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ZnO and Aluminum doped ZnO nanoparticles (Al/ZnO NPs) were successfully synthesized by the sol-gel method. Together with the effect of calcination temperatures (200, 300 and 400 °C) and Al dosage (1%, 3%, 5% and 10%) on structural, morphological and optical properties of Al/ZnO NPs, their photocatalytic degradation of methyl orange (MO) dye was investigated. The calcination temperatures at 200, 300 and 400 °C in forming structure of ZnO NPs led to spherical nanoparticle, nanorod and nanoflake structures with a well-crystalline hexagona