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Tb(Ⅲ)-trimesic acid (TMA) luminescent complexes were synthesized in the polyvinylpyrrolidone (PVP) matrix. The elemental analysis, inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and fourier-transform infrared spectroscopy (FT-IR) indicated that its chemical constitution is PVP/Tb(MTA)·4H2O. The XRD patterns showed that the complex is a new kind of crystal. The TEM image indicates that the complex is rod shaped. The rod diameter is about 200 nm, and the length ranges from hundred of nanometer to a few micrometers. In addition, the dispersity is better. TG-DTA curves indicate that the complex is thermally stable before 463 ℃. Photoluminescence analysis indicates that the complex emits Tb3+ characteristic luminescence under ultraviolet excitation.