The ordered oxynitrides mesoporous materials were successfully prepared by the nitridation of Al-MCM-41 and SBA-15 mesoporous materials (containing template) in flowing NH3 environment. The composition and structure of the synthesized materials were analyzed by CNH analysis, IR spectrum, Si MAS NMR, N-2 sorption, low-angle XRD, and HRTEM. The results of analysis show that the obtained oxnitrides mesoporous materials by nitriding at higher temperature (1273similar to1323K) and long soaking time (8similar to24h) still possess good order, high nitrogen content (10similar to21wt%), high surface area (700similar to900m(2) g(-1)), and narrow pore distribution.