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Cu-Eu red fluorescent and magnetic microporous structure complex and preparation method thereof

A technology of red fluorescence and microporous structure, which is applied in the field of luminescent materials and magnetic materials, to achieve the effects of improving luminous efficiency, improving light conversion efficiency, and novel geometric topological structure

Inactive Publication Date: 2015-04-01
NORTHEASTERN UNIV
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The preparation of this 3d-4f heterometallic microporous framework complex mainly faces the following problems: a. Transition metal ions and rare earth ions tend to form the same metal ion complexes due to chelation
Therefore, it is not yet possible to accurately predict which ligands can coordinate and link different metal ions

Method used

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  • Cu-Eu red fluorescent and magnetic microporous structure complex and preparation method thereof
  • Cu-Eu red fluorescent and magnetic microporous structure complex and preparation method thereof
  • Cu-Eu red fluorescent and magnetic microporous structure complex and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Synthesis of red fluorescent single crystals with metal-organic framework microporous structure. Add CuCl in a beaker at a molar ratio of 3:2:6:12 2 , EuCl 3 , 3,4 dipicolinic acid and triethylamine. Reflux for 2 hours and filter to obtain a light blue solution. After standing for three days, sky blue hexagonal microcrystals appeared, with a yield of 45%. Pick a blue-green crystal of 0.2mm×0.18mm×0.12mm, use Xcalibur single crystal X-ray diffractometer, use Mo Kα ray (λ=0.71073nm) monochromated by graphite, and collect diffraction by φ-ω scanning data. Diffraction intensities were Lp corrected. The empirical absorption correction was carried out. The single crystal structure was solved by the direct method, and all non-hydrogen atoms were found by the difference Fourier synthesis method, and the coordinates of all non-hydrogen atoms were corrected by the least square method. The molecular structure of the complex is shown in figure 2 shown. Depend on figure 2 ...

Embodiment 2

[0047] Add 3,4 dipicolinic acid and triethylamine in ethanol to prepare solution A in a molar ratio of 6:12, and mix Cu(NO 3 ) 2 , Eu(NO3) 3 Dissolve in water to prepare solution B, mix solution A and solution B, stir for about 8 hours, filter to obtain a light blue solution, after standing for three days, sky blue hexagonal microcrystals appear. Further analysis of the structure of complex 1 as image 3 , it can be seen that the complex has a three-dimensional hole structure, and the hole radius is about 0.6nm. Table 1 is a partial Eu...Cu and Cu...Cu spacing table. It can be seen from Figure 4 that each copper ion connects four 3,4-pyridinedicarboxylic acid molecules, and each 3,4-pyridinedicarboxylic acid molecule bridges two copper ions to form an extended irregular two-dimensional plane , Europium ions are located between these two-dimensional planes, linking the copper ion coordination units to form a three-dimensional framework structure. Among them, Eu1 connects 4...

Embodiment 3

[0052] Add 3,4 dipicolinic acid and triethylamine in ethanol at a molar ratio of 6:12 to prepare solution A, and dissolve CuSO at a molar ratio of 3:2 4 , Eu(CH 3 COO) 3 Dissolve in water to prepare solution B, mix solution A and solution B, stir for about 10 hours, filter, and stand still to obtain a single crystal. Drying in the air gave blue powder with a yield of 46%. Compound 1 was further tested by polycrystalline powder diffraction as shown in Figure 5 , according to the simulation value of the single crystal structure and the experimental test value are in good agreement, which proves that the prepared powder has a high purity. In order to further test the stability of the complex, a thermogravimetric test was performed at room temperature -750°C. Depend on Image 6 It can be seen that the complex begins to lose crystal water in the range of 65-180°C, and the weight loss rate is about 24%, which is more consistent with the theoretical value. The complex began to...

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Abstract

The invention discloses a Cu-Eu red fluorescent and magnetic microporous structure complex and a preparation method thereof. The preparation method comprises the following steps: by taking pyridine dicarboxylic acid as a bridging ligand, dissolving pyridine dicarboxylic acid into deionized water according to a certain molar ratio, adding CuCl2 and EuCl3, stirring and filtering to obtain a light blue solution, and standing for three days to obtain blue-green hexagonal micro-crystals. A prepared 3d-4f metal compound can be used for greatly improving the photo-conversion efficiency based on the ligand, copper ions and pyridine dicarboxylic acid can play roles as antennae and can be used for transferring the energy of ultraviolet light to rare earth ions, and by virtue of the 3d-4f metal compound, the copper ions and pyridine dicarboxylic acid, novel geometric and topological structures can be provided, and the overall luminous efficiency of the complex can also be improved. According to the complex disclosed by the invention, metal ions are in anti-ferromagnetic coupling in a range of 300-100K, and the metal ions have ferromagnetic coupling interaction effects in a range of less than 100K.

Description

technical field [0001] The invention relates to the technical fields of luminescent materials and magnetic materials, in particular to a Cu-Eu red fluorescent and magnetic microporous structure complex and a preparation method thereof. Background technique [0002] The design and preparation of metal-organic framework complexes have attracted more and more attention. Here, the framework substances often have flexible or rigid capillary channels, which can be used in molecular recognition and separation, physical gas adsorption, sensors, ion exchange and heterogeneous Catalysts and other aspects have very important applications. [0003] After the ligands of rare earth complexes are irradiated by ultraviolet light or visible light and undergo π-π* absorption, they transition from the ground state S0 to the lowest excited singlet state S1, and then undergo intersystem crossing to the excited triplet state T 1 or T 2 , followed by the lowest excited triplet state T 1 , to ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00C09K11/06H01F1/42
Inventor 刘宣文余业奇王燕燕郭瑞
Owner NORTHEASTERN UNIV
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