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.

Pd-doped SiO2 organic-inorganic hybrid material (Pd/M-SiO2) was prepared by sol-gel method and characterized by XRD, FTIR spectra and TG/DTG analysis. The most probable kinetic mechanism function, apparent activation energy and pre-exponential factor of the thermal decomposition for Pd/M-SiO2 material were calculated using the combined Coast-Redfern intergral and Αchar differential methods. Pd element in noncalcined Pd/M-SiO2 materials exists in PdCl2 form. FTIR spectroscopy confirmed the existence of hydrophobic Si−CH3 groups. The thermal decomposition process of Pd/M-SiO2 materials can be divided into four stages, with different mechanism functions. The activation energies are 76.37, 146.85, 208.90 and 413.89 kJ·mol−1 for the four stages, respectively, and the pre-exponential factors are 5.04×1012, 7.14×1013, 2.93×1012 and 6.56×1019 s−1, respectively. There is no obvious influence of the existence of metallic Pd0 on the thermal decomposition of methyl.