Solvothermal synthesis, structure and characterization of 1D chain and 2D layered rare earth sulfates in the presence of cyclic diamines

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• 作者：Gen-Wu Ge ; Zhi-Yuan Qi ; Zhi-Gang Ni ; Yi-Zhi Li ; Hong-Bin Du ; ^{hbdu@nju.edu.cn} ; Xiao-Zeng You
• 关键词：Sulfate ; Rare earth ; Structure ; Synthesis ; Photoluminescence
• 刊名：Inorganic Chemistry Communications
• 出版年：2012
• 期刊代码：39_13877003
• 类别：ch
• 出版时间：June, 2012
• 卷：20
• 期：Complete
• 页码：228-233
• 文件大小：1239 K

摘要

Three new rare earth sulfates were solvothermally synthesized and characterized by X-ray diffraction, elemental analysis, thermogravimetric, and photoluminescent studies. Compounds [(NH₄)(C₆N₂H₁₂)][Ln(SO₄)₃] (LnEu, 1; Gd, 2) were synthesized in the solvent of DMA with 1,4-diazabicyclo-[2,2,2]-octane (DABCO) as a structure-directing agent (SDA), which are isomorphous and adopt a two-dimensional layered structure with 8-membered rings made of LnO₈ polyhedra and SO₄ tetrahedra. The protonated DABCO molecules lie between the layers while the ammonium cations are located within the layers. Compound [(C₄N₂H₁₂)_1.5][Er(SO₄)₃(H₂O)] (3) was synthesized in the mixed solvent of water and ethanol with piperazine (PIP) as a SDA. The structural analyses showed that 3 is constructed from ErO₉ polyhedra and SO₄ tetrahedra to form a one-dimensional chained structure with edge-sharing 4-membered rings. The protonated PIP molecules and coordination H₂O molecules form extensive intra- and inter-chain hydrogen bonding to generate a 3-dimensional supramolecular network. The three compounds exhibit good thermal stability. Compound 1 exhibits intense red luminescence upon excitation owing to the Eu³⁺ ion.