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Zn reinforced rare earth sulfur oxide up-conversion luminescent material and preparation method thereof

A rare earth oxysulfide, luminescent material technology, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of reducing the symmetry of crystal structure and phonon energy, uneven particle size, weak luminous intensity, etc., to reduce symmetry Effects of sex and phonon energy, simple reaction conditions, enhanced luminous intensity

Active Publication Date: 2016-05-25
防城港市唐氏食品有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The first object of the present invention is to provide a Zn-enhanced rare earth oxysulfide up-conversion luminescent material to solve the problem of weak luminous intensity of existing rare-earth oxysulfide up-conversion luminescent materials. The Zn-enhanced rare earth oxysulfide Up-conversion luminescent material, because Zn doping optimizes the crystal structure of rare earth oxysulfide, reduces crystal structure symmetry and phonon energy, and greatly enhances luminous intensity by 50% to 120%.
[0006] The second object of the present invention is to provide a preparation method of the Zn-enhanced rare earth oxysulfide up-conversion luminescent material, which uses the method of precipitant reverse dripping to prepare rare earth oxide raw materials, so as to solve the problem of existing purchase of rare earth Oxide raw materials have uneven particle size and serious agglomeration problems. The prepared rare earth oxide raw materials have the advantages of spherical particles, uniform particle size, good dispersion, no need for ball milling, and can be used directly.

Method used

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  • Zn reinforced rare earth sulfur oxide up-conversion luminescent material and preparation method thereof
  • Zn reinforced rare earth sulfur oxide up-conversion luminescent material and preparation method thereof
  • Zn reinforced rare earth sulfur oxide up-conversion luminescent material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0047] A Zn-enhanced rare earth oxysulfide up-conversion luminescent material, its chemical formula is (La 0.8175 Yb 0.16 Ho 0.0075 Zn 0.015 ) 2 o 2 S.

[0048] The preparation method of the rare earth sulfur oxide up-conversion luminescent material comprises the following steps:

[0049] S11, according to the chemical formula (La 0.8175 Yb 0.16 Ho 0.0075 Zn 0.015 ) 2 o 2 S, weigh the required raw material 20.171gLa (NO 3 ) 3 ·6H 2 O, 4.095gYb (NO 3 ) 3 ·5H 2 O, 0.187gHo(NO 3 ) 3 ·5H 2 O and 0.254gZn(NO 3 ) 2 ·6H 2 O, above-mentioned raw material is dissolved, is mixed with nitrate solution; According to the amount of raw material, takes by weighing 7.902g oxalic acid, and is mixed with oxalic acid solution;

[0050] S12. Drop the nitrate solution described in step S11 into the precipitant solution, and stir; after the titration, continue to stir, and seal the titrated solution, leave it to age, and filter;

[0051] S13. Wash and dry the precipitate fil...

Embodiment 2

[0054] A Zn-enhanced rare earth oxysulfide up-conversion luminescent material, its chemical formula is (La 0.775 Yb 0.2 Er 0.005 Zn 0.02 ) 2 o 2 S.

[0055] The preparation method of the rare earth sulfur oxide up-conversion luminescent material comprises the following steps:

[0056] S21, according to the chemical formula (La 0.775 Yb 0.2 Er 0.005 Zn 0.02 ) 2 o 2 S, weigh the required raw material 19.020gLa (NO 3 ) 3 ·6H 2 O, 5.091gYb (NO 3 ) 3 ·5H 2 O, 0.126gEr(NO 3 ) 3 ·5H 2 O and 0.337gZn(NO 3 ) 2 ·6H 2 O, above-mentioned raw material is dissolved, is mixed with nitrate solution; According to the amount of raw material, takes by weighing 7.145g oxalic acid, and is mixed with oxalic acid solution;

[0057] S22. Drop the nitrate solution described in step S21 into the oxalic acid solution, and stir; after the titration, continue to stir for 0.5 hours, seal the titrated solution, leave it to age for 10 hours, and filter;

[0058] S23. Wash the filtered...

Embodiment 3

[0061] A Zn-enhanced rare earth oxysulfide up-conversion luminescent material, its chemical formula is (La 0.8175 Yb 0.16 Ho 0.0075 Zn 0.015 ) 2 o 2 S.

[0062] The preparation method of the rare earth sulfur oxide up-conversion luminescent material comprises the following steps:

[0063] S31, according to the chemical formula (La 0.8175 Yb 0.16 Ho 0.0075 Zn 0.015 ) 2 o 2 S, weigh the required raw material 20.171gLa (NO 3 ) 3 ·6H 2 O, 4.095gYb (NO 3 ) 3 ·5H 2 O, 0.187gHo(NO 3 ) 3 ·5H 2 O and 0.254gZn(NO 3 ) 2 ·6H 2 O, above-mentioned raw material is dissolved, is mixed with nitrate solution; According to the amount of raw material, takes by weighing 7.902g oxalic acid, and is mixed with oxalic acid solution;

[0064] S32, drop the nitrate solution described in step S31 into the oxalic acid solution, and stir; after the titration, continue to stir for 1 hour, and seal the titrated solution, leave it to age for 12 hours, and filter;

[0065] S33. Wash the...

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Abstract

The invention provides a Zn reinforced rare earth sulfur oxide up-conversion luminescent material and a preparation method thereof. The chemical formula of the material is (Ln1-x-y-zYbxREyZnz)2O2S, wherein the x is greater than or equal to 0.04 and is smaller than or equal to 0.2, the y is greater than or equal to 0.005 and is smaller than or equal to 0.02, the z greater than or equal to 0.005 and is smaller than or equal to 0.02, the Ln is one of La, Y and Gd, and the RE is one of Er, Ho, Tm, Pr, Eu and Tb. The luminous intensity of the material is greatly improved and is improved by 50%-120%. The preparation method of the material adopts a precipitator return-titration method to obtain rare earth oxide raw materials and then adopts a gas sulfidization method, the reaction conditions are simple and easy to control, the method can well keep the morphology and particle size of rare earth oxides, most of the rare earth sulfur oxide up-conversion luminescent materials prepared by means of the method are spherical, uniform in particle size and relatively smaller in particle size distribution range, and D90 is equal to 0.2-0.5 microns.

Description

technical field [0001] The invention relates to the field of fine chemical industry, in particular to a Zn-enhanced rare earth sulfur oxide up-conversion luminescent material and a preparation method. Background technique [0002] In recent years, the improvement of the output power of near-infrared semiconductor laser diodes has provided an effective excitation pump source for up-conversion luminescent materials, and promoted the large-scale development of up-conversion luminescent materials. Infrared detection technology, anti-counterfeiting technology, biomolecular fluorescent labeling and solar cells have been applied in actual or potential fields. The host material is the main component of the up-conversion luminescent material, and its physical and chemical properties largely determine the overall performance of the up-conversion luminescent material. Due to its good thermal and chemical stability, sulfur oxide has a band gap of 4.6-4.8eV, which is suitable for doping...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/84
CPCC09K11/7771
Inventor 韩朋德姜晓萍程森于方丽焦宝祥吴其胜张其土
Owner 防城港市唐氏食品有限公司
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