High temperature reaction-vaporization techniques were used to produce AlF, GaF and InF in the vapor and condensed states. The efficiency of the eqs. M+AlF3→MF, M+CaF2→MF, where M=Al, Ga or In, were determined by a loss in weight method. The maximum purity obtained was about 65 percent. The microwave absorption spectra of these monofluorides varified their presence in the vapor from the reaction mixtures above as well as in the vapor from the condensates obtained by quenching the vapor produced in these reactions.