The ordered lamellar nanostructured zirconias were prepared via atmospheric reflux and hydrothermal hybrid method in ethanol-water system by using zirconium oxychloride as zirconium source and sodium dodecyl sulfonate (SDS) as template agent, which were characterized by X-ray diffraction (XRD). The results showed that the ordered lamellar nanostructured zirconias were composed of tetragonal phase for 110 and 125°C and tetragonal/monoclinic phase for 140 and 155°C. As the hydrothermal temperature raised, the monoclinic phase began to appear, and the crystallization is promoted, but the ordered lamellar nanostructure was shrinking prior to expanding in size, ranged from 1.33 to 1.55 nm, and tended to decrease in amount gradually. For the sample prepared at 110°C, the Fourier-transform infrared spectroscopy (FT-IR) pattern demonstrated that the inorganic phase is tetragonal zirconia and there remain small amount of template SDS. And the calcined lamellar nanostructure with a 1.2 nm periodicity was observed by transmission electron microscopy (TEM). This indicates the lamellar structure shrunk from 1.51 to 1.2 nm and was preserved after calcination at 500°C, showing good thermal stability.