Photosensitive ZrO2/BzAc gel films on silicon and quartz substrates with chelate complexes as precursors are fabricated using the sol-gel method. The characteristics of UV and IR spectra of the photosensitive gel films, and their variations in the process of laser irradiation and heat treatment, are investigated. Given different incident angles, the gratings with different pitches are fabricated by interference of two coherent beams of a 325-nm He-Cd laser in ZrO2/BzAc photosensitive gel films, which are exposed to the interference fringe after laser irradiation and leached in ethanol. Subsequently, the optical resolution is also investigated. The minimum pitch of the grating obtained from the experiment is 300 nm. After being heat treated at 600°C, the organism is volatilized and the gel film grating turns into an inorganic film grating, which can combine with the substrates firmly. The x-ray diffraction (XRD) result shows that inorganic films mainly consist of polycrystalline tetragonal ZrO2.