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Ternary rare-earth organic framework crystal material as well as synthesis method and application of ternary rare-earth organic framework crystal material

A crystal material, rare earth organic technology, applied in the direction of luminescent materials, chemical instruments and methods, instruments, etc., can solve the problems of ternary rare earth-organic framework materials that have not been seen, achieve high thermal stability and air stability, high sensitivity, fast response effect

Active Publication Date: 2017-05-31
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no report on ternary rare earth-organic framework materials as ratio thermometers

Method used

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  • Ternary rare-earth organic framework crystal material as well as synthesis method and application of ternary rare-earth organic framework crystal material
  • Ternary rare-earth organic framework crystal material as well as synthesis method and application of ternary rare-earth organic framework crystal material
  • Ternary rare-earth organic framework crystal material as well as synthesis method and application of ternary rare-earth organic framework crystal material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] The preparation of embodiment 1 sample

[0076] At least one of europium source, terbium source and gadolinium source was added to 10 mL of water to make solution I; The number of moles of europium element + the number of moles of terbium element + the number of moles of gadolinium element) was added to 10mL of organic solvent to obtain solution II; the solution I and solution II were mixed evenly, and put into a closed hydrothermal kettle. After keeping for a certain period of time, the obtained solid is centrifuged and vacuum-dried to obtain the crystal material. The obtained samples have good stability in air and organic solvents. The obtained samples were subjected to elemental analysis to obtain the corresponding x value and y value of each sample in formula I.

[0077] The relationship between the serial number of the obtained crystal material and the added amount of europium source, terbium source and gadolinium source, the type of organic solvent used, holding...

Embodiment 2

[0080] Embodiment 2 fluorescence test

[0081] Gained sample 1-1 to embodiment 1 # ~1-3 # , 2-1 # ~2-5 # , 3-1 # ~3-4 # and pure ligand H 4 L was tested for fluorescence.

[0082] Sample 1-1 # ~1-3 # and pure ligand H 4 The result of L is as follows:

[0083] pure ligand H 4 L exhibits a broad peak emission from 370-475 nm at an excitation wavelength of 341 nm, with the peak centered at 412 nm. Sample 1-1# The test results are as figure 2 As shown, under the excitation light of 335nm, Me 2 NH 2 ·EuL(H 2 O) 4 Shows Eu characteristic luminescence at 587nm, 610nm, 652nm, 696nm, corresponding to Eu ions 5 D. 0 → 7 f J (J=1-4) energy level transition; the emission peak of ligand L is very weak. Sample 1-2 # The test results are as image 3 As shown, under the excitation light of 335nm, Me 2 NH 2 ·TbL(H 2 O) 4 Shows the characteristic luminescence of terbium ions at 489nm, 542nm, 584nm, and 620nm, corresponding to terbium ions 5 D. 4 → 7 f J (J=6-3) e...

Embodiment 3

[0093] Embodiment 3 sample structure analysis and thermal stability experiment

[0094] For sample 1-1 # ~1-3 # , 2-1 # ~2-5 # , 3-1 # ~3-4 # The X-ray powder diffraction tests were carried out, and the crystallographic data were obtained by powder fitting method.

[0095] Sample 1-1 # ~1-3 # Comparison of the X-ray powder diffraction pattern and the XRD pattern obtained according to the fitting data Figure 18 shown. Sample 1-1 # ~1-3 # The fitting results are shown in Table 2. Sample 1-1 # The bond length and bond angle data in are shown in Table 3; samples 1-2 # The bond length and bond angle data in are shown in Table 4; samples 1-3 # The bond length and angle data in are shown in Table 5.

[0096] Depend on Figure 18 As can be seen from Table 2, the fitting XRD spectrum obtained according to the fitting data is consistent with the actual detection results, R 1 and wR 2 The (reflection) data is small, indicating that the fitting result is accurate.

[0...

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Abstract

The invention relates to a ternary rare-earth organic framework crystal material. A chemical formula of the ternary rare-earth organic framework crystal material is [Me2NH2][EuxTbyGd1-x-yL(H2O)4], wherein x is more than 0 and less than or equal to 0.05 and y is more than 0 and less than or equal to 0.1; Me represents methyl, L represents an organic ligand formed by pyridine-2,6-isophthalic acid; a crystal belongs to an orthorhombic crystal system and a space group is Pnma; the crystal belongs to the orthorhombic crystal system and the pace group is Pnma; the lattice parameters are as follows: a=8.500 to 8.506 angstroms, b=17.28 to 17.35 angstroms, c=12.05 to 12.15 angstroms, alpha=90, beta=90, gamma=90 and Z=4. The ternary rare-earth organic framework crystal material provided by the invention has very high heat stability and air stability; under the stimulation of ultraviolet light, characteristic emission of europium ions and terbium ions can be emitted simultaneously; the ternary rare-earth organic framework crystal material has very good linear response on temperature at the ratio of 77K to 450K, so that the ternary rare-earth organic framework crystal material can be used for temperature detection in a wide range.

Description

technical field [0001] A ternary rare earth organic framework crystal material, its synthesis method and application in temperature detection belong to the field of crystal materials. Background technique [0002] Metal-organic frameworks (MOFs) are a new type of porous crystalline material formed by the coordination of metal ions or metal clusters and organic bridging ligands. Metal-organic framework materials have special topology, regularity of internal arrangement, and specific size and shape of pores, but the framework materials show greater structural variability, tunable characteristics, and richer physical and chemical properties. In luminescent metal-organic framework materials, not only inorganic metal ions and organic ligands can provide luminescent properties, but also guest molecules or ions assembled in the pores of the framework materials can also produce luminescence. The site configuration, crystal structure and its interaction with guest molecules in the c...

Claims

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Application Information

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IPC IPC(8): C08G83/00C09K11/06G01K11/20
CPCC08G83/008C09K11/06C09K2211/1425C09K2211/1466C09K2211/182G01K11/20
Inventor 陈莲杨燕余沐昕江飞龙洪茂椿
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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