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ZnO nanosheets with nanograin distributions, high mesoporosity, and ultrathin thickness have garnered considerable attention owing to their intriguing properties, such as high surface-to-volume ratio and chemical reactivity. Although various methods for fabricating two-dimensional structures have been reported, the surfactant-assisted method is advantageous as it produces nanosheet structures at the water–air interface without affecting the crystal structure of the material. This study developed an innovative surfactant-assisted synthesis method to fabricate flower-like Zinc Oxide (f-ZnO) nanostructures. The synthesis, performed at a mild temperature of 70 °C, yields f-ZnO with high surface area-to-volume ratios and porous morphology. The f-ZnO demonstrates photoelectrochemical (PEC) performance due to increased interfacial contact with electrolytes and the formation of a wurtzite ZnO crystal structure. Additionally, f-ZnO exhibits sensitivity and selectivity as a hydrogen sulfide (H2S) gas sensor. This facile synthesis method opens new avenues for developing functional oxide nanostructures for sensors, catalysts, and energy storage systems.