Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)In the present investigation the morphological study of self-supported translucent films, constituted of semi-inorganic polymeric materials prepared by sol-gel process from poly(phenylsilsesquioxane) (PPSQ) and poly(dimethylsiloxane) (PDMS), modified by diphenylsilanediol (DPS), phenyltriethoxysilane (PTES) and/or tetraethoxysilane (TEOS), is reported. Small-angle X-ray scattering evidenced phase segregation between PPSQ and PDMS in the PPSQ/PDMS film (M1). The addition of TEOS to the sol, constituted by PPSQ and PDMS, led to morphological changes, characterized by nanoparticles of PPSQ and/or SiO(2) embedded in the PDMS-rich matrix. On its course, the use of diphenylsilanediol and phenyltriethoxysilane mixture, as an additive, led to more homogeneous films in comparison to PPSQ/PDMS. (C) 2009 Elsevier B.V. All rights reserved.35534-3617261732Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)