CN103865530A - Near ultraviolet exited red phosphor powder and preparation method thereof - Google Patents
Near ultraviolet exited red phosphor powder and preparation method thereof Download PDFInfo
- Publication number
- CN103865530A CN103865530A CN201410081674.9A CN201410081674A CN103865530A CN 103865530 A CN103865530 A CN 103865530A CN 201410081674 A CN201410081674 A CN 201410081674A CN 103865530 A CN103865530 A CN 103865530A
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- near ultraviolet
- preparation
- red fluorescence
- powder
- red phosphor
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- 239000000843 powder Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title abstract 7
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 5
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 5
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 229910021421 monocrystalline silicon Inorganic materials 0.000 abstract description 5
- 230000003595 spectral effect Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract description 2
- 229910021419 crystalline silicon Inorganic materials 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract 1
- 238000009413 insulation Methods 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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Abstract
The invention discloses near ultraviolet exited red phosphor powder and a preparation method thereof. The composition ratio general formula of the near ultraviolet exited red phosphor powder is Sr2-2xB2O5: xEu<3+>, xNa<+>, wherein x is greater than or equal to 0.01 and is less than or equal to 0.20. The preparation method of the near ultraviolet exited red phosphor powder comprises the following steps: (1) weighing raw components according to the composition ratio general formula; (2) fully and uniformly mixing the raw components, and obtaining fine powder uniform in particle through the first time grinding and the first time sieving; (3) preburning, calcining and cooling the fine powder, carrying out the second time grinding and the second time sieving, and thus obtaining the red phosphor powder. The red phosphor powder disclosed by the invention can be excited by near ultraviolet and can be used for increasing red light components in LEDs; the near ultraviolet exited red phosphor powder can also be applied to the preparation of monocrystalline silicon batteries and is capable of improving the spectral response of the monocrystalline silicon batteries to sunlight and the efficiency of crystalline silicon batteries; the preparation method disclosed by the invention adopts a high-temperature solid phase synthesis method and is low in heating temperature and energy consumption; used equipment is single, the equipment investment is little, the process is simple, and the cost is low.
Description
Technical field
The present invention is specifically related to a kind of near ultraviolet excitated red fluorescence powder and preparation method thereof.
Background technology
LED as the 4th generation solid light source, the features such as energy-conservation because having, efficient, environmental protection receive much concern, development in recent years rapidly.The white light LEDs of existing market is with the blue-light excited YAG:Ce of 465nm
3+fluorescent material Yellow light-emitting low temperature, then blue light and gold-tinted are synthesized to white light.But in the spectrum of this white light LEDs transmitting, red light is on the low side, and colour temperature is higher, and colour rendering index is lower, departs from people's visual sense curve, is not suitable for interior lighting.Therefore, the ruddiness composition in increase white light is significant.At present, the material taking InGaN/GaN as matrix is easy to prepare efficient near ultraviolet (350-400nm) LED, adopts near ultraviolet excitated three primary colors fluorescent powder can solve the too weak difficult problem of ruddiness composition in conventional white light LED.
In addition, Shockley and Queisser once the article pointed out in " Journal of Applied Physics " (1961, Vol.32, PP510-519) that the theoretical limit efficiency of single crystal silicon battery was 40.7% (being SQ limit efficiency).And crystal silicon in the market reaches far away theoretical limit, this is because crystal silicon battery can only absorb the visible light part in sunlight, if add last layer spectrum transition material on the surface of crystal silicon battery, can convert UV-light or infrared light to visible ray, just can increase the spectral response of crystal silicon battery to sunlight.This method can be used as one of method improving crystal silicon battery efficiency.
But red fluorescence powder cost of the prior art is higher and be difficult to meet the technical need of 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 red fluorescence powder is provided.
Another object of the present invention is to provide the preparation method of above-mentioned red fluorescence powder.
Concrete technical scheme of the present invention is as follows:
A near ultraviolet excitated red fluorescence powder, the general formula of its combination matching is: Sr
2-2xb
2o
5: xEu
3+, xNa
+, wherein 0.01≤x≤0.20.
In a preferred embodiment of the invention, its raw material composition comprises Strontium carbonate powder, boric acid, europium sesquioxide and contains the agent of Na charge conservation.
In a preferred embodiment of the invention, described is sodium carbonate containing the agent of Na charge conservation.
In a preferred embodiment of the invention, its granularity is 5-20 μ m.
Another technical scheme of the present invention is as follows:
The preparation method of above-mentioned red fluorescence powder, comprises the steps:
(1) take each feed composition according to described combination matching general formula;
(2) each feed composition is fully mixed, evengranular fine powder grinds and sieves to obtain for the first time through for the first time;
(3) by above-mentioned fine powder through pre-burning, calcining, cooling, through grinding for the second time and sieving for the second time, obtain described red fluorescence powder.
In a preferred embodiment of the invention, the granularity of the fine powder of described step (2) is 20～60 μ m.
In a preferred embodiment of the invention, the calcined temperature in described step (3) is 300～500 DEG C, and the time is 1～2 hour.
In a preferred embodiment of the invention, the calcining temperature in described step (3) is 700～900 DEG C, and the time is 3～5 hours.
In a preferred embodiment of the invention, being cooled in described step (3) is cooled to 100 DEG C.
The invention has the beneficial effects as follows:
1, the general formula of the combination matching of near ultraviolet excitated red fluorescence powder of the present invention is:
Sr
2-2xb
2o
5: xEu
3+, xNa
+, wherein 0.01≤x≤0.20, can be excited by near-ultraviolet ray, can be for increasing the ruddiness composition in traditional LED; Can also be for the preparation of monocrystalline silicon battery, increase the spectral response of monocrystalline silicon battery to sunlight.Improve crystal silicon battery efficiency;
2, preparation method of the present invention adopts high temperature solid-state synthetic method, and Heating temperature is low, less energy consumption; The equipment using is single, and facility investment is few, and technique is simple, with low cost.
Brief description of the drawings
Fig. 1 is the emmission spectrum of the near ultraviolet excitated red fluorescence powder prepared of the embodiment of the present invention 1;
Fig. 2 is the excitation spectrum of the near ultraviolet excitated red fluorescence powder prepared of the embodiment of the present invention 1;
Fig. 3 is the comparative result figure of the emmission spectrum of the embodiment of the present invention 1 and 4 prepared near ultraviolet excitated red fluorescence powders, and wherein a curve is S
r2-xb
2o
5: xEu
3+transmitting spectrogram, b curve is Sr
2-2xb
2o
5: xEu
3+, xNa
+transmitting spectrogram.
Embodiment
By reference to the accompanying drawings technical scheme of the present invention is further detailed and is described by embodiment below.
Embodiment 1
(1) press combination matching general formula Sr
2-xb
2o
5: xEu
3+(x=0.05), take Strontium carbonate powder 0.9620 ± 0.0005g, boric acid 0.4237 ± 0.0005g, europium sesquioxide 0.0293 ± 0.0005g with electronic balance;
(2) Strontium carbonate powder taking, boric acid, europium sesquioxide raw material being placed in to weighing bottle fully mixes, the raw material mixing is placed in to agate mortar, and mixture is fully ground with agate mortar rod, after grinding, sieve obtain fine powder (granularity be 20～60 μ m);
(3) levigate powder is poured in 20ml cylindrical ceramic crucible, then ceramic crucible is placed in to the heating zone centre of KSS-1700 DEG C of box high-temperature energy-conservation electric furnace;
(4) close electric furnace furnace chamber, the heating schedule of electric furnace is set, Heating temperature is risen to 400 DEG C, insulation 1h, then rise to 800 DEG C, insulation 2h;
(5) according to heating schedule, heat completely, electric furnace is lowered the temperature automatically, when sample naturally cools to 100 DEG C in stove, closes furnace power;
(6) open electric stove hearth, crucible is taken out in burner hearth, sample is poured in agate mortar, grind with mortar rod, and sieve, repeatedly grind and sieve, granularity is controlled at 5～20 μ m, obtain described near ultraviolet excitated red fluorescence powder, as shown in Figure 1, excitation spectrum as shown in Figure 2 for its emmission spectrum.
Embodiment 2
Similar to Example 1, its difference is: first at 400 DEG C of insulation 1h, then rise to 800 DEG C, insulation 3h.
Embodiment 3
Similar to Example 1, its difference is: first at 400 DEG C of insulation 1h, then rise to 900 DEG C, insulation 3h.
Embodiment 4
Similar to Example 1, its difference is: by combination matching general formula
Sr
2-2xb
2o
5: xEu
3+, xNa
+(x=0.05), take Strontium carbonate powder 0.9373 ± 0.0005g, boric acid 0.4237 ± 0.0005g, europium sesquioxide 0.0293 ± 0.0005g, sodium carbonate 0.0088 ± 0.0005g with electronic balance, the emmission spectrum of red fluorescence powder that gained is near ultraviolet excitated and the comparative result of the emmission spectrum of embodiment 1 prepared red fluorescence powder are as shown in Figure 3.
Embodiment 5
Similar to Example 4, its difference is: first at 400 DEG C of insulation 1h, then rise to 900 DEG C, insulation 4h.
In above-described embodiment, in the time of 0.01≤x≤0.2, those of ordinary skill in the art can determine and obtain identical or close technique effect.
The above, be only preferred embodiment of the present invention, therefore can not limit according to this scope of the invention process, the equivalence done according to the scope of the claims of the present invention and description changes and modifies, and all should still belong in the scope that the present invention contains.
Claims (9)
1. a near ultraviolet excitated red fluorescence powder, is characterized in that: the general formula of its combination matching is: Sr
2-2xb
2o
5: xEu
3+, xNa
+, wherein 0.01≤x≤0.20.
2. a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 1, is characterized in that: its raw material composition comprises Strontium carbonate powder, boric acid, europium sesquioxide and contains the agent of Na charge conservation.
3. a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 2, is characterized in that: described is sodium carbonate containing the agent of Na charge conservation.
4. a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 1, is characterized in that: its granularity is 5-20 μ m.
5. the preparation method of a kind of near ultraviolet excitated red fluorescence powder as described in arbitrary claim in claim 1 to 4, is characterized in that: comprise the steps:
(1) take each feed composition according to described combination matching general formula;
(2) each feed composition is fully mixed, evengranular fine powder grinds and sieves to obtain for the first time through for the first time;
(3) by above-mentioned fine powder through pre-burning, calcining, cooling, through grinding for the second time and sieving for the second time, obtain described red fluorescence powder.
6. the preparation method of a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 5, is characterized in that: the granularity of the fine powder of described step (2) is 20～60 μ m.
7. the preparation method of a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 6, is characterized in that: the calcined temperature in described step (3) is 300～500 DEG C, and the time is 1～2 hour.
8. the preparation method of a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 7, is characterized in that: the calcining temperature in described step (3) is 700～900 DEG C, and the time is 3～5 hours.
9. the preparation method of a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 8, is characterized in that: being cooled in described step (3) is cooled to 100 DEG C.
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|---|---|---|---|
| CN201410081674.9A CN103865530B (en) | 2014-03-07 | 2014-03-07 | A kind of near ultraviolet excitated red fluorescence powder and preparation method thereof |
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|---|---|---|---|
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| CN103865530B CN103865530B (en) | 2015-10-21 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106753347A (en) * | 2016-11-18 | 2017-05-31 | 厦门大学 | A kind of near ultraviolet excitated red fluorescence powder and preparation method thereof |
| CN106718422A (en) * | 2017-01-10 | 2017-05-31 | 厦门大学 | A kind of preparation method of degradable multifunctional fibre element agricultural film |
| CN106753364A (en) * | 2016-11-18 | 2017-05-31 | 厦门大学 | Borate red fluorescent powder of europium doping and preparation method thereof |
| CN111653657A (en) * | 2020-07-08 | 2020-09-11 | 泉州市康电光电科技有限公司 | Illumination process for plant solar photosynthesis |
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| CN102337125A (en) * | 2011-07-21 | 2012-02-01 | 长春理工大学 | Borate fluorescent powder for warm white LED (light-emitting diode) |
| CN103094394A (en) * | 2013-01-18 | 2013-05-08 | 厦门大学 | Down-conversion crystalline silicon solar cell and preparation method thereof |
-
2014
- 2014-03-07 CN CN201410081674.9A patent/CN103865530B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102337125A (en) * | 2011-07-21 | 2012-02-01 | 长春理工大学 | Borate fluorescent powder for warm white LED (light-emitting diode) |
| CN103094394A (en) * | 2013-01-18 | 2013-05-08 | 厦门大学 | Down-conversion crystalline silicon solar cell and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 王海英 等: "Eu3+掺杂的硼酸鳃系列荧光体的合成及其发光性能", 《无机材料学报》 * |
| 王荣 等: "白光LED用荧光材料Sr3B2O6∶Eu3+，Na+的制备及发光性能", 《发光学报》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106753347A (en) * | 2016-11-18 | 2017-05-31 | 厦门大学 | A kind of near ultraviolet excitated red fluorescence powder and preparation method thereof |
| CN106753364A (en) * | 2016-11-18 | 2017-05-31 | 厦门大学 | Borate red fluorescent powder of europium doping and preparation method thereof |
| CN106718422A (en) * | 2017-01-10 | 2017-05-31 | 厦门大学 | A kind of preparation method of degradable multifunctional fibre element agricultural film |
| CN111653657A (en) * | 2020-07-08 | 2020-09-11 | 泉州市康电光电科技有限公司 | Illumination process for plant solar photosynthesis |
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| Publication number | Publication date |
|---|---|
| CN103865530B (en) | 2015-10-21 |
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Effective date of registration: 20220222 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 |
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