ZnO nanostructures were synthesised in a hydrothermal reaction of zinc acetate in the presence of molybdophosphoric acid (H3[PMo12O40]) as well as its vanadium-substituted acid (H4[PMo11VO40]) at various times, temperatures, and concentrations. The ZnO nanostructures were characterised by X-ray diffraction, transmission electron microscopy, and Fourier transform infrared spectroscopy. The results demonstrated that the synthesised products are crystalline with a zincite hexagonal phase. Various ZnO nanostructures, such as nanoparticles, microrods, and nanosheets, were produced by changing the experimental conditions. The photocatalytic degradation of methyl orange was also investigated using the ZnO nanoparticles thus prepared. These particles exhibited high performance in the photocatalytic degradation of MO and almost 100 % decolourisation occurred within only 20 min.

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