TiO(2)/ZrO(2) binary oxide film was self-assembled using anionic surfactant (sodium dodecyl sulfonate (SDS)) as template and obtained at the air-water interface. X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) were used to characterize the obtained film. The film was composed of many lamellar nanorods with a d spacing of 3.2 nm, and the lamellas were perpendicular to the lengthwise position of the rods. The energy-dispersive spectrum (EDS) was used for determining the titanium/zirconium atomic ratio. After being calcined, the sample decomposed to a mixture of anatase titania and tetragonal zirconia, and all the lamellar structure was broken.