CN104710982A - Rare earth ion co-doped aluminosilicate novel green glow fluorescent powder and preparation method thereof - Google Patents
Rare earth ion co-doped aluminosilicate novel green glow fluorescent powder and preparation method thereof Download PDFInfo
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- CN104710982A CN104710982A CN201510115144.6A CN201510115144A CN104710982A CN 104710982 A CN104710982 A CN 104710982A CN 201510115144 A CN201510115144 A CN 201510115144A CN 104710982 A CN104710982 A CN 104710982A
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Abstract
The invention provides a rare earth ion co-doped aluminosilicate novel green glow fluorescent powder and a preparation method thereof, and belongs to the technical field of luminescent materials. The chemical constitution of the green glow fluorescent powder is aAl2O3.bSiO2.cCeO2.dTb4O7, wherein a, b, c and d are mole fractions; a/b is equal to 3/2; c is larger than or equal to 0 and less than or equal to 2.0%; d is larger than or equal to 0 and less than or equal to 5.0%; c and d are not 0 at the same time. The preparation method comprises the following steps: weighing raw materials according to the stoichiometric proportion of the elements in the chemical formula; fully mixing the raw materials; conducting ball milling on the raw materials at indoor temperature; putting the sample conducted by full ball milling in a high-temperature pipe furnace pumped by reducing atmosphere; calcining the sample for 2-6 hours at 1450-1550 DEG C; taking the sample out for crushing grinding after the furnace chamber is cooled to indoor temperature; adding H3BO3 flux, water washing or/and SiO2 coating treatment in following to obtain the fluorescent powder. The fluorescent powder prepared from the method is favorable in crystallinity and particle surface, high in luminous intensity (particularly excellent in temperature resistance), and suitable for being used as ultraviolet light excited LED green glow fluorescent powder.
Description
Technical field
The invention belongs to LED luminescent material preparing technical field, novel green light fluorescent powder of aluminosilicate being specifically related to a kind of rare earth ion codoped and preparation method thereof.
Background technology
White light emitting diode (WLED) possesses the advantages such as efficiency is high, life-span length, energy-conserving and environment-protective and replaces conventional illumination sources just gradually and become lighting source of new generation because of it.Fluorescent material can absorb ultraviolet/near ultraviolet or blue light then sends visible ray, is the critical material in LED solid luminescence technology.The implementation of current white light mainly contains three kinds: (1) by red, green, blue three-color LED Chip Packaging together, is mixed to get white light by each coloured light; (2) blue-light LED chip excites yellow fluorescent powder, and gold-tinted and blue light obtain white light; (3) UV LED chip excites three primary colors fluorescent powder to obtain white light.Wherein, not only driving circuit is complicated for the 1st kind of mode, and production cost is high, and heat dissipation problem is difficult to solve.Therefore, commercial many employings the 2nd kind of mode synthesize white light, but cause its color developing not good owing to lacking ruddiness.In order to meet the demand for development of LED illumination technology, researching and developing a kind of new and effective, green light fluorescent powder with superior luminescence color and thermal stability, to realize the synthesis mode of the 3rd kind of white light, will more wide application demand be had.
So far, the green emitting phosphor of exploitation both at home and abroad mainly contains silicate systems, aluminates system and oxynitride system etc., but they have the relative merits of oneself.Silicate substrate fluorescent material excitation wave length and width, can be applicable to exciting of different wave length chip well, can be widely used and have certain industrialized scale, as the M of orthosilicate system
2siO
4: Eu
2+(M:Ca, Sr, Ba) and Ca
3si
2o
7: Eu
2+; But its poor heat stability (light decay when 150 DEG C is greater than 50%), limits its large-scale application.Conventional aluminum silicate system fluorescent material can launch green glow under (closely) burst of ultraviolel, cheap, and preparation easily; But its raw materials requires relatively high purity, and between component phase composite and phase transformation complicated, fluorescence efficiency is lower, as BaMgAl
10o
17: Eu, Mn.Silica-based oxynitride is the very fast a kind of phosphor hosts of latest developments, can be excited, then coordinate the change of rare earth ion and chemical constitution, can realize the utilizing emitted light of different wave length: such as, β-SiAlON:Eu by blue light and ultraviolet high efficiency
2+be the class nitrogen oxide green fluorescent powder that application is more at present, it coordinates with blue chip can produce specular removal, but its shortcoming is preparation condition harshness (needing High Temperature High Pressure), large-scale commercial production difficulty.
Meanwhile, take mullite as matrix, the phosphor material powder of doping different rare earth ions, can obtain excellent luminescent properties, start to attract many research to pay close attention to: such as, adopts water heat transfer Eu
2+the mullite fluorescent material of doping, adopts sol-gel method to prepare Tb
3+the mullite fluorescent material of doping, also has in addition by preparation of sol-gel Ce
3+, Tb
3+eu prepared by the mullite fluorescent material mixed altogether and high temperature solid-state method
2+, Tb
3+the 3/2 mullite fluorescent material mixed altogether.But interpolation boric acid is fusing assistant, high temperature solid-state method is adopted to prepare Ce
3+, Tb
3+the mullite fluorescent material mixed altogether not yet occurs.
Summary of the invention
The object of the invention is the novel green light fluorescent powder of aluminosilicate developing a kind of rare earth ion codoped, namely can be excited by UV LED chip and launch high strength, the fluorescent material of stable green glow.
Technical problem to be solved by this invention is to provide that a kind of technique is simple, quality product is high, cost is low, can be widely used in luminescent material manufacture in novel green light fluorescent powder of aluminosilicate and preparation method thereof of a kind of rare earth ion codoped.
The novel green light fluorescent powder of aluminosilicate of a kind of rare earth ion of the present invention codoped, its primary chemical consists of:
aAl
2O
3﹒bSiO
2﹒cCeO
2﹒dTb
4O
7
Wherein a, b, c, d are molar fraction, a/b=3/2,0≤c≤2.0%, 0≤d≤5.0%; And be zero during c, d difference.
Experimentally result, the preferred value of c and d is respectively 1.3% and 2%, along with Ce
3+, Tb
3+ion doping concentration is started from scratch increase, and the excitation peak of fluorescent material and the intensity of emission peak strengthen gradually, and light intensity is as the same; When reaching preferred concentration value, excitation peak and emission peak intensity and light intensity reach the strongest; After exceeding optimum concn, occur concentration quenching under high doping, light intensity reduces gradually.
In addition, be promote high temperature solid state reaction, react fully and carry out, a certain amount of fusing assistant can be added, with H mixing altogether in fluorescent material
3bO
3for fusing assistant effect is better, its optimum addition is 5wt%.Along with H
3bO
3interpolation, fusing assistant is melting in reaction process, provides a semifluid environment, is conducive to the crystallinity improving speed of reaction and reaction product; But work as H
3bO
3when addition is greater than 5wt%, excessive H
3bO
3al can be caused
20b
4o
36the generation of cenotype.
3Al of the present invention
2o
3﹒ 2SiO
2refer to 3/2 mullite.
The Tb adulterated in mullite matrix
3+be provide luminescence center as activator, utilize Tb
3+special level structure, by the transition absorption of electronics between different energy level with launch photon, shows the transmitting of different colours light.The Ce adulterated in matrix
3+be as sensitizing agent to improve the absorption of activator ion to light, namely utilize Ce-Tb transmission ofenergy, by non-radiative energy transition, luminous energy passed to activator ion from sensitizer ion, then luminous by activator ion energy level transition.
The Ce of the mullite that the present invention relates to
3+, Tb
3+ion doping belongs to structural vacancy doping, and the advantage of this doping way is that luminescence center is subject to the impact of lattice environment more weak, has excellent stability.Rare earth ion Ce
3+and Tb
3+suitable doping scope be respectively 0 ~ 2.0% and 0 ~ 20.0%, wherein optimum doping concentration is that 1.3mol% and 8.0mol% is (namely with aforementioned 0≤c≤2.0% respectively, 0≤d≤5.0%, the preferred value of c and d is respectively 1.3% consistent with 2% effect); Now Tb
3+and Ce
3+between there is the transmission ofenergy of greater efficiency, fluorescent material shows good green emission, and has good thermal stability: when envrionment temperature is 260 DEG C, and fluorescent material sample luminous intensity is 91% under room temperature, is obviously better than general commercial fluorescent material.
For improving Al further
6si
2o
13: the crystallinity of Ce, Tb fluorescent material and luminescent properties, add H
3bO
3as fusing assistant, and carry out certain aftertreatment.Under content is no more than 5wt% situation, fusing assistant H
3bO
3can high temperature solid state reaction be promoted, reaction is fully carried out smoothly, and be unlikely to the luminescent properties damaging fluorescent material.
In the present invention, the preparation method of aforementioned fluorescent powder, comprises the steps:
(1) by aAl
2o
3﹒ bSiO
2﹒ cCeO
2﹒ dTb
4o
7the stoichiometric ratio of each element in chemical formula, takes aluminum oxide, silicon-dioxide, cerium oxide and terbium sesquioxide raw material;
(2) raw material taken fully is mixed, and at room temperature ball milling;
(3) pour the sample after abundant ball milling into boron nitride crucible, put into the high temperature process furnances being connected with reducing atmosphere, calcine 2 ~ 6 hours at 1450 ~ 1550 DEG C;
(4) treat that furnace chamber is cooled to room temperature, take out sample and carry out crushing grinding;
(5) fusing assistant is added in follow-up employing, and deionized water carries out ultrasonic wave water washing or/and carry out SiO
2process such as coated grade.
Described ball milling carries out in agate mortar, and the time is 30 ~ 40min, until the basic uniformity of the color of raw material.
Described reducing atmosphere is 95%N
2+ 5%H
2mixed gas.
The described crushing grinding time is about 30min, makes the sample broke of caking and is ground to small grains, and size distribution is below 30 μm.
Described fusing assistant is H
3bO
3, best results when addition is 5wt%, is conducive to the tiny and even of reactant particle.
When deionized water carries out ultrasonic wave water washing, the Al that 1.5g is prepared
6si
2o
13: 100ml beaker poured into by Ce, Tb fluorescent material, adds 70ml deionized water, carries out ultrasonic disperse washing, and the time is 2h, cleaned to carry out suction filtration and drying and processing to mixed solution afterwards, and make particle dispersion good, size distribution is at 5 ~ 10 μm.
Described SiO
2coated process utilizes tetraethoxy (TEOS) hydrolytic action in an acidic solution to produce Si (OH)
4, then heat-treat at 600 DEG C, insulation 2h, makes the Si (OH) on fluorescent powder grain surface
4be converted into unformed amorphous Si O fine and close continuously
2film, now fluorescent powder grain size not too large change.SiO
2best covering amount is 15wt%.
Last handling process comprise washing and coated.Adopt ultra-sonic dispersion method to carry out washing and can reduce fluorescent powder grain reunion degree, improve dispersed and specific surface area, thus the luminous intensity of fluorescent material is improved.Chemical method is utilized to carry out SiO to fluorescent powder grain
2coated, especially work as SiO
2when content is 15wt%, the surface topography of fluorescent powder grain be improved significantly, and thermostability is highly improved.
Compared with existing result of study, the present invention has following beneficial effect:
1. the present invention adopts high temperature solid-state method to prepare fluorescent material, has that output is large, production cost is low and can the advantage of suitability for industrialized production, and it is simple to prepare fluorescent material flow process, and powder surface defect is few.
2. the fluorescent material prepared of the present invention is by rare earth ion Ce
3+and Tb
3+mix altogether, Ce
3+as sensitizer ion, effectively can strengthen the absorption of activator ion to light by transmission ofenergy, luminous intensity is significantly improved.
3. the present invention with the addition of fusing assistant and has carried out washing and coated aftertreatment in preparation process, and significantly can improve reaction conditions, obtain particle fine uniform, surface topography is good, the fluorescent material of good heat stability.
4. the fluorescent material excitation wavelength range prepared of the present invention is wide, and luminous intensity is high, has good thermostability, effectively can be excited generate bright green glow by UV-light.
5. this fluorescent material can be subject to exciting of the luminous element of emmission spectrum in 200 ~ 300nm region, the light of dominant absorption wavelength near 300nm, produce within the scope of 420 ~ 620nm, dominant emission peak at the emmission spectrum of about 540nm, and has the good thermal stability energy being better than general commercial fluorescent material.
Accompanying drawing explanation
Fig. 1 is excitation spectrum and the emmission spectrum of embodiment 1;
Fig. 2 is excitation spectrum and the emmission spectrum of embodiment 2;
Fig. 3 be embodiment 4 with the addition of H
3bO
3fluorescent material XRD figure spectrum;
Fig. 4 is that embodiment 2 is adding H with example 4
3bO
3the fluorescence emission spectrum comparison diagram of front and back.
Fluorometric investigation condition is: 150W xenon lamp, and PMT voltage is 400V, and sweep speed for 1200nm/min, light inlet and light-emitting window slit are 5nm, step-length 1nm.
Embodiment
Explain the present invention with accompanying drawing with the following Examples, but technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment 1
Weigh aluminum oxide 5.998g (0.588mol), silicon-dioxide 2.352g (0.392mol), terbium sesquioxide 1.496g (0.02mol), mixed, in agate mortar, ground 30min.The raw material of full and uniform mixing is poured in boron nitride crucible, puts corundum sheet at crucible underlay, put into high temperature process furnances and sinter, pass into reducing atmosphere 95%N
2+ 5%H
2, arranging sintering temperature is 1470 DEG C, and soaking time is 5h.Treat that furnace chamber is cooled to room temperature, taking-up sample carries out crushing grinding and is about 30min, can obtain Al
6si
2o
13: Tb fluorescent material.Now Tb
3+doping content be 8mol%, excitation and emission spectra is as shown in Figure 1.
Embodiment 2
Weigh aluminum oxide 5.918g (0.5802mol), silicon-dioxide 2.321g (0.3868mol), terbium sesquioxide 1.496g (0.02mol), cerium oxide 0.2236g (0.013mol), mixed, in agate mortar, ground 30min.The raw material of full and uniform mixing is poured in boron nitride crucible, puts corundum sheet at crucible underlay, put into high temperature process furnances and sinter, pass into reducing atmosphere 95%N
2+ 5%H
2, sintering temperature is 1470 DEG C, and soaking time is 5h.Treat that furnace chamber is cooled to room temperature, taking-up sample carries out crushing grinding and is about 30min, can obtain Al
6si
2o
13: Tb, Ce green light fluorescent powder.Now Ce
3+and Tb
3+doping content be respectively 1.3mol% and 8.0mol%, excitation and emission spectra is as shown in Figure 2.Take 297nm as excitation wavelength, the luminous quantum efficiency of fluorescent material is 24.21%, has good thermostability simultaneously: the luminous intensity of fluorescent material 260 DEG C time, is 91% of luminous intensity under room temperature.
Embodiment 3
Weigh aluminum oxide 5.918g (0.5802mol), silicon-dioxide 2.321g (0.3868mol), terbium sesquioxide 1.496g (0.02mol), cerium oxide 0.2236g (0.013mol), mixed, in agate mortar, ground 30min.The raw material of full and uniform mixing is poured in boron nitride crucible, puts corundum sheet at crucible underlay, put into high temperature process furnances and sinter, pass into reducing atmosphere 95%N
2+ 5%H
2, sintering temperature is 1470 DEG C, and soaking time is 5h.Treat that furnace chamber is cooled to room temperature, taking-up sample carries out crushing grinding and is about 30min, can obtain Al
6si
2o
13: Tb, Ce green light fluorescent powder; Follow-uply carry out 15wt%SiO again
2coated process: specifically utilize tetraethoxy (TEOS) hydrolytic action in an acidic solution to produce Si (OH)
4, then heat-treat at 600 DEG C, insulation 2h, makes the Si (OH) on fluorescent powder grain surface
4be converted into unformed amorphous Si O fine and close continuously
2film.Now fluorescent material Ce
3+and Tb
3+doping content be respectively 1.3mol% and 8.0mol%, when taking 297nm as excitation wavelength, luminous quantum efficiency is 18.33%; But having better thermostability: light-emitting phosphor intensity 260 DEG C time, is 98.8% of luminous intensity under room temperature.
Embodiment 4
Weigh aluminum oxide 5.918g (0.5802mol), silicon-dioxide 2.321g (0.3868mol), terbium sesquioxide 1.496g (0.02mol), cerium oxide 0.2236g (0.013mol), boric acid 0.524g (0.0085mol), mixed, and ground 30min in agate mortar.Again the raw material of full and uniform mixing is poured in boron nitride crucible, put corundum sheet at crucible underlay, put into high temperature process furnances and sinter, pass into reducing atmosphere 95%N
2+ 5%H
2, arranging sintering temperature is 1470 DEG C, and soaking time is 5h.Treat that furnace chamber is cooled to room temperature, taking-up sample carries out crushing grinding and is about 30min, can obtain the Al of B element doping
6si
2o
13: Tb, Ce green light fluorescent powder.Add the fluorescent material XRD figure spectrum after different content boric acid as shown in Figure 3.When taking 297nm as excitation wavelength, luminous quantum efficiency is 21.96%; Its luminous intensity 260 DEG C time is about 76% under room temperature.
Embodiment 5
Weigh aluminum oxide 5.918g (0.5802mol), silicon-dioxide 2.321g (0.3868mol), terbium sesquioxide 1.496g (0.02mol), cerium oxide 0.2236g (0.013mol), boric acid 0.524g (0.0085mol), mixed, in agate mortar, ground 30min.The raw material of full and uniform mixing is poured in boron nitride crucible, puts corundum sheet at crucible underlay, put into high temperature process furnances and sinter, pass into reducing atmosphere 95%N
2+ 5%H
2, arranging sintering temperature is 1470 DEG C, and soaking time is 5h.Treat that furnace chamber is cooled to room temperature, taking-up sample carries out crushing grinding and is about 30min, can obtain the Al of B element doping
6si
2o
13: Tb, Ce green light fluorescent powder.Take the fluorescent material sample that 1.5g has prepared, pour in 100ml beaker, add the deionized water of 70ml, under certain power, carry out ultrasonic disperse cleaning, the time is 2h, carries out suction filtration after cleaning to mixed solution, dries, milled processed.When taking 297nm as excitation wavelength, its luminescent spectrum as shown in Figure 4; Compared with the fluorescent material not adding boric acid flux with example 2, luminous intensity is significantly improved.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple inferences or replacement can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (10)
1. the novel green light fluorescent powder of the aluminosilicate of rare earth ion codoped, is characterized in that, new phosphors chemical constitution is aAl
2o
3﹒ bSiO
2﹒ cCeO
2﹒ dTb
4o
7, wherein a, b, c, d are molar fraction, a/b=3/2,0≤c≤2.0%, 0≤d≤5.0%, and are zero when c, d are different.
2. the novel green light fluorescent powder of aluminosilicate of a kind of rare earth ion codoped according to claim 1, is characterized in that, CeO
2be preferably 1.3%.
3. the novel green light fluorescent powder of aluminosilicate of a kind of rare earth ion codoped according to claim 1, is characterized in that, Tb
4o
7be preferably 2%.
4. the novel green light fluorescent powder of aluminosilicate of a kind of rare earth ion codoped according to the arbitrary claim of claim 1-3, is characterized in that, on described fluorescent material basis, and the fusing assistant H of interpolation
3bO
3, H
3bO
3massfraction for fluorescent material is 5wt%.
5. the novel green-emitting fluorescent powder, preparation method thereof of the aluminosilicate of rare earth ion codoped, is characterized in that, the novel green light fluorescent powder of aluminosilicate of the rare earth ion codoped as described in claim as arbitrary in claim 1-4, comprises the steps:
(1) by aAl
2o
3﹒ bSiO
2﹒ cCeO
2﹒ dTb
4o
7the stoichiometric ratio of each element in chemical formula, takes aluminum oxide, silicon-dioxide, cerium oxide and terbium sesquioxide raw material;
(2) raw material taken fully is mixed, and at room temperature ball milling;
(3) sample after abundant ball milling is put into the high temperature process furnances being connected with reducing atmosphere, calcine 2 ~ 6 hours at 1450 ~ 1550 DEG C;
(4) treat that furnace chamber is cooled to room temperature, take out sample and carry out crushing grinding;
(5) fusing assistant is added in follow-up employing, and deionized water carries out ultrasonic wave water washing or/and carry out SiO
2process such as coated grade.
6. preparation method according to claim 5, is characterized in that: under described room temperature, ball milling carries out in agate mortar, and the time is 30 ~ 40 minutes.
7. preparation method according to claim 5, is characterized in that: described reducing atmosphere is volume ratio 95%N
2+ 5%H
2mixed gas.
8. preparation method according to claim 5, is characterized in that: the described crushing grinding time is about 30 minutes, makes the sample broke of caking and is ground to small grains, and size distribution is below 30 μm.
9. preparation method according to claim 5, is characterized in that: described is fusing assistant H
3bO
3, H
3bO
3massfraction for fluorescent material is 5wt%.
10. preparation method according to claim 5, is characterized in that: when described employing deionized water carries out ultrasonic wave water washing, pour the fluorescent material of 1.5g into 100ml beaker, add 70ml deionized water, then carry out ultrasonic disperse washing, and the time is 2h; Cleaned and carried out suction filtration and drying and processing to mixed solution afterwards, make particle dispersion good, size distribution is at 5 ~ 10 μm; Or described SiO
2during coated process, be utilize tetraethoxy (TEOS) hydrolytic action in an acidic solution to produce Si (OH)
4, at 600 DEG C, then heat-treat insulation 2h, make the Si (OH) on fluorescent powder grain surface
4be converted into unformed amorphous Si O fine and close continuously
2film, SiO
2best covering amount is 15wt%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106277791A (en) * | 2016-08-13 | 2017-01-04 | 华南理工大学 | A kind of high temperature resistant silicon hydrochlorate luminous ceramic glaze and preparation method thereof |
| CN111378441A (en) * | 2018-12-29 | 2020-07-07 | 长春理工大学 | Improve rare earth doping SrSi2B2O8:Tb3+Technology for green light luminous intensity of fluorescent material |
| CN115785943A (en) * | 2022-10-19 | 2023-03-14 | 广州珠江光电新材料有限公司 | Blue-green fluorescent powder with core-shell structure and preparation method thereof |
| CN116285983A (en) * | 2023-03-30 | 2023-06-23 | 安徽工业大学 | Manganese-doped red-green light fluorescent powder with self-reduction effect and preparation method and application thereof |
| US11718567B2 (en) * | 2017-07-14 | 2023-08-08 | Canon Kabushiki Kaisha | Powder for ceramic manufacturing, ceramic manufactured object, and manufacturing method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881705A (en) * | 2014-03-26 | 2014-06-25 | 吉林大学 | Cerium, terbium or europium codoping activated aluminosilicate blue green fluorescent powder and preparation method thereof |
-
2015
- 2015-03-16 CN CN201510115144.6A patent/CN104710982B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881705A (en) * | 2014-03-26 | 2014-06-25 | 吉林大学 | Cerium, terbium or europium codoping activated aluminosilicate blue green fluorescent powder and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106277791A (en) * | 2016-08-13 | 2017-01-04 | 华南理工大学 | A kind of high temperature resistant silicon hydrochlorate luminous ceramic glaze and preparation method thereof |
| CN106277791B (en) * | 2016-08-13 | 2019-04-09 | 华南理工大学 | A kind of high temperature resistant silicon hydrochlorate luminous ceramic glaze and preparation method thereof |
| US11718567B2 (en) * | 2017-07-14 | 2023-08-08 | Canon Kabushiki Kaisha | Powder for ceramic manufacturing, ceramic manufactured object, and manufacturing method thereof |
| CN111378441A (en) * | 2018-12-29 | 2020-07-07 | 长春理工大学 | Improve rare earth doping SrSi2B2O8:Tb3+Technology for green light luminous intensity of fluorescent material |
| CN115785943A (en) * | 2022-10-19 | 2023-03-14 | 广州珠江光电新材料有限公司 | Blue-green fluorescent powder with core-shell structure and preparation method thereof |
| CN115785943B (en) * | 2022-10-19 | 2023-08-08 | 广州珠江光电新材料有限公司 | Blue-green fluorescent powder with core-shell structure and preparation method thereof |
| CN116285983A (en) * | 2023-03-30 | 2023-06-23 | 安徽工业大学 | Manganese-doped red-green light fluorescent powder with self-reduction effect and preparation method and application thereof |
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