SiO 2 /ZrO 2 gel films were derived from Zr-butoxide modified chemically with β-diketones and then mixed with Tetraethyl orthosilicate via Sol-Gel process. The obtained gel films showed an absorption band, in characteristic of the π-π* transition of chelate ring at around 334 nm, and its refractive index was changed from 1.463~1.647. The Si-O-Zr, Zr-O bands were detected by FTIR. The result indicated that SiO 2 and ZrO 2 integrated uniformly in the films on micro molecule magnitude. The negative tone gel films were irradiated with high pressure mercury lamp through mask and then leached in ethyl alcohol. The above process gave uniform surface-relief gratings of periods at 2.0µm. The present study had proved that the photosensitive gel films were versatile for the fabrication of micro optical devices.