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Method for preparing NaYF4 type up-conversion materials

A conversion material and basic technology, applied in the field of manufacturing up-conversion luminescent materials, can solve the problems of high technical requirements, complex synthesis components, and difficult to imitate, and achieve the effects of simple preparation process, good reproducibility and low cost

Inactive Publication Date: 2009-11-11
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the currently widely used UV-excited and luminescent marking materials, infrared up-conversion marking materials have complex synthetic components, high technical requirements, and are difficult to imitate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0028] The invention provides a method for preparing NaYF 4 :Er x , Yb y (Among them, 0.0014 :Er x , Yb y (Where 0.001

[0029] The preparation method of the present invention includes the following steps:

[0030] 1) A step of preparing a basic solution, that is, a step of obtaining a NaF aqueous solution containing metal ions of Y, Yb, and Er.

[0031] Add NaF and inorganic salts containing Y, Yb, and Er into water, and stir to obtain a NaF aqueous solution containing Y, Yb, and Er metal ions (referred to as "basic solution" in this article), where NaF is in the aqueous solution. The concentration is 0.02-2 mol / L, and relative to 1 mol of NaF, the molar ratios of the metal ions of Y, Yb and Er are in the range of 0.5-1, 0.01-0.5, and 0.001-0.1, respectively.

[0032] For the inorganic salt containing Y, Yb or Er, one or more of nitrate, sulfate, chloride, etc. can be selected, and nitrate is preferred. These inorganic salts and NaF...

Embodiment 1

[0043] Mix 3.3644g (0.0495mol) of yttrium oxide, 0.7882g (0.01mol) of ytterbium oxide and 0.0382g (0.005mol) of erbium oxide into a slurry with distilled water. While heating, add 14mol / L concentrated nitric acid to dissolve until it becomes colorless Transparent solution. 1.6796 (0.1 mol) sodium fluoride was added to 50 mL of deionized water, and electromagnetically stirred until completely dissolved. Add the rare earth metal ion solution to the NaF solution and continue to stir to obtain a mixed solution, add 0.8 g (0.004 mol) polyethylene glycol (PEG200), stir at constant temperature for 10 minutes, and then add 0.3843 g (0.002 mol) of citric acid to obtain a white mixed solution. After 10 minutes, add 48.048g (0.8mol) of urea and continue to stir. After stirring for 10 minutes at constant temperature, add 0.6184g (0.025mol) of boric acid powder, continue stirring for 10 minutes, and then move it into a 50℃ constant temperature water bath to react for 2 hours. Take out 10mL and...

Embodiment 2

[0045] Mix 3.3644g (0.0495mol) of yttrium oxide, 0.7882g (0.01mol) of ytterbium oxide and 0.0382g (0.005mol) of erbium oxide into a slurry with distilled water. While heating, add 14mol / L concentrated nitric acid to dissolve until it becomes colorless Transparent solution. 1.6796 g (0.1 mol) of sodium fluoride was added to 50 mL of deionized water, and electromagnetically stirred until completely dissolved. Add the rare earth ion solution to the NaF solution and continue to stir to obtain a mixed solution, add 0.8 g (0.004 mol) of polyethylene glycol (PEG200), stir at constant temperature for 10 minutes, and then add 0.3843 g (0.002 mol) of citric acid to obtain a white mixed solution. After 10 minutes, add 60.056g (0.8mol) glycine and continue to stir. After stirring at constant temperature for 10 minutes, add 0.6184g (0.025mol) of boric acid powder, continue stirring for 10 minutes, then move to 50℃ constant temperature water bath to react for 2 hours, take out 10mL and load int...

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Abstract

The invention provides a method for preparing NaYF4 type up-conversion materials, which comprises: a step of adding NaF and inorganic salts which respectively contain Y, Yb and Er into water to obtain a uniform basic solution, a step of adding an incendiary agent into the basic solution to obtain uniform mixed liquid, and a step of placing the mixed liquid into a crucible for microwave heating to generate combusting foaming reaction, thereby obtaining the up-conversion materials.

Description

Technical field [0001] The present invention relates to a method for manufacturing an up-conversion luminescent material, in particular to a method for manufacturing a composite fluoride up-conversion material activated by rare earth ions. Background technique [0002] Among the photoluminescent materials, up-conversion materials refer to materials that can emit fluorescence with a shorter wavelength than the excitation wavelength when excited by light, that is, absorb low-frequency light and emit high-frequency light, so it is called frequency up-conversion. As an up-conversion luminescent material, since the excited infrared light source is invisible to the human eye, this type of material has a basic anti-counterfeiting function. Compared with currently widely used UV-excited and luminescent marking materials, infrared up-conversion marking materials have complex synthetic components, high technical requirements, and are difficult to imitate. Therefore, the use of high-efficie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85
Inventor 孙家跃杜海燕杨志萍周威
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY