CN103865530B - A kind of near ultraviolet excitated red fluorescence powder and preparation method thereof - Google Patents
A kind of near ultraviolet excitated red fluorescence powder and preparation method thereof Download PDFInfo
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- CN103865530B CN103865530B CN201410081674.9A CN201410081674A CN103865530B CN 103865530 B CN103865530 B CN 103865530B CN 201410081674 A CN201410081674 A CN 201410081674A CN 103865530 B CN103865530 B CN 103865530B
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Abstract
The invention discloses a kind of near ultraviolet excitated red fluorescence powder and preparation method thereof, the general formula of its combination matching is: Sr
2-2xb
2o
5: xEu
3+, xNa
+, wherein 0.01≤x≤0.20; Its preparation method comprises the steps: (1) takes each feed composition according to described combination matching general formula; (2) each feed composition is fully mixed, through first time grinding and the evengranular fine powder that sieves to obtain for the first time; (3) by above-mentioned fine powder through pre-burning, calcining, cooling, through second time grinding and second time sieve, obtain described red fluorescence powder.Red fluorescence powder of the present invention can be excited by near-ultraviolet ray, and may be used for increases the red color light component in traditional LED; For the preparation of monocrystalline silicon battery, monocrystalline silicon battery can also be increased to the spectral response of sunlight, improves 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.
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 forth generation solid light source, receives much concern because having the features such as energy-conservation, efficient, environmental protection, and 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 white light.But in the spectrum that this white light LEDs is launched, 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 red color light component increased in white light is significant.At present, be that the material of matrix is easy to prepare efficient near ultraviolet (350-400nm) LED with InGaN/GaN, adopt near ultraviolet excitated three primary colors fluorescent powder can solve the difficult problem that in conventional white light LED, red color light component is too weak.
In addition, in " Journal of Applied Physics " (1961, Vol.32, PP510-519), Shockley and Queisser once the article pointed out that the theoretical limit efficiency of single crystal silicon battery was 40.7% (i.e. 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 UV-light or infrared light be converted to visible ray, just can increase the spectral response of crystal silicon battery to sunlight.This method can as one of method improving crystal silicon battery efficiency.
But red fluorescence 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 red fluorescence powder is provided.
Another object of the present invention is to the preparation method that above-mentioned red fluorescence powder is provided.
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 μm.
Another technical scheme of the present invention is as follows:
The preparation method of above-mentioned red fluorescence powder, comprises the steps:
(1) each feed composition is taken according to described combination matching general formula;
(2) each feed composition is fully mixed, through first time grinding and the evengranular fine powder that sieves to obtain for the first time;
(3) by above-mentioned fine powder through pre-burning, calcining, cooling, through second time grinding and second time sieve, 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 μm.
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, may be used for increasing the red color light component in traditional LED; 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.
Accompanying drawing explanation
Fig. 1 is the emmission spectrum of near ultraviolet excitated red fluorescence powder prepared by the embodiment of the present invention 1;
Fig. 2 is the excitation spectrum of near ultraviolet excitated red fluorescence powder prepared by the embodiment of the present invention 1;
The comparative result figure of the emmission spectrum of the near ultraviolet excitated red fluorescence powder of Fig. 3 prepared by the embodiment of the present invention 1 and 4, 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 below by way of embodiment technical scheme of the present invention is further detailed and is described.
Embodiment 1
(1) by combination matching general formula Sr
2-xb
2o
5: xEu
3+(x=0.05), Strontium carbonate powder 0.9620 ± 0.0005g, boric acid 0.4237 ± 0.0005g, europium sesquioxide 0.0293 ± 0.0005g is taken with electronic balance;
(2) Strontium carbonate powder taken, boric acid, europium sesquioxide raw material are placed in weighing bottle and fully mix, the raw material mixed is placed in agate mortar, and with agate mortar rod, mixture is fully ground, sieve after grinding and obtain fine powder (granularity is 20 ~ 60 μm);
(3) levigate powder is poured in 20ml cylindrical ceramic crucible, then ceramic crucible is placed in 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 complete, electric furnace is lowered the temperature automatically, when sample naturally cools to 100 DEG C in stove, closes furnace power;
(6) electric stove hearth is opened, crucible is taken out in burner hearth, sample is poured in agate mortar, grind with mortar rod, and sieve, grinding is sieved repeatedly, Task-size Controlling is at 5 ~ 20 μm, 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 comparative result of the emmission spectrum of the emmission spectrum of the red fluorescence powder that gained is near ultraviolet excitated and the red fluorescence powder obtained by embodiment 1 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, when 0.01≤x≤0.2, those of ordinary skill in the art can determine to obtain identical or close technique effect.
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 (7)
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, its raw material composition comprises Strontium carbonate powder, boric acid, europium sesquioxide and sodium carbonate.
2. a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 1, is characterized in that: its granularity is 5-20 μm.
3. the preparation method of a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 1 or 2, is characterized in that: comprise the steps:
(1) each feed composition is taken according to described combination matching general formula;
(2) each feed composition is fully mixed, through first time grinding and the evengranular fine powder that sieves to obtain for the first time;
(3) by above-mentioned fine powder through pre-burning, calcining, cooling, through second time grinding and second time sieve, obtain described near ultraviolet excitated red fluorescence powder.
4. the preparation method of a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 3, is characterized in that: the granularity of the fine powder of described step (2) is 20 ~ 60 μm.
5. the preparation method of a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 4, it is characterized in that: the calcined temperature in described step (3) is 300 ~ 500 DEG C, the time is 1 ~ 2 hour.
6. the preparation method of a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 5, it is characterized in that: the calcining temperature in described step (3) is 700 ~ 900 DEG C, the time is 3 ~ 5 hours.
7. the preparation method of a kind of near ultraviolet excitated red fluorescence powder as claimed in claim 6, is characterized in that: being cooled in described step (3) is cooled to 100 DEG C.
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| CN103865530B true CN103865530B (en) | 2015-10-21 |
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| CN106753364A (en) * | 2016-11-18 | 2017-05-31 | 厦门大学 | Borate red fluorescent powder of europium doping and preparation method thereof |
| 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 |
| 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 |
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 |
-
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 |
|---|
| Eu3+掺杂的硼酸鳃系列荧光体的合成及其发光性能;王海英 等;《无机材料学报》;20041120;第19卷(第6期);2 实验部分 * |
| 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》.2011,第32卷(第10期),全文. * |
| 高压合成的硼酸锯掺Eu2+离子发光特性的研究;许伟 等;《高压物理学报》;19880930;第2卷(第3期);全文 * |
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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 |