CN102786929A - Red phosphor - Google Patents
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- CN102786929A CN102786929A CN2012102686098A CN201210268609A CN102786929A CN 102786929 A CN102786929 A CN 102786929A CN 2012102686098 A CN2012102686098 A CN 2012102686098A CN 201210268609 A CN201210268609 A CN 201210268609A CN 102786929 A CN102786929 A CN 102786929A
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- fluorescence powder
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 238000005303 weighing Methods 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 27
- 238000001354 calcination Methods 0.000 abstract description 20
- 230000005284 excitation Effects 0.000 abstract description 17
- 239000000203 mixture Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 3
- 238000004020 luminiscence type Methods 0.000 abstract description 2
- 238000001228 spectrum Methods 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 239000004570 mortar (masonry) Substances 0.000 description 9
- 241001025261 Neoraja caerulea Species 0.000 description 4
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 206010023126 Jaundice Diseases 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Images
Classifications
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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
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- Luminescent Compositions (AREA)
Abstract
The invention relates to a red phosphor, which belongs to the field of luminescence techniques and is expressed by the general chemical formula of A(3-2x)BxCxDO6, wherein A is at least one of Ca, Sr and Ba, B is at least one of Li, Na and K, C is Eu, D is at least one of W and Mo, and x is larger than 0 and is smaller than or equal to 0.6. The preparation method comprises the following steps: weighing and uniformly grinding the materials according the proportion of the general chemical formula, calcining the mixture for 6-20 h at 1000-1400 DEG C, cooling the mixture to a room temperature, calcining the mixture for 6-20 h at 1000-1400 DEG C again, and crushing after the mixture is cooled. The red phosphor has the advantages of good chemical stability and high excitation efficiency, can be matched with near-ultraviolet or blue light LEDs, and is a novel red phosphor for white-light LEDs.
Description
Technical field
The present invention relates to a kind of red fluorescence powder, belong to the luminescence technology field.
Background technology
The birth of semiconductor light emitting diode device (LED) is pointed out new hope for illumination.LED is owing to have characteristics such as less energy-consumption, high-level efficiency, long lifetime, compared significant advantage with lighting sources commonly used such as in the past incandescent light, electricity-saving lamps.The white light implementation that at present with LED is main a new generation's illumination system has following several kinds: the first, and through the led chip (normally red-green-blue) of different colours is integrated and be mixed into white light.But the bias voltage of different chips is different, and circuit control is had relatively high expectations, and cost is very high.Second kind is the lighting theory of using for reference luminescent lamp, at led chip surface-coated fluorescent material, obtains white light.At first develop yttrium aluminum garnet (YAG) fluorescent material of jaundice light like this year day in 1996 Japan Ri Ya company, cooperate blue-ray LED to obtain high efficiency white light source.Blue light excitation YAG fluorescent material, the part blue light is absorbed by fluorescent material and inspires gold-tinted, and the rest part blue light becomes white light with yellow light mix.This white light implementation cost is lower, be the mode that extensively adopts at present, yet this fluorescent material lacks the ruddiness composition, so colour rendering index is bad, and its colour temperature is higher, and is difficult to regulate, and can not obtain warm radiant.Also having the auxiliary mode that produces white light of a kind of fluorescent material is to utilize near ultraviolet LED to excite red-green-blue fluorescent material to mix to realize white light; This ultraviolet leds has stronger excitation intensity and the efficiency of conversion of Geng Gao; Yet wherein red fluorescence powder is lower with respect to bluish-green light-emitting phosphor efficient, like Y
2O
2S:Eu fluorescent material, energy conversion efficiency is low, and poor stability.
At present, still lack excellent performance on the market, use three primary colors fluorescent powder based on the white-light illuminating LED of near ultraviolet or blue light diode, especially can be by near-ultraviolet light and blue-light excited red fluorescence powder.
Summary of the invention
The purpose of this invention is to provide a kind of near ultraviolet or blue-light excited red fluorescence powder and preparation method thereof; The ruddiness composition that makes it solve emmission spectrum in prior art is few and make its colour rendering index on the low side; The problem that can not synthesize single white light; And make its chemicalstability good, launching efficiency is high, can be simultaneously by near ultraviolet and blue-light excited.
The chemical general formula of red fluorescence powder of the present invention is A
3-2xB
xC
xDO
6, wherein A is at least a among Ca, Sr, the Ba, and B is at least a among Li, Na, the K, and C is Eu, and D is at least a among W, the Mo, 0<x≤0.6.
In the said structure formula, preferred A is Ca, and B is K, and C is Eu, and D is W.At this moment, red fluorescence powder is luminous best.
The preparation method of red fluorescence powder of the present invention is:
(1) takes by weighing the carbonate of following raw material: A, the carbonate of B, the oxide compound of C and the oxide compound of D by the proportioning in the above-mentioned chemical general formula;
(2) the former abrasive lapping and the mixing that step (1) are taken by weighing;
(3) raw material of mixing is calcined 6-20h at 1000-1400 ℃, be cooled to room temperature then, calcine 6-20h at 1000 ℃-1400 ℃ again after the grinding;
(4) grind after the product cooling that step (3) obtains, promptly get.
Preferably in raw material, add raw material total mass 3-4 ethanol doubly when grinding in the step (2), can make grinding more abundant, easily mixing.
Above-mentioned preparation method is a solid-phase synthesis, and fluorescent material of the present invention also can adopt chemical synthesis, for example can adopt the precipitator method or sol-gel method to carry out chemosynthesis.
Red fluorescence powder chemicalstability of the present invention is good; Launching efficiency is high; Can excite at UV-light (300nm), near ultraviolet (395nm), blue light (466nm) and obtain to be positioned at the emitting red light about 618nm down; Can mate with near ultraviolet and blue-ray LED, be a kind of novel red fluorescent powder for white radiation LED.
Description of drawings
Fig. 1 is Y
2O
2The exciting light spectrogram of fluorescent material and emmission spectrum figure in the S:Eu and the embodiment of the invention 1.
Fig. 2 is the exciting light spectrogram of fluorescent material in the embodiment of the invention 2.
Fig. 3 is the emmission spectrum figure of fluorescent material among the embodiment of the invention 3-5.
Fig. 4 is the graph of relation of the luminous intensity and the x value of fluorescent material.
Fig. 5 is the emmission spectrum figure of fluorescent material in the embodiment of the invention 7.
Fig. 6 is the exciting light spectrogram and the emmission spectrum figure of fluorescent material in the embodiment of the invention 8.
Fig. 7 is the exciting light spectrogram and the emmission spectrum figure of fluorescent material in the embodiment of the invention 9.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described further.
Embodiment 1
Preparation red fluorescence powder Ca
2K
0.5Eu
0.5WO
6
Take by weighing CaCO
3(analytical pure) 2.0017 grams, K
2CO
3(analytical pure) 0.3455 gram, Eu
2O
3(3N) 0.8798 gram, WO
3(analytical pure) 2.3184 grams.Add 17 gram ethanol, fully grind with agate mortar, send into retort furnace after mixing at 1100 ℃ of calcining 6h, again at 1200 ℃ of calcining 18h, the cooling back grinds, and promptly gets after the cooling.
The emmission spectrum and the excitation spectrum of gained fluorescent material are seen Fig. 1, can find out its PLE at 300nm by Fig. 1,395nm; All there is stronger exciting at the 466nm place; Wherein near the charge transfer state transition that comes from W-O of the broadband excitation the 300nm excites, and other wire excites and then comes from Eu ionic f-f transition and excite, and its excitation wavelength just in time is positioned near ultraviolet and blue light position; With led chip excitation wavelength coupling, be fit near ultraviolet and blue-ray LED and excite.The main emission peak of its emission spectrum sends bright red light at 618nm.Y in the comparison diagram 1
2O
2S:Eu and Ca
2K
0.5Eu
0.5WO
6The PLE of two kinds of materials can be seen near ultraviolet and blue light portion C a
2K
0.5Eu
0.5WO
6The advantage that significantly excites is arranged.When the exciting light with the 395nm of identical wavelength excites two samples under the same conditions, Ca
2K
0.5Eu
0.5WO
6Emissive porwer be Y
2O
2Four times of S:Eu have good luminescent properties more.
Embodiment 2
Preparation red fluorescence powder Ca
2.8K
0.1Eu
0.1W
0.9Mo
0.1O
6
Take by weighing CaCO
3(analytical pure) 2.8028 grams, K
2CO
3(analytical pure) 0.0691 gram, Eu
2O
3(3N) 0.176 gram, WO
3(analytical pure) 2.0865 grams, MoO
3(analytical pure) 0.1439 gram.Add 16 gram ethanol, fully grind with agate mortar, send into retort furnace after mixing at 1000 ℃ of calcining 16h, again at 1300 ℃ of calcining 10h, the cooling back grinds, and promptly gets after the cooling.
The excitation spectrum of gained fluorescent material is seen Fig. 2, can not found out with carrying out the Mo doped samples by Fig. 2 and compare that its banded PLE becomes wideer; Expand near ultraviolet long wavelength direction; Its launching efficiency is uprised, and at 395nm, the 466nm place has still kept original excitation intensity; Wideer with led chip coupling excitation wavelength range, be fit near ultraviolet and blue-ray LED and excite.
Embodiment 3
Preparation red fluorescence powder Ca
2.9Li
0.05Eu
0.05WO
6
Take by weighing CaCO by stoicheiometry
3(analytical pure) 2.9026 grams, Li
2CO
3(analytical pure) 0.0167 gram, Eu
2O
3(3N) 0.088 gram, WO
3(analytical pure) 2.3184 grams.Add 20 gram ethanol, fully grind with agate mortar, send into retort furnace after mixing at 1200 ℃ of calcining 12h, again at 1200 ℃ of calcining 12h, the cooling back grinds, and promptly gets after the cooling.The emmission spectrum of gained fluorescent material is seen Fig. 3 (excitation wavelength is 395nm).
Embodiment 4
Preparation red fluorescence powder Ca
2.9Na
0.05Eu
0.05WO
6
Take by weighing CaCO by stoicheiometry
3(analytical pure) 2.9026 grams, Na
2CO
3(analytical pure) 0.0207 gram, Eu
2O
3(3N) 0.088 gram, WO
3(analytical pure) 2.3184 grams.Add 20 gram ethanol, fully grind with agate mortar, send into retort furnace after mixing at 1200 ℃ of calcining 12h, again at 1200 ℃ of calcining 12h, the cooling back grinds, and promptly gets after the cooling.The emmission spectrum of gained fluorescent material is seen Fig. 3 (excitation wavelength is 395nm).
Embodiment 5
Preparation red fluorescence powder Ca
2.9K
0.05Eu
0.05WO
6
Take by weighing CaCO by stoicheiometry
3(analytical pure) 2.9026 grams, K
2CO
3(analytical pure) 0.0345 gram, Eu
2O
3(3N) 0.088 gram, WO
3(analytical pure) 2.3184 grams.Add 20 gram ethanol, fully grind with agate mortar, send into retort furnace after mixing at 1200 ℃ of calcining 12h, again at 1200 ℃ of calcining 12h, the cooling back grinds, and promptly gets after the cooling.The emmission spectrum of gained fluorescent material is seen Fig. 3 (excitation wavelength is 395nm).
Can find out K by Fig. 3
+Do the charge compensation agent with respect to Li
+, Na
+Effect is best, and three kinds of charge compensation agent can make the luminous of fluorescent material be enhanced.It excites and emission figure spectral shape does not change.
Embodiment 6
Preparation red fluorescence powder Ca
2.8K
0.1Eu
0.1WO
6
Take by weighing WO by stoicheiometry
3(analytical pure) 2.3184 grams, CaCO
3(analytical pure) 2.8028 grams, K
2CO
3(analytical pure) 0.0691 gram, Eu
2O
3(3N) 0.176 gram.Add 20 gram ethanol, fully grind with agate mortar, send into retort furnace after mixing at 1400 ℃ of calcining 10h, again at 1300 ℃ of calcining 8h, the cooling back grinds, and promptly gets after the cooling.
Through getting 0<different x value between x≤0.6 can prepare the Ca of different x values in order to last method
3-2xK
xEu
xWO
6Fluorescent material, fluorescent material Ca
3-2xK
xEu
xWO
6Luminous intensity and the value graph of relation of x see Fig. 4, can find out by Fig. 4 at K
+Do under the situation of charge compensation agent, luminous intensity increases with the increase of x value, and when the x value surpassed 0.5, luminous intensity began to descend, and the optimum value of x value is between 0.4 ~ 0.6.
Embodiment 7
Preparation red fluorescence powder Ca
2K
0.25Na
0.25Eu
0.5WO
6
Take by weighing CaCO
3(analytical pure) 2.0017 grams, K
2CO
3(analytical pure) 0.1727 gram, Na
2CO
3(analytical pure) 0.1324 gram, Eu
2O
3(3N) 0.8798 gram, WO
3(analytical pure) 2.3184 grams.Add 21 gram ethanol, fully grind with agate mortar, send into retort furnace after mixing at 1200 ℃ of calcining 12h, again at 1200 ℃ of calcining 12h, the cooling back grinds, and promptly gets after the cooling.
Mix the red fluorescence powder Ca of K, Na altogether
2K
0.25Na
0.25Eu
0.5WO
6Excite with emmission spectrum and see Fig. 5; Can find out by Fig. 5 and to mix K, Na altogether and to mix K separately or Na plays same effect; But some small variations appear; The relative excitation intensity at 395nm and 466nm place changes to some extent, and with respect to the relative excitation intensity grow of the sample of mixing K separately (embodiment 1) 466nm, but the introducing of Na can make overall excitation intensity descend to some extent with respect to the sample of mixing K separately (embodiment 1).
Embodiment 8
Preparation red fluorescence powder CaSrK
0.5Eu
0.5WO
6
Take by weighing CaCO
3(analytical pure) 1.0009 grams, SrCO
3(analytical pure) 1.4763 grams, K
2CO
3(analytical pure) 0.3455 gram, Eu
2O
3(3N) 0.8798 gram, WO
3(analytical pure) 2.3184 grams.Add 24 gram ethanol, fully grind with agate mortar, send into retort furnace after mixing at 1200 ℃ of calcining 12h, again at 1200 ℃ of calcining 12h, the cooling back grinds, and promptly gets after the cooling.
Mix the red fluorescence powder CaSrK of Sr altogether
0.5Eu
0.5WO
6Excite with emmission spectrum and see Fig. 6, can find out that by Fig. 6 the introducing of Sr makes PLE that bigger variation take place, overall excitation intensity has bigger decline, the band excitation intensity decline at 300nm place is apparent in view, and the relative excitation intensity at 466nm place becomes the strongest.
Embodiment 9
Preparation red fluorescence powder Sr
2K
0.5Eu
0.5WO
6
Take by weighing SrCO by stoicheiometry
3(analytical pure) 2.9526 grams, K
2CO
3(analytical pure) 0.3455 gram, WO
3(analytical pure) 2.3184 grams, Eu
2O
3(3N) 0.8798 gram.Add 20 gram ethanol, fully grind with agate mortar, send into retort furnace after mixing at 1300 ℃ of calcining 18h, again at 1100 ℃ of calcining 12h, the cooling back grinds, and promptly gets after the cooling.Excite and the emmission spectrum of gained fluorescent material are seen Fig. 7.
Claims (4)
1. a red fluorescence powder is characterized in that, chemical general formula is A
3-2xB
xC
xDO
6, wherein A is at least a among Ca, Sr, the Ba, and B is at least a among Li, Na, the K, and C is Eu, and D is at least a among W, the Mo, 0<x≤0.6.
2. red fluorescence powder as claimed in claim 1 is characterized in that, A is Ca, and B is K, and C is Eu, and D is W.
3. the preparation method of claim 1 or 2 said red fluorescence powders is characterized in that, comprises the steps:
(1) takes by weighing the carbonate of following raw material: A, the carbonate of B, the oxide compound of C and the oxide compound of D by the proportioning in the chemical general formula;
(2) the former abrasive lapping and the mixing that step (1) are taken by weighing;
(3) raw material of mixing is calcined 6-20h at 1000 ℃-1400 ℃, be cooled to room temperature then, calcine 6-20h at 1000 ℃-1400 ℃ again after the grinding;
(4) the product cooling back that step (3) is obtained grinds, and promptly gets.
4. the preparation method of red fluorescence powder as claimed in claim 3 is characterized in that, in raw material, adds raw material total mass 3-4 ethanol doubly when grinding in the step (2).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102686098A CN102786929B (en) | 2012-07-31 | 2012-07-31 | Red phosphor |
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|---|---|---|---|
| CN2012102686098A CN102786929B (en) | 2012-07-31 | 2012-07-31 | Red phosphor |
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| Publication Number | Publication Date |
|---|---|
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| CN102786929B CN102786929B (en) | 2013-11-13 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105505389A (en) * | 2014-09-22 | 2016-04-20 | 青岛农业大学 | Near ultraviolet light or blue light excited white light LED fluorescent material and preparation method thereof |
| CN105969352A (en) * | 2016-06-04 | 2016-09-28 | 王颖畅 | Red phosphor for LED light source and preparation method of red phosphor |
| CN109705864A (en) * | 2018-11-23 | 2019-05-03 | 长春理工大学 | A kind of red fluorescence powder and preparation method thereof that luminous efficiency is high |
| CN110055066A (en) * | 2019-03-21 | 2019-07-26 | 惠州学院 | A kind of red fluorescence powder and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962545A (en) * | 2010-09-26 | 2011-02-02 | 中山大学 | Alkaline earth molybdate rare earth light conversion material and preparation method thereof |
-
2012
- 2012-07-31 CN CN2012102686098A patent/CN102786929B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962545A (en) * | 2010-09-26 | 2011-02-02 | 中山大学 | Alkaline earth molybdate rare earth light conversion material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| S.YE ET AL: "Photoluminescence and energy transfer of phosphor series Ba2−zSrzCaMo1−yWyO6Eu,Li for white light UVLED applications", 《APPLIED PHYSICS B》 * |
| S.YE ET AL: "Photoluminescence and energy transfer of phosphor series Ba2−zSrzCaMo1−yWyO6Eu,Li for white light UVLED applications", 《APPLIED PHYSICS B》, vol. 91, 7 May 2008 (2008-05-07), XP019627025 * |
| XUELIANG ZHANG ET AL: "Luminescence properties of Sr2ZnWO6:Eu3+ phosphors", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105505389A (en) * | 2014-09-22 | 2016-04-20 | 青岛农业大学 | Near ultraviolet light or blue light excited white light LED fluorescent material and preparation method thereof |
| CN105969352A (en) * | 2016-06-04 | 2016-09-28 | 王颖畅 | Red phosphor for LED light source and preparation method of red phosphor |
| CN109705864A (en) * | 2018-11-23 | 2019-05-03 | 长春理工大学 | A kind of red fluorescence powder and preparation method thereof that luminous efficiency is high |
| CN110055066A (en) * | 2019-03-21 | 2019-07-26 | 惠州学院 | A kind of red fluorescence powder and preparation method thereof |
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| CN102786929B (en) | 2013-11-13 |
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Granted publication date: 20131113 Termination date: 20160731 |