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本文以Na2WO4·2H2O,H3BO3及Eu(NO3)3·6H2O等为原料,利用常规溶液合成法制备了一种基于硼钨酸盐的稀土多金属氧酸盐K7.5H4.5[Eu(BW11O39)(W5O18)]?21.5H2O(1)。借助于X-射线单晶衍射仪(SXRD)、X-射线粉末衍射仪(PXRD)、红外光谱仪(IR)、热分析仪(TG-DTA)、以及荧光光谱仪(PL)等对样品的结构、热稳定性及发光性能进行了表征。结果表明,该化合物结晶于三斜晶系,Pī空间群,a=1.2648(3)nm,b=1.7290(4)nm,c=1.7637(4)nm,?=110.584(4)°,?=94.111(4)°,?=96.546(4)°,V=3.5610(15)nm3,H47.5O78.5BK7.5Eu W16,Mr=4701.2823,Dc=4.340 Mg/m3,μ(Mo Kα)=27.151 mm?1,F(000)=4045,GOF=1.019,Z=2,the final R1=0.0389 and w R2=0.0960 for I>2?(I)。该稀土多金属氧酸盐是以多金属氧酸盐阴离子[Eu(BW11O39)(W5O18)]12?为构筑块的三维无机框架结构,该阴离子呈现夹心型构型,Eu3+离子位于两个缺位阴离子[BW11O39]9?和[W5O18]6?的中间,该化合物呈现较高的热稳定性,在紫外光(λex=394 nm)激发下,发射出较强的红光。
In this paper, a kind of borotungstate based rare earth polyoxometallate K7.5H4.5 [Eu (BW11O39)] was prepared by the conventional solution synthesis method using Na2WO4 · 2H2O, H3BO3 and Eu (NO3) 3 · 6H2O as raw materials, (W5O18)]? 21.5H2O (1). The structure of the sample was characterized by means of X-ray single crystal diffraction (XRD), X-ray powder diffraction (PXRD), infrared spectroscopy (IR), thermal analysis (TG-DTA) and fluorescence spectroscopy (PL) Thermal stability and luminescent properties were characterized. The results show that the compound crystallizes in the triclinic system with a = 1.2648 (3) nm, b = 1.7290 (4) nm and c = 1.7637 (4) nm, 94.111 (4) °, = 96.546 (4) °, V = 3.5610 (15) nm3, H47.5O78.5BK7.5Eu W16, Mr = 4701.2823, Dc = 4.340 Mg / m3, μ (Mo Kα) = 27.151 mm ? 1, F (000) = 4045, GOF = 1.019, Z = 2, the final R1 = 0.0389 and w R2 = 0.0960 for I> 2? The rare-earth polyoxometallate is a three-dimensional inorganic framework structure based on a polyoxometalate anion [Eu (BW11O39) (W5O18)] 12 ?, wherein the anion has a sandwich type configuration and Eu3 + ions are located at two vacancies In the middle of the anion [BW11O39] 9? And [W5O18] 6 ?, the compound shows high thermal stability and emits strong red light when excited by ultraviolet light (λex = 394 nm).