系列Ag-Ln配聚物的研制及发光性能
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摘要
本文采用水热合成反应方法，合成了6种Ag-Ln(Ln=Ho，Tb，Gd，Nd，Sm，Pr)杂多核配合物，另有4种无限结构的稀土配聚物，1种稀土配合物。全部得到了单晶体，经过X-光射线衍射测定，确定了它们的分子结构，分子式如下：(1){[Ho_2Ag_4(INA)_8(H_2O)_(10)]·2NO_3·2H_2O}_n (2){[Tb_2Ag_4(INA)_8(H_2O)_(10)]·2NO_3·2H_2O}_n (3){[Gd_2Ag_4(INA)_8(H_2O)_(10)]·2NO_3·2H_2O}_n (4){[NdAg_2(INA)_4·(H_2O)_2]·NO_3·H_2O}_n (5){[SmAg_2(INA)_4·(H_2O)_2]·NO_3·H_2O}_n (6){[PrAg_2(INA)_4·(H_2O)_2]·NO_3·H_2O}_n (7)[Er_4(btec)_3(H_2O)_4]_n (8)[Er(C_8H_7O_3)_3]_n (9)[Yb(C_8H_7O_3)_3]_n (10)[Sm(INA)_3(H_2O)_2]_n (11)Nd_2(C_7H_4O_2Cl)_6(phen)_2(H_2O)_2
重点研究了它们在可见区和近红外区的发光性能。化合物(2)发射很强的绿光，化合物(5)，(10)的发光在整个光谱的橙色区域，化合物(1)，(4)，(7)，(8)，(9)，(11)在可见区的发光相对较弱，而在近红外区却表现出明显的稀土离子的特征发射，化合物(6)在近红外区没有检测到Pr(Ⅲ)的特征发射。通过对各产物特别是d-f杂多核配合物光物理的对比研究以及相关的定量考察，我们发现d块和f块之间以及有机配体和中心金属之间的相互影响能够改变分子内部能级，使分子产生较强的发射光。同时，起天线作用的辅助配体及第二个金属离子的引入，不但可以改变结构，更值得注意的是它们往往可以起到敏化稀土离子发光的作用，从而调变并增强体系发光。此外，我们还对化合物进行了IR，UV-VIS-NIR光谱的测定和分析，以有利于化合物发光性能的考察，分析和对比。
Six novel Ag-Ln (Ln=Ho, Tb, Gd, Nd, Sm, Pr) coordination polymershave been synthesized under hydrothermal condition, besides of four rareearth coordination polymers and one dinuclear rare earth complex. Thecrystal structures are determined by X-ray diffraction and their formulasare presented as following: (1){[Ho_2Ag_4(INA)_8(H_2O)_(10)]·2NO_3·2H_2O}_n (2){[Tb_2Ag_4(INA)_8(H_2O)_(10)]·2NO_3·2H_2O}_n (3){[Gd_2Ag_4(INA)_8(H_2O)_(10)]·2NO_3·2H_2O}_n (4){[NdAg_2(INA)_4·(H_2O)_2]·NO_3·H_2O}_n (5){[SmAg_2(INA)_4·(H_2O)_2]·NO_3·H_2O}_n (6){[PrAg_2(INA)_4·(H_2O)_2]·NO_3·H_2O}_n (7)[Er_4(btec)_3(H_2O)_4]_n (8)[Er(C_8H_7O_3)_3]_n (9)[Yb(C_8H_7O_3)_3]_n (10)[Sm(INA)_3(H_2O)_2]_n (11)Nd_2(C_7H_4O_2Cl)_6(phen)_2(H_2O)_2
Their photoluminescences are mainly studied. Complex (2) canexhibit intense green light. Complexes (5), (10) can exhibit light in therange of orange color. And complexes (1), (4), (7), (8), (9), (11) canexhibit week light in visible region but strong light in NIR. But complex(6) does not exhibit any emission spectrum in the NIR. We found thatthrough quantitative analysis the influence between d-block and f-block,organic ligands and center metals can change the intramolecular energylevel, which can increace quantum efficiency. At the same time, someinvestigations have shown that the introduction of an auxiliary ligand or asecond metal ion can alter not only the architectures but also thephotoluminescent properties. In addition, their IR, UV-VIS-NIR spectraare measured and investigated which are important to further analyse andcontrast the luminescent property.
重点研究了它们在可见区和近红外区的发光性能。化合物(2)发射很强的绿光，化合物(5)，(10)的发光在整个光谱的橙色区域，化合物(1)，(4)，(7)，(8)，(9)，(11)在可见区的发光相对较弱，而在近红外区却表现出明显的稀土离子的特征发射，化合物(6)在近红外区没有检测到Pr(Ⅲ)的特征发射。通过对各产物特别是d-f杂多核配合物光物理的对比研究以及相关的定量考察，我们发现d块和f块之间以及有机配体和中心金属之间的相互影响能够改变分子内部能级，使分子产生较强的发射光。同时，起天线作用的辅助配体及第二个金属离子的引入，不但可以改变结构，更值得注意的是它们往往可以起到敏化稀土离子发光的作用，从而调变并增强体系发光。此外，我们还对化合物进行了IR，UV-VIS-NIR光谱的测定和分析，以有利于化合物发光性能的考察，分析和对比。
Six novel Ag-Ln (Ln=Ho, Tb, Gd, Nd, Sm, Pr) coordination polymershave been synthesized under hydrothermal condition, besides of four rareearth coordination polymers and one dinuclear rare earth complex. Thecrystal structures are determined by X-ray diffraction and their formulasare presented as following: (1){[Ho_2Ag_4(INA)_8(H_2O)_(10)]·2NO_3·2H_2O}_n (2){[Tb_2Ag_4(INA)_8(H_2O)_(10)]·2NO_3·2H_2O}_n (3){[Gd_2Ag_4(INA)_8(H_2O)_(10)]·2NO_3·2H_2O}_n (4){[NdAg_2(INA)_4·(H_2O)_2]·NO_3·H_2O}_n (5){[SmAg_2(INA)_4·(H_2O)_2]·NO_3·H_2O}_n (6){[PrAg_2(INA)_4·(H_2O)_2]·NO_3·H_2O}_n (7)[Er_4(btec)_3(H_2O)_4]_n (8)[Er(C_8H_7O_3)_3]_n (9)[Yb(C_8H_7O_3)_3]_n (10)[Sm(INA)_3(H_2O)_2]_n (11)Nd_2(C_7H_4O_2Cl)_6(phen)_2(H_2O)_2
Their photoluminescences are mainly studied. Complex (2) canexhibit intense green light. Complexes (5), (10) can exhibit light in therange of orange color. And complexes (1), (4), (7), (8), (9), (11) canexhibit week light in visible region but strong light in NIR. But complex(6) does not exhibit any emission spectrum in the NIR. We found thatthrough quantitative analysis the influence between d-block and f-block,organic ligands and center metals can change the intramolecular energylevel, which can increace quantum efficiency. At the same time, someinvestigations have shown that the introduction of an auxiliary ligand or asecond metal ion can alter not only the architectures but also thephotoluminescent properties. In addition, their IR, UV-VIS-NIR spectraare measured and investigated which are important to further analyse andcontrast the luminescent property.
引文
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[2] Sixto Domi'nguez, Julia Torres, Florencia Peluffo, et al. Mixed 3d/4f polynuclear complexes with 2, 20-oxydiacetate as bridging ligand: Synthesis, structure and chemical speciation of La-M compounds (M=bivalent cation). Journal of Molecular Structure, 2007, 829:57-64
[3] Takafumi Kido, Shigeyuki Nagasato, Yukinari Sunatsuki, Naohide Matsumoto. A cyclic tetranuclear Cu2Gd2 complex with an s=8 ground state derived from ferromagnetic spin-couping between copper (Ⅱ) and gadolinium(Ⅲ)ions arrayed alternately. Chem.Commun. 2000:2113-2114
[4] Raquel Rodri'guez-Cortin, Fernando Avecilla, Carlos Platas-Iglesias, et al. Structural and Photophysical Properties of Heterobimetallic 4f-Zn Iminophenolate Cryptates. Inorganic Chemistry, 2002, 41, (21): 5336-5349
[5] 良玉仓，洪茂春，曹荣等。含吡啶-2，5-二羧酸稀土-锌配位聚合物合成结构和性能。无机化学学报，2002，18(1)：100-107
[6] Yi-Shan Song, Bing Yan. A novel unexpected luminescent quarternary coordination polymer {Sm_3(C_8H_4O_4)_4(C_(12)N_2H_8)_2(NO_3)}n with three high asymmetrical central Sm fragments by hydrothermal assembly. Inorganica Chimica Acta, 2005, 358:191-195
[7] Ercules E.S. Teotonio, Hermi F. Brito, Maria Cla'udia F.C. Felinto, et al. Preparation, crystal structure and optical spectroscopy of the rare earth complexes (RE~(3+)=Sm, Eu, Gd and Tb) with 2-thiopheneacetate anion.Journal of Molecular Structure, 2005, 751:85-94
[8] Ze Liu, Fushan Wen, Wenlian Li. Synthesis and electroluminescence properties of europium (Ⅲ)complexes with new second ligands. Thin Solid Films 2005, 478: 265-270
[9] Andrew P. Bassett, Steven W. Magennis, Peter B. Glover, et al. Highly Luminescent, Triple- and Quadruple-Stranded, Dinuclear Eu, Nd, and Sm(III) Lanthanide Complexes Based on Bis-Diketonate Ligands. J. AM. CHEM. SOC. 2004, 126: 9413-9424
[10]Bin Zhao, Xiao-Yan Chen, Peng Cheng, et al. Coordination Polymers Containing 1D Channels as Selective Luminescent Probes. J. AM. CHEM. SOC, 2004, 126: 15394-15395
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