Dual-rare-earth-metal organic frame material used in temperature detection and preparation method of dual-rare-earth-metal organic frame material

A metal-organic framework and double rare earth technology, applied in thermometers, luminescent materials, organic chemistry, etc., can solve the problems of narrow temperature sensitive range and low sensitivity, and achieve high sensitivity, high luminous efficiency, and simple preparation process.

Inactive Publication Date: 2013-09-25
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the application of metal-organic frameworks in fluorescent temperature sensors is quite rare, and there is a narrow range of temperature sensitivity and low sensitivity (less than 0.9% K -1 ) and other shortcomings

Method used

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  • Dual-rare-earth-metal organic frame material used in temperature detection and preparation method of dual-rare-earth-metal organic frame material
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  • Dual-rare-earth-metal organic frame material used in temperature detection and preparation method of dual-rare-earth-metal organic frame material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The organic ligand containing pyridinecarboxylic acid group is 5-(pyridin-4-yl)-isophthalic acid, x is 0.1, n is 2.0, and the synthetic route is as follows:

[0019] (1) Mix 0.3mmol of europium nitrate and terbium nitrate (molar ratio Eu 3+ :Tb 3+ =1:9) was added to 10mL of water to make a rare earth brine solution;

[0020] (2) Add 0.3 mmol of 5-(pyridin-4-yl)-isophthalic acid to 50 mL of water to make an aqueous solution of organic ligands;

[0021] (3) The above two solutions were mixed, then placed in a closed hydrothermal kettle, and reacted at a constant temperature of 160°C for 2 days to obtain a double rare earth metal organic framework material with a yield of 65%.

[0022] The obtained double rare earth metal organic framework material is a colorless transparent crystal with a crystal size of 0.5-2mm, and has good stability in most organic solvents and water, and its main luminescence peaks are located at 546 and 615nm, respectively. The ratio of intensity ...

Embodiment 2

[0026] The organic ligand containing pyridinecarboxylic acid group is 5-(pyridin-3-yl)-isophthalic acid, x is 0.1, n is 2.0, and the synthetic route is as follows:

[0027] (1) Mix 0.3mmol of europium nitrate and terbium nitrate (molar ratio Eu 3+ :Tb 3+ =1:9) into 30mL of DMF solution;

[0028] (2) Dissolve 0.3mmol of 5-(pyridin-3-yl)-isophthalic acid in 30mL of DMF solution;

[0029] (3) The above two solutions were mixed, then put into a sealed strain bottle, and reacted at a constant temperature of 100°C for 3 days to obtain a double rare earth metal organic framework material with a yield of 72%.

[0030] The obtained double rare earth metal-organic framework material is a colorless transparent crystal with a crystal size of 0.2-1.5mm and has good stability in most organic solvents. Its main luminescence peaks are located at 546 and 615nm, respectively. The ratio of the peak intensity has a good linear relationship with the temperature. The double rare earth metal-orga...

Embodiment 3

[0032] The organic ligand containing pyridinecarboxylic acid group is 5-(pyridin-2-yl)-isophthalic acid, x is 0.2, n is 3.0, the synthetic route of double rare earth metal-organic framework material is as follows:

[0033] (1) Mix 0.3mmol of europium nitrate and terbium nitrate (molar ratio Eu 3+ :Tb 3+ =2:8) into 30mL ethanol solution;

[0034] (2) Add 0.3mmol of 5-(pyridin-2-yl)-isophthalic acid to 30mL of ethanol solution;

[0035] (3) The above two solutions were mixed, then put into a closed hydrothermal kettle, and reacted at a constant temperature of 150°C for 3 days to obtain a double rare earth metal organic framework material with a yield of 82%.

[0036] The obtained double rare earth metal-organic framework material is a colorless transparent crystal with a crystal size of 0.3-1.5mm and has good stability in most organic solvents. Its main luminescence peaks are located at 546 and 615nm, respectively. The ratio of the peak intensity has a good linear relationshi...

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Abstract

The invention relates to a dual-rare-earth-metal organic frame material used in temperature detection and a preparation method of the dual-rare-earth-metal organic frame material. The dual-rare-earth-metal organic frame material has a structure general formula (Tb1-xEux)Ln, wherein L is an organic ligand containing a pyridine carboxylic acid group, x is more than 0 or not more than 0.5, and n is equal to 1-4. The dual-rare-earth-metal organic frame material is prepared through a hydrothermal or solvothermal reaction. The dual-rare-earth-metal organic frame material is simple in preparation process, high in yield and good in stability. The dual-rare-earth-metal organic frame material simultaneously has characteristic light-emitting peaks of rare earths of europium and terbium, is capable of realizing self-calibrating temperature detection because a good linear relation exists between a strength ratio of the two peaks and the temperature, and is high in sensitivity reaching 3.53.K<-1>; the dual-rare-earth-metal organic frame material to be expected as a novel temperature sensing material is practically applied to the field of low-temperature detection because the light-emitting color within a temperature range of 14-300K changes with the change of the temperature.

Description

technical field [0001] The invention relates to a double rare earth metal organic framework material for temperature detection and a preparation method thereof. Background technique [0002] Temperature is a very important physical parameter in the field of scientific research and industrial application. At present, various temperature sensors have been invented to detect temperature, such as traditional thermocouples, thermal resistances and radiation thermometers. Most of these temperature sensors can only be used in traditional occasions, and cannot meet the requirements of many fields, especially high-tech fields, such as temperature detection in extremely low temperature areas. Compared with traditional temperature sensors, fluorescent temperature sensors are mainly based on the dependence of fluorescence intensity or lifetime on temperature. Good sex and other characteristics. Therefore, the research and development of fluorescent temperature sensor has been paid mor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00C09K11/06G01K11/16
Inventor 钱国栋饶兴堂崔元靖杨雨宋涛
Owner ZHEJIANG UNIV
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