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Binary rare earth organic framework crystal material, as well as synthesis method and application thereof

A crystalline material, rare earth organic technology, applied in organic chemistry methods, luminescent materials, organic chemistry, etc., can solve the problems of poor thermal stability and solvent stability, instability, application limitations, etc., and achieve high air stability and response speed. Fast, strong anti-interference ability

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

[0005] There have been some reports on the use of double rare earth-organic framework materials for temperature detection, but the more commonly used double rare earth ratio thermometers are not sensitive in the normal temperature region and high temperature region, so that their application is limited to the temperature range of room temperature and below
On the other hand, metal-organic frameworks are usually unstable in air due to their poor thermal and solvent stability, which also limits their applications.

Method used

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  • Binary rare earth organic framework crystal material, as well as synthesis method and application thereof
  • Binary rare earth organic framework crystal material, as well as synthesis method and application thereof
  • Binary rare earth organic framework crystal material, as well as synthesis method and application thereof

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Effect test

Embodiment 1

[0072] The preparation of embodiment 1 sample

[0073] 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.

[0074] 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

[0077] Embodiment 2 fluorescence test

[0078] 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.

[0079] Sample 1-1 # ~1-3 # and pure ligand H 4 The result of L is as follows:

[0080] 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) 4Shows 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) ...

Embodiment 3

[0090] Embodiment 3 sample structure analysis and thermal stability experiment

[0091] 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.

[0092] 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.

[0093] 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 provides a binary rare earth organic framework crystal material. The chemical formula of the binary rare earth organic framework crystal material is [Me2NH2][EuxTb1-xL(H2O)4], wherein x is greater than 0 and less than or equal to 5; Me represents methyl; L represents an organic ligand formed by pyridine-2,6 m-phthalic acid; crystals belong to an orthorhombic system, the space group is Pnma, and the cell parameters are as follows: a=8.500 to 8.506 Angstrom, b=17.28 to 17.35 Angstrom, and c=12.05 to 12.15 Angstrom; alpha is equal to 90, beta is equal to 90, gamma is equal to 90, and Z is equal to 4. The binary rare earth organic framework crystal material is extremely high in heat stability and air stability, and can be used for temperature detection within a wide range of 77K to 450K; the temperature range covers a low temperature region, a physiological temperature region and a high temperature region, and is the widest detection temperature range which can be realized at the present.

Description

technical field [0001] A binary rare earth organic framework crystal material, its synthesis method and its application in temperature detection belong to the field of crystal materials. Background technique [0002] Temperature is a very important physical parameter in the fields of scientific research and industrial applications, and temperature detectors are one of the most frequently used sensors in modern testing and industrial process control. Various instruments and materials have been designed and invented for temperature detection. Fluorescent temperature sensors are mainly based on the dependence of fluorescence intensity or lifetime on temperature. Compared with traditional sensing technologies, fluorescent temperature detection has the advantages of anti-electromagnetic interference, high-voltage insulation, stability and reliability, high precision, high sensitivity, tiny size, long life and Corrosion resistance, good adaptability and so on. [0003] Metal-org...

Claims

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Application Information

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IPC IPC(8): C07F5/00C09K9/02C09K11/06G01K11/20
CPCC07B2200/13C07F5/003C09K9/02C09K11/06C09K2211/182G01K11/20
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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