A kind of oxyfluoride red up-conversion material and preparation method thereof

A conversion material, oxyfluoride technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of inconvenient large-scale production, harsh preparation conditions, low color purity, etc., achieve good up-conversion performance, simple preparation method, Chemically stable effect

Inactive Publication Date: 2016-01-13
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the development of up-conversion materials, the luminous efficiency of green up-conversion materials is relatively high, while red up-conversion materials not only have fewer varieties, but also have low efficiency and low color purity.
[0005] Chinese patent CN101195747A discloses a red up-conversion phosphor NaY prepared under hydrothermal conditions of 180-220°C 1-x-y-z (Yb x Ho y Ce z ) F 4 method, the hydrothermal method used has a long production cycle and high safety management requirements, so the production cost is high, and the red light emission is enhanced through the quenching effect of Ce, which will cause the overall luminous intensity to decrease
[0006] Chinese patent CN101457143A discloses a method for preparing red up-conversion phosphors by combustion method, which is not convenient for large-scale production and seriously pollutes the environment
[0007] To sum up, the existing preparation technology of red up-conversion luminescent materials, or the preparation conditions are relatively harsh, or the production cost is high, or the environmental pollution is serious, or it is not easy to produce on a large scale, and new formulations and process technologies are urgently needed way

Method used

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  • A kind of oxyfluoride red up-conversion material and preparation method thereof
  • A kind of oxyfluoride red up-conversion material and preparation method thereof
  • A kind of oxyfluoride red up-conversion material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Put 4.7309g YCl 3 ·6H 2 O, 1.55gYbCl 3 ·6H 2 O, 0.1527gErCl 3 ·6H 2 Dissolve O in 50g of deionized water, stir to fully dissolve it, and obtain a transparent mixed solution of Y, Yb and Er;

[0040] (2) Dissolve 2.3718 g of solid ammonium bicarbonate in 30 g of deionized water to obtain a transparent ammonium bicarbonate solution;

[0041] (3) Under stirring conditions, add ammonium bicarbonate solution to the mixed solution of Y, Yb and Er, aging for 1 hour, and slowly react to obtain a slurry;

[0042] (4) Filter the slurry obtained above, collect the precipitate, wash the precipitate with deionized water 2 to 3 times, and dry it at 80°C for 10 hours to obtain a white powder;

[0043] (5) The white powder is calcined in a muffle furnace at a calcining temperature of 1200°C and a calcining time of 3h to obtain a white solid;

[0044] (6) Mix and grind the white solid with 0.0415 g of lithium fluoride and 1.1408 g of ammonium bifluoride to obtain a precursor;

[0045] (7) Plac...

Embodiment 2

[0049] (1) Add 2.9113g YCl 3 ·6H 2 O, 3.8749gYbCl 3 ·6H 2 O, 0.1527gErCl 3 ·6H 2 Dissolve O in 50g of deionized water, stir to fully dissolve it, and obtain a transparent mixed solution of Y, Yb and Er;

[0050] (2) Dissolve 2.8824 g of solid ammonium carbonate in 30 g of deionized water to obtain a transparent ammonium carbonate solution;

[0051] (3) Under stirring conditions, add the ammonium carbonate solution to the mixed solution of Y, Yb and Er, age for 1 hour, and slowly react to obtain a slurry;

[0052] (4) Filter the slurry obtained above, collect the precipitate, wash the precipitate with ethanol 2 to 3 times, and dry it at 80°C for 10 hours to obtain a white powder;

[0053] (5) The white powder is calcined in a muffle furnace, the calcining temperature is 1100℃, and the calcining time is 3h to obtain a white solid;

[0054] (6) Mix and grind the white solid with 0.0415g lithium fluoride and 1.4816g ammonium fluoride to obtain a precursor;

[0055] (7) Place the precursor in...

Embodiment 3

[0058] (1) Put 5.398g of YCl 3 ·6H 2 O, 0.775gYbCl 3 ·6H 2 O, 0.0763gErCl 3 ·6H 2 Dissolve O in 50g of deionized water, stir to fully dissolve it, and obtain a transparent mixed solution of Y, Yb and Er;

[0059] (2) Dissolve 2.3718 g of solid ammonium bicarbonate in 30 g of deionized water to obtain a transparent ammonium bicarbonate solution;

[0060] (3) Under stirring conditions, add ammonium bicarbonate solution to the mixed solution of Y, Yb and Er, aging for 1 hour, and slowly react to obtain a slurry;

[0061] (4) Filter the slurry obtained above, collect the precipitate, wash the precipitate with deionized water 2 to 3 times, and dry it at 100°C for 8 hours to obtain a white powder;

[0062] (5) The white powder is calcined in a muffle furnace, the calcining temperature is 1000℃, and the calcining time is 4h to obtain a white solid;

[0063] (6) Mix and grind the white solid with 0.0415g lithium fluoride and 0.5704g ammonium bifluoride to obtain a precursor;

[0064] (7) Place t...

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Abstract

The invention relates to a red up-conversion material of oxyfluoride and a preparation method thereof. The molecular formula of the red up-conversion material of oxyfluoride is Y(5-x-y)YbxEryO4F7, wherein 0.5<=x<=2.5, and 0.05<=y<=0.25; lithium-containing compounds such as Li2CO3 and LiF are used as a fluxing agent and a spectrum regulator. The red up-conversion material of oxyfluoride provided by the invention has the advantages of stable performance, high strength, pure chroma and the like; under the 980nm laser excitation, the material can realize red up-conversion luminescence and make up for the shortcomings of few colors and varieties of the up-conversion luminous material, thereby having a good application prospect in the fields of three-dimensional display, anti-counterfeiting, medicine, high-density data storage and the like; moreover, the preparation process is finished in an air atmosphere without needing special atmosphere protection, thereby greatly reducing the production difficulty and cost and being suitable for large-scale production.

Description

Technical field [0001] The invention relates to an oxyfluoride red upconversion material and a preparation method thereof. Background technique [0002] The red upconversion material is a fluorescent material that can convert near-infrared light into visible light. Its characteristic is that the emitted photon energy is greater than the absorbed photon energy, which is an anti-Stokes phenomenon. The red upper conversion material is widely used, mainly in the fields of three-dimensional display, anti-counterfeiting, medicine, and high-density data storage. [0003] Among the rare earth ions, Er 3+ Because it can be effectively excited by 808nm and 980nm infrared light, it is often used as the emission center in up-conversion luminescent materials. And Yb 3+ It can effectively increase the absorption area of ​​980nm infrared light by the up-conversion luminescent material and improve the efficiency of up-conversion. It is an ideal sensitizer. In the selection of up-conversion matri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/86
Inventor 阳效良周碧遥向志锋刘小海文晴肖思国
Owner XIANGTAN UNIV
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