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Method for preparing up-conversion fluorescent matrix material NaYF4 nano crystal

A technology of matrix materials and nanocrystals, which is applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems of large particle size of nanoparticles, and achieve the effects of stable product quality, simple process and equipment, and good repeatability

Inactive Publication Date: 2007-03-28
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1157462C discloses a kind of preparation method that adopts aminocarboxyl complexing agent, but the particle size of the nanoparticle that this technology prepares is bigger, mainly distributes in 37-166 nanometer

Method used

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  • Method for preparing up-conversion fluorescent matrix material NaYF4 nano crystal
  • Method for preparing up-conversion fluorescent matrix material NaYF4 nano crystal
  • Method for preparing up-conversion fluorescent matrix material NaYF4 nano crystal

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Experimental program
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Effect test

Embodiment 1

[0023] a) Weigh 0.01 mol of yttrium oxide, add a sufficient amount of perchloric acid with a concentration of 0.1 mol / l and a pH value of 6, heat and dissolve to generate 0.02 mol of yttrium perchlorate, add deionized water to make up to 100ml , be made into the yttrium perchlorate solution of 0.2mol / l, adjust its pH value to be 2;

[0024] b) preparing a 0.6mol / l trisodium citrate solution;

[0025] c) uniformly mixing the solutions of steps a) and b), wherein the molar ratio of yttrium perchlorate to trisodium citrate solution is 1:3;

[0026] d) Take another 2.1g of sodium fluoride solution, add deionized water, dissolve, adjust the pH value of the solution to 10, stir rapidly, add the solution obtained in step c) at room temperature, and age for 1 hour; the total rare earth ions and fluorine in the solution The molar ratio of sodium chloride was 1:1.2; centrifuged, washed three times with deionized water, washed once with absolute ethanol, and dried in a vacuum oven at 60...

Embodiment 2

[0028] a) Weigh 0.01mol of yttrium oxide, add a sufficient amount of hydrochloric acid with a concentration of 0.5mol / l and a pH value of 0, heat and dissolve to generate 0.02mol of yttrium chloride, add deionized water to make the volume to 100ml, and prepare into a 0.2 mol / l yttrium chloride solution, and adjust its pH to 0.

[0029] b) Prepare 0.2 mol / l trisodium citrate solution.

[0030] c) uniformly mixing the solutions of a) and b), wherein the molar ratio of trisodium citrate solution to yttrium chloride is 1:1.

[0031] d) Weigh another 2.1 g of sodium fluoride solution, add 60 ml of deionized water, dissolve, adjust the pH value of the solution to 10, stir rapidly, add to the solution obtained in step c) at 45 ° C, and age at room temperature for 5 hours; The molar ratio of total rare earth ions to sodium fluoride was 1:30; centrifuged, washed three times with deionized water and once with absolute ethanol, and dried in a vacuum oven at 30°C.

Embodiment 3

[0033] a) Weigh 0.01 mol of yttrium oxide, add a sufficient amount of perchloric acid with a concentration of 0.3 mol / l and a pH value of 4, heat and dissolve to generate 0.02 mol of yttrium perchlorate, add deionized water to dilute to 100 ml , be made into 0.2mol / l yttrium perchlorate solution, and adjust its pH value to 6.

[0034] b) Prepare 1 mol / l trisodium citrate solution.

[0035] c) Step a) is mixed with the solution of b), wherein the molar ratio of trisodium citrate solution to yttrium perchlorate is 1:5.

[0036] d) Separately weigh 2.1 g of sodium fluoride solution, add 60 ml of deionized water, dissolve, and adjust the pH value of the solution to 10. Stir quickly, add to the solution obtained in step c) at 0°C, and age at room temperature for 3 hours; the molar ratio of total rare earth ions to sodium fluoride in the solution is 1:10; centrifuge, wash with deionized water 3 times, and dry Wash once with ethanol and dry in a vacuum oven at 80°C.

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Abstract

The invention discloses supra transition luminescence substrate material NaYF4 nanometer crystal preparing method. It includes the following steps: (1) dissolving rare earth yttrium oxide in perchloric acid or hydrochloric acid with 0.1-0.5mol / l density and 0-6 pH to produce perchloric acid yttrium or yttrium chloride solution; (2) preparing hydroxyl carboxyl series complexing agent with 0.2-1.0mol / l density, mixing it with the (1) solution, adjusting the pH at 0-6; the mol ratio of the perchlorate or hydrochloride and hydroxyl carboxyl series complexing agent is 1:1-5; (3) preparing sodium fluoride aqueous solution with 0.02-1mol / l density and 10 pH, adding the (2) solution at 0-45 degree centigrade, aging for 1-5h; the mol ratio of the sodium fluoride and the total rare earth ion is 1:1.2-30; (4) separating precipitate, washing, drying to gain nanometer NaYF4 particle. The produced NaYF4 particle has the advantages of controllable size with 10-25 nanometer, simple technology and device, good product quality and repeatability.

Description

technical field [0001] The present invention relates to a kind of preparation method of nanometer up-conversion fluorescent host material, relate to nanometer up-conversion fluorescent host material NaYF more precisely 4 The preparation technology of nano crystal belongs to the field of preparation technology of nano fluorescent material. Background technique [0002] Up-conversion fluorescent materials are a kind of luminescent materials that can emit short-wavelength light under the excitation of long-wavelength light. Cooperating with infrared light-emitting diodes or semiconductor infrared lasers, such materials can be made into light-emitting diodes or lasers of different colors (Opt Lett 1997; 22:808-810.). In recent years, the use of up-conversion fluorescent materials as fluorescent labeling materials for biomolecules has attracted widespread attention. This type of material is used as a fluorescent material probe with low interference and high detection sensitivity...

Claims

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Application Information

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IPC IPC(8): C09K11/85
Inventor 周兴平李珊珊倪似愚陈小立朱泉
Owner DONGHUA UNIV
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