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本文分别采用水热和溶剂热的方法,以乙二胺和哌嗪为有机模板剂分别合成了两种新的三维孔道结构的稀土硫酸盐[Gd2(SO4)5(H2O)2][C2N2H10]2(1),[Eu2(SO4)5(H2O)2][C4N2H12]2(2),并且通过单晶X射线衍射、元素分析、红外、热重对两种化合物进行了表征。化合物1和2都属于单斜晶系,P21/c空间群。化合物1:a=0.652 1(4)nm,b=1.692 0(9)nm,c=2.023 3(11)nm,β=95.168(7)°,Z=4。化合物2:a=1.972 1(2)nm,b=1.927 1(2)nm,c=1.323 20(14)nm,β=92.307 0(10)°,Z=8。单晶结构分析表明,这两种化合物的无机骨架都是由SO4连接具有交替十六元环与八元环二维层形成的三维孔道结构。化合物2的固体荧光分析表明,在396 nm的激发波长下表现出Eu3+的特有发光性质。
In this paper, two new three-dimensional porous structures of rare earth sulfate [Gd2 (SO4) 5 (H2O) 2] [C2N2H10] were synthesized by hydrothermal and solvothermal methods using ethylenediamine and piperazine as organic template respectively. 2 (1), [Eu2 (SO4) 5 (H2O) 2] [C4N2H12] 2 (2) were synthesized and characterized by single crystal X-ray diffraction, elemental analysis, infrared and thermogravimetry. Compounds 1 and 2 belong to the monoclinic space group P21 / c. Compound 1: a = 0.652 1 (4) nm, b = 1.692 0 (9) nm, c = 2.023 3 (11) nm, β = 95.168 (7) °, Z = 4. Compound 2: a = 1.972 1 (2) nm, b = 1.927 1 (2) nm, c = 1.323 20 (14) nm, β = 92.307 0 (10) °, Z = 8. Single crystal structure analysis shows that the inorganic frameworks of these two compounds are connected by SO4 with three-dimensional pore structure formed by two-dimensional layers of alternating 16-membered ring and 8-membered ring. Solid-state fluorescence analysis of Compound 2 showed that Eu3 + has unique luminescence properties at an excitation wavelength of 396 nm.