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Four phenoxysilicon networks for nonlinear optical (NLO) applications were designed and prepared by an extended sol-gel process without additional H20 and catalyst. All poled polymer network films possess high second-order nonlinear optical coefficients (d33) of 10-?～10-8 esu. The investigation of NLO temporal stability at room temperature and elevated temperature (120°C) indicated that these films exhibit high d33 stability because the orientation of the chromophores are locked in the phenoxysilicon organic/inorganic networks.