Metilen biru merupakan pewarna organik berbahaya dari limbah industri tekstil yang menyebabkan permasalahan lingkungan yang serius. Degradasi metilen biru dapat dilakukan melalui proses fotokatalisis dengan semikonduktor berbasis oksida logam seperti NiO dan CuBi2O4. Pada penelitian ini, NiO disintesis melalui metode sol-gel, sedangkan CuBi2O4 disintesis melalui metode solvotermal. Nanokomposit NiO/CuBi2O4 telah berhasil dikembangkan dengan memodifikasi NiO dan CuBi2O4 melalui metode grinding-annealing, yang dikonfirmasi oleh hasil karakterisasi XRD, FTIR, TEM, dan UV-Vis DRS. Penurunan nilai energi celah pita NiO dari 3,39 eV akibat keberadaan CuBi2O4 dapat diamati. Energi celah pita NiO pada NiO/CuBi2O4 1:1, 1:2, dan 2:1 yang diperoleh dari hasil karakterisasi UV-Vis DRS adalah 2,95 eV, 2,89 eV, dan 3,15 eV. Selain itu, aktivitas fotokatalitik NiO, CuBi2O4, dan NiO/CuBi2O4 sebagai katalis juga dievaluasi melalui degradasi metilen biru di bawah radiasi sinar tampak selama 3 jam. Hasil menunjukkan bahwa modifikasi NiO dengan CuBi2O4 dapat meningkatkan aktivitas fotokatalitik. Persentase fotodegradasi metilen biru dengan 10 mg katalis NiO/CuBi2O4 2:1 adalah 74,12% dengan konstanta laju sebesar 6,07×10–3 menit–1, yang lebih tinggi dibandingkan NiO dan CuBi2O4 tanpa modifikasi

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Methylene blue is a hazardous organic dye from textile industrial effluents which causes serious environmental problems. Degradation of methylene blue could be carried out through photocatalysis process using metal oxide-based semiconductors such as NiO and CuBi2O4. In this study, NiO was synthesized by sol-gel method, while CuBi2O4 was synthesized by solvothermal method. NiO/CuBi2O4 nanocomposite was successfully developed by modifying NiO and CuBi2O4 through grinding-annealing method, which was confirmed by the results of XRD, FTIR, TEM, and UV-Vis DRS characterization. The decrease in bandgap energy value of NiO from 3.39 eV due to the presence of CuBi2O4 could be observed. The bandgap energies of NiO in NiO/CuBi2O4 1:1, 1:2, and 2:1 obtained from the results of UV-Vis DRS characterization were 2.95 eV, 2.89 eV, and 3.15 eV. Furthermore, the photocatalytic activity of NiO, CuBi2O4, and NiO/CuBi2O4 as catalysts were also evaluated by methylene blue degradation under visible light irradiation for 3 hours. The results showed that modification NiO with CuBi2O4 could enhance the photocatalytic activity. The percentage of methylene blue photodegradation using 10 mg NiO/CuBi2O4 2:1 catalyst was 74.12% with a rate constant of 6.07×10–3 min–1, which was higher than NiO and CuBi2O4 without modification.