CN103788943B - A kind of near ultraviolet excitated borate blue fluorescent powder and preparation method thereof - Google Patents
A kind of near ultraviolet excitated borate blue fluorescent powder and preparation method thereof Download PDFInfo
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- CN103788943B CN103788943B CN201410081670.0A CN201410081670A CN103788943B CN 103788943 B CN103788943 B CN 103788943B CN 201410081670 A CN201410081670 A CN 201410081670A CN 103788943 B CN103788943 B CN 103788943B
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- fluorescent powder
- blue fluorescent
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- 239000000843 powder Substances 0.000 title claims abstract description 42
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 2
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 2
- AMGRXJSJSONEEG-UHFFFAOYSA-L strontium dichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Sr]Cl AMGRXJSJSONEEG-UHFFFAOYSA-L 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 239000010703 silicon Substances 0.000 abstract description 5
- 229910021421 monocrystalline silicon Inorganic materials 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 230000004044 response Effects 0.000 abstract description 3
- 239000003086 colorant Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 230000003595 spectral effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 1
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/52—PV systems with concentrators
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Abstract
The invention discloses a kind of near ultraviolet excitated borate blue fluorescent powder and preparation method thereof, the general formula of its combination matching is: Sr
2-2xclO
3: xTm
3+, xLi
+, wherein 0≤x≤0.2; Its preparation method comprises the steps: (1) takes each feed composition according to described combination matching general formula; (2) each feed composition fully mixed and grind to obtain evengranular fine powder through first time; (3) by above-mentioned fine powder through pre-burning, calcining, cooling, through second time grinding, obtain described borate blue fluorescent powder.Borate blue fluorescent powder of the present invention can be excited by the near-ultraviolet ray of 358nm, and has blue emission at 457nm, may be used near ultraviolet excitated three primary colors fluorescent powder system; For the preparation of monocrystalline silicon battery, monocrystalline silicon battery can also be increased to the spectral response of sunlight.Improve crystal silicon battery efficiency; Preparation method of the present invention adopts high temperature process heat method, and Heating temperature is low, less energy consumption; The equipment used is single, and facility investment is few, and technique is simple, with low cost, and product performance are stablized.
Description
Technical field
The present invention is specifically related to a kind of near ultraviolet excitated borate blue fluorescent powder and preparation method thereof.
Background technology
White light LEDs because it is energy-conservation, efficient, long lifetime and environmental protection be called as solid lighting lamp of new generation and the fields such as entering rapidly illumination, automobile, personal communication apparatus that receives much concern.This novel green light source must for the lighting source of a new generation, to energy-saving and environmental protection, provide the aspects such as the quality of life of people to have extensively and profound significance.The scheme of current acquisition white light LEDs mainly contains two kinds, and one is that multi-chip is combined.Respectively by launching the LED combination of red, green, blue, mixing three kinds of light and forming white-light emitting.It is high that the white light of this scheme has brightness, stability and the advantage such as color developing is good, but cost is high, and driving circuit is complicated, does not have large-scale production at present.Another kind is fluorescent material conversion, excites the YAG:Ce3+ fluorescent material sending out yellow fluorescence, remaining blue light and gold-tinted are compounded to form white light with blue-ray LED.The white light shortage red color components colour temperature obtained when this scheme is higher, and color developing is lower, seriously constrains the development of white light LEDs.Obtain white light version by near ultraviolet excitated red, green, blue fluorescent material now to become and more and more come into one's own, therefore develop efficiently near ultraviolet excitated red, green, blue fluorescent material and become particularly important.
Single-crystal mass silicon is under solar illuminating, and main response spectrum is interval in visible region, is not all effectively utilized, therefore constrains the raising of single-crystal mass silicon solar cell efficiency at visible ray and infrared part.Can lower transition material be passed through, by sunlight medium ultraviolet light fractional conversion to visible ray, improve the efficiency of crystal silicon solar energy battery.Therefore develop new and effective transition material, the efficiency improving solar cell also becomes more and more important.
But blue colour fluorescent powder cost of the prior art is higher and be difficult to the technical need meeting above-mentioned two aspects.
Summary of the invention
The object of the invention is to overcome prior art defect, a kind of near ultraviolet excitated borate blue fluorescent powder is provided.
Another object of the present invention is to the preparation method that above-mentioned near ultraviolet excitated borate blue fluorescent powder is provided.
Concrete technical scheme of the present invention is as follows:
A near ultraviolet excitated borate blue fluorescent powder, the general formula of its combination matching is Sr
2-2xclO
3: xTm
3+, xLi
+, x is Tm
3+, Li
+molecular fraction in this compound, wherein 0≤x≤0.2.
In a preferred embodiment of the invention, described x=0,0.01,0.03,0.05,0.07,0.09,0.11,0.13,0.15,0.17,0.19 or 0.20.
In a preferred embodiment of the invention, its raw material composition comprises Strontium carbonate powder, boric acid, Strontium dichloride hexahydrate, trioxide and Quilonum Retard.
Another technical scheme of the present invention is as follows:
A preparation method for above-mentioned near ultraviolet excitated borate blue fluorescent powder, comprises the steps:
(1) each feed composition is taken according to described combination matching general formula;
(2) each feed composition fully mixed and grind to obtain evengranular fine powder through first time;
(3) by above-mentioned fine powder through pre-burning, calcining, cooling, through second time grinding, obtain described near ultraviolet excitated borate blue fluorescent powder.
In a preferred embodiment of the invention, in described step (3) from room temperature to the time of calcined temperature be 60 ~ 80 minutes, calcined temperature is 300 ~ 500 DEG C, and the time is 1 ~ 2 hour.
Further preferred, in described step (3) from room temperature to the time of calcined temperature be 70 minutes, calcined temperature is 400 DEG C, and the time is 1 hour.
In a preferred embodiment of the invention, the time being warming up to calcining temperature from calcined temperature in described step (3) is 80 ~ 100 minutes, and calcining temperature is 700 ~ 900 DEG C, and the time is 2 ~ 8 hours.
Further preferred, the time being warming up to calcining temperature from calcined temperature in described step (3) is 90 minutes, and calcining temperature is 800 DEG C, and the time is 6 hours.
In a preferred embodiment of the invention, being cooled in described step (3) is cooled to room temperature.
The invention has the beneficial effects as follows:
1, the general formula of the combination matching of near ultraviolet excitated borate blue fluorescent powder of the present invention is: Sr
2-2xc
lbO
3: xTm
3+, xLi
+, x is Tm
3+, Li
+molecular fraction in this compound, wherein 0≤x≤0.2, can be excited by the near-ultraviolet ray of 358nm, and have blue emission at 457nm, may be used near ultraviolet excitated three primary colors fluorescent powder system; For the preparation of monocrystalline silicon battery, monocrystalline silicon battery can also be increased to the spectral response of sunlight.Improve crystal silicon battery efficiency;
2, preparation method of the present invention adopts high temperature process heat method, and Heating temperature is low, less energy consumption; The equipment used is single, and facility investment is few, and technique is simple, with low cost, and product performance are stablized.
Accompanying drawing explanation
Fig. 1 is the XRD figure of near ultraviolet excitated borate blue fluorescent powder prepared by the embodiment of the present invention;
Fig. 2 is the exciting light spectrogram of near ultraviolet excitated borate blue fluorescent powder under 457nm prepared by the embodiment of the present invention;
Fig. 3 be embodiment of the present invention x=0.05,0.07, the utilizing emitted light spectrogram of near ultraviolet excitated borate blue fluorescent powder under 358nm of 0.09 and 0.11;
Fig. 4 is the CIR1931 chromaticity coordinates figure of the near ultraviolet excitated borate blue fluorescent powder of embodiment of the present invention x=0.07.
Embodiment
By reference to the accompanying drawings below by way of embodiment technical scheme of the present invention is further detailed and is described.
Embodiment 1
Sr
2-2xclO
3: 0.07Tm
3+, 0.07Li
+near ultraviolet excitated borate blue fluorescent powder
As shown in the table according to the proportioning raw materials of above-mentioned general formula:
| Raw material | H 3BO 3 | Sr 2CO 3 | SrCl 2·6H 2O | Tm 2O 3 | Li 2CO 3 |
| Weight | 0.3174g | 1.0037g | 0.6666g | 0.0675g | 0.0129g |
(1) accurately take above raw material, in agate crucible, fully the even 20min of grinding obtains evengranular fine powder, mixes in rear loading ceramic crucible.
(2) above-mentioned fine powder is put into the program of retort furnace according to setting, first rise to 400 DEG C of insulation 60min from room temperature through 70min, 800 DEG C of insulation 6h are risen to again through 90 minutes, after calcination procedure terminates, after being taken out to room temperature by sample furnace cooling, more namely obtain described near ultraviolet excitated borate blue fluorescent powder (its XRD as shown in Figure 1) with agate crucible grind into powder.
The near ultraviolet excitated borate blue fluorescent powder prepared excites the blue light (as shown in Figures 2 and 3) effectively can launching 457nm under 358nm.Its CIE chromaticity coordinates is in blue region (0.144,0.145) (as shown in Figure 4)
In above-described embodiment, when x=0,0.01,0.03,0.05,0.07,0.09,0.11,0.13,0.15,0.17,0.19 or 0.20 time, those of ordinary skill in the art can determine to obtain identical or close expected technique effect by the method for above-described embodiment.
In addition, when the processing parameter of aforesaid method changes in following scope, this area this technician common can obtain identical or close expected technique effect:
In described step (3) from room temperature to the time of calcined temperature be 60 ~ 80 minutes, calcined temperature is 300 ~ 500 DEG C, and the time is 1 ~ 2 hour.
The time being warming up to calcining temperature from calcined temperature in described step (3) is 80 ~ 100 minutes, and calcining temperature is 700 ~ 900 DEG C, and the time is 2 ~ 8 hours.
The above, be only preferred embodiment of the present invention, therefore can not limit scope of the invention process according to this, the equivalence change namely done according to the scope of the claims of the present invention and description with modify, all should still belong in scope that the present invention contains.
Claims (8)
1. a near ultraviolet excitated borate blue fluorescent powder, is characterized in that: the general formula of its combination matching is: Sr
2-2xclBO
3: xTm
3+, xLi
+, x is Tm
3+, Li
+molecular fraction in this compound, wherein x=0.05,0.07,0.09,0.11,0.13,0.15,0.17,0.19 or 0.20.
2. a kind of near ultraviolet excitated borate blue fluorescent powder as claimed in claim 1, is characterized in that: its raw material composition comprises Strontium carbonate powder, boric acid, Strontium dichloride hexahydrate, trioxide and Quilonum Retard.
3. the preparation method of a kind of near ultraviolet excitated borate blue fluorescent powder as claimed in claim 1, is characterized in that: comprise the steps:
(1) each feed composition is taken according to described combination matching general formula;
(2) each feed composition fully mixed and grind to obtain evengranular fine powder through first time;
(3) by above-mentioned fine powder through pre-burning, calcining, cooling, through second time grinding, obtain described near ultraviolet excitated borate blue fluorescent powder.
4. the preparation method of a kind of near ultraviolet excitated borate blue fluorescent powder as claimed in claim 3, it is characterized in that: in described step (3) from room temperature to the time of calcined temperature be 60 ~ 80 minutes, calcined temperature is 300 ~ 500 DEG C, and the time is 1 ~ 2 hour.
5. the preparation method of a kind of near ultraviolet excitated borate blue fluorescent powder as claimed in claim 4, it is characterized in that: in described step (3) from room temperature to the time of calcined temperature be 70 minutes, calcined temperature is 400 DEG C, and the time is 1 hour.
6. the preparation method of a kind of near ultraviolet excitated borate blue fluorescent powder as claimed in claim 4, it is characterized in that: the time being warming up to calcining temperature from calcined temperature in described step (3) is 80 ~ 100 minutes, calcining temperature is 700 ~ 900 DEG C, and the time is 2 ~ 8 hours.
7. the preparation method of a kind of near ultraviolet excitated borate blue fluorescent powder as claimed in claim 6, it is characterized in that: the time being warming up to calcining temperature from calcined temperature in described step (3) is 90 minutes, calcining temperature is 800 DEG C, and the time is 6 hours.
8. the preparation method of a kind of near ultraviolet excitated borate blue fluorescent powder as claimed in claim 6, is characterized in that: being cooled in described step (3) is cooled to room temperature.
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|---|---|---|---|
| CN201410081670.0A CN103788943B (en) | 2014-03-07 | 2014-03-07 | A kind of near ultraviolet excitated borate blue fluorescent powder and preparation method thereof |
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| CN103788943B true CN103788943B (en) | 2015-09-09 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101608117A (en) * | 2009-03-23 | 2009-12-23 | 华中科技大学 | The chloroboric acid salt base fluorescent powder that a kind of light-emitting diodes is effective |
| CN102408891A (en) * | 2010-09-26 | 2012-04-11 | 海洋王照明科技股份有限公司 | Fluoborate fluorescent powder and preparation method thereof |
-
2014
- 2014-03-07 CN CN201410081670.0A patent/CN103788943B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101608117A (en) * | 2009-03-23 | 2009-12-23 | 华中科技大学 | The chloroboric acid salt base fluorescent powder that a kind of light-emitting diodes is effective |
| CN102408891A (en) * | 2010-09-26 | 2012-04-11 | 海洋王照明科技股份有限公司 | Fluoborate fluorescent powder and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Enhanced red-emitting by charge compensation in Eu3+-activated Ca2BO3Cl phosphors;Fan Yang et. al.;《Ceramics International》;20120504;第38卷;6197-6201 * |
| Fan Yang et. al..YAl3(BO3)4:Tm3+,Dy3+:A potential tunable single-phased white-emitting phosphors.《Optik》.2012,第124卷2004-2007. * |
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Effective date of registration: 20220216 Address after: 518000 8b, building 5, phase III, China Merchants Haiyue, Nanshan District, Shenzhen, Guangdong Patentee after: Yang Peng Address before: 361000 Siming South Road, Xiamen, Fujian Province, No. 422 Patentee before: XIAMEN University |