Nano-class conversion fluorescence material on fluoride matrix and its preparing process

A fluorescent material and fluoride technology, applied in the field of nano fluorescent materials and their preparation, can solve the problems of high calcination temperature and small particle size range, and achieve the effects of low calcination temperature, uniform particle size and high repeatability

Inactive Publication Date: 2002-10-30
CAPITALBIO CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantage is that the controllable particle size range is small (50-60 nanometers), and the temperature required for calcination is high

Method used

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  • Nano-class conversion fluorescence material on fluoride matrix and its preparing process
  • Nano-class conversion fluorescence material on fluoride matrix and its preparing process
  • Nano-class conversion fluorescence material on fluoride matrix and its preparing process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Weigh 11.2905 grams of yttrium oxide, add enough hydrochloric acid (or nitric acid), heat to dissolve and evaporate to dryness. Add 500 ml of deionized water to dissolve, and the concentration of yttrium ions in the solution is 0.2 mol.L-1 at this time, which can be stored as a stock solution for a long time. Same as above, respectively weigh 18.125 g of gadolinium oxide, 16.3 g of lanthanum oxide, 19.7 g of ytterbium oxide, 19.1 g of erbium oxide, 19.3 g of thulium oxide, and 18.9 g of holmium oxide, each of which is made into 500 ml of 0.2 mol.L -1 stock solution. Take 16 milliliters of yttrium ion solution, 3.4 milliliters of ytterbium ion solution, and 0.6 milliliter of erbium ion solution in proportion, and place them in a 100 milliliter three-necked bottle. At this time, the molar ratio of rare earth ions in the solution is yttrium ion: ytterbium ion: erbium ion=80:17:3;

[0033] (2) In the above product, add 0.2 mol.L -1 20 ml of ethylenediaminetetraacetic...

Embodiment 2

[0038] (1) Take 17.4 milliliters of yttrium ion solution, 2.6 milliliters of ytterbium ion solution, and 0.02 milliliter of thulium ion solution in proportion, and place them in a 100 milliliter three-necked bottle. At this time, the molar ratio of rare earth ions in the solution is yttrium ion:ytterbium ion:thulium ion=87:13:0.1;

[0039] (2) In the above product, add 0.2mol.L -1 15 ml of ethylenediaminetetraacetic acid (EDTA) disodium salt solution;

[0040] (3) Weigh 2.1 g of sodium fluoride, add 65 ml of deionized water, and prepare an aqueous solution. At room temperature, under rapid stirring, the solution of step (2) was injected to form a precipitate, and the stirring reaction was continued for 1 hour;

[0041] (4) centrifugal separation and precipitation and washing with water three times, drying, and making a precursor;

[0042] (5) Putting the precursor into a high-temperature furnace and calcining at 400° C. for 4 hours to obtain a nano-scale up-conversion fluor...

Embodiment 3

[0044] (1) Take 16 milliliters of yttrium ion solution, 3.86 milliliters of ytterbium ion solution, and 0.04 milliliter of holmium ion solution in proportion, and place them in a 100 milliliter three-necked bottle. At this time, the molar ratio of rare earth ions in the solution is yttrium ion:ytterbium ion:holmium ion=80:19.8:0.2;

[0045] (2) In the above product, add 0.2mol.L -1 EDTA sodium salt 10 ml;

[0046] (3) Weigh 2.1 g of sodium fluoride, add 70 ml of deionized water, and prepare an aqueous solution. At room temperature, under rapid stirring, the above solution was injected to form a precipitate, and the stirring reaction was continued for 1 hour;

[0047] (4) centrifugal separation and precipitation and washing with water three times, drying, and making a precursor;

[0048] (5) Putting the precursor into a high-temperature furnace and calcining at 400° C. for 5 hours to obtain a nano-scale up-conversion fluorescent material with an average particle size of 77 n...

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Abstract

A nano-class conversion fluorescent material used for biomolecular fluorescent marker is prepared through dissolving yttrium (or lanthanum or gadolinium) oxide in acid to obtain solution A, adding aminocarboxylic comple, adding it to the solution of fluoride, centrifugal treating, drying to obtain precursor, and high-temp calcining. Its advantages are 37-166 nm of granularity, low calcining temp and strong fluorescence.

Description

technical field [0001] The invention belongs to a nanometer fluorescent material and a preparation process thereof, in particular to a nanometer up-conversion fluorescent material doped with rare earth ions using fluoride as a matrix and a preparation method thereof. Background technique [0002] Upconversion fluorescent material is a luminescent material that can emit visible light under the excitation of infrared light. Ytterbium and erbium co-doped fluoride is a highly efficient up-conversion fluorescent material, which emits strong green fluorescence and relatively weak red fluorescence under 946-970 nm infrared excitation (Yu Xianen, Practical Luminescent Materials. and Photoluminescence Mechanism, China Light Industry Press, 1997, Beijing). [0003] Due to its special properties, upconversion fluorescent materials can be used to prepare light-emitting diodes, solid-matrix visible light lasers, and highly sensitive biomolecular fluorescent labeling materials (Zarling, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85C09K11/08C09K11/77
CPCC09K11/7772C09K11/7773Y10S977/834Y10S977/83
Inventor 衣光舜孙宝全陈德朴周玉祥程京
Owner CAPITALBIO CORP
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