Schiff base 4-(p-dimethylaminobenzaldehydeamino)-4H-1,2,4-triazole(L) was synthesized from 4-amino-1,2,4-triazole and p-dimethylaminobenzaldehyde using acetic acid as the catalyst. The solid complexes RE3L6(NO3)6(H2O)2 (RE=Cu, Co, Zn, Cd; x=3-6) were synthesized with 4-(p-dimethylaminobenzaldehydeamino)-4H-1,2,4-triazole and nitrate of transition metals in ethanol and characterized by elemental analysis, infrared spectroscopy, UV spectrum, and fluorescence spectrum. Experimental results showed that the free ligand is a thermally stable material, and its ethanol solution emitted intense blue fluorescence at the peak wavelength of 416 nm. The absorption band at about 406 nm can be assigned to the intrinsic absorption of CN. Compared with the fluorescence emission of free ligand in ethanol solution, the emission of the complex of RE3L6(NO3)6(H2O)2 was red-shifted to 445 nm and narrow in solution. RE(Ⅱ) was coordinated with N atomy of triazole in 4-(p-dimethylaminobenzaldehydeamino)-4H-1,2,4-triazole.