The purpose of this study is to synthesize transition metal doped mesoporous silica catalyst and to characterize its surface in an attempt to decomposition of N2O. Transition metal used to surface modification were Ru, Pd, Cu and Fe concentration was adjusted to 0.05 M. The prepared mesoporous silica catalysts were characterized by X-ray diffraction, BET surface area, BJH pore size, Scanning Electron Microscopy and X-ray fluorescence. The results of XRD for mesoporous silica catalysts showed typical the hexagonal pore system. BET results showed the mesoporous silica catalysts to have a surface area of 537 ∼973 m2/g and pore size of 2∼4 nm. The well-dispersed particle of mesoporous silica catalysts were observed by SEM, the presence and quantity of transition metal loading to mesoporous surface were detected by XRF. The N2O decomposition efficiency on mesoporous silica catalysts were as follow: Ru>Pd>Cu>Fe. The results suggest that transition metal doped mesoporous silica is effective catalyst for decomposition of N2O.