In this research work, pure tetragonal zirconia (t-ZrO 2 ) nanosheets and semi-spherical nanoparticles were successfully prepared by modified Pechini method. In this approach, ZrOCl 2 ·8H 2 O, triethanolamine (TEA) and citric acid (CA) were used as the source of Zr 4+ , the chelating and polymerization agent, respectively. The effects of heat treatment and TEA:CA:Zr 4+ mole ratios on the structure, morphology and zirconia particle size were investigated. The microstructure of the products was characterized by X-ray diffractometry (XRD), thermogravimetric analysis (TGA), field emission scanning electron microscopy (FE-SEM) and Fourier transform infrared (FT-IR) analysis. The zirconia nanosheets exhibit photoluminescence at room temperature with a broad emission in the blue region of the visible spectrum. Finally, the effect of calcination temperature on the photocatalyst properties of nanosheets was investigated. The photocatalytic activity of as-prepared samples was tested for degradation of methyl orange, methyl red, Reactive Blue 21, Reactive Red 120 and Reactive Orange 5 solutions. It is found that t-ZrO 2 nanoparticles have higher photocatalytic activity than the other samples under UV light. Moreover the effect of pH was studied on the photocatalytic degradation of the methyl orange.