CN101376522A - Fluorescent powder for white light LED and preparation thereof - Google Patents
Fluorescent powder for white light LED and preparation thereof Download PDFInfo
- Publication number
- CN101376522A CN101376522A CNA2008101522696A CN200810152269A CN101376522A CN 101376522 A CN101376522 A CN 101376522A CN A2008101522696 A CNA2008101522696 A CN A2008101522696A CN 200810152269 A CN200810152269 A CN 200810152269A CN 101376522 A CN101376522 A CN 101376522A
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- China
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- fluorescent powder
- preparation
- white led
- ceo
- baf
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- 0 C*CC(C)(CCC(C*C(*)CCC*C*CC(C(C)(C)*)N=O)N=O)*C Chemical compound C*CC(C)(CCC(C*C(*)CCC*C*CC(C(C)(C)*)N=O)N=O)*C 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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- Luminescent Compositions (AREA)
Abstract
The invention discloses fluorescent powders used in a white light emitting diode and a preparation method. The chemical structural formula of the fluorescent powders used in the white light emitting diode is Y(3-x)BaxAl5O12:Ce, wherein, x ranges from 0.3 to 1.8. The preparation method comprises the steps as follows: (1) Y2O3, BaCO3, Al2O3, CeO2, BaF2 and H3BO3 are weighed; (2) BaF2 and H3BO3 are put in an agate mortar for being evenly mulled and mixed, Y2O3, BaCO3, Al2O3 and CeO2 are then added, and a mixture is obtained after even lapping finish; (3) the mixture is put in a corundum crucible, and is burnt for 2 to 4 hours in a nitrogen flow which contains inflammable air at the temperature ranging from 1050 to 1300 DEG C to obtain the fluorescent powders used in the white light emitting diode. By adopting the preparation method, the luminous intensity of the produced fluorescent powders used in the white light emitting diode is at least more than 10 percent stronger than that of Y3Al5O12:Ce, and the fluorescent powders are used in the fields such as lighting, automobiles, personal communication equipment, etc.
Description
Technical field
The present invention relates to a kind of fluorescent powder for white LED and preparation method.
Background technology
So-called semiconductor lighting is meant with the solid-state illumination of white light emitting diode (W-LED) as new light sources.The employing semiconductor lighting has many good qualities.Energy-conservation: under the same brightness, the power consumption of semiconductor lamp only is 1/10 of an incandescent light.Life-span is long: the stable performance shock resistance, the LED light fixture can reach 5~10 years work-ing life.Environmental protection: can avoid the thermal radiation of incandescent light and make the mercury pollution that uses luminescent lamp to produce, be the generation environmental protection energy.Volume is little: profile is small and exquisite, is convenient to shape-designing.Based on above advantage, the someone thinks: high-brightness white-light LED will be the mankind behind Edison's invention incandescent-lamp bulb, one of greatest invention, therefore, the semiconductor lighting Study on Technology has caused the attention of national governments and industrial community.
Usually, the principle of luminosity of white light LEDs is that the blue light part that the LED substrate sends is absorbed by YAG:Ce fluorescent material, and the yellow light mix that blue light of another part and YAG:Ce fluorescent material send can obtain white light.So in recent years, the research of YAG:Ce fluorescent material had obtained very big progress.
At present, solid phase method (seeing Chinese patent CN1364851A) is adopted in the preparation of YAG:Ce fluorescent material usually, just, raw material is through after the mixing and ball milling, calcine more than the 6h down at comparatively high temps (1400~1600 ℃), pulverize ball milling then, product granularity is bigger as a result, and calcining back ball milling reduces the luminous intensity of YAG:Ce fluorescent material.In addition, the temperature of reaction highly energy-consuming is big, and trivalent cerium ion at high temperature is oxidized to tetravalent state easily, thereby influences the luminosity of YAG:Ce fluorescent material.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of fluorescent powder for white LED is provided.
Second purpose of the present invention provides a kind of preparation method of fluorescent powder for white LED.
The 3rd purpose of the present invention provides another kind of fluorescent powder for white LED.
The 4th purpose of the present invention provides the preparation method of another kind of fluorescent powder for white LED.
Technical scheme of the present invention is summarized as follows:
A kind of fluorescent powder for white LED, its chemical structural formula is: Y
3-xBa
xAl
5O
12: Ce, wherein x is 0.3~1.8.
A kind of preparation method of fluorescent powder for white LED, be made up of following step:
(1) be that 0.5148~1.1923:0.2368~1.4208:1.0196:0.0413:0.3113~0.3746:0.3113~0.3746 takes by weighing Y by mass ratio
2O
3, BaCO
3, Al
2O
3, CeO
2, BaF
2And H
3BO
3
(2) with described BaF
2And H
3BO
3Put into agate mortar and grind and be mixed evenly, add described Y again
2O
3, BaCO
3, Al
2O
3And CeO
2, grind mixing and get mixture;
(3) described mixture is put into corundum crucible, the volumn concentration of hydrogen be in 5% the nitrogen gas stream in 1050~1300 ℃ of following calcination 2~4h, fluorescent powder for white LED Y
3-xBa
xAl
5O
12: Ce, wherein x is 0.3~1.8.
Preferably described Y
2O
3, BaCO
3, Al
2O
3, CeO
2, BaF
2And H
3BO
3Mass ratio be 0.9213:0.7104:1.0196:0.0413:0.3366:0.3366.
Another kind of fluorescent powder for white LED, its chemical structural formula is: Y
3-xSr
xAl
5O
12: Ce, wherein x is 0.3~1.8.
The preparation method of another kind of fluorescent powder for white LED, be made up of following step:
(1) be that 0.5148~1.1923:0.1772~1.0629:1.0196:0.0413:0.3038~0.3298:0.3038~0.3298 takes by weighing Y by mass ratio
2O
3, SrCO
3, Al
2O
3, CeO
2, BaF
2And H
3BO
3
(2) with described BaF
2And H3BO
3Put into agate mortar and grind and be mixed evenly, add described Y again
2O
3, SrCO
3, Al
2O
3And CeO
2, grind mixing and get mixture;
(3) described mixture is put into corundum crucible, the volumn concentration of hydrogen be in 5% the nitrogen gas stream in 1050~1300 ℃ of following calcination 2~4h, fluorescent powder for white LED Y
3-xSr
xAl
5O
12: Ce, wherein x is 0.3~1.8.
Preferably described Y
2O
3, SrCO
3, Al
2O
3, CeO
2, BaF
2And H
3BO
3Mass ratio be 0.9213:0.5315:1.0196:0.0413:0.3142:0.3142.
The present invention utilizes charge-compensation effects successfully to prepare the fluorescent powder for white LED Y of luminous intensity height, ball milling free by adopting relatively mild high temperature solid state reaction (1050~1300 ℃)
3-xM
xAl
5O
12: Ce (M=Sr, Ba).This fluorescent material does not appear in the newspapers so far.
Fluorescent powder for white LED Y by the inventive method production
3-xM
xAl
5O
12: Ce (M=Sr, Ba), luminous strength ratio Y
3Al
6O
12: the luminous intensity of Ce is big at least more than 10%, can be used for preparing white light emitting diode, is used for fields such as illumination, automobile, personal communication apparatus.
Description of drawings
Fig. 1 is Y of the present invention
3-xM
xAl
5O
12: Ce (M=Sr, Ba) and Y
3Al
5O
12: Ce fluorescence emission spectrogram.
Embodiment
So-called relatively mild high temperature solid-state method is the solid reaction mixture that mixes at lower temperature lower calcination, and because of mixture comprises the lower composition of melting point, reaction product can generate under lower temperature of reaction.Because temperature of reaction is lower, has avoided the resultant sintering, thereby improved luminosity.
So-called charge compensation is meant that in reaction system carrying out two kinds of processes that electric charge raises and electric charge reduces simultaneously can compensate mutually, and the result of compensation carries out two kinds of processes easily.
The present invention is directed to the deficiencies in the prior art, design a kind of breakthrough traditional method, adopt relatively mild high temperature solid state reaction (temperature is lower 300~500 ℃ than traditional method) and utilize the fluorescent powder for white LED Y of charge-compensation effects (replace the negative charge compensation quadrivalent cerium that tervalent Y produces with the Sr of divalence or Ba and change into the needed negative charge of trivalent cerium) preparation
3-xM
xAl
5O
12: (M=Sr Ba), reduces by 300~500 ℃ of calcining temperatures, has shortened the Y of calcination time and traditional high temperature solid-state method preparation Ce
3Al
5O
12: Ce fluorescent material is compared, and luminous intensity improves about 10%.
The present invention is further illustrated below in conjunction with specific embodiment.
Y of the present invention
2O
3, and CeO
2Purity is 99.99%, BaCO
3, SrCO
3, Al
2O
3, BaF
2And H
3BO
3Purity is 99.9%.
Embodiment 1
Take by weighing:
Y
2O
3 BaCO
3 Al
2O
3 CeO
2 BaF
2 H
3BO
3
1.1923g 0.2368g 1.0196g 0.0413g 0.3113g 0.3113g
Earlier load weighted flux BaF
2And H
3BO
3Put into agate mortar and grind and be mixed evenly, add again and press measured other the four kinds of reactant Y of weighing balance
2O
3, BaCO
3, Al
2O
3And CeO
2, grind mixing again, get mixture; Mixture is put into corundum crucible, the volumn concentration of hydrogen be in 5% the nitrogen gas stream in 1300 ℃ of following calcination 3h, fluorescent powder for white LED Y
2.7Ba
0.3Al
5O
12: Ce.
Embodiment 2
Take by weighing:
Y
2O
3 BaCO
3 Al
2O
3 CeO
2 BaF
2 H
3BO
3
0.9213g 0.7104g 1.0196g 0.0413g 0.3366g 0.3366g
Earlier load weighted flux BaF
2And H
3BO
3Put into agate mortar and grind and be mixed evenly, add again and press measured other the four kinds of reactant Y of weighing balance
2O
3, BaCO
3, Al
2O
3And CeO
2, grind mixing again and get mixture; Mixture is put into corundum crucible, the volumn concentration of hydrogen be in 5% the nitrogen gas stream in 1250 ℃ of following calcination 2h, fluorescent powder for white LED Y
2.1Ba
0.9Al
5O
12:Ce.
Embodiment 3
Take by weighing:
Y
2O
3 BaCO
3 Al
2O
3 CeO
2 BaF
2 H
3BO
3
0.5148g 1.4208g 1.0196g 0.0413g 0.3746g 0.3746g
Earlier load weighted flux BaF
2And H
3BO
3Put into agate mortar and grind and be mixed evenly, add again and press measured other the four kinds of reactant Y of weighing balance
2O
3, BaCO
3, Al
2O
3And CeO
2, grind mixing again and get mixture; Mixture is put into corundum crucible, the volumn concentration of hydrogen be in 5% the nitrogen gas stream in 1200 ℃ of following calcination 4h, fluorescent powder for white LED Y
1.2Ba
1.8Al
5O
12:Ce.
Embodiment 4
Y
2O
3 SrCO
3 Al
2O
3 CeO
2 BaF
2 H
3BO
3
1.1923g 0.1772g 1.0196g 0.0413g 0.3038g 0.3038g
Earlier load weighted flux BaF
2And H
3BO
3Put into agate mortar and grind and be mixed evenly, add again and press measured other the four kinds of reactant Y of weighing balance
2O
3, SrCO
3, Al
2O
3And CeO
2, grind mixing again and get mixture; Mixture is put into corundum crucible, the volumn concentration of hydrogen be in 5% the nitrogen gas stream in 1150 ℃ of following calcination 3h, fluorescent powder for white LED Y
2.7Sr
0.3Al
5O
12: Ce.
Embodiment 5
Y
2O
3 SrCO
3 Al
2O
3 CeO
2 BaF
2 H
3BO
3
0.9213g 0.5315g 1.0196g 0.0413g 0.3142g 0.3142g
Earlier load weighted flux BaF
2And H
3BO
3Put into agate mortar and grind and be mixed evenly, add again and press measured other the four kinds of reactant Y of weighing balance
2O
3, SrCO
3, Al
2O
3And CeO
2, grind mixing again and get mixture; Mixture is put into corundum crucible, the volumn concentration of hydrogen be in 5% the nitrogen gas stream in 1100 ℃ of following calcination 4h, fluorescent powder for white LED Y
2.1Sr
0.9Al
5O
12: Ce.
Embodiment 6
Y
2O
3 SrCO
3 Al
2O
3 CeO
2 BaF
2 H
3BO
3
0.5148g 1.0629g 1.0196g 0.0413g 0.3298g 0.3298g
Earlier load weighted flux BaF
2And H
3BO
3Put into agate mortar and grind and be mixed evenly, add again and press measured other the four kinds of reactant Y of weighing balance
2O
3, SrCO
3, Al
2O
3And CeO
2, grind mixing again and get mixture; Mixture is put into corundum crucible, the volumn concentration of hydrogen be in 5% the nitrogen gas stream in 1050 ℃ of following calcination 2h, fluorescent powder for white LED Y
1.2Sr
1.8Al
5O
12: Ce.
Fig. 1 is Y of the present invention
2.7M
0.3Al
5O
12: Ce (M=Sr, Ba) and Y
3Al
5O
12: Ce fluorescence emission spectrogram.1 is Y among the figure
2.7Ba
0.3Al
5O
12: Ce
0.06The fluorescence emission spectrogram; 2 is Y
2.7Sr
0..3Al
5O
12: Ce
0.06The fluorescence emission spectrogram; 3 is Y
3Al
5O
12: Ce
0.06The fluorescence emission spectrogram.As can be seen from the figure, Y
2.7M
0.3Al
5O
12: Ce (M=Sr, luminous strength ratio Y Ba)
3Al
5O
12: the luminous intensity of Ce is big at least more than 10%.
Claims (6)
1. a fluorescent powder for white LED is characterized in that, its chemical structural formula is: Y
3-xBa
xAl
5O
12: Ce, wherein x is 0.3~1.8.
2. the preparation method of a kind of fluorescent powder for white LED of claim 1 is characterized in that being made up of following step:
(1) be that 0.5148~1.1923:0.2368~1.4208:1.0196:0.0413:0.3113~0.3746:0.3113~0.3746 takes by weighing Y by mass ratio
2O
3, BaCO
3, Al
2O
3, CeO
2, BaF
2And H
3BO
3
(2) with described BaF
2And H
3BO
3Put into agate mortar and grind and be mixed evenly, add described Y again
2O
3, BaCO
3, Al
2O
3And CeO
2, grind mixing and get mixture;
(3) described mixture is put into corundum crucible, the volumn concentration of hydrogen be in 5% the nitrogen gas stream in 1050~1300 ℃ of following calcination 2~4h, fluorescent powder for white LED Y
3-xBa
xAl
5O
13: Ce, wherein x is 0.3~1.8.
3. the preparation method of a kind of fluorescent powder for white LED according to claim 2 is characterized in that described Y
2O
3, BaCO
3, Al
2O
3, CeO
2, BaF
2And H
3BO
3Mass ratio be 0.9213:0.7104:1.0196:0.0413:0.3366:0.3366.
4. a fluorescent powder for white LED is characterized in that, its chemical structural formula is: Y
3-xSr
xAl
5O
12: Ce, wherein x is 0.3~1.8.
5. the preparation method of a kind of fluorescent powder for white LED of claim 4 is characterized in that being made up of following step:
(1) be that 0.5148~1.1923:0.1772~1.0629:1.0196:0.0413:0.3038~0.3298:0.3038~0.3298 takes by weighing Y by mass ratio
2O
3, SrCO
3, Al
2O
3, CeO
2, BaF
2And H
3BO
3
(2) with described BaF
2And H
3BO
3Put into agate mortar and grind and be mixed evenly, add described Y again
2O
3, SrCO
3, Al
2O
3And CeO
2, grind mixing and get mixture;
(3) described mixture is put into corundum crucible, the volumn concentration of hydrogen be in 5% the nitrogen gas stream in 1050~1300 ℃ of following calcination 2~4h, fluorescent powder for white LED Y
3-xSr
xAl
5O
12: Ce, wherein x is 0.3~1.8.
6. the preparation method of a kind of fluorescent powder for white LED according to claim 5 is characterized in that described Y
2O
3, SrCO
3, Al
2O
3, CeO
2, BaF
2And H
3BO
3Mass ratio be 0.9213:0.5315:1.0196:0.0413:0.3142:0.3142.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNA2008101522696A CN101376522A (en) | 2008-10-09 | 2008-10-09 | Fluorescent powder for white light LED and preparation thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNA2008101522696A CN101376522A (en) | 2008-10-09 | 2008-10-09 | Fluorescent powder for white light LED and preparation thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN101376522A true CN101376522A (en) | 2009-03-04 |
Family
ID=40420267
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNA2008101522696A Pending CN101376522A (en) | 2008-10-09 | 2008-10-09 | Fluorescent powder for white light LED and preparation thereof |
Country Status (1)
Country | Link |
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CN (1) | CN101376522A (en) |
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US20110254435A1 (en) * | 2010-04-20 | 2011-10-20 | China Glaze Co., Ltd. | Phosphors and white light illumination devices utilizing the same |
CN102234510A (en) * | 2010-05-06 | 2011-11-09 | 中国制釉股份有限公司 | Fluorescent material and white light emitting device |
CN102337132A (en) * | 2011-07-19 | 2012-02-01 | 彩虹集团公司 | Method for preparing surface-coated yellow fluorescent powder |
CN102352248A (en) * | 2011-09-19 | 2012-02-15 | 上海穗杉实业有限公司 | Fluorescent powder for white light-emitting diodes (LEDs) and backlight LEDs |
CN102604634A (en) * | 2012-02-10 | 2012-07-25 | 南通南京大学材料工程技术研究院 | Yellow fluorescent powder for white light emitting diode (LED) |
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JP2015180741A (en) * | 2010-07-14 | 2015-10-15 | インテマティックス・コーポレーションIntematix Corporation | Green-emitting, garnet-based phosphors for general and backlighting applications |
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CN103265955A (en) * | 2013-02-19 | 2013-08-28 | 江门市慧存光电材料有限公司 | Method for enhancing YAG fluorescent powder thermal stability |
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