CN104087290A - Method for preparing nitride red phosphor - Google Patents
Method for preparing nitride red phosphor Download PDFInfo
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- CN104087290A CN104087290A CN201410335293.9A CN201410335293A CN104087290A CN 104087290 A CN104087290 A CN 104087290A CN 201410335293 A CN201410335293 A CN 201410335293A CN 104087290 A CN104087290 A CN 104087290A
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- fluorescent powder
- red fluorescent
- nitride red
- preparation
- roasting
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Links
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title abstract description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title abstract 3
- 239000011575 calcium Substances 0.000 claims abstract description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 239000010703 silicon Substances 0.000 claims abstract description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 4
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 4
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 31
- 239000002994 raw material Substances 0.000 claims description 25
- 238000002360 preparation method Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 9
- 229910052582 BN Inorganic materials 0.000 description 8
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 5
- 229910004261 CaF 2 Inorganic materials 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000000428 dust Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 208000013840 Non-involuting congenital hemangioma Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 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 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
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- Luminescent Compositions (AREA)
Abstract
The invention discloses a method for preparing nitride red phosphor. The chemical structural formula of the nitride red phosphor is (Ca1-xSr1-x)Si5N8:Eu2x, wherein Ca is elemental calcium, Sr is elemental strontium, Si is elemental silicon, N is elemental nitrogen, Eu is elemental europium, and x is more than or equal to 0.05 and less than or equal to 0.20. The requirement of the needed equipment is simple, glove box operation is not needed, no carbon powder is needed for reducing, impurity carbon residues do not exist in the product, the operating process is simplified, batch production is easily realized, and the synthesized target product has the advantages of high luminous efficiency and stable chemical property and does not contain impurity carbon.
Description
Technical field
The invention discloses a kind of LED of being mainly used in warm white interior lighting, LED street lamp, the preparation method of the nitride red fluorescent powder of the illumination such as LED backlight of LCD and demonstration.
Background technology
Compare white light LEDs with traditional lighting light source and there is the advantages such as low voltage, less energy-consumption, long lifetime, therefore receive increasing concern both at home and abroad.Obtain at present the maximum mode of white light LEDs and be blue-light LED chip with the yttrium aluminum garnet yellow fluorescent powder (YAG:Ce) activating with cerium thereby compound generation white light, important component part as LED, LED fluorescent material is subject to people and more and more pays close attention in recent years, but it is not high that YAG yellow fluorescent powder also exists luminous efficiency at present, and cause the shortcomings such as colour rendering index is low owing to lacking emitting red light composition.Therefore,, in order to obtain the more LED white light of high color rendering index (CRI), need to add red fluorescence powder.
Schnick W team and Hintze H T team have carried out extensive work in early days, successfully synthesize M
2si
5n
8silica-based nitride is also adulterated and has been obtained 600-630nm transmitting red material by Eu, obtains very soon application in LED.And by OSRAM and NICH IADeng company the earliest for the making of warm white LED.M
2si
5n
8: the synthetic very difficulty of Eu system material, adopts the nitrogenize of active alkaline-earth metal simple substance to form active binary nitride in the people's such as Schnick W work in early days and then synthesizes in more than 1700 ℃ high temperature and nitrogen with activity two imido silicon.These methods relate to active reactant, and condition is harsh, link is complicated, is unfavorable for industrialization volume production and application request.For the ease of suitability for industrialized production, reduce energy consumption, reduce cost, from former, expect that technique updates, to meet large-scale industrial production.Therefore, can stable in the airly there is the lower preparation M that become of simultaneous reactions temperature
2si
5n
8: the developing direction of Eu.
Summary of the invention
The object of this invention is to provide a kind of luminous efficiency good, brightness is high, and the nitride red fluorescent powder of carbon-containing impurities not, it effectively excites between 300-350 nm, emission wavelength, between 600-700 nm, can better meet a kind of nitride red fluorescent powder (Ca of the application requiring of white light LEDs
1-
x sr
1-
x ) Si
5n
8: Eu
2
x preparation method.
The present invention is achieved through the following technical solutions: a kind of preparation method of nitride red fluorescent powder, and the reaction equation of preparing nitride red fluorescent powder is:
(1-x)CaCN
2+(Sr
1-xEu
2x)CO
3+5/3Si
3N
4→(Ca
1-xSr
1-xEu
2x)SiN+CO↑+CO
2↑ (1)
1/2(1-x)CaCN
2+1/2(Sr
1-xEu
2x)CO
3+1/3Si
3N
4→(Ca
1-xEu
x)Al
ySiN
3+1/2CO↑+1/2CO
2↑ (2)
(Sr
1-xEu
2x)CO
3+(Ca
1-xSr
1-xEu
2x)SiN+2/3Si
3N
4+2(Ca
1-xEu
x)Al
ySiN
3
→2(Ca
1-xSr
1-xEu
2x)Si
5N
8+2yAlN+CO↑+CO
2↑ (3)
The chemical structural formula of described nitride red fluorescent powder is as follows: (Ca
1-
x sr
1-
x ) Si
5n
8: Eu
2
x , wherein Ca is calcium constituent, and Sr is strontium element, and Si is element silicon, and N is nitrogen element, Eu is europium element, wherein 0.05≤
x≤ 0.20;
The preparation method's of nitride red fluorescent powder step is as follows:
A, with CaCN
2, SrCO
3, Eu
2o
3and Si
3n
4for raw material;
B, according to chemical structural formula, form and stoichiometric ratio takes above-mentioned raw materials;
C, in above-mentioned sample, add solubility promoter, above-mentioned raw materials is fully mixed with solubility promoter, the scope of the mass ratio of solubility promoter and raw material is 0.1%-0.5%;
D, by the above-mentioned raw material mixing at high temperature solid-state kiln roasting;
Product after E, roasting obtains nitride red fluorescent powder through ball milling, washing, after dry.
Further improvement of the present invention is: silicon nitride is amorphous amorphous particle, and particle size is 300-500 nm.
Further improvement of the present invention is: solubility promoter is the fluorochemical of II valency rare earth element.
Further improvement of the present invention is: the atmosphere in high temperature solid-state stove is N
2; Gaseous tension is 0.1 Pa, flow velocity 50-100 mL/min.
Further improvement of the present invention is: raw material is roasting in two steps: the first step maturing temperature is 1000 ℃-1200 ℃, and the time is 2-3h; Second step maturing temperature is 1500 ℃-1550 ℃, and the time is 4-6 h, and reaction end gas is focused on to rear discharge.
Further improvement of the present invention is: holding vessel during raw material roasting is Mo crucible.
Further improvement of the present invention is: the product obtaining after roasting sieves after levigate, then washing, and described washing is successively through overpickling, then through washing, wherein acid is hydrochloric acid, nitric acid or phosphoric acid, and the volumetric molar concentration of acid is 5%-15%.
The present invention compared with prior art has the following advantages:
1, the synthetic required wide material sources of target product, without carbon dust or H
2reduce, in target product, inclusion-free carbon is residual;
2, synthetic target product equipment is simple, normal pressure N
2atmosphere, safety coefficient is high, simultaneously without glove box operation, has avoided the operating process of glove box complexity, has improved efficiency.
accompanying drawing explanation:
Fig. 1 be embodiment 1 excite figure;
Fig. 2 is the utilizing emitted light spectrogram of embodiment 1;
Fig. 3 is the XRD spectra of embodiment 1.
embodiment:
In order to deepen the understanding of the present invention, below in conjunction with embodiment and accompanying drawing, the invention will be further described, and this embodiment only, for explaining the present invention, does not form limiting the scope of the present invention.
The reaction equation of preparing nitride red fluorescent powder is:
(1-x)CaCN
2+(Sr
1-xEu
2x)CO
3+5/3Si
3N
4→(Ca
1-xSr
1-xEu
2x)SiN+CO↑+CO
2↑ (1)
1/2(1-x)CaCN
2+1/2(Sr
1-xEu
2x)CO
3+1/3Si
3N
4→(Ca
1-xEu
x)Al
ySiN
3+1/2CO↑+1/2CO
2↑ (2)
(Sr
1-xEu
2x)CO
3+(Ca
1-xSr
1-xEu
2x)SiN+2/3Si
3N
4+2(Ca
1-xEu
x)Al
ySiN
3
→2(Ca
1-xSr
1-xEu
2x)Si
5N
8+2yAlN+CO↑+CO
2↑ (3)
The chemical structural formula of nitride red fluorescent powder is as follows: (Ca
1-
x sr
1-
x ) Si
5n
8: Eu
2
x , wherein Ca is calcium constituent, and Sr is strontium element, and Si is element silicon, and N is nitrogen element, Eu is europium element, wherein 0.05≤
x≤ 0.20;
The preparation method's of nitride red fluorescent powder step is as follows:
A, with CaCN
2, SrCO
3, Eu
2o
3and Si
3n
4for raw material;
B, according to chemical structural formula, form and stoichiometric ratio takes above-mentioned raw materials;
C, in above-mentioned sample, add solubility promoter, above-mentioned raw materials is fully mixed with solubility promoter, the scope of the mass ratio of solubility promoter and raw material is 0.1%-0.5%;
D, by the above-mentioned raw material mixing at high temperature solid-state kiln roasting;
Product after E, roasting obtains nitride red fluorescent powder through ball milling, washing, after dry.
Silicon nitride is amorphous amorphous particle, and particle size is 300-500 nm, and solubility promoter is the fluorochemical of II valency rare earth element, and the atmosphere in high temperature solid-state stove is N
2; Gaseous tension is 0.1 Pa, flow velocity 50-100 mL/min, and raw material is roasting in two steps: the first step maturing temperature is 1000 ℃-1200 ℃, and the time is 2-3h; Second step maturing temperature is 1500 ℃-1550 ℃, time is 4-6 h, reaction end gas is focused on to rear discharge, holding vessel during raw material roasting is Mo crucible, and the product obtaining after roasting sieves after levigate, then washing, described washing is successively through overpickling, through washing, wherein acid is hydrochloric acid, nitric acid or phosphoric acid again, and the volumetric molar concentration of acid is 5%-15%.
Equipment requirements required for the present invention is simple, without glove box operation, does not use carbon dust to reduce simultaneously, and in products therefrom, inclusion-free carbon is residual, has simplified operating procedure, is easy to batch production; It is high that synthetic target product has luminous efficiency, stable chemical nature, the advantages such as carbon free from foreign meter.
Embodiment 1:
Take respectively CaCN
22.400g, SrCO
34.207g, Eu
2o
30.528g, Si
3n
47.000g, AlN 0.038g and CaF
20.024g adds ethanol wet mixing 6 hours by above raw material in beaker, put into oven drying 24 hours, after crossing 120 mesh sieves, mix, pack in boron nitride crucible, make its 1100 ℃ of roasting 10 hours in nitrogen atmosphere, product of roasting is taken out afterwards and ground, excessively after 200 mesh sieves, put into boron nitride crucible, put it into 1550 ℃ of roastings of nitrogen atmosphere 12 hours.Products therefrom washs with 10% nitric acid after grinding and sieving, and then by deionized water wash post-drying, obtains Ca
0.95sr
0.95si
5n
8: Eu
0.1nitride red fluorescent powder.
Embodiment 2:
Take respectively CaCN
22.160g, SrCO
33.986g, Eu
2o
31.056g, Si
3n
47.000g, AlN 0.035g and CaF
20.026g adds ethanol wet mixing 6 hours by above raw material in beaker, put into oven drying 24 hours, after crossing 120 mesh sieves, mix, pack in boron nitride crucible, put it in nitrogen atmosphere 1510 ℃ of roastings 10 hours, product of roasting is taken out afterwards and ground, excessively after 200 mesh sieves, put into boron nitride crucible, put it into 1550 ℃ of roastings of nitrogen atmosphere 12 hours.Products therefrom washs with 10% nitric acid after grinding and sieving, and then by deionized water wash post-drying, obtains Ca
0.9sr
0.9si
5n
8: Eu
0.2nitride red fluorescent powder.
Embodiment 3:
Take respectively CaCN
22.040g, SrCO
33.764g, Eu
2o
31.584g, Si
3n
47.000g, AlN 0.033g and CaF
20.028g adds ethanol wet mixing 6 hours by above raw material in beaker, put into oven drying 24 hours, after crossing 120 mesh sieves, mix, pack in boron nitride crucible, put it in nitrogen atmosphere 1510 ℃ of roastings 10 hours, product of roasting is taken out afterwards and ground, excessively after 200 mesh sieves, put into boron nitride crucible, put it into 1550 ℃ of roastings of nitrogen atmosphere 12 hours.Products therefrom washs with 10% nitric acid after grinding and sieving, and then by deionized water wash post-drying, obtains Ca
0.85sr
0.85si
5n
8: Eu
0.3nitride red fluorescent powder.
Embodiment 4:
Take respectively CaCN
21.920g, SrCO
33.543g, Eu
2o
32.112g, Si
3n
47.000g, AlN 0.031g and CaF
20.033g adds ethanol wet mixing 6 hours by above raw material in beaker, put into oven drying 24 hours, after crossing 120 mesh sieves, mix, pack in boron nitride crucible, put it in nitrogen atmosphere 1510 ℃ of roastings 10 hours, product of roasting is taken out afterwards and ground, excessively after 200 mesh sieves, put into boron nitride crucible, put it into 1550 ℃ of roastings of nitrogen atmosphere 12 hours.Products therefrom washs with 10% nitric acid after grinding and sieving, and then by deionized water wash post-drying, obtains Ca
0.8sr
0.8si
5n
8: Eu
0.4nitride red fluorescent powder.
Finally it should be noted that: obviously, above-described embodiment is only for example of the present invention is clearly described, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without also giving all embodiments.And the apparent variation of being amplified out thus or change are still among protection scope of the present invention.
Claims (7)
1. a preparation method for nitride red fluorescent powder, is characterized in that: the reaction equation of preparing nitride red fluorescent powder is:
(1-x)CaCN
2+(Sr
1-xEu
2x)CO
3+5/3Si
3N
4→(Ca
1-xSr
1-xEu
2x)SiN+CO↑+CO
2↑ (1)
1/2(1-x)CaCN
2+1/2(Sr
1-xEu
2x)CO
3+1/3Si
3N
4→(Ca
1-xEu
x)Al
ySiN
3+1/2CO↑+1/2CO
2↑ (2)
(Sr
1-xEu
2x)CO
3+(Ca
1-xSr
1-xEu
2x)SiN+2/3Si
3N
4+2(Ca
1-xEu
x)Al
ySiN
3
→2(Ca
1-xSr
1-xEu
2x)Si
5N
8+2yAlN+CO↑+CO
2↑ (3)
The chemical structural formula of described nitride red fluorescent powder is as follows: (Ca
1-
x sr
1-
x ) Si
5n
8: Eu
2
x , wherein Ca is calcium constituent, and Sr is strontium element, and Si is element silicon, and N is nitrogen element, Eu is europium element, wherein 0.05≤
x≤ 0.20;
The preparation method's of nitride red fluorescent powder step is as follows:
A, with CaCN
2, SrCO
3, Eu
2o
3and Si
3n
4for raw material;
B, according to chemical structural formula, form and stoichiometric ratio takes above-mentioned raw materials;
C, in above-mentioned sample, add solubility promoter, above-mentioned raw materials is fully mixed with solubility promoter, the scope of the mass ratio of solubility promoter and raw material is 0.1%-0.5%;
D, by the above-mentioned raw material mixing at high temperature solid-state kiln roasting;
Product after E, roasting obtains nitride red fluorescent powder through ball milling, washing, after dry.
2. a kind of preparation method of nitride red fluorescent powder according to claim 1, it is characterized in that: described silicon nitride is amorphous amorphous particle, and particle size is 300-500 nm.
3. a kind of preparation method of nitride red fluorescent powder according to claim 1, is characterized in that: described solubility promoter is the fluorochemical of II valency rare earth element.
4. a kind of preparation method of nitride red fluorescent powder according to claim 1, is characterized in that: the atmosphere in described high temperature solid-state stove is N
2; Gaseous tension is 0.1 Pa, flow velocity 50-100 mL/min.
5. a kind of preparation method of nitride red fluorescent powder according to claim 1, is characterized in that: the roasting in two steps of described raw material: the first step maturing temperature is 1000 ℃-1200 ℃, and the time is 2-3h; Second step maturing temperature is 1500 ℃-1550 ℃, and the time is 4-6 h, and reaction end gas is focused on to rear discharge.
6. a kind of preparation method of nitride red fluorescent powder according to claim 1, is characterized in that: holding vessel during described raw material roasting is Mo crucible.
7. a kind of preparation method of nitride red fluorescent powder according to claim 1, it is characterized in that: the product obtaining after described roasting sieves after levigate, then washing, described washing is successively through overpickling, again through washing, wherein acid is hydrochloric acid, nitric acid or phosphoric acid, and the volumetric molar concentration of acid is 5%-15%.
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| CN107365070A (en) * | 2017-09-13 | 2017-11-21 | 上海应用技术大学 | A kind of white light LEDs red green composite fluorescence glass and preparation method thereof |
| CN110256072A (en) * | 2019-02-28 | 2019-09-20 | 江苏罗化新材料有限公司 | Fluorescent transparent ceramics and preparation method thereof |
| CN112457021A (en) * | 2020-12-17 | 2021-03-09 | 新沂市锡沂高新材料产业技术研究院有限公司 | Ceramic fluorescent sheet for LED and pressureless sintering method thereof |
| CN112745835A (en) * | 2021-01-26 | 2021-05-04 | 厦门大学 | Small-particle-size high-quantum-efficiency nitride fluorescent powder, preparation method and application thereof, light-emitting device and display device |
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| CN110256072A (en) * | 2019-02-28 | 2019-09-20 | 江苏罗化新材料有限公司 | Fluorescent transparent ceramics and preparation method thereof |
| CN112457021A (en) * | 2020-12-17 | 2021-03-09 | 新沂市锡沂高新材料产业技术研究院有限公司 | Ceramic fluorescent sheet for LED and pressureless sintering method thereof |
| CN112745835A (en) * | 2021-01-26 | 2021-05-04 | 厦门大学 | Small-particle-size high-quantum-efficiency nitride fluorescent powder, preparation method and application thereof, light-emitting device and display device |
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