An aspect of organophilic modification for the delamination is described for the layered rare-earth hydroxides in this paper. The interlayer property of RE 2 (OH) 5 NO 3 ·nH 2 O, where RE=Eu (LEuH) and Tb (LTbH), was modified by the exchange reaction of nitrate ion with oleate anion that is one of the representative dispersion agents in nonpolar solvents. The bilayer arrangement of long oleate anions in the gallery of RE 2 (OH) 5 NO 3 ·nH 2 O could effectively weaken the stacking of the hydroxide layers. Highly organophilic environment of the interlayer space promoted the introduction of toluene to delaminate the layered structure into their individual sheets. When irradiated with 365 nm UV, the resulting transparent colloidal solutions of toluene containing LEuH and LTbH nanosheets yielded typical red and green emissions, respectively, which are visible to the naked eye.