A method for preparing highly crystalline nano nitride phosphor

A nitride phosphor, high crystallinity technology, applied in nano optics, chemical instruments and methods, nanotechnology, etc., can solve the problems of decreased luminous efficiency, difficult to accurately control the packaging process, low yield rate, etc., to eliminate light loss , Improve light extraction efficiency, crystallinity recovery effect

Active Publication Date: 2020-10-02
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the particles are too thick, there are two defects: (1) During the encapsulation process, the phosphor particles settle in the encapsulant because the specific gravity is much higher than that of the liquid encapsulant, which makes it difficult to accurately control the encapsulation process and uneven distribution of phosphor particles , the light color consistency of white LED is difficult to guarantee, the light color is uneven, and the yield rate is low
[0005] Due to the extremely high synthesis temperature, it is difficult to prepare nano-nitride phosphors using existing conventional methods
However, if the size of nitride phosphor particles is reduced to the nanometer scale by using mechanical pulverization methods such as ball milling and jet milling, the crystallinity of phosphor particles will be severely damaged, resulting in a significant drop in luminous efficiency.
However, if the mechanically pulverized nano-nitride phosphor is calcined at a high temperature for the second time, although its crystallinity can be restored, it will cause the nanoparticles to sinter and grow again.
So far, there is no report on highly crystalline dispersed nano-nitride particles and transparent nitride fluorescent glue

Method used

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  • A method for preparing highly crystalline nano nitride phosphor
  • A method for preparing highly crystalline nano nitride phosphor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1: Prepare 2 L of potassium sulfate solution with a concentration of 0.1 mol / L with deionized water, add polyacrylic acid with a salt mass of 5%, and dissolve it. The potassium sulfate solution containing polyacrylic acid is dropped into 50 liters of ethanol under the condition of stirring, the precipitate is washed with ethanol for 1-2 times, and the potassium sulfate nano crystal can be obtained after drying. Weigh 10 grams of nano-potassium sulfate, disperse it in 200 ml of ethanol, add 0.5 grams of stearic acid, and keep stirring at 50° C. for 2 hours. After centrifuging the nano-potassium sulfate ethanol dispersion, disperse the nano-potassium sulfate in 100ml xylene, add 10g of nano-CaAlSiN obtained by mechanical pulverization 3 : Eu phosphor, stirred at 80°C for 2 hours, centrifuged, dried, calcined at 1000°C in a nitrogen atmosphere for 2 hours, washed with water, dried to obtain highly crystalline dispersed nano-CaAlSiN 3 : Eu phosphor.

Embodiment 2

[0043] Example 2: Prepare 2 L of potassium sulfate solution with a concentration of 0.1 mol / L with deionized water, add polyacrylic acid with a salt mass of 5%, and dissolve it. The potassium sulfate solution containing polyacrylic acid is dropped into 50 liters of ethanol under the condition of stirring, the precipitate is washed with ethanol for 1-2 times, and the potassium sulfate nano crystal can be obtained after drying. Weigh 1 gram of nanopotassium sulfate, disperse it in 200ml of ethanol, add 0.01 gram of stearic acid, and keep stirring at 50°C for 2 hours. After centrifuging the nano-potassium sulfate ethanol dispersion, disperse the nano-potassium sulfate in 100ml xylene, add 0.1g of nano-CaAlSiN obtained by mechanical pulverization 3 : Eu phosphor, stirred at 80°C for 2 hours, centrifuged, dried, calcined at 1000°C in a nitrogen atmosphere for 2 hours, washed with water, dried to obtain highly crystalline dispersed nano-CaAlSiN 3 : Eu phosphor.

Embodiment 3

[0044] Example 3: Prepare 2 L of potassium sulfate solution with a concentration of 0.1 mol / L with deionized water, add polyacrylic acid with a salt mass of 5%, and dissolve it. The potassium sulfate solution containing polyacrylic acid is dropped into 50 liters of ethanol under the condition of stirring, the precipitate is washed with ethanol for 1-2 times, and the potassium sulfate nano crystal can be obtained after drying. Weigh 5 grams of nano-potassium sulfate, disperse it in 200 ml of ethanol, add 0.1 gram of stearic acid, and keep stirring at 50° C. for 2 hours. After centrifuging the nano-potassium sulfate ethanol dispersion, disperse the nano-potassium sulfate in 100ml xylene, add 5g of nano-CaAlSiN obtained by mechanical pulverization 3 : Eu phosphor, stirred at 80°C for 2 hours, centrifuged, dried, calcined at 1000°C in a nitrogen atmosphere for 2 hours, washed with water, dried to obtain highly crystalline dispersed nano-CaAlSiN 3 : Eu phosphor.

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Abstract

The invention discloses a method for preparing highly crystalline nano nitride fluorescent powder. The method comprises the steps that: firstly, nano-size potassium sulfate particles are prepared, thenano-potassium sulfate particles are surface-modified to uniformly disperse the particles in xylene, mechanically pulverized nano nitride fluorescent powder particles are dispersed and isolated in xylene, precipitate is dried and then calcined in an inert atmosphere, and after washing, the nano nitride fluorescent powder with high crystallinity, high dispersion, and excellent luminescence properties can be obtained. The method for preparing the highly crystalline nano nitride fluorescent powder can rapidly prepare high-quality nano nitride fluorescent powder in batches, and the nano nitride fluorescent powder can be made into transparent fluorescent glues, can not only eliminate light scattering loss, but also solve a problem of inconsistency of white LED light color caused by settlement.

Description

technical field [0001] The invention relates to a technology for preparing highly crystalline nano nitride phosphor powder, which belongs to the technical field of luminescent materials. Background technique [0002] (Sr / Ca)AlSiN 3 :Eu and Sr 2 Si 5 N 8 :Eu system nitride red phosphor is widely used in commercial white LEDs due to its high luminous efficiency and pure light color. [0003] At present, commercial nitride phosphors are all prepared by high-temperature solid-phase method, and the synthesis temperature is as high as 1400°C to 1700°C. The prepared phosphor particles are coarse, and the particle size is generally about 10-20 μm. Because the particles are too thick, there are two defects: (1) During the encapsulation process, the phosphor particles settle in the encapsulant because the specific gravity is much higher than that of the liquid encapsulant, which makes it difficult to accurately control the encapsulation process and uneven distribution of phosphor ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/64B82Y20/00B82Y40/00C09J183/04C09J163/00C09J11/04
CPCB82Y20/00B82Y40/00C08K3/34C08K9/00C08K9/04C08K2003/3045C08K2201/011C09J11/04C09J163/00C09J183/04C09K11/7734
Inventor 董岩卞仙王宇婷邵起越蒋建清
Owner SOUTHEAST UNIV
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