Au particles dispersed thin metal oxide films were prepared from precursor films containing HAuCl4 with H2S gas diffusion method. HAuCl4 was uniformly dissolved in the films as promoted by hydroxypropyl cellulose (HPC). The mechanism of the Au particle formation was studied. It was found that HAuCl4 was converted directly to Au metal particles upon contacting with H2S gas. Au particles generated by this method were characterized with small particle size, sharp size distribution and high volume fraction in the films. The surface plasma resonance absorption of Au particles shifted to longer wavelength when TiO2 component was introduced in the matrix.