CN102786929B - Red phosphor - Google Patents
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- CN102786929B CN102786929B CN2012102686098A CN201210268609A CN102786929B CN 102786929 B CN102786929 B CN 102786929B CN 2012102686098 A CN2012102686098 A CN 2012102686098A CN 201210268609 A CN201210268609 A CN 201210268609A CN 102786929 B CN102786929 B CN 102786929B
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- calcining
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- red fluorescence
- fluorescent material
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 21
- 238000000227 grinding Methods 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 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
- 230000005284 excitation Effects 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 3
- 238000004020 luminiscence type Methods 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 238000000695 excitation spectrum Methods 0.000 description 9
- 239000004570 mortar (masonry) Substances 0.000 description 9
- 238000001228 spectrum Methods 0.000 description 5
- 241001025261 Neoraja caerulea Species 0.000 description 4
- 238000000295 emission spectrum Methods 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
- 238000005286 illumination Methods 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000002500 ions Chemical class 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 having the characteristics such as less energy-consumption, high-level efficiency, long lifetime, with lighting sources commonly used such as in the past incandescent light, electricity-saving lamps, compared significant advantage.At present the white light implementation take LED as main a new generation's illumination system has following several: the first, and integrated and be mixed into white light by the LED chip with different colours (normally red-green-blue).But the bias voltage of different chips is different, and circuit is controlled and had relatively high expectations, and cost is very high.The second is the lighting theory of using for reference luminescent lamp,, at LED chip surface-coated fluorescent material, obtains white light.At first Ri Ya company as Japanese in this year day in 1996 develops yttrium aluminum garnet (YAG) fluorescent material of Yellow light-emitting low temperature, coordinates 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 efficiency, as Y
2O
2S:Eu fluorescent material, energy conversion efficiency is low, and poor stability.
At present, still lack excellent performance on market, based on the white-light illuminating LED three primary colors fluorescent powder 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 chemical stability 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 in Ca, Sr, Ba, and B is at least a in Li, Na, K, and C is Eu, and D is at least a in W, 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) take 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 above-mentioned chemical general formula;
(2) the former abrasive lapping that step (1) is taken also mixes;
The raw material that (3) will mix, at 1000-1400 ℃ of calcining 6-20h, then is cooled to room temperature, calcines 6-20h at 1000 ℃-1400 ℃ again after grinding;
(4) the cooling rear grinding of product that obtains of step (3), obtain.
Preferably add raw material total mass 3-4 ethanol doubly in raw material while grinding in step (2), can make grinding more abundant, easily mix.
Above-mentioned preparation method is 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 chemical stability of the present invention is good, launching efficiency is high, can excite lower acquisition to be positioned at the emitting red light of 618nm left and right at UV-light (300nm), near ultraviolet (395nm), blue light (466nm), 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 utilizing emitted light spectrogram in S:Eu and the embodiment of the present invention 1.
Fig. 2 is the exciting light spectrogram of fluorescent material in the embodiment of the present invention 2.
Fig. 3 is the utilizing emitted light spectrogram of fluorescent material in embodiment of the present invention 3-5.
Fig. 4 is the graph of relation of luminous intensity and the x value of fluorescent material.
Fig. 5 is the utilizing emitted light spectrogram of fluorescent material in the embodiment of the present invention 7.
Fig. 6 is exciting light spectrogram and the utilizing emitted light spectrogram of fluorescent material in the embodiment of the present invention 8.
Fig. 7 is exciting light spectrogram and the utilizing emitted light spectrogram of fluorescent material in the embodiment of the present invention 9.
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing.
Embodiment 1
Prepare red fluorescence powder Ca
2K
0.5Eu
0.5WO
6
Take 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, with agate mortar, fully grind, send into after mixing retort furnace 1100 ℃ the calcining 6h, cooling after again 1200 ℃ the calcining 18h, cooling rear grinding, obtain.
Emmission spectrum and the excitation spectrum of gained fluorescent material are seen Fig. 1, its excitation spectrum is at 300nm as seen from Figure 1,395nm, there is stronger exciting at the 466nm place, wherein near the charge transfer state transition that comes from W-O of the broadband excitation 300nm excites, and other wire excites the f-f transition that comes from the Eu ion to 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, at 618nm, sends bright red light.Y in comparison diagram 1
2O
2S:Eu and Ca
2K
0.5Eu
0.5WO
6The excitation spectrum of bi-material can be seen near ultraviolet and blue light part Ca
2K
0.5Eu
0.5WO
6The advantage that significantly excites is arranged.When the exciting light of the 395nm with identical wavelength excites two samples under the same conditions, Ca
2K
0.5Eu
0.5WO
6Emissive porwer be Y
2O
2More than four times of S:Eu, have good luminescent properties.
Embodiment 2
Prepare red fluorescence powder Ca
2.8K
0.1Eu
0.1W
0.9Mo
0.1O
6
Take 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, with agate mortar, fully grind, send into after mixing retort furnace 1000 ℃ the calcining 16h, cooling after again 1300 ℃ the calcining 10h, cooling rear grinding, obtain.
The excitation spectrum of gained fluorescent material is seen Fig. 2, as seen from Figure 2 with do not carry out the Mo doped samples and compare, its banded excitation spectrum becomes wider, expand near ultraviolet long wavelength direction, its launching efficiency is uprised, and at 395nm, the 466nm place has still kept original excitation intensity, wider with LED chip coupling excitation wavelength range, be fit near ultraviolet and blue-ray LED and excite.
Embodiment 3
Prepare red fluorescence powder Ca
2.9Li
0.05Eu
0.05WO
6
Take 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, with agate mortar, fully grind, send into after mixing retort furnace 1200 ℃ the calcining 12h, cooling after again 1200 ℃ the calcining 12h, cooling rear grinding, obtain.The emmission spectrum of gained fluorescent material is seen Fig. 3 (excitation wavelength is 395nm).
Embodiment 4
Prepare red fluorescence powder Ca
2.9Na
0.05Eu
0.05WO
6
Take 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, with agate mortar, fully grind, send into after mixing retort furnace 1200 ℃ the calcining 12h, cooling after again 1200 ℃ the calcining 12h, cooling rear grinding, obtain.The emmission spectrum of gained fluorescent material is seen Fig. 3 (excitation wavelength is 395nm).
Embodiment 5
Prepare red fluorescence powder Ca
2.9K
0.05Eu
0.05WO
6
Take 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, with agate mortar, fully grind, send into after mixing retort furnace 1200 ℃ the calcining 12h, cooling after again 1200 ℃ the calcining 12h, cooling rear grinding, obtain.The emmission spectrum of gained fluorescent material is seen Fig. 3 (excitation wavelength is 395nm).
As seen from Figure 3, K
+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
Prepare red fluorescence powder Ca
2.8K
0.1Eu
0.1WO
6
Take 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, with agate mortar, fully grind, send into after mixing retort furnace 1400 ℃ the calcining 10h, cooling after again 1300 ℃ the calcining 8h, cooling rear grinding, obtain.
, by getting x values different between 0＜x≤0.6, can prepare the Ca of different x values in order to upper 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, as seen from Figure 4 at K
+Do in 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 started to descend, and the optimum value of x value is between 0.4 ~ 0.6.
Embodiment 7
Prepare red fluorescence powder Ca
2K
0.25Na
0.25Eu
0.5WO
6
Take 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, with agate mortar, fully grind, send into after mixing retort furnace 1200 ℃ the calcining 12h, cooling after again 1200 ℃ the calcining 12h, cooling rear grinding, obtain.
Mix altogether the red fluorescence powder Ca of K, Na
2K
0.25Na
0.25Eu
0.5WO
6Excitation and emission spectra see Fig. 5, mixing altogether K, Na and mixing separately K or Na plays same effect as seen from Figure 5, but the variation that some are small appears, the relative excitation intensity at 395nm and 466nm place changes to some extent, with respect to the sample of mixing separately K (embodiment 1) 466nm relative excitation intensity grow, but the introducing of Na can make overall excitation intensity descend to some extent with respect to the sample of mixing separately K (embodiment 1).
Embodiment 8
Prepare red fluorescence powder CaSrK
0.5Eu
0.5WO
6
Take 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, with agate mortar, fully grind, send into after mixing retort furnace 1200 ℃ the calcining 12h, cooling after again 1200 ℃ the calcining 12h, cooling rear grinding, obtain.
Mix altogether the red fluorescence powder CaSrK of Sr
0.5Eu
0.5WO
6Excitation and emission spectra see Fig. 6, the introducing of Sr makes excitation spectrum that larger variation occur as seen from Figure 6, overall excitation intensity has larger 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
Prepare red fluorescence powder Sr
2K
0.5Eu
0.5WO
6
Take 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, with agate mortar, fully grind, send into after mixing retort furnace 1300 ℃ the calcining 18h, cooling after again 1100 ℃ the calcining 12h, cooling rear grinding, obtain.The excitation and emission spectra of gained fluorescent material is seen Fig. 7.
Claims (2)
1. a red fluorescence powder, is characterized in that, chemical general formula is A
3-2xB
xC
xDO
6, wherein A is Ca, and B is K, and C is Eu, and D is W, 0＜x≤0.6.
2. the preparation method of the described red fluorescence powder of claim 1, is characterized in that, comprises the steps:
(1) take 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 chemical general formula;
(2) the former abrasive lapping that step (1) is taken also mixes;
The raw material that (3) will mix, at 1000 ℃-1400 ℃ calcining 6-20h, then is cooled to room temperature, calcines 6-20h at 1000 ℃-1400 ℃ again after grinding;
(4) the cooling rear grinding of product that step (3) is obtained, obtain;
Add raw material total mass 3-4 ethanol doubly while grinding in step (2) in raw material.
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| 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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|---|---|
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| CN102786929B true CN102786929B (en) | 2013-11-13 |
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| 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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| CN101962545B (en) * | 2010-09-26 | 2013-07-10 | 中山大学 | Alkaline earth molybdate rare earth light conversion material and preparation method thereof |
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2012
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Non-Patent Citations (2)
| Title |
|---|
| Luminescence properties of Sr2ZnWO6:Eu3+ phosphors;Xueliang Zhang et al;《Journal of Alloys and Compounds》;20080317;第469卷;第L6-L9页 * |
| Xueliang Zhang et al.Luminescence properties of Sr2ZnWO6:Eu3+ phosphors.《Journal of Alloys and Compounds》.2008,第469卷第L6-L9页. |
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