Vanadium xerogels intercalated by n -hexadecylamine were prepared in the presence of hexane. The interlayer spacing of the vanadium xerogel was saturated by n -hexadecylamine at a composition of ( n -hexadecylamine) 2.2V2O5 center dot 0.6H(2)O. The space between the n -hexadecylamine molecules in the layer was available for adsorption of dye molecules. Large amounts of rhodamine 6G (2.9 wt%), pyrene (1.8 wt%), and p -terphenyl (3.6 wt%) were monomerically intercalated. The I-1/I-3 ratios of the emission peak for pyrene in the intercalation compounds were approximately 0.9, suggesting a nonpolar environment of the interlayer space. The N , N -diethlaminoazobenzene molecules in intercalation compounds were highly confined between n -hexadecylamine molecules.