Pd/Ag/SiO2 sols and powder materials were prepared by adding AgNO3 and Pd (NO3)2·2H2O into a methyl-modified silica sol. Tetraethylorthosilicate and methyltriethoxysilane were used as the silica precursor for the sol-gel reaction. The obtained SiO2 sols and powder materials were characterized by sol particle size distribution, zeta potential analysis, UV-Vis spectra, Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) measurement. It was found that most of the particle sizes of the prepared Pd/Ag/SiO2 sols are about 2~10 nm with narrow size distribution. The zeta potential of Pd/Ag/SiO2 sol with Pd/Ag molar ratio of 7.5/2.5 presents the highest value. The FTIR analysis substantiates that the Si-CH3 groups exist in the silica network and the formed Pd/Ag/SiO2 sol particles possess linear structure. XRD characterization indicates that the Pd2+ and Ag+ in the Pd/Ag/SiO2 materials had be reduced to Pd0 and Ag0, respectively, after annealed in a nitrogen atmosphere at 350°C.