New nanocomposites were synthesized by the reaction between a polyhedral oligomeric silsesquioxane (POSS) with eight epoxy groups (epoxy-POSS) and diglycidyl ether of bisphenol A (DGEBA) using Jeffamine D230 as curing agent. The reactivity of the systems was extensively studied by Raman spectroscopy. The hybrid materials were characterized by different techniques like thermogravimetric analysis, dynamical mechanical analysis, X-ray photoelectron spectroscopy, differential scanning calorimetry, and scanning electron microscopy. The oSi-O-Sio cages of the POSS component form aggregates, which was shown by the conversion data obtained from the Raman spectra and confirmed by the DSC curves, XPS spectra, and SEM images.