Abstract The heterogeneous fluorination of diethylsilane, ethylvinylsilane and divinylsilane with SbF 3 was studied by measuring the yields of the fluorinated products as a function of reaction time. As the reactions proceed, the monofluorinated species (two of them are new compounds) exhibit maxima in their percentage yields with respect to time. The proton NMR and IR spectra of the three silanes and their six fluorinated products are reported.