Lanthanum lithium titanate, belonging to the solid solution La0.66Li0.33TiO3, was prepared by sol-gel method from LiNO3, La(NO3)(3)center dot 6H(2)O and Ti(OC4H9)(4) in ideal cation stoichiometry for La0.66Li0.33TiO3. The synthesized product was characterized by X-ray powder diffractometry (XRD) and thermal analyses (DTA-TG). Electron microscopy investigations (SEM and TEM) was used to evaluate the morphology of synthesized La0.66Li0.33TiO3. The bulk quantities of nano-sized particles of layered La0.66Li0.33TiO3 have been obtained at 1,000 degrees C using the modified sol-gel method. The mean diameter of La0.66Li0.33TiO3 nano-crystals was about 123 nm.