The synthesis of sol-gel materials induced by ultrasonic action (sonolysis) is implemented as an alternative method for the fabrication of highly pure organic-inorganic composites with good monolithic and optical properties. A newly synthesized liquid crystalline mesogen (named here RED-PEGM-7) was introduced as dopant specie within the SiO(2) matrix in order to create an active nonlinear optical hybrid material at room temperature. A comparative characterization of the structural properties between a pure reference sample and several doped composites was performed by X-ray diffraction (XRD) and atomic force microscopy (AFM); where, an optimal dissolution concentration of tetraethoxysilane (TEOS) and the liquid crystalline (LC) mesogen, to obtain good mechanical and nonlinear optical properties in thin film layers has been found.