A metal-organic framework ［Zn (3,4’-Hdpdc)2(4,4’-bpy)］ (Zn-MOF) has been synthesized by hydrothermal reaction with the Zn(NO3)2·6H2O, 3,4’-biphenyl dicarboxylic acid (3,4’-H2dpdc) and 4,4’-bipyridine (4,4’-bpy) , and its crystal structure was confirmed by X-ray single crystal diffraction. The complex was the monoclinic system, C2/c space group. The complex had a “Z”-shaped chain structure formed by the 4,4’-bpy ligand and Zn(Ⅱ) ion. The Zn-MOF exhibited intense ligand-based blue luminescence with the maximum excitation wavelength of 278 nm, and the emission band was in the range of 341~537 nm from the π*—π transition of the ligand. The emission maximum was at 406 nm. The luminescence properties of the complex toward Ln(Ⅲ) metal ions in methanol/aqueous solutions were studied. Fluorescence spectrum show the characteristic emission peaked of Tb (Ⅲ) ions at 490, 545, 585 and 624 nm, which corresponded to 5D4→7FJ (J=6～3) transitions of Tb (Ⅲ), the strongest emission peaked at 545 nm (5D4→7F5), for the green light. The experimental results showed that the Zn-MOF can sensitize the Tb(Ⅲ) ion in the methanol solution and in water, and thus the compound can be used as a fluorescent probe to detect Tb(Ⅲ) ions in methanol solutions and in water.