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In this book, it has demonstrated that the nanocomposites of ZnO-NiO coated MWNTs acting as photocatalyst have been successfully synthesized by co precipitation method and fully characterized. The photocatalytic activity of the photocatalyst was determined by examining the Photodegradation of methyl orange under UV (280 nm) and visible light (480 nm) irradiation. Moreover ZnO nanoparticles were also prepared by using the same method for a comparative study. The results show that photocatalysts are active both in UV and visible light region but the photocatalytic activity is greater under UV irradiation. The degradation rate was increased after acid oxidized MWNTs were coated by ZnO as compared to that by pristine ZnO nanoparticles. In addition, the degradation rate of photo catalysts was further enhanced when NiO was loaded on the surface of MWNTs being maximum for 3% NiO loading on ZnO coated MWNTs. This method can prove the most advantageous for textile dye removal.