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A preparation method of rare earth ion doped yttrium fluoride green up-conversion fluorescent material

A technology of rare earth ions and fluorescent materials, applied in the field of preparation of rare earth doped luminescent materials, can solve the problems of harsh experimental technical conditions control, unfavorable large-scale industrial production, and difficult to guarantee purity, and achieves good up-conversion performance and equipment. The effect of low cost and stable product quality

Active Publication Date: 2016-07-06
FUZHOU UNIV
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  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the preparation methods of rare earth ion-doped yttrium fluoride fluorescent materials mainly include the following three types: 1. Solid-state reaction method, such as the technical scheme described in Chinese patent CN101746805B, powdery water and yttrium nitrate, powdery fluoride Mix the ammonium evenly, and grind it in a mortar for a solid phase reaction. After the reaction is complete, a jelly is obtained. Dry the jelly and grind it to obtain a powder. The powder is kept at 300~500°C for 3~ under the protection of an inert atmosphere. 6 hours, get nanoscale YF 3 , the advantage of the solid phase method is that the output of the prepared powder is relatively large, the synthesis process is simple, and the price is relatively low, but the solid phase method consumes a lot of energy during the preparation process, the final powder is relatively thick, the efficiency is relatively low, and the purity is not easy Guarantee; 2. Electrospinning method, which sprays and stretches liquid-phase polymers or melts in a high-voltage electrostatic environment to obtain very fine fibers. By this method, extremely long fibers can be obtained on the receiving screen. nanowire
As the technical scheme described in Chinese patent CN102817108B, first prepare PVP / [PVP+Y(NO 3 ) 3 +Tb(NO 3 ) 3 ] Composite coaxial fibers, followed by heat treatment to obtain Y 2 o 3 :5%Tb 3+ hollow nanofibers, followed by the double-crucible method, with ammonium bifluoride to Y 2 o 3 :5%Tb 3+ Hollow nanofibers were fluorinated to obtain YF 3 :5%Tb 3+ Green luminescent hollow nanofibers, this method has relatively high requirements for equipment, and the control of experimental technical conditions is also relatively harsh, and the preparation process is cumbersome; Compound ions are mixed with arginine and fluoride to form a mixed solution, and then the mixed solution is hydrothermally reacted at different temperatures and times to obtain a precursor, and then the precursor is heat-treated at different temperatures to obtain a hollow yttrium fluoride For luminescent balls, the hydrothermal method does not require high-temperature sintering, but the production cycle is long and the production cost is high, which is not conducive to large-scale industrial production
[0003] In summary, although there are many methods for preparing rare earth ion-doped yttrium fluoride fluorescent materials, there are many disadvantages in the production process. The preparation technology of rare earth doped luminescent materials with low cost and easy scale production is very meaningful

Method used

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  • A preparation method of rare earth ion doped yttrium fluoride green up-conversion fluorescent material
  • A preparation method of rare earth ion doped yttrium fluoride green up-conversion fluorescent material
  • A preparation method of rare earth ion doped yttrium fluoride green up-conversion fluorescent material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Weigh 0.306g solid powder yttrium acetate hexahydrate, 0.076g solid powder ytterbium acetate pentahydrate, and 0.013g solid powder erbium acetate pentahydrate;

[0031] 2) Measure 4ml of isopropanol, 4ml of ethanol, 1ml of trifluoroacetic acid, and 3ml of water, add solid powder into it, stir for 3 hours, and obtain transparent sol A;

[0032] 3) Transfer transparent sol A to a high-temperature-resistant crucible, and dry in an oven for 3 hours to obtain colloidal substance B;

[0033] 4) Put the colloidal substance B in a high-temperature furnace, raise the temperature of the furnace from room temperature to 300 °C at a rate of 4 °C / min, keep it for 1 hour, and take it out after cooling to room temperature with the furnace;

[0034] 5) Grinding to get YF 3 : Yb 3+ , Er 3+ powder.

Embodiment 2

[0036] 1) Weigh 0.306g solid powder yttrium acetate hexahydrate, 0.076g solid powder ytterbium acetate pentahydrate, and 0.013g solid powder erbium acetate pentahydrate;

[0037] 2) Measure 4ml of isopropanol, 4ml of ethanol, 1ml of trifluoroacetic acid, and 3ml of water, add solid powder into it, stir for 3 hours, and obtain transparent sol A;

[0038] 3) Transfer transparent sol A to a high-temperature-resistant crucible, and dry in an oven for 3 hours to obtain colloidal substance B;

[0039] 4) Put the colloidal substance B in a high-temperature furnace, raise the temperature of the furnace from room temperature to 400 °C at a rate of 4 °C / min, keep it warm for 1 hour, and take it out after cooling to room temperature with the furnace;

[0040] 5) Grinding to get YF 3 : Yb 3+ , Er 3+ powder.

Embodiment 3

[0042] 1) Weigh 0.306g solid powder yttrium acetate hexahydrate, 0.076g solid powder ytterbium acetate pentahydrate, and 0.013g solid powder erbium acetate pentahydrate;

[0043] 2) Measure 4ml of isopropanol, 4ml of ethanol, 1ml of trifluoroacetic acid, and 3ml of water, add solid powder into it, stir for 3 hours, and obtain transparent sol A;

[0044] 3) Transfer transparent sol A to a high-temperature-resistant crucible, and dry in an oven for 3 hours to obtain colloidal substance B;

[0045] 4) Put the colloidal substance B in a high-temperature furnace, raise the temperature of the furnace from room temperature to 500 °C at a rate of 4 °C / min, keep it warm for 1 hour, and take it out after cooling to room temperature with the furnace;

[0046] 5) Grinding to get YF 3 : Yb 3+ , Er 3+ powder.

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Abstract

The invention provides a preparation method of a rare-earth-ion-doped yttrium fluoride green upconversion fluorescent material, which has the advantages of simple preparation technique, low heat treatment temperature and high product purity and can implement large-scale production. The method comprises the following steps: adding rare-earth acetate into a mixed solvent composed of isopropanol, ethanol and water, adding trifluoroacetic acid, and stirring uniformly to obtain a transparent sol A; drying the transparent sol A to obtain a colloid substance, carrying out heat treatment, heating from room temperature to 300-500 DEG C, keeping the temperature for some time, carrying out furnace cooling to room temperature, and grinding to obtain rare-earth-ion-doped yttrium fluoride fluorescent powder; applying the transparent sol onto a glass or silicon chip substrate by whirl coating, airing at room temperature for 15-30 minutes, drying in a drying box at 100 DEG C, carrying out annealing treatment in a high-temperature furnace, heating to 300-500 DEG C at the heating rate of 1-10 DEG C / minute, keeping the temperature, and cooling to obtain the rare-earth-ion-doped yttrium fluoride fluorescent film.

Description

technical field [0001] The invention belongs to the technical field of preparation of rare earth doped luminescent materials, and in particular relates to a preparation method of rare earth ion doped yttrium fluoride green up-conversion fluorescent materials. Background technique [0002] At present, the preparation methods of rare earth ion-doped yttrium fluoride fluorescent materials mainly include the following three types: 1. Solid-state reaction method, such as the technical scheme described in Chinese patent CN101746805B, powdery water and yttrium nitrate, powdery fluoride Mix the ammonium evenly, and grind it in a mortar for solid-phase reaction. After the reaction is complete, a jelly is obtained. Dry the jelly and grind it to obtain a powder. The powder is kept at 300-500°C for 3~ under the protection of an inert atmosphere. 6 hours, get nanoscale YF 3 , the advantage of the solid-phase method is that the output of the prepared powder is relatively large, the synth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85
Inventor 李凌云潘坚福于岩孙李珍
Owner FUZHOU UNIV
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