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Nitrogen oxide fluorescent powder used in white-light LED, and preparation method thereof

A nitrogen oxide and phosphor technology is applied in the field of nitrogen oxide phosphor for white light LED and its preparation, which can solve the problems affecting the uniformity of product phase and morphology, the performance of phosphor samples, and the large difference in melting temperature, etc. problems, to achieve a wide range of chips, avoid performance deterioration, and easy post-processing.

Inactive Publication Date: 2014-11-12
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently commonly used fluxes are boric acid, alkali metal fluoride, ammonium chloride, etc. Their disadvantage is that it is easy to introduce impurity ions and reduce the brightness of phosphor powder; It will lead to uneven crystallization of phosphor powder during sintering, which will affect the uniformity of product phase and shape
In addition, different sintering and heating systems will also have a great impact on the performance of the final phosphor sample

Method used

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  • Nitrogen oxide fluorescent powder used in white-light LED, and preparation method thereof
  • Nitrogen oxide fluorescent powder used in white-light LED, and preparation method thereof
  • Nitrogen oxide fluorescent powder used in white-light LED, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The preparation method of a kind of nitrogen oxide phosphor powder for white light LED of this embodiment comprises the following steps:

[0034] (1) Weigh and mix the raw materials; the raw materials are made of Si 3 N 4 , CaCO 3 , SiO 2 、Eu 2 o 3 Composition, the molar ratio is CaCO 3 : SiO 2 : Si 3 N 4 : Eu2 o 3 =(1-x):2-3y:y:x / 2, where x=0.03, y=2 / 3;

[0035] (2) Add a flux to the raw materials and mix well to obtain a mixture; the flux is Zn(CH 3 COO) 2 , the weight is 40% of the mixture;

[0036] (3) Put the mixture into the crucible and place it in the furnace tube of the horizontal high-temperature tube furnace;

[0037] (4) Vacuum the horizontal high temperature tube furnace to 10 -5 Pa, and then filled with 1 atmosphere of nitrogen with a purity greater than 99.99%;

[0038] (5) Repeat step (4) 3 times;

[0039] (6) Vacuumize the furnace to 10 -5 Pa, then fill the furnace with a reducing gas (nitrogen-hydrogen mixture) with a purity greater th...

Embodiment 2

[0050] The preparation method of a kind of nitrogen oxide phosphor powder for white light LED of this embodiment comprises the following steps:

[0051] (1) Weigh and mix the raw materials; the raw materials are made of Si 3 N 4 , CaO, SiO 2 、Eu 2 o 3 Composition, molar ratio CaO:SiO 2 : Si 3 N 4 : Eu 2 o 3 =(1-x):2-3y:y:x / 2, where x=0.005, y=0.5;

[0052] (2) Adding a flux to the raw materials and mixing to obtain a mixture; the flux is ZnO, and the weight is 50% of the mixture;

[0053] (3) Put the mixture into the crucible and place it in the furnace tube of the horizontal high-temperature tube furnace;

[0054] (4) Vacuum the horizontal high temperature tube furnace to 10 -3 After Pa, it is filled with nitrogen with a purity greater than 99.99% at 0.5 atmospheric pressure;

[0055] (5) Repeat step (4) 5 times;

[0056] (6) Vacuumize the furnace to 10 -3 After Pa, fill the furnace with reducing gas (hydrogen) with a purity greater than 99.99%;

[0057] (7) Af...

Embodiment 3

[0062] The preparation method of a kind of nitrogen oxide phosphor powder for white light LED of this embodiment comprises the following steps:

[0063] (1) Weigh and mix the raw materials; the raw materials are made of Si 3 N 4 , CaC 2 o 4 , SiO 2 、Eu 2 o 3 Composition, the molar ratio is CaC 2 o 4 : SiO 2 : Si 3 N 4 : Eu 2 o 3 =(1-x):2-3y:y:x / 2, where x=0.05, y=1 / 3;

[0064] (2) Adding a flux to the raw materials and mixing to obtain a mixture; the flux is ZnCO 3 , the weight is 30% of the mixture;

[0065] (3) Put the mixture into the crucible and place it in the furnace tube of the horizontal high-temperature tube furnace;

[0066] (4) Vacuum the horizontal high temperature tube furnace to 10 -1 Pa, and then filled with 2 atmospheres of nitrogen with a purity greater than 99.99%;

[0067] (5) Repeat step (4) 4 times;

[0068] (6) Vacuumize the furnace to 10 -1 After Pa, fill the furnace with reducing gas (ammonia) with a purity greater than 99.99%;

[0...

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Abstract

The invention discloses a preparation method of nitrogen oxide fluorescent powder used in white-light LED. According to the invention, Si3N4, CaO or precursor thereof, SiO2, and Eu2O3 are adopted as raw materials, wherein a molar ratio of CaO:SiO2:Si3N4:Eu2O3=(1-x):2-3y:y:x / 2. x is no smaller than 0.005 and no greater than 0.05, and y is no smaller than 1 / 3 and no greater than 2 / 3. A zinc-containing compound is added as a flux, and the nitrogen oxide fluorescent powder is prepared. With the method, pure-phase nitrogen oxide Ca1-xSi2O2N2:xEu<2+> fluorescent powder can be prepared. The fluorescent powder has the advantages of good physiochemical stability and good thermal stability. Crystallinity of synthesized block-shaped crystal powder is better, and luminescence is better. Bright yellow light can be emitted under the excitation of long-wavelength ultraviolet light. With the preparation method, the process steps are simple, cost is low, popularization is easy, and large-scale industrialized production can be carried out.

Description

technical field [0001] The invention relates to the field of luminescent materials, in particular to a nitrogen oxide fluorescent powder for white LEDs and a preparation method thereof. Background technique [0002] As a new type of all-solid-state lighting source, white LED has attracted much attention. Because of its many advantages such as long life, high efficiency, green environmental protection, no pollution, energy saving, good color rendering, no flicker, no infrared and ultraviolet radiation, it is regarded as a green lighting source in the 21st century and has broad application prospects and Huge potential market. [0003] At present, the white light LED that is widely used in the world is composed of a blue light LED and a yellow phosphor that can be effectively excited by blue light, which was first reported in 1996. Many American and Japanese companies have adopted this method to launch white LED products. The current typical yellow phosphor that can be effec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/59
CPCY02B20/181Y02B20/00
Inventor 张勤远马艳艳叶柿季小红
Owner SOUTH CHINA UNIV OF TECH
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