CN103666472A - Method for improving luminescent intensity and stability of synthesized YAG (yttrium aluminum garnet):Ce fluorescent powder - Google Patents
Method for improving luminescent intensity and stability of synthesized YAG (yttrium aluminum garnet):Ce fluorescent powder Download PDFInfo
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Abstract
The invention belongs to the technical field of rare earth luminescent materials, and mainly relates to a method for obviously improving the luminescent intensity and stability of synthesized YAG (yttrium aluminum garnet):Ce fluorescent powder. The main process comprises the following steps: mixing raw materials according to composition requirements, and calcining at 1400-1700 DEG C to obtain YAG:Ce raw fluorescent powder; performing ball milling dispersion on the YAG:Ce raw fluorescent powder in an acidic water medium, filtering, and drying to obtain surface-acidic raw fluorescent powder; adding cosolvent, uniformly mixing, and performing reducing calcination in hydrogen gas and hydrogen-nitrogen mixed gas at 1400-1600 DEG C for 2-50 hours; and performing furnace cooling to room temperature under the protection of a reducing atmosphere, washing with water, performing grinding dispersion, filtering, washing, and drying to obtain the fluorescent powder. The acid treatment on the surface of the YAG:Ce fluorescent powder can guarantee the cerium reducing effect in the subsequent high-temperature calcination process and improve the dispersity of the YAG fluorescent powder. Thus, the YAG:Ce powder produced by the invention has the characteristics of high luminescent intensity, less luminance decrease, favorable dispersity and stability and the like. The YAG:Ce powder is suitable for synthesis of new fluorescent powder, and can be also used for reforming and upgrading waste fluorescent powder.
Description
Technical field
The invention belongs to rare earth luminescent material technical field, be specifically related to a kind of simple method that improves synthetic YAG:Ce fluorescent material brightness and stability.
Background technology
In recent years, White-light LED illumination has the features such as " energy-conservation ", " environmental protection ", " efficiently " and " long lifetime " because of it, is called as the lighting source of the new generation of green environmental protection after incandescent light, electricity-saving lamp.Along with the lifting of LED chip and encapsulation technology level and the main application market of LED are shown as the main transformation to general lighting from decorating, there is greatly the trend that replaces traditional lighting.
Because the production technology of blue-light LED chip is comparatively ripe, so the volume production scheme of white light LEDs remains the classical way that LED chip combines with fluorescence transition material.This scheme of its main flow is: blue-ray LED (450-470nm)+fluorescent material.White LED light source can be divided into cold white light and warm white again according to colour temperature, and wherein cold white light LEDs is mainly blue-ray LED+YAG:Ce fluorescent material, and this combination accounts for the more than 70 percent of market.This scheme is the YAG phosphor combination by blue-light LED chip and the Yellow light-emitting low temperature that can effectively be excited by blue light, and wherein a part of blue light of blue-ray LED is absorbed by YAG:Ce and launches gold-tinted.The gold-tinted producing becomes white light with remaining blue light.Regulate and control their strength ratio, can obtain various in-white light of high color temperature.Warm white LED main LED chip+YAG:Ce fluorescent material and the combination of nitride rouge and powder on market, wherein the proportion of YAG:Ce fluorescent material and Nitride phosphor is approximately 10:1 left and right, and YAG:Ce fluorescent material remains main part thus.Therefore,, no matter from cold white light or the development of warm white LED, within the quite a long time from now on, YAG:Ce fluorescent material will be all that white light LEDs is applied of paramount importance fluorescent material.In addition,, along with the further expansion in LED market, the market share of fluorescent material is also bound to get a promotion.Because day by day ripe along with the universal SMD encapsulation technology gradually of power-type LED etc., the consumption of single LEDs fluorescent material can significantly increase.Certainly, when the demand of YAG:Ce fluorescent material is increased sharply, to its specification of quality, also will be more and more higher.First, high light efficiency is the primary goal of LED, so require YAG:Ce fluorescent material to have higher light conversion efficiency.Secondly, after encapsulation, the light decay of LED is little, and chromaticity coordinates drift is also little, and Here it is requires YAG:Ce fluorescent material will have higher stability.When again, MODEL OF THE PHOSPHOR PARTICLE SIZE is moderate, dispersiveness will be got well.See that from the market current small power is many in 7-10 micron left and right by YAG:Ce MODEL OF THE PHOSPHOR PARTICLE SIZE, high-power with YAG:Ce fluorescent material in order to keep stability and brightness, granularity is many about 12-16 micron.YAG:Ce fluorescent material so large granularity is easy to cause precipitation when joining powder, affects packaging effect.So require YAG:Ce fluorescent material must have good dispersiveness.Regrettably domestic manufacturer is difficult to produce the YAG:Ce fluorescent material that simultaneously meets above requirement at present, still has larger gap with the production technology level of American-European Japan and Korea S and China Taiwan.Such as: the LED of China, with YAG:Ce fluorescent material market, by Ying Temei and the producer such as grand, ruled for a long time.Therefore the YAG:Ce fluorescent material that, development has a high-performance independent intellectual property right is significant.Meanwhile, in order to guarantee the high brightness requirement of synthetizing phosphor powder, in production process, can produce the substandard products of larger proportion, in fluorescent material use procedure, also can produce some waste and old fluorescent material.If can do suitable aftertreatment to these fluorescent material, to reach application requiring, for improving synthetic yield, economizing on resources and reducing production costs also has very important significance.
In recent ten years, very extensive to the research of YAG:Ce fluorescent material.As far back as US Patent No. 5998925 in 1999 just to YAG:Ce at Y/Gd ratio, Al/Ga than on adjusts and optimizes, the peak value that it can emmission spectrum can be changed between 530-570nm, be applied to the light that blue-light LED chip can produce different-colour, obtained good effect.Similarly research also has US Patent No. 6069440 etc., and since then to YAG:Ce fluorescent material, improvement obtains the actually rare of the achievement of attracting attention.Recent domestic also mainly concentrates on the improvement of novel synthesis to the research of YAG:Ce.
For example, liquid phase method synthetic aspect: Hsuan-Min Lee etc. has synthesized dispersed good YAG:Ce fluorescent material by spray-drying process recently.The features such as Kyeong Youl Jung etc. adopt the synthetic YAG:Ce powder of the method for microwave heating, and it is short that the synthetic YAG of this method has generated time, and temperature is low, good dispersity.Jia etc. synthesize YAG:Ce powder by solvent-thermal method and have also obtained good effect.In addition also have numerous reports such as the synthetic YAG:Ce powder of the novel coprecipitation method of report such as the synthetic YAG:Ce powder of employing colloidal sol-combustion method low temperature such as Yan and Yang.
Patent aspect, US Patent No. 6409938 has been reported oxalate precipitation method for a long time, and take aluminum fluoride and synthesized YAG:Ce powder as solubility promoter.Chinese patent CN1254747 also once reported with the synthetic YAG:Ce powder of homogeneous precipitation method.What the patent CN100543110C of Xiamen University adopted is the low degree of aggregation of the synthetic acquisition of heterogeneous precipitation method, and granularity is the YAG:Ce fluorescent material of 3-15 micron.Chinese patent CN101077974A has synthesized nano level YAG:Ce powder in microemulsion system.CN101831298A adopts the synthetic YAG:Ce powder of sol-gel method.The patent CN101497790A of CaiHong Group combustion synthesis YAG:Ce, thinks with ammonium sulfate and urea to be that incendiary material has good effect.
As can be seen here, it is very many adopting the report of the synthetic YAG:Ce fluorescent material of different liquid phase methods.But still there are a lot of problems in the industrial mass production of liquid phase method at present.First, the material cost that liquid phase method is produced YAG:Ce is higher, and technique is more complicated also, and is difficult to produce in enormous quantities as solid phase method.Secondly, liquid phase method is often introduced all kinds of organic impuritys, and these impurity are difficult to remove totally, will inevitably exert an influence to the YAG:Ce fluorescent material brightness of producing.Again, although on the synthetic small grain size YAG:Ce of liquid phase method, there is clear superiority, can synthesis nano YAG:Ce, the practical application of nano level YAG:Ce in white light LEDs is very limited.The YAG:Ce Powder Particle Size that great power LED needs at present is all wanted 10 more than micron.Yet synthetic granularity is bigger than normal, the YAG:Ce powder liquid phase method that stability is high is not preponderated.
Solid phase method is one of production method of developing the earliest, and the method technique is simple, and cost is low, and efficiency is high, easily mass-produced.It is method the most frequently used in current industrial mass production.Relevant report is very many, and Won etc. has reported employing BaF in recent years
2modified version solid phase method for solubility promoter.The patent CN1880402A of Xiamen Tong Shida illumination has reported that solid phase method synthesizes YAG:Ce powder, mentions and adopts CeF
3make solubility promoter and have good effect.Chinese patent CN101838536A has also reported that solid phase method synthesizes YAG:Ce powder, adopts Sb and Bi to make sensitizing agent, has increased the luminous intensity of Ce etc.And adopted twice and the original YAG:Ce of reparation lattice.The patent No. is that CN100554364C has reported employing BaF
2and H
3bO
3for solubility promoter, adopt airflow crash raw material, the YAG:Ce powder that the mode production granularity of ball milling free is less etc.Although also carried out large quantity research, the YAG:Ce opaque amount that China produces still has larger gap, and the LED light efficiency being mainly reflected in after envelope turns is low, and light decay is but very large, and the chromaticity coordinates drift of 1000 hours is also very serious.In addition also often there is the problems such as aperture, hot spot in the product after encapsulation.Major cause is exactly that the YAG:Ce powder produced of present China exists low lightness, numerous shortcomings such as poor stability and bad dispersibility.
Summary of the invention
The object of this invention is to provide a kind of physical and chemical performance that can synthesize and stablize, luminous efficiency is high, the novel method of YAG:Ce fluorescent material for the LED of good dispersity, and to meet high brightness, the needs of low light attenuation white-light LED encapsulation.
It is simple that another object of the present invention is to provide a kind of method, easy handling, and cost is low, is easy to the transformation and upgrade method of industrialized waste and old YAG:Ce fluorescent material.
The present invention is by having adopted 2 high-temperature calcinations to synthesize to achieve the above object.Calcining is for the first time mainly synthetic YAG:Ce fecula, lattice reduction feature due to yttrium aluminum garnet, rare earth will enter corresponding case with trivalent, most ceriums are existed with trivalent, but its surface crystallization is not fine, also have quadrivalent cerium and exist, need to make it be reduced to trivalent at follow-up reduction calcination process.For improving the reduction effect of cerium, need to carry out acidic cleaning to synthetic fecula, make its surface with certain acidity.And add suitable solubility promoter and calcine for the second time under reducing atmosphere.Now solubility promoter used can be the muriate of ammonium, one or more in fluorochemical, in their high-temperature calcination processes under reducing atmosphere, can volatilize.The weight of fusing assistant accounts for the 0.1-5% of material total mass, preferably 0.5-2%.Calcining temperature is at 1400-1650
0c scope, calcination time 2-50 hour.
Concrete steps and the condition of preparing fluorescent material provided by the invention is as follows:
To contain aluminium, yttrium, the simple substance of gadolinium and cerium and compound (oxide compound, oxyhydroxide, nitrate, carbonate, muriate) they are raw material, by chemical formula Y
3-a-bgd
bal
5o
12: Ce
athe mol ratio requiring accurately takes corresponding raw material (value of a is 0.02≤a≤0.08 preferably, and the value of b is 0.02≤b≤1.5 preferably), and adds one or more solubility promoters, and it is mixed; Mixture is put into crucible, at 1500-1650
01-20 hour is calcined and be incubated to C temperature range, and preferably 4-8 hour, cools to room temperature with the furnace; The product Hubei Province obtaining is broken, pair roller, dry screen, pickling, washing, centrifugal, dry, obtain acid YAG:Ce fecula; In the acid fecula of gained, add one or more solubility promoters, it is mixed; Mixture is put into crucible, under reducing atmosphere at 1400-1650
02-50 hour is calcined and be incubated to C temperature range, cools to room temperature with the furnace; The product Hubei Province obtaining is broken, pair roller, dry screen, washing, wet screening, centrifugal, dry, obtain required fluorescent material product.
The invention provides a kind of method of simple and effective raising YAG:Ce light-emitting phosphor strength and stability.Its principal feature is to adopt two step calcination methods.Calcining for the first time can be carried out under air atmosphere, and main purpose is to prepare YAG:Ce fluorescence fecula, subsequently by pickling ball milling, obtains surface and is acid fine particle, and calcining is for the second time at 1400-1650 under suitable solubility promoter existence and protection of reducing atmosphere
0between C, carry out high temperature reduction calcining, obtain high efficiency fluorescent material.Key of the present invention is to guarantee the acid requirement of reduction calcination process, because cerium is more easily restored to trivalent under acidic conditions, can also improve the dispersiveness of YAG:Ce powder.Therefore it is high that the YAG:Ce powder that the present invention produces has brightness, and light decay is little, the features such as dispersiveness and good stability.
Effect of the present invention and advantage:
(1) a relatively traditional flux method, is used the present invention to produce YAG fluorescent material and has better crystallinity and dispersiveness, can greatly improve brightness and the stability of synthetic YAG:Ce fluorescent material.
(2) fluorescent material physical and chemical performance of the present invention is stable, and with the oxygen in environment, water, carbonic acid gas etc. do not react, heat-resisting, nontoxic, nuisanceless.
(3) the simple easy handling of fluorescent material preparation method of the present invention, had both been suitable for the synthetic of new fluorescent material, also can be used for the transformation and upgrade of waste and old fluorescent material, had good application prospect.
With the synthetic YAG:Ce fluorescent material of the present invention, have illumination effect good, physical and chemical performance is stable, good dispersity and be easy to the features such as suitability for industrialized production.In White-light LED illumination field, have broad application prospects.
Accompanying drawing explanation
Fig. 1 is the XRD diffractogram of synthetizing phosphor powder.
The fluorescent material of proof synthesized has identical phase structure.
The YAG of Tu2Wei factory and hot-water cure fluorescence fecula are carried out the fluorescence spectrum Comparative map after secondary reduction under different flux.
In figure, 1 for not adding fusing assistant; 2 ammonium bifluorides; 3 Neutral ammonium fluorides; 4 ammonium chlorides; 5 YAG of factory.
Fig. 3 is that YAG and acid treatment fluorescence fecula are carried out the fluorescence spectrum Comparative map after secondary reduction under different flux.
In figure, 1 for not adding fusing assistant; 2 ammonium bifluorides; 3 Neutral ammonium fluorides; 4 ammonium chlorides; 5 YAG of factory.
Embodiment
Routine Y:Al:Ce=2.94:5:0.06 takes Y in molar ratio
2o
3, Al (OH)
3, CeO
2,, be more than analytical pure, add appropriate NaF fusing assistant, above-mentioned raw materials is mixed, proceed to and in alumina crucible, tamp and be placed in high temperature reaction stove high-temperature calcination, and pass into reducing gas, temperature is 1600 ℃, soaking time 6h.To be cooledly to taking out sample after room temperature, grind, by 100 object sieve dry screens, the XRD of sample characterizes and sees Fig. 1 sample A.By the powder hot wash of gained, then cross 200 object wet screenings, the sample of wet screening gained is put into 100 ℃ of oven for drying, obtain washing fluorescence fecula, standby.
Get the washing fluorescence fecula of embodiment 1 gained, be placed in hydrogen-nitrogen mixed gas for tube furnace (5%-95%) and carry out secondary reduction, temperature is 1450 ℃, soaking time is 4h, after being cooled to room temperature, take out sample grinding, the fluorescence emission spectrum of gained sample is shown in Fig. 2 sample 1, and the XRD of sample characterizes and sees that Fig. 1 sample B, its fluorescence intensity are 1.03 times of the YAG of factory product.
Get the washing fluorescence fecula of embodiment 1 gained, add 8 ‰ NH4HF2 to be placed in hydrogen-nitrogen mixed gas for tube furnace (5%-95%) and carry out secondary reduction, temperature is 1450 ℃, soaking time is 4h, after being cooled to room temperature, take out sample grinding, the fluorescence emission spectrum of gained sample is shown in Fig. 2 sample 2, and its fluorescence intensity is 1.02 times of the YAG of factory product.
Embodiment 4
The washing fluorescence fecula of getting embodiment 1 gained, adds 8 ‰ NH
4f is placed in hydrogen-nitrogen mixed gas for tube furnace (5%-95%) and carries out secondary reduction, temperature is 1450 ℃, soaking time is 4h, after being cooled to room temperature, take out sample grinding, the XRD of gained sample characterizes and sees Fig. 1 sample C, the fluorescence emission spectrum of sample is shown in Fig. 2 sample 3, and its fluorescence intensity is 1.09 times of the YAG of factory product.
Get the washing fluorescence fecula of embodiment 1 gained, add 8 ‰ NH4Cl, be placed in hydrogen-nitrogen mixed gas for tube furnace (5%-95%) and carry out secondary reduction, temperature is 1450 ℃, soaking time is 4h, after being cooled to room temperature, take out sample grinding, the fluorescence emission spectrum of gained sample is shown in Fig. 2 sample 4, and its fluorescence intensity is 1.06 times of the YAG of factory product.
Embodiment 6
Routine Y:Al:Ce=2.94:5:0.06 takes Y in molar ratio
2o
3, Al (OH)
3, CeO
2,, be more than analytical pure, add appropriate NaF fusing assistant, above-mentioned raw materials is mixed, proceed to and in alumina crucible, tamp and be placed in high temperature reaction stove high-temperature calcination, and pass into reducing gas, temperature is 1600 ℃, soaking time 6h.To be cooledly to taking out sample after room temperature, grind, by 100 object sieve dry screens, the powder of gained is washed with rare HNO3, use again distilled water wash 2-3 time, then cross 200 object wet screenings, the sample of wet screening gained is put into 100 ℃ of oven for drying, obtain pickling fluorescence fecula, standby.
Embodiment 7
Get the pickling fluorescence fecula of embodiment 6 gained, be placed in hydrogen-nitrogen mixed gas for tube furnace (5%-95%) and carry out secondary reduction, temperature is 1450 ℃, soaking time is 4h, after being cooled to room temperature, take out sample grinding, the XRD of gained sample characterizes and sees Fig. 1 sample D, and the fluorescence emission spectrum of sample is shown in Fig. 3 sample 1, and its fluorescence intensity is 1.15 times of the YAG of factory product.
Embodiment 8
The pickling fluorescence fecula of getting embodiment 6 gained, adds 8 ‰ NH
4hF
2fusing assistant, is placed in hydrogen-nitrogen mixed gas for tube furnace (5%-95%) and carries out secondary reduction, and temperature is 1450 ℃, and soaking time is 4h, is cooled to take out sample after room temperature and grind, and the XRD of gained sample characterizes and sees Fig. 1 sample E.The fluorescence emission spectrum of sample is shown in Fig. 3 sample 2, and its fluorescence intensity is 1.33 times of the YAG of factory product.
Embodiment 9
The pickling fluorescence fecula of getting embodiment 6 gained, adds 8 ‰ NH
4f fusing assistant, is placed in hydrogen-nitrogen mixed gas for tube furnace (5%-95%) and carries out secondary reduction, and temperature is 1450 ℃, soaking time is 4h, after being cooled to room temperature, take out sample grinding, the fluorescence emission spectrum of gained sample is shown in Fig. 3 sample 3, and its fluorescence intensity is 1.12 times of the YAG of factory product.
Embodiment 10
The pickling fluorescence fecula of getting embodiment 6 gained, adds 8 ‰ NH
4cl fusing assistant, is placed in hydrogen-nitrogen mixed gas for tube furnace (5%-95%) and carries out secondary reduction, and temperature is 1450 ℃, soaking time is 4h, after being cooled to room temperature, take out sample grinding, the fluorescence emission spectrum of gained sample is shown in Fig. 3 sample 4, and its fluorescence intensity is 1.14 times of the YAG of factory product.
In table 1, the increase rate of the fluorescence intensity ratio factory fluorescent phosphor intensity of gained sample in above-described embodiment has been listed in contrast.Can find out, the sample that restores calcining after overpickling has higher fluorescence intensity.Wherein, the fluorescent material intensity of pickling fluorescence fecula fluoridize hydrogen ammonium secondary reduction is the highest.
Pickling is carried out in pickling of the present invention also available other acid, makes fluorescence fecula possess acidity.
Table 1 hot water and pickling fluorescence fecula add the solubility promoter secondary reduction Hou Yu YAG of factory and compare the percentage ratio that luminous intensity improves
| Fusing assistant | Nothing | Ammonium bifluoride | Neutral ammonium fluoride | Ammonium chloride |
| Hot water wash | 3.31 | 1.85 | 8.93 | 6.13 |
| Pickling | 15.38 | 33.06 | 11.99 | 13.77 |
Claims (9)
1. one kind is improved the method for synthesizing YAG:Ce light-emitting phosphor strength and stability, it is characterized in that, adopt secondary high-temperature method for calcinating, the synthetic YAG:Ce fluorescence fecula of calcining first, secondary clacining carries out under reducing atmosphere, establishes acid pickling step first between calcining and secondary clacining.
2. a kind of method that improves synthetic YAG:Ce light-emitting phosphor strength and stability according to claim 1, is characterized in that, its concrete steps are:
1) simple substance and the compound of take containing aluminium, yttrium, gadolinium and cerium are raw material, by chemical formula Y
3-a-bgd
bal
5o
12: Ce
athe mol ratio requiring takes corresponding raw material, then mixture is put into crucible, at 1500-1650
01-20 hour is calcined and be incubated to C temperature range, cools to room temperature with the furnace;
2) the product Hubei Province obtaining is broken, pair roller, dry screen, pickling, washing, centrifugal, dry, obtain acid YAG fecula;
3) in the acid YAG fecula of gained, put into crucible, under reducing atmosphere at 1400-1650
01-50 hour is calcined and be incubated to C temperature range, cools to room temperature with the furnace; The product Hubei Province obtaining is broken, pair roller, dry screen, washing, wet screening, centrifugal, dry, obtain required fluorescent material product.
3. a kind of method that improves synthetic YAG:Ce light-emitting phosphor strength and stability according to claim 2, is characterized in that value 0.02≤a≤0.08 of described a, value 0.02≤b≤1.5 of b.
4. a kind of method that improves synthetic YAG:Ce light-emitting phosphor strength and stability according to claim 2, is characterized in that, 1), 3) all add solubility promoter in step.
5. a kind of method that improves synthetic YAG:Ce light-emitting phosphor strength and stability according to claim 4, is characterized in that described 3) add NH in step
4hF
2fusing assistant.
6. a kind of method that improves synthetic YAG:Ce light-emitting phosphor strength and stability according to claim 1 and 2, it is characterized in that, described acid pickling step is: will calcine first the powder dilute acid wash of gained, use again distilled water wash 2-3 time, then cross 200 object wet screenings, the sample of wet screening gained is put into 100 ℃ of oven for drying, obtain pickling fluorescence fecula, standby.
7. a kind of method that improves synthetic YAG:Ce light-emitting phosphor strength and stability according to claim 1 and 2, is characterized in that, described calcining first under reducing atmosphere carried out.
8. a kind of method that improves synthetic YAG:Ce light-emitting phosphor strength and stability according to claim 2, is characterized in that described 3) in step, be placed in tube furnace and carry out secondary reduction with hydrogen-nitrogen mixed gas.
9. a kind of method that improves synthetic YAG:Ce light-emitting phosphor strength and stability according to claim 8, is characterized in that, its ratio of described hydrogen-nitrogen mixed gas is 5%-95%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957653A (en) * | 2017-03-30 | 2017-07-18 | 上海应用技术大学 | One kind enhancing YAG:The method of Ce fluorescent material yellow emission intensity |
| CN110311047A (en) * | 2019-06-28 | 2019-10-08 | 云谷（固安）科技有限公司 | A kind of display panel and display device |
| CN111057547A (en) * | 2019-12-27 | 2020-04-24 | 江苏师范大学 | Silicon carbide modified YAG (yttrium aluminum garnet) Ce fluorescent powder and preparation method thereof |
| CN112574748A (en) * | 2020-12-10 | 2021-03-30 | 烟台希尔德材料科技有限公司 | Preparation method of aluminate fluorescent powder with high thermal stability |
-
2013
- 2013-08-31 CN CN201310387834.8A patent/CN103666472A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957653A (en) * | 2017-03-30 | 2017-07-18 | 上海应用技术大学 | One kind enhancing YAG:The method of Ce fluorescent material yellow emission intensity |
| CN110311047A (en) * | 2019-06-28 | 2019-10-08 | 云谷（固安）科技有限公司 | A kind of display panel and display device |
| CN111057547A (en) * | 2019-12-27 | 2020-04-24 | 江苏师范大学 | Silicon carbide modified YAG (yttrium aluminum garnet) Ce fluorescent powder and preparation method thereof |
| CN112574748A (en) * | 2020-12-10 | 2021-03-30 | 烟台希尔德材料科技有限公司 | Preparation method of aluminate fluorescent powder with high thermal stability |
| CN112574748B (en) * | 2020-12-10 | 2023-05-26 | 烟台希尔德材料科技有限公司 | Preparation method of aluminate fluorescent powder with high thermal stability |
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Application publication date: 20140326 |