transfer and charge migration. This composite material shows outstanding electrocatalytic performance for hydrazine detection, with a broad linear range (0.48−6106.58 μM), low detection limit (0.286 μM, S/N = 3), and high sensitivity (0.037 μA μM⁻1). Moreover, when tested for hydrazine detection in water samples, the sensor achieved a recovery rate of 95.7–105 %, highlighting its high sensitivity and rapid response in practical applications.
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