Two kinds of Tb（Ⅲ） complexes with tetrapodal ligand, [TbL（NO3）] 3+ and [TbL] 3+ （L: 1,1,1′,1′-tera（2-pyridinecarboxylester）-di（trimethylpropane）） were intercalated into the interlayer space of montmorillonite （MT） by ion exchange and coordination reaction of L with the Tb 3+ ion existing in the interlayer space of Tb-MT respectively. The obtained luminescent supramolecular composite materials, [TbL（NO3）] 2+ -MT and [TbL] 3+ -MT were characterized by elemental analysis, XRD, FT-IR, UV-vis and thermal analysis. At the same time, the luminescent properties of the materials were also studied. The results show that the intercalated materials with regular layered structure, good thermal stability and the interlayer spacing （d 001 ） approximates to the size of the complex ions which are located in the interlayer space of MT in the form of a monolayer. The material emit characteristic green emission of Tb 3+ strongly under excitation of ultraviolet light. It is also found that the thermal stabilities and relative luminescence intensities of the Tb 3+ species are distinctly improved after the Tb（Ⅲ） complexes are intercalated into the MT. The excitation wavelengths of the complexes are modulated to red shift in the composite materials.
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