This work demonstrates a sustainable green synthesis of nickel oxide (NiO) nanoparticles using plant extracts from neem (Azadirachta indica), guava (Psidium guajava), and onion peel (Allium cepa), yielding NiO-N, NiO-G, and NiO-O respectively. The nanoparticles exhibited strong visible-light absorption, favorable morphology, high crystallinity, and crystallite sizes of 23 nm (NiO-N), 15 nm (NiO-G), and 13 nm (NiO-O) with surface areas of 64.17, 38.44 and 39.85 m²/g. Advanced characterizations (XRD, UV-Vis, PL, Raman, FESEM, FTIR, Zeta potential, XPS, BET) confirmed NiO nanoparticles formation, Ni-rich surface regions, and mixed-valence Ni²⁺/Ni³ ⁺ states enriched with oxygen vacancies. Photocatalytic studies under visible and natural sunlight revealed efficient degradation of Methyl Orange (89–96 %), Brilliant Green (87–90 %), and Ciprofloxacin (65–78.2 %), with enhanced performance in sunlight (up to 98 % for MO, 94 % for BG, and 85 % for CIF) within 160 mins. Radical scavenging experiments identified •OH as the dominant reactive species, supported by h⁺ and e⁻ contributions. The catalysts exhibited high stability and reusability, with only 7 % efficiency loss after four cycles. These findings highlight the potential of green-synthesized NiO nanoparticles as robust, eco-friendly photocatalysts for sustainable wastewater treatment.
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