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The design and development of efficient and electrocatalytic sensitive nickel oxide nanomaterials have attracted attention as they are considered cost-effective, stable, and abundant electrocatalytic sensors. However, although innumerable electrocatalysts have been reported, their large-scale production with the same activity and sensitivity remains challenging. In this study, we report a simple protocol for the gram-scale synthesis of uniform NiO nanoflowers (approximately 1.75 g) via a hydrothermal method for highly selective and sensitive electrocatalytic detection of hydrazine. The resultant material was characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, and X-ray diffraction. For the production of the modified electrode, NiO nanoflowers were dispersed in Nafion and drop-cast onto the surface of a glassy carbon electrode (NiO NF/GCE). By cyclic voltammetry, it was possible to observe the excellent performance of the modified electrode toward hydrazine oxidation in alkaline media, providing an oxidation overpotential of only +0.08 V vs Ag/AgCl. In these conditions, the peak current response increased linearly with hydrazine concentration ranging from 0.99 to 98.13 μmol L -1 . The electrocatalytic sensor showed a high sensitivity value of 0.10866 μA L μmol -1 . The limits of detection and quantification were 0.026 and 0.0898 μmol L -1 , respectively. Considering these results, NiO nanoflowers can be regarded as promising surfaces for the electrochemical determination of hydrazine, providing interesting features to explore in the electrocatalytic sensor field., Competing Interests: The authors declare no competing financial interest., (© 2023 The Authors. Published by American Chemical Society.)