A soft process for the intercalation of different ammonium cations into vanadium pentoxide was developed. By refluxing an aqueous solution containing ammonium , tetramethylammonium (CH3)4N+, and tetraethylammonium (C2H5)4N+ with V2O5 powders, intercalation compounds containing corresponding ammonium cations were obtained. The compound with aniline C6H5NH2 was also synthesized by the same process. The compounds with (CH3)4N+, (C2H5)4N+, and also C6H5NH2 had diffraction patterns consisting of very sharp 00l lines. The spacing for sandwiching the intercalates (the identity period), (CH3)4N+, (C2H5)4N+, and C6H5NH2, was 1.29, 1.31, and 1.39 nm, respectively.