Novel organic/inorganic hybrid material was synthesized from poly(acrylazapropyl-trimethoxysilane)-b-poly(N(epsilon)-trifluoroacetyl-L-lysine) (P(AAPTMS)-b-P(TLL)) block copolymer using the sol-gel process. The treatment with ammonia solution permitted the hydrolysis of both trifluoro acetyl and trimethoxysilyl groups of the hydride copolymer followed by the condensation of the silanol groups, leading to crosslinked copolymers. The resulting cross-linked hybrid material was characterized using FT-IR, (29)Si NMR, DSC, TGA, and environmental scanning electron microscopy. These techniques evidenced that a siloxane network was obtained. Amphiphilic poly peptide/inorganic hybrid copolymers were achieved and self-organized as particles in water. (C) 2009 Elsevier Ltd. All rights reserved.