The complexes of Zn^2+, Ni^2+ with 4-amino-3,5-dimethyl-1,2,4-triazole and 4-amino-i, 2,4-triazote were synthesized in water, respectively. By elemental analysis, coordination titration and molar conductivities studies, the compositions of the complexes were suggested as Zna (NCS)6 (L1)6 (NO3)2 and Ni3 (NCS)6 (L2)6 (NO3)2 respectively. The ligands and coordination compounds were studied by means of IR spectra, UV and fluorescence excitation and emission spectra. The IR spectra studies indicate that triazolate was bonded with RE ( Ⅱ ) through nitrogen atoms in the heterocyclic ring. The fluorescence spectra showed that the fluorescence emission intensity of Ni3 (NCS) 6 (L2) 6 (NO3) 2 was stronger than that of Zn3 (NCS) 6 ( L1 ) 6 (NO3) 2.