Mesostructured zirconia has been synthesized by using zirconium chloride and PEO nonionic ethoxylated sorbitan ester (Tween-20, -40, -60 or -80) as a zirconium source and structure-directing agent in an aqueous medium. To remove the occluded surfactants, UV/ozone treatment has been utilized instead of calcination due to thermal instability. This results from a special molecular structure of Tween surfactant. From XRD, SEM and TEM analyses, the materials treated with UV light and in-situ generated ozone has a wormhole structure and ill-defined or well-defined spherical particles.