We simply synthesized the triethoxysilane bearing the second-order nonlinear optical(NLO) active chromophore or chalcone derivatives. In order to improve the poor temporal stability of second-order NLO effect in sol-gel matrix, we introduced the photo-crosslink between the side chain. themselves. Photo-crosslink formation was confirmed with UV-VIS absorption and infrared vibrational spectroscopy. Under a polarized light, we investigated the decaying behavior of molecular order parameter after corona poling.