CN102703074A - Preparation method of yellow fluorescent powder - Google Patents

Preparation method of yellow fluorescent powder Download PDF

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Publication number
CN102703074A
CN102703074A CN2012100630562A CN201210063056A CN102703074A CN 102703074 A CN102703074 A CN 102703074A CN 2012100630562 A CN2012100630562 A CN 2012100630562A CN 201210063056 A CN201210063056 A CN 201210063056A CN 102703074 A CN102703074 A CN 102703074A
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fluorescent powder
preparation
yellow fluorescent
fusing assistant
powder according
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曾小青
周彦
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WUHU XUPU FLUORESCENT MATERIAL TECHNOLOGY CO LTD
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WUHU XUPU FLUORESCENT MATERIAL TECHNOLOGY CO LTD
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Abstract

The invention discloses a preparation method of yellow fluorescent powder. The method comprises the following steps of: uniformly mixing the raw materials Y2O3, Gd2O3, CeO2 and Al2O3 with a combined flux; putting the mixture in a corundum crucible; firing at 1,500-1,600 DEG C in the presence of reducing atmosphere for 2-6 hours; cooling to room temperature to obtain a loose block phosphor; and grinding the block phosphor and performing ball-milling dispersion, washing and drying to obtain the fluorescent powder, wherein the dosage of the combined flux accounts for 0.1-5% of the total amount of the raw materials. Compared with the prior art, the combined flux is added to the raw materials before high-temperature sintering; and the combined flux comprises a crystallization accelerator, a particle shape control agent and a particle loosening agent. Through the method, spherical or similar-spherical mono-disperse granular fluorescent powder without surface defects can be obtained.

Description

A kind of preparation method of yellow fluorescent powder
Technical field
The invention belongs to the preparation method of yellow fluorescent powder, and particularly (Y, Gd) 3Al 5O1 2: the preparation method of Ce yellow fluorescent powder, this fluorescent material can be encapsulated into white light emitting diode with the led chip of blue-light-emitting, and white light emitting diode can be used for illumination.
Background technology
White light emitting diode (LED) is a kind of efficient and environment-friendly type semiconductor lighting product; Luminous efficiency high (can reach 200 lumens/watt in theory); Long service life (can reach 100,000 hours in theory), non-environmental-pollution becomes follow-on illuminating product with replacing present power saving fluorescent lamp.White light LEDs has two kinds of implementations, and the one, combinations red, green, blue three kinds of LED; The 2nd, adopt blue-ray LED combination yellow or red, green emitting phosphor, perhaps adopt purple LED combinations red, green, blue colour fluorescent powder.First kind of mode complicacy, costliness, and the second way is simple, cheap, so the second way obtains fast development.Fluorescent RE powder is as one of critical material of white light LEDs, and with luminous efficiency that influences this product and life-span, developing and produce the high-end fluorescent RE powder that is fit to this product will lay the foundation for the development of semiconductor lighting.White light LEDs mainly adopts blue-ray LED combination yellow fluorescent powder at present, and promptly a part of blue-light excited fluorescent material produces gold-tinted, and gold-tinted and the combination of another part blue light realize white light.The commercialization of this white light LEDs has been applied in compact illuminations such as decoration, torch, car light.Another kind of white light LEDs adopts blue-ray LED display predetermined colors in combination, green emitting phosphor, and promptly a part of blue-light excited fluorescent material produces red and green glow, and red-green glow and the combination of another part blue light realize white light.This product color developing is high, can be used as illumination, can also be as the backlight of LCD.
Blue-light excited fluorescent RE powder has been developed fluorescent material such as yellow, green and redness at present, comparative maturity be yellow fluorescent powder, aluminate and silicate systems are arranged, wherein ripe with aluminates system.Aluminates system is meant Ce 3+Ion-activated (Y, Gd) 3Al 5O 12(YAG), its luminous efficiency (450nm excites) can reach 90%.Adopt this fluorescent material, the white light LEDs luminous efficiency of small power (＜0.2 watt) reaches 150 lumens/watt, has surpassed the luminous efficiency (100 lumens/watt) of present power saving fluorescent lamp.Along with the exploitation of the white light LEDs of high-power (＞0.2 watt), YAG fluorescent material will obtain increasing application.
Summary of the invention
The purpose of this invention is to provide a kind of new (Y, Gd) 3Al 5O 12: the preparation method of Ce yellow fluorescent powder, this method combination fusing assistant at high temperature through the crystallization that is used for improving fluorescent material of combination fusing assistant, is controlled the pattern of fluorescent material and is prevented sintering.Thereby obtain well-crystallized, sphere or type sphere, the fluorescent material of free of surface defects.
The technical scheme of technical solution problem of the present invention is: a kind of preparation method of yellow fluorescent powder, and with raw material Y 2O 3, Gd 2O 3, CeO 2, Al 2O 3Mix with the combination fusing assistant, in the corundum crucible of packing into, after reducing atmosphere, 1500-1600 ℃ are fired 2-6 hour and be cooled to the block fluor that room temperature obtains loosening; With obtaining fluorescent material after block fluor pulverizing, Ball milling, washing and the drying, the consumption of combination fusing assistant is the 0.1-5% of raw material total amount, preferably 1-3%.
Described combination fusing assistant is by crystallization promoter, granule-morphology control agent, particle raising agent; The crystallization promoter quality accounts for the 20-60% of combination fusing assistant total amount; The granule-morphology control agent accounts for the 30-50% of combination fusing assistant total amount, and the particle raising agent accounts for the 10-30% of combination fusing assistant total amount.
Described crystallization promoter is a fluorochemical, is specially: LiF, NaF, KF, BaF 2, SrF 2, CaF 2, MgF 2, AlF 3, Na 3AlF 6, GaF 3, YF 3, GdF 3
Described granule-morphology control agent is boric acid and borate, is specially H 3BO 3, B 2O 3, Li 2B 4O 7, Na 2B 4O 7, K 2B 4O 7, BaB 2O 4, SrB 2O 4, CaB 2O 4
Described particle raising agent is a carbonate, is specially: BaCO 3, SrCO 3, MgCO 3, CaCO 3, Li 2CO 3, Na 2CO 3, K 2CO 3
Described reducing atmosphere is 95%N 2-5%H 2(volumetric concentration).
Fluorochemical is an ionic compound among the present invention, has very strong crystallizing power, and its relative fusing point is low simultaneously, and its melt has dissolving raw material Y 2O 3, Gd 2O 3, Al 2O 3And CeO 2Ability, so as synthetic (Y, Gd) 3Al 5O 12: the crystallization promoter of Ce yellow fluorescent powder.
The modest viscosity of melt under boric acid and the borate high temperature, surface tension is moderate, can cover particle surface, and particle surface produce to be shunk, and reduces the particulate surface-area, so as synthetic (Y, Gd) 3Al 5O 12: the granule-morphology control agent of Ce yellow fluorescent powder.
Carbonate at high temperature can produce gas, and volume increases, and the contact surface between the particle is reduced, and is unlikely to produce sintering, thus as synthetic (Y, Gd) 3Al 5O 12: the particle raising agent of Ce yellow fluorescent powder.
In order to reach best effect, crystallization promoter, granule-morphology control agent and particle raising agent need certain ratio.Crystallization promoter and granule-morphology control agent are too much, then easy sintering; The particle raising agent is too many, reaction then occurs not exclusively;
The present invention compared with prior art adopts the combination fusing assistant to be added into raw material and forms at high temperature sintering, and the combination fusing assistant comprises crystallization promoter, granule-morphology control agent and particle raising agent.Use this method, can obtain the fluorescent material of sphere or type sphere, monodisperse particles, free of surface defects.
Description of drawings
Fig. 1 is embodiment 1 made (Y 2.96Ce 0.04) Al 5O 12Fluorescent material amplifies 10000 times stereoscan photograph.
Fig. 2 is embodiment 1 made (Y 2.96Ce 0.04) Al 5O 12The emmission spectrum of fluorescent material under 460nm excites.
Embodiment
Below in conjunction with embodiment the present invention is done detailed explanation.
Embodiment 1:
Take by weighing 336.72 gram Y respectively 2O 3, 6.96 gram CeO 2, 256.8 gram Al 2O 3Raw material, the H of adding raw material 2.5% 3BO 3, NaF, AlF 3, Na 2CO 3Fusing assistant, fusing assistant mass ratio are H 3BO 3: NaF: AlF 3: Na 2CO 3Be 1: 0.4: 0.6: 0.5, in the ball grinder of packing into, porphyrize and mixing on ball mill is in the aluminum oxide of packing into the corundum crucible, at 95%N 2-5%H 2Reducing atmosphere is heated to 1500-1600 ℃; Be incubated 2 hours postcooling to room temperature, agglomerate was pulverized 150 mesh sieves, carry out ball milling with 6 millimeters agate bead and water then; Through for several times wash to the washings specific conductivity less than 10 μ S/cm, filter then, 120 ℃ of oven dry promptly get (Y 2.96Ce 0.04) Al 5O 12Sample.Powder diameter is the 13-15 micron.The fluorescent material that obtains is type spherical, a monodisperse particles, and free of surface defects is as shown in Figure 1.Emmission spectrum is as shown in Figure 2.With the blue chip (emission wavelength is 450nm) of 450mW encapsulation back white light light efficiency be 100lm/W, colour temperature 8000K.
Embodiment 2:
Take by weighing 336.72 gram Y respectively 2O 3, 6.96 gram CeO 2, 256.8 gram Al 2O 3Raw material, the H of adding raw material 2.5% 3BO 3, NaF, AlF 3, Na 2CO 3Fusing assistant, fusing assistant mass ratio are H 3BO 3: NaF: AlF 3: Na 2CO 3Be 1: 0.4: 0.6: 0.5, in the ball grinder of packing into and add water, porphyrize and mixing on ball mill, 100 ℃ of one nights of drying, crushing screening is in the aluminum oxide of packing into the corundum crucible, at 95%N then 2-5%H 2Reducing atmosphere is heated to 1500-1600 ℃; Be incubated 2 hours postcooling to room temperature, agglomerate was pulverized 150 mesh sieves, carry out ball milling with 6 millimeters agate bead and water then; Through for several times wash to the washings specific conductivity less than 10 μ S/cm, filter then, 120 ℃ of oven dry promptly get (Y 2.96Ce 0.04) Al 5O 12Sample.Powder diameter is the 13-15 micron.
Embodiment 3:
Take by weighing 336.72 gram Y respectively 2O 3, 6.96 gram CeO 2, 256.8 gram Al 2O 3Raw material, the H of adding raw material 1.5% 3BO 3, NaF, AlF 3, Na 2CO 3Fusing assistant, fusing assistant mass ratio are H 3BO 3: NaF: AlF 3: Na 2CO 3Be 1: 0.4: 0.6: 0.5, in the ball grinder of packing into, porphyrize and mixing on ball mill is in the aluminum oxide of packing into the corundum crucible, at 95%N 2-5%H 2Reducing atmosphere is heated to 1500-1600 ℃; Be incubated 2 hours postcooling to room temperature, agglomerate was pulverized 150 mesh sieves, carry out ball milling with 6 millimeters agate bead and water then; Through for several times wash to the washings specific conductivity less than 10 μ S/cm, filter then, 120 ℃ of oven dry promptly get (Y 2.96Ce 0.04) Al 5O 12Sample.Powder diameter is the 8-9 micron.With the blue chip (emission wavelength is 452nm) of 60mW encapsulation back white light light efficiency be 110lm/W, colour temperature 6200K.
Embodiment 4:
Take by weighing 336.72 gram Y respectively 2O 3, 6.96 gram CeO 2, 256.8 gram Al 2O 3Raw material, the H of adding raw material 1.5% 3BO 3, NaF, AlF 3, Na 2CO 3Fusing assistant, fusing assistant mass ratio are H 3BO 3: NaF: AlF 3: Na 2CO 3Be 1: 0.4: 0.6: 0.5, in the ball grinder of packing into and add water, porphyrize and mixing on ball mill, 100 ℃ of one nights of drying, crushing screening is in the aluminum oxide of packing into the corundum crucible, at 95%N then 2-5%H 2Reducing atmosphere is heated to 1500-1600 ℃; Be incubated 2 hours postcooling to room temperature, agglomerate was pulverized 150 mesh sieves, carry out ball milling with 6 millimeters agate bead and water then; Through for several times wash to the washings specific conductivity less than 10 μ S/cm, filter then, 120 ℃ of oven dry promptly get (Y 2.96Ce 0.04) Al 5O 12Sample.Powder diameter is the 8-9 micron.
Embodiment 5:
Take by weighing 162.66 gram Y respectively 2O 3, 202.57 gram Gd 2O 3, 10.53 gram CeO 2, 222.56 gram Al 2O 3Raw material, the H of adding raw material 1.5% 3BO 3, NaF, AlF 3, Na 2CO 3Fusing assistant, fusing assistant mass ratio are H 3BO 3: NaF: AlF 3: Na 2CO 3Be 1: 0.4: 0.6: 0.5, in the ball grinder of packing into, porphyrize and mixing on ball mill is in the aluminum oxide of packing into the corundum crucible, at 95%N 2-5%H 2Reducing atmosphere is heated to 1450-1550 ℃; Be incubated 2 hours postcooling to room temperature, agglomerate was pulverized 150 mesh sieves, carry out ball milling with 6 millimeters agate bead and water then; Through for several times wash to the washings specific conductivity less than 10 μ S/cm, filter then, 120 ℃ of oven dry promptly get (Y 1.65Gd 1.28Ce 0.07) Al 5O 12Sample.Powder diameter is the 8-9 micron.

Claims (7)

1. the preparation method of a yellow fluorescent powder is characterized in that: with raw material Y 2O 3, Gd 2O 3, CeO 2, Al 2O 3Mix with the combination fusing assistant, in the corundum crucible of packing into, after reducing atmosphere, 1500-1600 ℃ are fired 2-6 hour and be cooled to the block fluor that room temperature obtains loosening; With obtaining fluorescent material after block fluor pulverizing, Ball milling, washing and the drying, the consumption of combination fusing assistant is the 0.1-5% of raw material total amount.
2. the preparation method of a kind of yellow fluorescent powder according to claim 1 is characterized in that: the consumption of combination fusing assistant is 1-3%.
3. the preparation method of a kind of yellow fluorescent powder according to claim 1; It is characterized in that: described combination fusing assistant is by crystallization promoter, granule-morphology control agent, particle raising agent; The crystallization promoter quality accounts for the 20-60% of combination fusing assistant total amount; The granule-morphology control agent accounts for the 30-50% of combination fusing assistant total amount, and the particle raising agent accounts for the 10-30% of combination fusing assistant total amount.
4. the preparation method of a kind of yellow fluorescent powder according to claim 1, it is characterized in that: described crystallization promoter is a fluorochemical, is specially: LiF, NaF, KF, BaF 2, SrF 2, CaF 2, MgF 2, AlF 3, Na 3AlF 6, GaF 3, YF 3, GdF 3
5. the preparation method of a kind of yellow fluorescent powder according to claim 1, it is characterized in that: described granule-morphology control agent is boric acid and borate, is specially H 3BO 3, B 2O 3, Li 2B 4O 7, Na 2B 4O 7, K 2B 4O 7, BaB 2O 4, SrB 2O 4, CaB 2O 4
6. the preparation method of a kind of yellow fluorescent powder according to claim 1, it is characterized in that: described particle raising agent is a carbonate, is specially: BaCO 3, SrCO 3, MgCO 3, CaCO 3, Li 2CO 3, Na 2CO 3, K 2CO 3
7. the preparation method of a kind of yellow fluorescent powder according to claim 1, it is characterized in that: described reducing atmosphere is 95%N 2-5%H 2(volumetric concentration).
CN2012100630562A 2012-03-12 2012-03-12 Preparation method of yellow fluorescent powder Pending CN102703074A (en)

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Cited By (5)

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CN105331365A (en) * 2015-11-25 2016-02-17 浙江阳光美加照明有限公司 Preparation method of LED fluorescent powder
CN106207152A (en) * 2015-05-08 2016-12-07 云南民族大学 Go to push up octahedral build LiMn2o4anode material for lithium-ion batteries
CN106544023A (en) * 2016-10-21 2017-03-29 北京宇极科技发展有限公司 A kind of preparation method of white light LEDs with the green powder of small particle LuAG
CN109486490A (en) * 2018-11-29 2019-03-19 江苏博睿光电有限公司 Garnet-based superfine fluorescent powder and preparation method thereof
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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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106207152A (en) * 2015-05-08 2016-12-07 云南民族大学 Go to push up octahedral build LiMn2o4anode material for lithium-ion batteries
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CN105331365A (en) * 2015-11-25 2016-02-17 浙江阳光美加照明有限公司 Preparation method of LED fluorescent powder
CN105331365B (en) * 2015-11-25 2017-08-29 浙江阳光美加照明有限公司 A kind of preparation method of LED fluorescent powder
CN106544023A (en) * 2016-10-21 2017-03-29 北京宇极科技发展有限公司 A kind of preparation method of white light LEDs with the green powder of small particle LuAG
CN109486490A (en) * 2018-11-29 2019-03-19 江苏博睿光电有限公司 Garnet-based superfine fluorescent powder and preparation method thereof
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: 20121003