CN104119911A - Method for preparing aluminate fluorescent powder for high luminous efficiency light emitting diode (LED) - Google Patents
Method for preparing aluminate fluorescent powder for high luminous efficiency light emitting diode (LED) Download PDFInfo
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- CN104119911A CN104119911A CN201410306224.5A CN201410306224A CN104119911A CN 104119911 A CN104119911 A CN 104119911A CN 201410306224 A CN201410306224 A CN 201410306224A CN 104119911 A CN104119911 A CN 104119911A
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- fluorescent powder
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- aluminate fluorescent
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Abstract
The invention discloses a method for preparing aluminate fluorescent powder for a high luminous efficiency light emitting diode (LED). The chemical composition of the fluorescent powder is Y3-xAl5O12:Cex. The method comprises the following steps: mixing three raw materials such as yttrium oxide (Y2O3), aluminum oxide (Al2O3) and cerium oxide (CeO2) and a fluxing agent ammonium chloride (NH4Cl), performing once firing in an inert atmosphere, screening, adding fluxing agents aluminum fluoride (AlF3) and lithium fluoride (LiF) in a reducing atmosphere for performing twice firing, performing ball milling dispersion, drying and screening, performing third firing in an oxidizing atmosphere, and screening to obtain the needed fluorescent powder. The aluminate fluorescent powder prepared by adopting the method has high luminous efficiency and high attenuation resistance and can be widely applied to high-power high luminous efficiency illuminating LEDs.
Description
Technical field
The present invention relates to a kind of fluorescent material preparation method, particularly the preparation method of aluminate fluorescent powder for a kind of high light efficiency LED.
Background technology
White light LEDs has energy-saving and environmental protection, green, the remarkable advantage such as efficient, as a kind of novel all solid state lighting source, is deeply subject to people's attention.In recent years, along with deepening continuously of semiconductive luminescent materials research, LED manufactured the development and application of novel process, novel material, and versicolor ultra-high brightness LED has been obtained breakthrough.The superiority such as LED illumination is high with its luminous efficiency, current consumption is few, long service life, safe reliability are strong, environmentally-friendly sanitary.
The implementation of white light LEDs is diversified, the implementation that the main yellow fluorescent powder that adopts blue led chip and can effectively be excited by blue light combines in current practical application, wherein, a large amount of yellow fluorescent powders that use are mainly the yttrium aluminum garnet system that cerium excites, i.e. Y
3-xal
5o
12: Ce
x(YAG).Along with the develop rapidly of LED illumination, have higher requirement with aluminate fluorescent powder to LED in market, at present the commercial fluorescent material shortcomings such as in use ubiquity luminous efficiency is on the low side, anti-decay property is poor.How to prepare there is high luminous efficiency, the aluminate fluorescent powder of strong anti-decay property becomes the technical problem that current urgent need solves.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide the preparation method of aluminate fluorescent powder for a kind of LED, can prepare the commercial LED aluminate fluorescent powder that luminescent properties is good, anti-decay property is superior.
To achieve these goals, the technical solution used in the present invention is:
A preparation method for aluminate fluorescent powder for LED, comprises the steps:
Step 1, inert atmosphere burns till:
By the molar ratio of Y, Al and Ce, take respectively yttrium oxide (Y2O3), aluminum oxide (Al2O3) and three kinds of raw materials of cerium oxide (CeO2) and add fusing assistant ammonium chloride (NH4Cl), after mixing, sintering 3-6 hour in the inert atmosphere of 1200-1400 ℃;
Step 2, reducing atmosphere is burnt till:
The product that burn till in step 1 are crossed to 100 mesh sieves, add in mass ratio aluminum fluoride (AlF3) and the 0.1-0.5% lithium fluoride (LiF) of 1-3%, after mixing, sintering 5-8 hour in the reducing atmosphere of 1400-1600 ℃;
Step 3, oxidizing atmosphere burns till:
The product that burn till in step 2 are crossed to 100 mesh sieves, in powder: the ratio of water: zirconia ball=1:2:2.5 is disperseed 12-36 hour, be dried, sieve, sintering 0.5-2 hour in the oxidizing atmosphere of 500-700 ℃, taking out sieves can obtain high light efficiency LED aluminate fluorescent powder.
The add-on of ammonium chloride in described step 1 (NH4Cl) is the 0.5-1.5% of the common quality of yttrium oxide (Y2O3), aluminum oxide (Al2O3) and cerium oxide (CeO2).
Inert atmosphere described in described step 1 is the mixed gas of nitrogen and argon gas, nitrogen: argon gas=90:10-95:5.
Reducing atmosphere described in described step 2 is ammonia atmosphere.
Oxidizing atmosphere described in described step 3 is oxygen atmosphere.
The present invention adopts the preparation method of aluminate fluorescent powder for a kind of high light efficiency LED, and the YAG fluorescent material of preparation has high luminous efficiency and strong antidamping ability, can widespread use in high-power high light efficiency illumination LED.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details.
A preparation method for aluminate fluorescent powder for LED, comprises the steps:
Step 1, inert atmosphere burns till:
By the molar ratio of Y, Al and Ce, take respectively yttrium oxide (Y2O3), aluminum oxide (Al2O3) and three kinds of raw materials of cerium oxide (CeO2) and add fusing assistant ammonium chloride (NH4Cl), after mixing, sintering 3-6 hour in the inert atmosphere of 1200-1400 ℃;
Step 2, reducing atmosphere is burnt till:
The product that burn till in step 1 are crossed to 100 mesh sieves, add in mass ratio aluminum fluoride (AlF3) and the 0.1-0.5% lithium fluoride (LiF) of 1-3%, after mixing, sintering 5-8 hour in the reducing atmosphere of 1400-1600 ℃;
Step 3, oxidizing atmosphere burns till:
The product that burn till in step 2 are crossed to 100 mesh sieves, in powder: the ratio of water: zirconia ball=1:2:2.5 is disperseed 12-36 hour, be dried, sieve, sintering 0.5-2 hour in the oxidizing atmosphere of 500-700 ℃, taking out sieves can obtain high light efficiency LED aluminate fluorescent powder.
The add-on of ammonium chloride in described step 1 (NH4Cl) is the 0.5-1.5% of the common quality of yttrium oxide (Y2O3), aluminum oxide (Al2O3) and cerium oxide (CeO2).
Inert atmosphere described in described step 1 is the mixed gas of nitrogen and argon gas, nitrogen: argon gas=90:10-95:5.
Reducing atmosphere described in described step 2 is ammonia atmosphere.
Oxidizing atmosphere described in described step 3 is oxygen atmosphere.
Embodiment mono-
The chemical constitution molecular formula of the present embodiment fluorescent material is: Y
3-xal
5o
12: Ce
x, x=0.01 wherein.
Preparation method's step of the present embodiment is as follows:
Step 1, inert atmosphere burns till:
Take respectively 76.47g yttrium oxide (Y2O3), 98.23g aluminum oxide (Al2O3), 0.52 cerium oxide (CeO2) and 0.88g ammonium chloride (NH4Cl), after mixing, in the mixed gas of the nitrogen of 1200 ℃ and argon gas, sintering is 6 hours, nitrogen: argon gas=90:10;
Step 2, reducing atmosphere is burnt till:
The product that burn till in step 1 are crossed to 100 mesh sieves, add in mass ratio 1% aluminum fluoride (AlF3) and 0.2% lithium fluoride (LiF), after mixing, in the ammonia atmosphere of 1450 ℃, sintering is 5 hours;
Step 3, oxidizing atmosphere burns till:
The product that burn till in step 2 are crossed to 100 mesh sieves, and in powder: the ratio of water: zirconia ball=1:2:2.5 is disperseed 18 hours, is dried, sieves, and in the oxygen atmosphere of 550 ℃, sintering is 0.5 hour, taking out sieves can obtain high light efficiency LED aluminate fluorescent powder.
Embodiment bis-
The chemical constitution molecular formula of the present embodiment fluorescent material is: Y
3-xal
5o
12: Ce
x, x=0.02 wherein.
Preparation method's step of the present embodiment is as follows:
Step 1, inert atmosphere burns till:
Take respectively 764.7g yttrium oxide (Y2O3), 982.32g aluminum oxide (Al2O3), 1.03 cerium oxide (CeO2) and 17g ammonium chloride (NH4Cl), after mixing, in the mixed gas of the nitrogen of 1300 ℃ and argon gas, sintering is 6 hours, nitrogen: argon gas=95:5;
Step 2, reducing atmosphere is burnt till:
The product that burn till in step 1 are crossed to 100 mesh sieves, add in mass ratio 1% aluminum fluoride (AlF3) and 0.5% lithium fluoride (LiF), after mixing, in the ammonia atmosphere of 1600 ℃, sintering is 6 hours;
Step 3, oxidizing atmosphere burns till:
The product that burn till in step 2 are crossed to 100 mesh sieves, and in powder: the ratio of water: zirconia ball=1:2:2.5 is disperseed 36 hours, is dried, sieves, and in the oxygen atmosphere of 650 ℃, sintering is 1.5 hours, taking out sieves can obtain high light efficiency LED aluminate fluorescent powder.
Embodiment tri-
The chemical constitution molecular formula of the present embodiment fluorescent material is: Y
3-xal
5o
12: Ce
x, x=0.05 wherein.
Preparation method's step of the present embodiment is as follows:
Step 1, inert atmosphere burns till:
Take respectively 229.41g yttrium oxide (Y2O3), 294.69g aluminum oxide (Al2O3), 7.8 cerium oxide (CeO2) and 5.30g ammonium chloride (NH4Cl), after mixing, in the mixed gas of the nitrogen of 1400 ℃ and argon gas, sintering is 5 hours, nitrogen: argon gas=95:5;
Step 2, reducing atmosphere is burnt till:
The product that burn till in step 1 are crossed to 100 mesh sieves, add in mass ratio 2.5% aluminum fluoride (AlF3) and 0.4% lithium fluoride (LiF), after mixing, in the ammonia atmosphere of 1600 ℃, sintering is 5 hours;
Step 3, oxidizing atmosphere burns till:
The product that burn till in step 2 are crossed to 100 mesh sieves, and in powder: the ratio of water: zirconia ball=1:2:2.5 is disperseed 30 hours, is dried, sieves, and in the oxygen atmosphere of 700 ℃, sintering is 1 hour, taking out sieves can obtain high light efficiency LED aluminate fluorescent powder.
Claims (5)
1. a preparation method for aluminate fluorescent powder for high light efficiency LED, is characterized in that, comprises the steps:
Step 1, inert atmosphere burns till:
By the molar ratio of Y, Al and Ce, take respectively yttrium oxide (Y2O3), aluminum oxide (Al2O3) and three kinds of raw materials of cerium oxide (CeO2) and add fusing assistant ammonium chloride (NH4Cl), after mixing, sintering 3-6 hour in the inert atmosphere of 1200-1400 ℃;
Step 2, reducing atmosphere is burnt till:
The product that burn till in step 1 are crossed to 100 mesh sieves, add in mass ratio aluminum fluoride (AlF3) and the 0.1-0.5% lithium fluoride (LiF) of 1-3%, after mixing, sintering 5-8 hour in the reducing atmosphere of 1400-1600 ℃;
Step 3, oxidizing atmosphere burns till:
The product that burn till in step 2 are crossed to 100 mesh sieves, in powder: the ratio of water: zirconia ball=1:2:2.5 is disperseed 12-36 hour, be dried, sieve, sintering 0.5-2 hour in the oxidizing atmosphere of 500-700 ℃, taking out sieves can obtain high light efficiency LED aluminate fluorescent powder.
2. according to the preparation method with aluminate fluorescent powder according to high light efficiency LED claimed in claim 1, it is characterized in that, the add-on of ammonium chloride in described step 1 (NH4Cl) is the 0.5-1.5% of the common quality of yttrium oxide (Y2O3), aluminum oxide (Al2O3) and cerium oxide (CeO2).
3. according to the preparation method with aluminate fluorescent powder according to high light efficiency LED claimed in claim 1, it is characterized in that, inert atmosphere described in described step 1 is the mixed gas of nitrogen and argon gas.
4. according to the preparation method with aluminate fluorescent powder according to high light efficiency LED claimed in claim 1, it is characterized in that, reducing atmosphere described in described step 2 is ammonia atmosphere.
5. according to the preparation method with aluminate fluorescent powder according to high light efficiency LED claimed in claim 1, it is characterized in that, oxidizing atmosphere described in described step 3 is oxygen atmosphere.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112739653A (en) * | 2018-12-28 | 2021-04-30 | 松下知识产权经营株式会社 | Method for producing halide |
| CN113046081A (en) * | 2019-12-27 | 2021-06-29 | 英特美光电（苏州）有限公司 | Aluminate fluorescent powder for LED light source |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101536193A (en) * | 2006-10-20 | 2009-09-16 | 英特曼帝克司公司 | Nano-YAG:Ce phosphor compositions and their methods of preparation |
| US20100301739A1 (en) * | 2009-06-01 | 2010-12-02 | Nitto Denko Corporation | Luminescent ceramic and light-emitting device using the same |
| CN102965109A (en) * | 2012-10-31 | 2013-03-13 | 彩虹集团公司 | Novel process for synthesis of LED fluorescent powder material |
-
2014
- 2014-06-30 CN CN201410306224.5A patent/CN104119911A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101536193A (en) * | 2006-10-20 | 2009-09-16 | 英特曼帝克司公司 | Nano-YAG:Ce phosphor compositions and their methods of preparation |
| US20100301739A1 (en) * | 2009-06-01 | 2010-12-02 | Nitto Denko Corporation | Luminescent ceramic and light-emitting device using the same |
| CN102965109A (en) * | 2012-10-31 | 2013-03-13 | 彩虹集团公司 | Novel process for synthesis of LED fluorescent powder material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112739653A (en) * | 2018-12-28 | 2021-04-30 | 松下知识产权经营株式会社 | Method for producing halide |
| CN112739653B (en) * | 2018-12-28 | 2023-03-28 | 松下知识产权经营株式会社 | Method for producing halide |
| CN113046081A (en) * | 2019-12-27 | 2021-06-29 | 英特美光电（苏州）有限公司 | Aluminate fluorescent powder for LED light source |
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Application publication date: 20141029 |