系列d-f异双核发光配合物的研制及性能
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摘要
(1):本文采用溶剂热合成方法,合成了12种M-Ln(M=Zn,Cd;Ln=Eu,Tb,Gd,Pr,Nd,Ho,Er,Yb) d-f异双核配合物,另有3种Ln_2(Ln=Pr,Ho,Er)同双核稀土配合物。全部得到了单晶体,经过X-光衍射测定,确定了它们的分子结构,分子式如下: EuCd(C_8H_7O_3)_5(phen)(H_2O) (1) TbCd(C_8H_7O_3)_5(phen)(H_2O) (2) GdCd(C_8H_7O_3)_5(phen)(H_2O) (3) PrCd(C_8H_7O_3)_5(phen)(H_2O) (4) NdCd(C_8H_7O_3)_5(phen)(H_2O) (5) HoCd(C_8H_7O_3)_5(phen)(H_2O) (6) ErCd(C_8H_7O_3)_5(phen)(H_2O) (7) EuZn(C_8H_7O_3)_5(phen)(H_2O) (8) TbZn(C_8H_7O_3)_5(phen)(H_2O) (9) ErZn(C_8H_7O_3)_5(phen)(H_2O) (10) YbZn(C_8H_7O_3)_5(phen)(H_2O) (11) HoZn(C_8H_7O_2)_5(phen)(H_2O) (12) Pr_2(C_7H_4O_2Cl)_6(phen)_2(H_2O)2 (13) Ho_2(C_7H_4O_2Cl)_6(phen)_2 (14) Er_2(C_7H_4O_2Cl)_6(phen)_2 (15)
(2):研究了这些化合物在可见区和近红外区的发光性能。化合物(1),(8)发射很强的红光,化合物(2),(9)发射很强的绿光;化合物(5),(6),(7),(11),(12),(14),(15)在可见区的荧光发射相对较弱,而在近红外区却表现出明显的稀土离子特征发射,化合物(13)在近红外区没有检测到文献报道的Pr(III)特征发射。
(3):通过对d-f配合物与相应过渡金属配合物发光性能的对比研究,进一步证实了以下规律:第一,当配体激发态能级与稀土离子激发态能级相匹配时,杂双核配合物中d块与f块之间的能量传递非常有效,导致d块发射减弱,甚至完全猝灭,而相对的f块发射却很强,即d块对f块发射起到很好的敏化作用;第二,虽然稀土离子具有丰富的能级可与配体激发态能级相匹配,但是由于稀土离子的近红外发光,导致可见区稀土离子特征发射较弱,且成带状谱,而相应的d块发射却较强,d块对f块发射的敏化作用不明显。第三,当配体与稀土离子激发态能级不匹配(由于稀土离子激发态能级过高或者过低)时,d块与f块之间的能量传递不能进行,在可见区观察不到稀土离子的特征发射,而d块发射却较强,d块对f块发射没有起到敏化作用。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综合考察,分析和对比。
Fifteen coordination complexes, including 12 d-f hetero-binuclear M-Ln complexes (M = Zn, Cd; Ln = Eu, Tb, Gd, Pr, Nd, Ho, Er, and Yb) and 3 homo-binuclear Ln-Ln complexes (Ln=Pr, Ho and Er), have been thermally synthesized and structurally characterized by X-ray diffraction. Their formulas are presented as following: EuCd(C_8H_7O_3)_5(phen)(H_2O) (1) TbCd(C_8H_7O_3)_5(phen)(H_2O) (2) GdCd(C_8H_7O_3)_5(phen)(H_2O) (3) PrCd(C_8H_7O_3)_5(phen)(H_2O) (4) NdCd(C_8H_7O_3)_5(phen)(H_2O) (5) HoCd(C_8H_7O_3)_5(phen)(H_2O) (6) ErCd(C_8H_7O_3)_5(phen)(H_2O) (7) EuZn(C_8H_7O_3)_5(phen)(H_2O) (8) TbZn(C_8H_7O_3)_5(phen)(H_2O) (9) ErZn(C_8H_7O_3)_5(phen)(H_2O) (10) YbZn(C_8H_7O_3)_5(phen)(H_2O) (11) HoZn(C_8H_7O_2)_5(phen)(H_2O) (12) Pr_2(C_7H_4O_2Cl)_6(phen)_2(H_2O)2 (13) Ho_2(C_7H_4O_2Cl)_6(phen)_2 (14) Er_2(C_7H_4O_2Cl)_6(phen)_2 (15)
The study on luminescent property in the visible and NIR regions reveals that complexes (1) and (8) emit strong red light, complexes (2) and (9) emit strong green light, and the left complexes besides (13) emit weak fluorescence in the visible region; all the 15 complexes except (13) show the characteristic emission of lanthanide ion in the NIR region.
Compare and contrast the luminescence of d-f complexes and corresponding transition metal complexes (d complexes), the following rules are confirmed:
(1) When the energy level of excited states between ligand and lanthanide ion is matching, the energy transferring between d block and f block in hetero-binuclear complexes is very efficient. This results in the strengthening of emission of f block and weakening of emission of d block, so much as quenching. That is to say, d block sensitize the emission of f block.
(2) Although the lanthanide ion possesses abundant energy levels and which can matches the energy level of excited states of ligand, luminescence of the lanthanide ion in the NIR region leads to the weakening of its characteristic emission in the visible region and the strengthening of emission of d block in the visible region. As a result, the emission of lanthanide ion in the visible region takes on zonal spectra, the sensitized action of d block is not obvious to the emission of f block
(3) When the energy level of excited states between ligand and lanthanide ion is not matching (the energy level of excited states of lanthanide ion is much higher or lower), the energy transferring between d block and f block in hetero-binuclear complexes does not take place. So the characteristic emission of lanthanide ion is not observed in the visible region, however the emission of d block is strong, i.e., d block does not sensitize the emission of f block.
In addition, the IR and UV-Vis-NIR of all complexes for the analysis and contrast of luminescent property are measured and analsized.
(2):研究了这些化合物在可见区和近红外区的发光性能。化合物(1),(8)发射很强的红光,化合物(2),(9)发射很强的绿光;化合物(5),(6),(7),(11),(12),(14),(15)在可见区的荧光发射相对较弱,而在近红外区却表现出明显的稀土离子特征发射,化合物(13)在近红外区没有检测到文献报道的Pr(III)特征发射。
(3):通过对d-f配合物与相应过渡金属配合物发光性能的对比研究,进一步证实了以下规律:第一,当配体激发态能级与稀土离子激发态能级相匹配时,杂双核配合物中d块与f块之间的能量传递非常有效,导致d块发射减弱,甚至完全猝灭,而相对的f块发射却很强,即d块对f块发射起到很好的敏化作用;第二,虽然稀土离子具有丰富的能级可与配体激发态能级相匹配,但是由于稀土离子的近红外发光,导致可见区稀土离子特征发射较弱,且成带状谱,而相应的d块发射却较强,d块对f块发射的敏化作用不明显。第三,当配体与稀土离子激发态能级不匹配(由于稀土离子激发态能级过高或者过低)时,d块与f块之间的能量传递不能进行,在可见区观察不到稀土离子的特征发射,而d块发射却较强,d块对f块发射没有起到敏化作用。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综合考察,分析和对比。
Fifteen coordination complexes, including 12 d-f hetero-binuclear M-Ln complexes (M = Zn, Cd; Ln = Eu, Tb, Gd, Pr, Nd, Ho, Er, and Yb) and 3 homo-binuclear Ln-Ln complexes (Ln=Pr, Ho and Er), have been thermally synthesized and structurally characterized by X-ray diffraction. Their formulas are presented as following: EuCd(C_8H_7O_3)_5(phen)(H_2O) (1) TbCd(C_8H_7O_3)_5(phen)(H_2O) (2) GdCd(C_8H_7O_3)_5(phen)(H_2O) (3) PrCd(C_8H_7O_3)_5(phen)(H_2O) (4) NdCd(C_8H_7O_3)_5(phen)(H_2O) (5) HoCd(C_8H_7O_3)_5(phen)(H_2O) (6) ErCd(C_8H_7O_3)_5(phen)(H_2O) (7) EuZn(C_8H_7O_3)_5(phen)(H_2O) (8) TbZn(C_8H_7O_3)_5(phen)(H_2O) (9) ErZn(C_8H_7O_3)_5(phen)(H_2O) (10) YbZn(C_8H_7O_3)_5(phen)(H_2O) (11) HoZn(C_8H_7O_2)_5(phen)(H_2O) (12) Pr_2(C_7H_4O_2Cl)_6(phen)_2(H_2O)2 (13) Ho_2(C_7H_4O_2Cl)_6(phen)_2 (14) Er_2(C_7H_4O_2Cl)_6(phen)_2 (15)
The study on luminescent property in the visible and NIR regions reveals that complexes (1) and (8) emit strong red light, complexes (2) and (9) emit strong green light, and the left complexes besides (13) emit weak fluorescence in the visible region; all the 15 complexes except (13) show the characteristic emission of lanthanide ion in the NIR region.
Compare and contrast the luminescence of d-f complexes and corresponding transition metal complexes (d complexes), the following rules are confirmed:
(1) When the energy level of excited states between ligand and lanthanide ion is matching, the energy transferring between d block and f block in hetero-binuclear complexes is very efficient. This results in the strengthening of emission of f block and weakening of emission of d block, so much as quenching. That is to say, d block sensitize the emission of f block.
(2) Although the lanthanide ion possesses abundant energy levels and which can matches the energy level of excited states of ligand, luminescence of the lanthanide ion in the NIR region leads to the weakening of its characteristic emission in the visible region and the strengthening of emission of d block in the visible region. As a result, the emission of lanthanide ion in the visible region takes on zonal spectra, the sensitized action of d block is not obvious to the emission of f block
(3) When the energy level of excited states between ligand and lanthanide ion is not matching (the energy level of excited states of lanthanide ion is much higher or lower), the energy transferring between d block and f block in hetero-binuclear complexes does not take place. So the characteristic emission of lanthanide ion is not observed in the visible region, however the emission of d block is strong, i.e., d block does not sensitize the emission of f block.
In addition, the IR and UV-Vis-NIR of all complexes for the analysis and contrast of luminescent property are measured and analsized.
引文
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