Solid scintillators are gaining interest due to their increased applications in radiation detection. A series of sol-gel monoliths were prepared from polystyrene and 4,4'-bis(triethoxysilyl)biphenyl through a room-temperature sol-gel method based on π-π interactions. The hybrid organic-inorganic scintillating dye is serving not only as a scintillator but also as a silica precursor, which has the advantage of eliminating leaching of the fluorescent sensitizer from the matrix as well as enhancing the loading of the dye without causing phase separation. The photoluminescence studies of the gel samples show emission in the blue region. The efficiencies of these plastic scintillators were measured through detection of alpha particles.