Zinc molybdate rod-like nanostructures have been successfully synthesized by precipitation method process in the presence of different surfactants. This study aimed to investigate the effects of different surfactant such as sodium dodecyl sulfate, polyethylene glycol, and cetyltrimethylammonium bromide and solvent on the morphology and particle size of final products. It was found that the size and morphology of the products could be greatly influenced by the aforementioned parameters. To the best of authors’ knowledge, this is the first report on the synthesis of ZnMoO₄ nanostructure with different morphologies in the presence of ethanol as a solvent. The as-synthesized products were characterized by XRD, SEM, UV–Vis, and EDS techniques. To evaluate the photocatalyst properties of nanocrystalline zinc molybdate, the photocatalytic degradation of methyl orange under visible light irradiation was carried out.