The novel HfO2/SiO2 gel films with property of radiation polymerization were prepared by means of sol-gel technique. The film was exposed to X-ray irradiation and the structural change in the hybrid glass thin film was
monitored by Fourier transform infrared(FTIR) sectroscopy, polymerization was clearly evidenced in the mid-IR spectra by the loss of intensity of the vinyl group ν(C=C) mode at 1638 cm-1. The Hafnium element in the film was detected by X-ray photoelectron spectroscopy(XPS). The atomic percentages obtained by XPS were 1.96%(Hf), 10.49%(Si), 27.63%(O), 59.91%(C), respectively. XPS result shows that the atomic ratio of Si to Hf is about 5∶1. The refractive indexes of the film at different wavelengths were also measured by the ellipsometer, which showed that they were raised. Because of the solubility difference between the exposed part and unexposed part, after the film was exposed through the mask by X-ray irradiation, a grating, with a highness of 0.8 μm and a period of 1 μm, was fabricated in the HfO2/SiO2 sol-gel glass, which showed that the film has a good property of radiation polymerization.