CN101376522A - Fluorescent powder for white light LED and preparation thereof - Google Patents

Fluorescent powder for white light LED and preparation thereof Download PDF

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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
Prior art keywords
fluorescent powder
preparation
white led
ceo
baf
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CNA2008101522696A
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Chinese (zh)
Inventor
孙淑清
刘静
周瑞婷
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Tianjin University
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Tianjin University
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Priority to CNA2008101522696A priority Critical patent/CN101376522A/en
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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

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

Fluorescent powder for white LED and preparation method
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.
CNA2008101522696A 2008-10-09 2008-10-09 Fluorescent powder for white light LED and preparation thereof Pending 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)
CN102786932A (en) * 2012-08-11 2012-11-21 金封焊宝有限责任公司 Novel preparation process of LED (light-emitting diode)
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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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
CN107502354A (en) * 2017-10-11 2017-12-22 哈尔滨工业大学 A kind of warm white LED fluorescent material and preparation method thereof
CN116425544A (en) * 2023-04-20 2023-07-14 江苏师范大学 High-brightness high-luminous-efficiency complex-phase fluorescent ceramic for laser illumination and preparation method thereof

Cited By (23)

* Cited by examiner, † Cited by third party
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TWI447965B (en) * 2010-01-22 2014-08-01 Tzu Kuei Wen Method for led chip package
US20110254435A1 (en) * 2010-04-20 2011-10-20 China Glaze Co., Ltd. Phosphors and white light illumination devices utilizing the same
US8747696B2 (en) * 2010-04-20 2014-06-10 China Glaze Co., Ltd. Phosphors and white light illumination devices utilizing the same
TWI394827B (en) * 2010-04-20 2013-05-01 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
CN102234510B (en) * 2010-05-06 2014-10-29 中国制釉股份有限公司 fluorescent material and white light emitting device
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
CN103270138A (en) * 2010-12-16 2013-08-28 宇部兴产株式会社 Ceramic composite for photoconversion, method for producing same, and light-emitting device comprising same
US9074126B2 (en) 2010-12-16 2015-07-07 Ube Industries, Ltd. Ceramic composite for light conversion
TWI500591B (en) * 2010-12-16 2015-09-21 Ube Industries A ceramic composite for optical conversion, a method for manufacturing the same, and a light-emitting device provided with the same
CN103270138B (en) * 2010-12-16 2015-04-29 宇部兴产株式会社 Ceramic composite for photoconversion, method for producing same, and light-emitting device comprising same
EP2653521A1 (en) * 2010-12-16 2013-10-23 Ube Industries, Ltd. Ceramic composite for photoconversion, method for producing same, and light-emitting device comprising same
EP2653521A4 (en) * 2010-12-16 2014-07-16 Ube Industries Ceramic composite for photoconversion, method for producing same, and light-emitting device comprising same
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)
CN102604634B (en) * 2012-02-10 2013-08-28 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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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
CN107502354A (en) * 2017-10-11 2017-12-22 哈尔滨工业大学 A kind of warm white LED fluorescent material and preparation method thereof
CN107502354B (en) * 2017-10-11 2020-11-06 哈尔滨工业大学 Fluorescent powder for warm white LED and preparation method thereof
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