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 voltammet...