CN103571478A - Synthesizing method of broadband-excited white-light LED (Light Emitting Diode) fluorescent powder - Google Patents
Synthesizing method of broadband-excited white-light LED (Light Emitting Diode) fluorescent powder Download PDFInfo
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- CN103571478A CN103571478A CN201310547062.XA CN201310547062A CN103571478A CN 103571478 A CN103571478 A CN 103571478A CN 201310547062 A CN201310547062 A CN 201310547062A CN 103571478 A CN103571478 A CN 103571478A
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- solution
- fluorescent powder
- light led
- white light
- led fluorescent
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- 239000000843 powder Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title abstract description 8
- 230000002194 synthesizing effect Effects 0.000 title abstract 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 230000005284 excitation Effects 0.000 claims abstract description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000000137 annealing Methods 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 11
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000010189 synthetic method Methods 0.000 claims description 13
- 239000000523 sample Substances 0.000 claims description 8
- 239000012488 sample solution Substances 0.000 claims description 8
- 238000000643 oven drying Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 230000002459 sustained effect Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 abstract description 9
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 abstract 3
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Inorganic materials [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 abstract 3
- 229910019614 (NH4)6 Mo7 O24.4H2 O Inorganic materials 0.000 abstract 2
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 abstract 2
- 229910002412 SrMoO4 Inorganic materials 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000005286 illumination Methods 0.000 description 3
- 239000005132 Calcium sulfide based phosphorescent agent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000011430 maximum method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a synthesizing method of broadband-excited white-light LED (Light Emitting Diode) fluorescent powder. The synthesizing method comprises the following steps of: preparing solutions through raw materials, namely, Sr(NO3)2, (NH4)6Mo7O24.4H2O and Eu2O3; adding nitric acid to the Eu2O3 solution until Eu2O3 is reacted completely to obtain Eu<3+>; dropping Eu<3+> to the Sr(NO3)2 solution; adding nitric acid to adjust the pH of the solution to be 2 to 5; dropping the (NH4)6Mo7O24.4H2O solution into the Sr(NO3)2 solution; uniformly agitating; feeding a sampled solution into a reaction kettle; transferring the reaction kettle into an oven to react; washing the reaction product with ethyl alcohol and deionized water; drying through the oven; transferring the dried sample into a muffle furnace; annealing to obtain the target product, namely, white-light LED fluorescent powder SrMoO4:Eu3<+>. The fluorescent powder prepared by the synthesizing method is relatively high in broadband excitation performance and can be applied to a red fluorescent material of white-light LED.
Description
Technical field
The present invention relates to field of light emitting materials, relate in particular to a kind of broadband excitation white light LED fluorescent powder synthetic method.
Background technology
1997, the Ya chemical company of Japan manufactured first white light-emitting diodes in the world.The principle of work of this diode is mainly the blue-light excited YAG:Ce fluorescent material that utilizes blue led chip to send, and makes fluorescent material send gold-tinted, and the gold-tinted that fluorescent material sends and the blue light of transmission are combined to form white light.This makes to lack red spectral component (more than 600nm) in the emmission spectrum of white light LEDs, and the color developing of light source is bad, can meet the requirement of general illumination, but needs higher color developing in the illumination of Ru Hua shop, special lighting field, Operation theatre illumination.White LED lamp mainly contains Y with ruddiness light-converting material
2o
3: Eu
3+and CaS:Eu
2+.Y
2o
3: Eu
3+red-emitting phosphors is most effective red-emitting phosphors under 254nm excites, but long wave ultraviolet light and blue-light excited under excite substantially invalid.CaS:Eu
2+system is the efficient red emission material of a class, can be by UV-light and blue-light excited, and emission peak is 650nm.But sulfide exists synthesis technique to produce the shortcomings such as obnoxious flavour, moisture resistivity are low.Serial of methods is prepared new Eu
3+molybdate, the tungstate red emission system of doping, Eu in this system
3+f-f transition in the excitation intensity of near ultraviolet and blue region, significantly improve, can produce very strong 616nm Eu
3+characteristic red light emission.Use at present maximum methods to comprise high temperature solid-state method, chemical coprecipitation, solvent-thermal method, hydrothermal method etc., wherein, hydrothermal method has many advantages: starting raw material can reach the even mixing on molecular level, preparation temperature is low, and the product purity of preparation is high, and crystal appearance and size are regular, these have all made up the deficiency of pyroprocess etc.: as reactant mixes inhomogeneous, in product, have impurity, produce agglomeration, crystal morphology and size are also irregular.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of broadband excitation white light LED fluorescent powder synthetic method.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of broadband excitation white light LED fluorescent powder synthetic method, comprises the steps:
By raw material Sr (NO
3)
2, (NH
4)
6mo
7o
244H
2o, Eu
2o
3wiring solution-forming, the raw material Sr (NO wherein taking
3)
2, (NH
4)
6mo
7o
244H
2o, Eu
2o
3mass ratio is 1:1:1～1:3:1;
At Eu
2o
3in solution, add nitric acid, until Eu
2o
3react completely and obtain Eu
3+;
By Eu
3+be added drop-wise to Sr (NO
3)
2in solution, and add nitric acid regulator solution pH 2～5;
Again by (NH
4)
6mo
7o
244H
2o solution splashes into Sr (NO
3)
2in solution and stir;
Sample solution is packed in reactor, then put reactor into baking oven reaction;
Reaction product is clean with ethanol and deionized water wash, put into oven drying;
After being dried, sample is put into retort furnace annealing and is obtained target product white light LED fluorescent powder SrMoO
4: Eu
3+.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described by raw material Sr (NO
3)
2, (NH
4)
6mo
7o
244H
2o, Eu
2o
3in wiring solution-forming step, described raw material Sr (NO
3)
2, (NH
4)
6mo
7o
244H
2o, Eu
2o
3purity be: Sr (NO
3)
2(analytical pure), (NH
4)
6mo
7o
244H
2o(analytical pure), Eu
2o(99.99%)
3.
Further, described sample solution is packed in reactor, then reactor is put in baking oven reactions steps, described temperature of reaction kettle is 150～200 ℃, sustained reaction 40～50h.
Further, described that reaction product is clean with ethanol and deionized water wash, put into oven drying step, described purity of alcohol is analytical pure, oven drying temperature is 50～80 ℃, continues 5～8h.
Further, after described being dried, sample is put into retort furnace annealing and is obtained target product white light LED fluorescent powder SrMoO
4: Eu
3+in step, described retort furnace annealing temperature is 500～800 ℃.
The invention has the beneficial effects as follows: the prepared fluorescent material of synthetic method of the present invention has good broadband excitation performance, can be used for the red fluorescence material of white light LEDs.
Accompanying drawing explanation
Fig. 1 is a kind of broadband excitation white light LED fluorescent powder of the present invention synthetic method schema.
Embodiment
Below in conjunction with accompanying drawing, principle of the present invention and feature are described, example, only for explaining the present invention, is not intended to limit scope of the present invention.
As shown in Figure 1, a kind of broadband excitation white light LED fluorescent powder synthetic method, comprises the steps:
By raw material Sr (NO
3)
2, (NH
4)
6mo
7o
244H
2o, Eu
2o
3wiring solution-forming, the raw material Sr (NO wherein taking
3)
2, (NH
4)
6mo
7o
244H
2o, Eu
2o
3mass ratio is 1:1:1～1:3:1;
At Eu
2o
3in solution, add nitric acid, until Eu
2o
3react completely and obtain Eu
3+;
By Eu
3+be added drop-wise to Sr (NO
3)
2in solution, and add nitric acid regulator solution pH 2～5;
Again by (NH
4)
6mo
7o
244H
2o solution splashes into Sr (NO
3)
2in solution and stir;
Sample solution is packed in reactor, then put reactor into baking oven reaction;
Reaction product is clean with ethanol and deionized water wash, put into oven drying;
After being dried, sample is put into retort furnace annealing and is obtained target product white light LED fluorescent powder SrMoO
4: Eu
3+.
Embodiment 1:
Get 10g Sr (NO
3)
2, 10g (NH
4)
6mo
7o
244H
2o, 10g Eu
2o
3wiring solution-forming; At Eu
2o
3in solution, add nitric acid, until Eu
2o
3react completely and obtain Eu
3+; By Eu
3+be added drop-wise to Sr (NO
3)
2in solution, and add nitric acid regulator solution pH 2～5; Again by 10g (NH
4)
6mo
7o
244H
2o solution splashes into Sr (NO
3)
2in solution and stir; Sample solution is packed in reactor, then reactor is put in baking oven at 150 ℃ into sustained reaction 40h; Reaction product is clean with ethanol and deionized water wash, put into baking oven at 50 ℃, continue dry 5h; After being dried, sample is put into annealing at 500 ℃ of retort furnaces and is obtained target product white light LED fluorescent powder SrMoO
4: Eu
3+.
Embodiment 2:
Get 10g Sr (NO
3)
2, 20g (NH
4)
6mo
7o
244H
2o, 10g Eu
2o
3wiring solution-forming; At Eu
2o
3in solution, add nitric acid, until Eu
2o
3react completely and obtain Eu
3+; By Eu
3+be added drop-wise to Sr (NO
3)
2in solution, and add nitric acid regulator solution pH 2～5; Again by 20g (NH
4)
6mo
7o
244H
2o solution splashes into Sr (NO
3)
2in solution and stir; Sample solution is packed in reactor, then reactor is put in baking oven at 180 ℃ into sustained reaction 45h; Reaction product is clean with ethanol and deionized water wash, put into baking oven at 60 ℃, continue dry 6h; After being dried, sample is put into annealing at 700 ℃ of retort furnaces and is obtained target product white light LED fluorescent powder SrMoO
4: Eu
3+.
Embodiment 3:
Get 10g Sr (NO
3)
2, 30g (NH
4)
6mo
7o
244H
2o, 10g Eu
2o
3wiring solution-forming; At Eu
2o
3in solution, add nitric acid, until Eu
2o
3react completely and obtain Eu
3+; By Eu
3+be added drop-wise to Sr (NO
3)
2in solution, and add nitric acid regulator solution pH 2～5; Again by 30g (NH
4)
6mo
7o
244H
2o solution splashes into Sr (NO
3)
2in solution and stir; Sample solution is packed in reactor, then reactor is put in baking oven at 200 ℃ into sustained reaction 50h; Reaction product is clean with ethanol and deionized water wash, put into baking oven at 80 ℃, continue dry 8h; After being dried, sample is put into annealing at 800 ℃ of retort furnaces and is obtained target product white light LED fluorescent powder SrMoO
4: Eu
3+.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (6)
1. a broadband excitation white light LED fluorescent powder synthetic method, is characterized in that, comprises the steps:
By raw material Sr (NO
3)
2, (NH
4)
6mo
7o
244H
2o, Eu
2o
3wiring solution-forming, the raw material Sr (NO wherein taking
3)
2, (NH
4)
6mo
7o
244H
2o, Eu
2o
3mass ratio is 1:1:1～1:3:1;
At Eu
2o
3in solution, add nitric acid, until Eu
2o
3react completely and obtain Eu
3+;
By Eu
3+be added drop-wise to Sr (NO
3)
2in solution, and add nitric acid regulator solution pH 2～5;
Again by (NH
4)
6mo
7o
244H
2o solution splashes into Sr (NO
3)
2in solution and stir;
Sample solution is packed in reactor, then put reactor into baking oven reaction;
Reaction product is clean with ethanol and deionized water wash, put into oven drying;
After being dried, sample is put into retort furnace annealing and is obtained target product white light LED fluorescent powder SrMoO
4: Eu
3+.
2. a kind of broadband excitation white light LED fluorescent powder synthetic method according to claim 1, is characterized in that, described by raw material Sr (NO
3)
2, (NH
4)
6mo
7o
244H
2o, Eu
2o
3in wiring solution-forming step, described raw material Sr (NO
3)
2, (NH
4)
6mo
7o
244H
2o, Eu
2o
3purity be: Sr (NO
3)
2(analytical pure), (NH
4)
6mo
7o
244H
2o(analytical pure), Eu
2o(99.99%)
3.
3. a kind of broadband excitation white light LED fluorescent powder synthetic method according to claim 1, it is characterized in that, described sample solution is packed in reactor, then reactor is put in baking oven reactions steps, described temperature of reaction kettle is 150～200 ℃, sustained reaction 40～50h.
4. a kind of broadband excitation white light LED fluorescent powder synthetic method according to claim 1, is characterized in that, described that reaction product is clean with ethanol and deionized water wash, put into oven drying step, described purity of alcohol is analytical pure, and oven drying temperature is 50～80 ℃, continues 5～8h.
5. according to the arbitrary described a kind of broadband excitation white light LED fluorescent powder synthetic method of claim 1 to 4, it is characterized in that, after described being dried, sample is put into retort furnace annealing and is obtained target product white light LED fluorescent powder SrMoO
4: Eu
3+in step, described retort furnace annealing temperature is 500～800 ℃.
6. according to the synthetic broadband excitation white light LED fluorescent powder of the arbitrary described broadband excitation white light LED fluorescent powder synthetic method of claim 1 to 5.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310547062.XA CN103571478A (en) | 2013-11-07 | 2013-11-07 | Synthesizing method of broadband-excited white-light LED (Light Emitting Diode) fluorescent powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310547062.XA CN103571478A (en) | 2013-11-07 | 2013-11-07 | Synthesizing method of broadband-excited white-light LED (Light Emitting Diode) fluorescent powder |
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| Publication Number | Publication Date |
|---|---|
| CN103571478A true CN103571478A (en) | 2014-02-12 |
Family
ID=50044202
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|---|---|---|---|
| CN201310547062.XA Pending CN103571478A (en) | 2013-11-07 | 2013-11-07 | Synthesizing method of broadband-excited white-light LED (Light Emitting Diode) fluorescent powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670624A (en) * | 2016-01-26 | 2016-06-15 | 中南大学 | Fluorescent powder capable of realizing blue light-white light conversion based on ultraviolet excitation and preparation method of fluorescent powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090174310A1 (en) * | 2008-01-03 | 2009-07-09 | Thomas Vogt | White Light Phosphors for Fluorescent Lighting |
| WO2012079226A1 (en) * | 2010-12-14 | 2012-06-21 | 海洋王照明科技股份有限公司 | Tungstate fluorescent materials and preparation methods thereof |
-
2013
- 2013-11-07 CN CN201310547062.XA patent/CN103571478A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090174310A1 (en) * | 2008-01-03 | 2009-07-09 | Thomas Vogt | White Light Phosphors for Fluorescent Lighting |
| WO2012079226A1 (en) * | 2010-12-14 | 2012-06-21 | 海洋王照明科技股份有限公司 | Tungstate fluorescent materials and preparation methods thereof |
Non-Patent Citations (4)
| Title |
|---|
| P. S. DUTTA 等: "Eu3+ Activated Molybdate and Tungstate Based Red Phosphors", 《JOURNAL OF SOLID STATE SCIENCE AND TECHNOLOGY》 * |
| 唐红霞等: "发光二极管用红色荧光粉SrMoO4:Eu3+的制备和发射性质", 《物理学报》 * |
| 孟献丰等: "水热法制备SrMoO4:Eu3+红色发光材料及其发光性能", 《功能材料》 * |
| 戴沈华等: "微波水热法合成Eu3+掺杂的SrMoO4红色荧光粉", 《南京工业大学学报(自然科学版)》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670624A (en) * | 2016-01-26 | 2016-06-15 | 中南大学 | Fluorescent powder capable of realizing blue light-white light conversion based on ultraviolet excitation and preparation method of fluorescent powder |
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Application publication date: 20140212 |