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) 2.2 V 2 O 5 Á0.6 H 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.