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The transformations induced by ion irradiation in films of polycarbosilane and gels derived from tetraethoxysilane, methyltriethoxysilane and triethoxysilane have been studied. Hydrogen is released selectively under the effect of electronic excitations at a rate depending on the probability of H radicals to combine for forming molecules inside the film. The radiolysis efficiency of C—H bonds is the lowest and that of Si—H bonds the highest. Beside the conversion of the polymeric structure into an amorphous ceramic, ion irradiation induces the precipitation of C or Si clusters, according to the precursor, leading to a noticeable luminescence in the visible. This precipitation has been put into evidence for the first time by energy filtered electron microscopy.