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以卤代苯甲酸和1,10-邻菲哕啉为配体,合成了9种Tb(Ⅲ)的三元配合物,以EDTA配位滴定分析和元素分析确定了各配合物的组成。通过红外光谱分析对配合物的结构进行了初步表征,在配合物中羧基氧原子和1,10-邻菲啰啉中的氮原子均参与了配位。采用TG-DTG技术对配合物的热稳定性进行了研究,9种配合物均有较好的热稳定性,它们的热稳定性顺序为:Tb(o-ClBA)_3phen>Tb(o-BrBA)_3phen>Tb(p- ClBA)_3phen>Tb(m-BrBA)_3phen·H_2O>Tb(o-FBA)_3phen>Tb(p-BrBA)_3phen>Tb(p-FBA)_3phen>Tb(m- ClBA)_3phen≈Tb(m-FBA)_3phen·H_2O。在同一条件下测得了各配合物固体粉末的激发和发射光谱,结果表明:相同取代基和相同取代位置的各组配合物的两个较强发射峰(~5D_4-~7F_6和~5D_4-~7F_5)的荧光强度顺序分别为:Tb(o-FBA)_3phen>Tb(p-FBA)_3phen>Tb(m-FBA)_3phen·H_2O,Tb(m-ClBA)_3phen>Tb(p-ClBA)_3phen>Tb (o-ClBA)_3phen,Tb(p-BrBA)_3phen>Tb(o-BrBA)_3phen>Tb(m-BrBA)_3phen·H_2O和Tb(o-FBA)_3phen>Tb (o-BrBA)_3phen>Tb(o-ClBA)_3phen,Tb(m-ClBA)_3phen>Tb(m-FBA)_3phen·H_2O>Tb(m-BrBA)_3phen·H_2O,Tb(p-BrBA)_3phen>Tb(p-ClBA)_3phen>Tb(p-FBA)_3phen[其中o(m,p)-F(Cl,Br)BA为邻(间,对)氟(氯,溴)苯甲酸根,phen为1,10-邻菲哕啉]。
Nine ternary complexes of Tb (Ⅲ) were synthesized by using halogenated benzoic acid and 1,10-phenanthroline as ligands. The composition of each complex was determined by EDTA coordinate titration and elemental analysis. The structure of the complex was preliminarily characterized by infrared spectroscopy. The carboxyl oxygen atoms and nitrogen atoms in 1,10-phenanthroline were all coordinated in the complex. The thermostability of the complexes was studied by TG-DTG technique. All the nine complexes have good thermal stability. The order of their thermal stability is Tb (o-ClBA) 3phen> Tb (o-BrBA ) _3phen> Tb (p-ClBA) _3phen> Tb (m-BrBA) _3phen · H_2O> Tb (o-FBA) _3phen> Tb ) _3phen≈Tb (m-FBA) _3phen · H_2O. Under the same conditions, the excitation and emission spectra of the solid powders were measured. The results showed that the two strong emission peaks (~ 5D_4 ~ 7F_6 and ~ 5D_4 ~ (P-FBA) _3phen> Tb (m-FBA) _3phen · H_2O, Tb (m-ClBA) _3phen> Tb (p-ClBA) _3phen Tb (o-BrBA) _3phen> Tb (o-BrBA) _3phen> Tb (m-BrBA) _3phen.H2O and Tb (o-FBA) (P-BrBA) _3phen> Tb (m-ClBA) _3phen> Tb (m-ClBA) _3phen> Tb (Phenylene) is 1, 10-o-phenylene group, which is o (m, p) -F Phenanthroline].