Palladium and palladium-alloy are investigated by great quantities of researchers [1-5],but there is no report about palladium-doping in hydrophobic silica material and its thermal analysis kinetics nowadays.Pd/SiO2 hybrid material was prepared using sol-gel method,by introducing metallic palladium into hydrophobic silica material.The decomposition process and thermal analysis kinetics of Pd/SiO2 hybrid material were investigated,and the activation energies and frequency factors were figured out by Doyle equation combined with the common 41 kinds of solid decomposition mechanism functions [6].