CN104046357A - YAG fluorescent powder used in semiconductor illumination and preparation method thereof - Google Patents
YAG fluorescent powder used in semiconductor illumination and preparation method thereof Download PDFInfo
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- CN104046357A CN104046357A CN201410223326.0A CN201410223326A CN104046357A CN 104046357 A CN104046357 A CN 104046357A CN 201410223326 A CN201410223326 A CN 201410223326A CN 104046357 A CN104046357 A CN 104046357A
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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
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Abstract
A YAG fluorescent powder used in semiconductor illumination disclosed by the invention is a powder formed by Y3Al5O12:Ce<3+> microspheres with diameter of 1-2 mum. The preparation method adopts inorganic salt as a precursor and a sol gel method to obtain theY3Al5O12:Ce<3+> fluorescent microspheres at lower heat treatment temperature. The invention has the advantages of simple preparation process, convenient operation, short preparation time and low heat treatment temperature, can greatly reduce energy consumption, and is suitable for industrial mass production. YAG fluorescent microspheres obtained by the invention have the characteristics of regular shape, uniformly distributed size and excellent luminescence properties and can be widely used for the production of white LED lighting device.
Description
Technical field
The present invention relates to YAG fluorescent material being applied to semiconductor lighting and preparation method thereof, belong to technical field of semiconductor illumination.
Background technology
In recent years, due to the fast lifting of blue light, purple light and ultraviolet light-emitting diode (LED) performance, the development of LED Lighting Industry rapidly.Compare with existing illuminating device, the many merits such as LED illumination has energy-saving and environmental protection, cost is low, efficiency is high, the time of response is short, long service life, shock resistance and vibration resistance, thereby become the ideal chose of illuminating device of new generation.
LED, as environment-friendly type a new generation lighting source, mainly refers to white light LEDs.At present, mainly by blue led chip, to excite YAG yellow fluorescent powder to realize white luminous for comparatively ripe white light LED part.In suitability for industrialized production, the main high temperature solid-phase sintering technique that adopts is prepared YAG yellow fluorescent powder, and ubiquity preparation technology is loaded down with trivial details, and sintering temperature is high by (>=1600
othe problems such as C), energy consumption is huge, production cost height.Meanwhile, due to the limitation of technology of preparing, also there is the problems such as particle shape is irregular, and dimensional change is large in existing commercialization YAG yellow fluorescent powder, has a strong impact on the optical property of white light LED part.Therefore, develop preparation technology simple, less energy consumption, cost are low, particle shape rule, and the YAG yellow fluorescent powder tool of even size distribution is of great significance.
Summary of the invention
The object of the present invention is to provide a kind of technique simple, with low cost, be applicable to suitability for industrialized production, regular shape be applied to YAG fluorescent material of semiconductor lighting and preparation method thereof
The YAG fluorescent material that is applied to semiconductor lighting of the present invention is by Y
3al
5o
12: Ce
3+the powder that microballoon forms, microsphere diameter is 1 ~ 2 μ m.
The preparation method who is applied to the YAG fluorescent material of semiconductor lighting, comprises the steps:
1) crystal aluminum chloride in mass ratio: six hydration Yttrium trichlorides: Cerium trichloride hexahydrate: ethanol: deionized water: methane amide: 1,2-propylene oxide=1:0.46:0.07～0.14:0.85～1.82:0.62～1.85:0.35～0.70:0.77～1.79, take crystal aluminum chloride, six hydration Yttrium trichlorides, Cerium trichloride hexahydrate, ethanol, deionized water, methane amide and 1,2 epoxy prapane;
2) under the condition of 15-25 ℃ of water bath with thermostatic control, crystal aluminum chloride in step 1), six hydration Yttrium trichlorides and Cerium trichloride hexahydrate are fully dissolved in the mixing solutions of deionized water, ethanol and methane amide, then add 1-2 propylene oxide, after being fully uniformly mixed, put into sealed vessel, then under 50 ~ 60 ℃ of constant temperatures, be incubated to mixing solutions formation gel;
3) by gel under 60 ~ 90 ℃ of constant temperatures dry 6 ~ 24 hours, then grinding distribution was processed it 2 ~ 6 hours at 500 ~ 700 ℃, then under reducing atmosphere in 800 ~ 1200 ℃ of sintering 2 ~ 8 hours, obtain YAG fluorescent material.
Above-mentioned reducing atmosphere is H
2and N
2the gas mixing for 1:19 by volume.
The present invention compares with technical background, has following advantage:
The equipment that the present invention uses is simple, easy to operate, and step is simple.In whole preparation process the time short, thermal treatment temp is low, integral body has significantly reduced energy consumption, is applicable to very much large-scale industrialization and produces.The YAG fluorescent microsphere that the present invention obtains has regular shape, even size distribution, and the features such as luminescent properties excellence, can be widely used in and make White-light LED illumination device.
In addition, by regulating additional proportion and the water bath with thermostatic control temperature of crystallization Cerium II Chloride, 1,2 epoxy prapane, deionized water and ethanol, can change the particle size of YAG fluorescence spheroid, thus the luminous intensity of regulation and control YAG fluorescent material.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the YAG fluorescent material of embodiment 1 preparation;
Fig. 2 is the X ray diffracting spectrum of the YAG fluorescent material of embodiment 1 preparation;
Fig. 3 is the PL fluorescence spectrum figure of the YAG fluorescent material of embodiment 1 preparation.
Embodiment
Embodiment 1
1) crystal aluminum chloride in mass ratio: six hydration Yttrium trichlorides: Cerium trichloride hexahydrate: ethanol: deionized water: methane amide: 1,2-propylene oxide=1:0.46:0.07:1.34:1.24:0.35:1.79, take crystal aluminum chloride, six hydration Yttrium trichlorides, Cerium trichloride hexahydrate, ethanol, deionized water, methane amide and 1,2 epoxy prapane;
2) under the condition of 25 ℃ of waters bath with thermostatic control, crystal aluminum chloride in step 1), six hydration Yttrium trichlorides and Cerium trichloride hexahydrate are fully dissolved in the mixing solutions of deionized water, ethanol and methane amide, then add 1-2 propylene oxide, after being fully uniformly mixed, put into sealed vessel, then under 60 ℃ of constant temperatures, be incubated to mixing solutions formation gel;
3) gel is placed under 60 ℃ of constant temperatures and is dried 24 hours, then grinding distribution is incubated 4 hours by it under the condition of 500 ℃, then at H
2and N
2under the gas atmosphere that 1:19 mixes by volume, in 800 ℃, be incubated 2 hours, cooling rear acquisition YAG fluorescent material.
The electron scanning micrograph of this YAG fluorescent material is shown in Fig. 1, and YAG fluorescent microsphere has regular shape as seen from the figure, the feature of even size distribution, and microsphere diameter is 1 ~ 2 μ m.Its X ray diffracting spectrum is shown in Fig. 2, shows that the YAG fluorescent material degree of crystallinity obtaining is very good; PL fluorescence spectrum figure is shown in Fig. 3, and as seen from the figure, the YAG fluorescent material that the present invention prepares has sent the light of 540nm under the exciting of 470nm light, and luminous intensity is strong, is suitable for very much making White-light LED illumination device.
Embodiment 2
1) crystal aluminum chloride in mass ratio: six hydration Yttrium trichlorides: Cerium trichloride hexahydrate: ethanol: deionized water: methane amide: 1,2-propylene oxide=1:0.46:0.14:1.34:1.24:0.35:1.79, take crystal aluminum chloride, six hydration Yttrium trichlorides, Cerium trichloride hexahydrate, ethanol, deionized water, methane amide and 1,2 epoxy prapane;
2) under the condition of 15 ℃ of waters bath with thermostatic control, crystal aluminum chloride in step 1), six hydration Yttrium trichlorides and Cerium trichloride hexahydrate are fully dissolved in the mixing solutions of deionized water, ethanol and methane amide, then add 1-2 propylene oxide, after being fully uniformly mixed, put into sealed vessel, then under 60 ℃ of constant temperatures, be incubated to mixing solutions formation gel;
3) gel is placed under 70 ℃ of constant temperatures and is dried 24 hours, then grinding distribution is incubated 4 hours by it under the condition of 600 ℃, then at H
2and N
2under the gas atmosphere that 1:19 mixes by volume, in 900 ℃, be incubated 4 hours, cooling rear acquisition regular shape, the YAG fluorescent microsphere of even size distribution.
Embodiment 3
1) crystal aluminum chloride in mass ratio: six hydration Yttrium trichlorides: Cerium trichloride hexahydrate: ethanol: deionized water: methane amide: 1,2-propylene oxide=1:0.46:0.07:0.85:1.85:0.35:1.79, take crystal aluminum chloride, six hydration Yttrium trichlorides, Cerium trichloride hexahydrate, ethanol, deionized water, methane amide and 1,2 epoxy prapane;
2) under the condition of 20 ℃ of waters bath with thermostatic control, crystal aluminum chloride in step 1), six hydration Yttrium trichlorides and Cerium trichloride hexahydrate are fully dissolved in the mixing solutions of deionized water, ethanol and methane amide, then add 1-2 propylene oxide, after being fully uniformly mixed, put into sealed vessel, then under 50 ℃ of constant temperatures, be incubated to mixing solutions formation gel;
3) gel is placed under 80 ℃ of constant temperatures and is dried 6 hours, then grinding distribution is incubated 4 hours by it under the condition of 600 ℃, then at H
2and N
2under the gas atmosphere that 1:19 mixes by volume, in 1000 ℃, be incubated 12 hours, cooling rear acquisition regular shape, the YAG fluorescent microsphere of even size distribution.
Embodiment 4
1) crystal aluminum chloride in mass ratio: six hydration Yttrium trichlorides: Cerium trichloride hexahydrate: ethanol: deionized water: methane amide: 1,2-propylene oxide=1:0.46:0.07:1.82:0.62:0.35:1.79, take crystal aluminum chloride, six hydration Yttrium trichlorides, Cerium trichloride hexahydrate, ethanol, deionized water, methane amide and 1,2 epoxy prapane;
2) under the condition of 25 ℃ of waters bath with thermostatic control, crystal aluminum chloride in step 1), six hydration Yttrium trichlorides and Cerium trichloride hexahydrate are fully dissolved in the mixing solutions of deionized water, ethanol and methane amide, then add 1-2 propylene oxide, after being fully uniformly mixed, put into sealed vessel, then under 55 ℃ of constant temperatures, be incubated to mixing solutions formation gel;
3) gel is placed under 80 ℃ of constant temperatures and is dried 20 hours, then grinding distribution is incubated 4 hours by it under the condition of 700 ℃, then at H
2and N
2under the gas atmosphere that 1:19 mixes by volume, in 900 ℃, be incubated 4 hours, cooling rear acquisition regular shape, the YAG fluorescent microsphere of even size distribution.
Embodiment 5
1) crystal aluminum chloride in mass ratio: six hydration Yttrium trichlorides: Cerium trichloride hexahydrate: ethanol: deionized water: methane amide: 1,2-propylene oxide=1:0.46:0.07:1.34:1.24:0.70:1.79, take crystal aluminum chloride, six hydration Yttrium trichlorides, Cerium trichloride hexahydrate, ethanol, deionized water, methane amide and 1,2 epoxy prapane;
2) under the condition of 20 ℃ of waters bath with thermostatic control, crystal aluminum chloride in step 1), six hydration Yttrium trichlorides and Cerium trichloride hexahydrate are fully dissolved in the mixing solutions of deionized water, ethanol and methane amide, then add 1-2 propylene oxide, after being fully uniformly mixed, put into sealed vessel, then under 50 ℃ of constant temperatures, be incubated to mixing solutions formation gel;
3) gel is placed under 80 ℃ of constant temperatures and is dried 24 hours, then grinding distribution is incubated 4 hours by it under the condition of 500 ℃, then at H
2and N
2under the gas atmosphere that 1:19 mixes by volume, in 900 ℃, be incubated 12 hours, cooling rear acquisition regular shape, the YAG fluorescent microsphere of even size distribution.
Embodiment 6
1) crystal aluminum chloride in mass ratio: six hydration Yttrium trichlorides: Cerium trichloride hexahydrate: ethanol: deionized water: methane amide: 1,2-propylene oxide=1:0.46:0.07:1.34:1.24:0.35:0.77, take crystal aluminum chloride, six hydration Yttrium trichlorides, Cerium trichloride hexahydrate, ethanol, deionized water, methane amide and 1,2 epoxy prapane;
2) under the condition of 17 ℃ of waters bath with thermostatic control, crystal aluminum chloride in step 1), six hydration Yttrium trichlorides and Cerium trichloride hexahydrate are fully dissolved in the mixing solutions of deionized water, ethanol and methane amide, then add 1-2 propylene oxide, after being fully uniformly mixed, put into sealed vessel, then under 50 ℃ of constant temperatures, be incubated to mixing solutions formation gel;
3) gel is placed under 80 ℃ of constant temperatures and is dried 24 hours, then grinding distribution is incubated 4 hours by it under the condition of 600 ℃, then at H
2and N
2under the gas atmosphere that 1:19 mixes by volume, in 1000 ℃, be incubated 4 hours, cooling rear acquisition regular shape, the YAG fluorescent microsphere of even size distribution.
Embodiment 7
1) crystal aluminum chloride in mass ratio: six hydration Yttrium trichlorides: Cerium trichloride hexahydrate: ethanol: deionized water: methane amide: 1,2-propylene oxide=1:0.46:0.07:1.34:1.24:0.35:1.79, take crystal aluminum chloride, six hydration Yttrium trichlorides, Cerium trichloride hexahydrate, ethanol, deionized water, methane amide and 1,2 epoxy prapane;
2) under the condition of 23 ℃ of waters bath with thermostatic control, crystal aluminum chloride in step 1), six hydration Yttrium trichlorides and Cerium trichloride hexahydrate are fully dissolved in the mixing solutions of deionized water, ethanol and methane amide, then add 1-2 propylene oxide, after being fully uniformly mixed, put into sealed vessel, then under 60 ℃ of constant temperatures, be incubated to mixing solutions formation gel;
3) gel is placed under 70 ℃ of constant temperatures and is dried 2 hours, then grinding distribution is incubated 4 hours by it, then H under the condition of 600 ℃
2and N
2under the gas atmosphere that 1:19 mixes by volume, in 800 ℃, be incubated 4 hours, cooling rear acquisition YAG fluorescent microsphere.
Claims (3)
1. be applied to a YAG fluorescent material for semiconductor lighting, it is characterized in that it is by Y
3al
5o
12: Ce
3+the powder that microballoon forms, microsphere diameter is 1～2 μ m.
2. the preparation method that is applied to the YAG fluorescent material of semiconductor lighting claimed in claim 1, comprises the steps:
1) crystal aluminum chloride in mass ratio: six hydration Yttrium trichlorides: Cerium trichloride hexahydrate: ethanol: deionized water: methane amide: 1,2-propylene oxide=1:0.46:0.07～0.14:0.85～1.82:0.62～1.85:0.35～0.70:0.77～1.79, take crystal aluminum chloride, six hydration Yttrium trichlorides, Cerium trichloride hexahydrate, ethanol, deionized water, methane amide and 1,2 epoxy prapane;
2) under the condition of 15～25 ℃ of waters bath with thermostatic control, crystal aluminum chloride in step 1), six hydration Yttrium trichlorides and Cerium trichloride hexahydrate are fully dissolved in the mixing solutions of deionized water, ethanol and methane amide, then add 1-2 propylene oxide, after being fully uniformly mixed, put into sealed vessel, then under 50～60 ℃ of constant temperatures, be incubated to mixing solutions formation gel;
3) by gel under 60～90 ℃ of constant temperatures dry 6～24 hours, then grinding distribution was processed it 2～6 hours at 500～700 ℃, then under reducing atmosphere in 800～1200 ℃ of sintering 2～8 hours, obtain YAG fluorescent material.
3. Application and preparation according to claim 2, in the method for the YAG of semiconductor lighting fluorescent material, is characterized in that described reducing atmosphere is H
2and N
2the gas mixing for 1:19 by volume.
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|---|---|---|---|
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| CN104046357B CN104046357B (en) | 2015-07-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106967430A (en) * | 2017-03-30 | 2017-07-21 | 浙江大学 | A kind of YAG:Mn4+Red fluorescent microspheres and preparation method thereof |
| CN109370590A (en) * | 2018-11-14 | 2019-02-22 | 五邑大学 | A kind of green emitting phosphor and its preparation method and application that near ultraviolet effectively excites |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826514A (en) * | 2012-09-06 | 2012-12-19 | 东南大学 | Method for preparing inorganic oxide aerogel by dehydrating and drying organic solvent |
| CN103551091A (en) * | 2013-11-25 | 2014-02-05 | 北京化工大学 | Method for drying aerogel |
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2014
- 2014-05-26 CN CN201410223326.0A patent/CN104046357B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826514A (en) * | 2012-09-06 | 2012-12-19 | 东南大学 | Method for preparing inorganic oxide aerogel by dehydrating and drying organic solvent |
| CN103551091A (en) * | 2013-11-25 | 2014-02-05 | 北京化工大学 | Method for drying aerogel |
Non-Patent Citations (2)
| Title |
|---|
| YUN CHAN KANG ET AL: "YAG:Ce phosphor particles prepared by ultrasonic spray pyrolysis", 《MATERIALS RESEARCH BULLETIN》 * |
| YUN CHAN KANG ET AL: "YAG:Ce phosphor particles prepared by ultrasonic spray pyrolysis", 《MATERIALS RESEARCH BULLETIN》, vol. 35, 31 December 2000 (2000-12-31) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106967430A (en) * | 2017-03-30 | 2017-07-21 | 浙江大学 | A kind of YAG:Mn4+Red fluorescent microspheres and preparation method thereof |
| CN109370590A (en) * | 2018-11-14 | 2019-02-22 | 五邑大学 | A kind of green emitting phosphor and its preparation method and application that near ultraviolet effectively excites |
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| CN104046357B (en) | 2015-07-15 |
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