CN101851509A - Method for preparing rare earth cerium ion-doped yttrium aluminum garnet fluorescent powder from network gel - Google Patents
Method for preparing rare earth cerium ion-doped yttrium aluminum garnet fluorescent powder from network gel Download PDFInfo
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- CN101851509A CN101851509A CN201010186575A CN201010186575A CN101851509A CN 101851509 A CN101851509 A CN 101851509A CN 201010186575 A CN201010186575 A CN 201010186575A CN 201010186575 A CN201010186575 A CN 201010186575A CN 101851509 A CN101851509 A CN 101851509A
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Abstract
The invention discloses a method for preparing rare earth cerium ion-doped yttrium aluminum garnet fluorescent powder from network gel, relates to fluorescent powder, and aims to obtain the fluorescent powder with low aggregation degree, small particle size and high performance. The method comprises the following steps of: dissolving yttrium oxide powder in excessive concentrated sulfuric acid and mixing dissolved yttrium oxide with solution of cerous nitrate and solution of aluminum nitrate to prepare metal ion solution, wherein the molar ratio of Y<3+> to Ce<3+> to Al<3+> is 2.94:0.06:5; adding NH4HCO3 into the metal ion solution and controlling the pH value of the metal ion solution to be between 3 and 5; adding an acrylamide monomer, a lattice reagent and an initiator into obtained solution and polymerizing the mixture to obtain wet gel; drying the wet gel to obtain dry gel; pre-sintering the dry gel to obtain pre-sintered powder; and adding a fluxing agent into the obtained pre-sintered powder and calcining the mixture to obtain the rare earth cerium ion-doped yttrium aluminum garnet fluorescent powder.
Description
Technical field
The present invention relates to a kind of fluorescent material, especially relate to a kind of method for preparing rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder with network gel.
Background technology
Be applied in the YAG:Ce fluorescent material on the white light LEDs, at first require the excitation wavelength of fluorescent material to be complementary, to reach higher light conversion efficiency with the emission wavelength of blue chip; Secondly, the exciting light of chip can be formed visual white light with the emission light of fluorescent material; The 3rd, the granularity of fluorescent material must be little, could guarantee that so more blue light sees through coat.So YAG:Ce fluorescent material must possess characteristics such as high purity, small particle size and high evenness, its grain-size, degree of crystallinity and dispersiveness have very big influence to the fluorescence property of fluorescent material.And these are decided by its preparation method to a great extent, and high-temperature solid phase reaction method is exactly a kind of traditional method of synthetic fluorescent material.This kind method technology is simple, efficient is high, cost is low, easy batch process, is one of the most general method of using at present.
1984, (G.de, H.J.A.van Dijk., Translucent Y such as G.de.With
3Al
5O
12Ceramics[J] .MaterialsResearch Bulletin, 1984,19 (12): 1669-1674.), adopt chemical pure level Al
2O
3And Y
2O
3Powder is a raw material, adds a small amount of SiO
2, after ball milling mixes, under the condition of 1500 ℃ of insulation 12h, synthesized the YAG powder.Liu Ruxi etc. (Liu Ruxi, Shi Jingren. white light emitting diode is with yttrium aluminium garnet fluorescent powder prescription and Mechanism Study [J]. Chinese rare-earth journal, 2002,20 (6): 495-501.), adopt solid phase method to synthesize fluorescent material, studied various ce
3+The crystalline structure of doping fluorescent material and luminescent spectrum, and with Gd, Ga ionic replacement Ce
3+Come influence to fluorescence property.But this method exists the equipment requirements height, the diameter of particle skewness of production, and granule-morphology is imperfect, the more shortcoming of rare earth material loss of costliness in the production.Therefore seek the heat subject that new synthetic method has become fluorescent material research.
Sol-gel method (sol-gel) is a kind of emerging wet chemical synthesis, utilizes it can obtain purity height, chemical constitution is even, particle diameter is less luminescent material, and need not to grind, and synthesis temperature is lower than traditional synthetic method.(Michael Veith, Sanjay Mathur, Aivaras Kareiva, Mohammad Jilavi, Michael Zimmera, VolkerHucha.Low temperature synthesis of nanocrystalline Y such as Michael Veith
3Al
5O
12(YAG) and Ce-doped Y
3Al
5O
12Viadifferent sol-gel methods[J] .Journal of materials chemistry, 1999,9:3069-3079), hydrolysis and concentrated Al in Pr (OH) solution, Y, the metal alkoxide of Ce has obtained gel, gel advances to handle later and calcining, has finally obtained fluorescent material.Employed metal alkoxide raw material is respectively Al
2(OBu
t)
6, Y
3(OBu
t)
9(Bu
tOH)
2And Ce
3(OBu
t)
9(Bu
tOH)
2(Yuexiao Pan such as Yuexiao Pan, Mingmei Wu, Qiang Su.Comparative investigation on synthesis andphotoluminescence of YAG:Ce phosphor[J] .Materials Science and Engineering B, 2004,106:251-256.), at Al, Y, in the nitrate solution of Ce, add sequestrant citric acid and hexylene glycol, at 200 ℃ of heating 5h.After the solvent evaporation, obtain the xanchromatic gel, obtained the fluorescent material of the Huang of nanoscale through high-temperature calcination.The weak point of sol-gel method is: Production Flow Chart long (be converted into by colloidal sol in the process of xerogel, moisture is wrapped in and is difficult in the colloid losing); Make raw material with metal alkoxide, cost is higher, and alkoxide has big toxicity, and is harmful to HUMAN HEALTH, easily environment caused very big pollution; Carbon ligand under non-oxidized substance atmosphere in the organic ligand is difficult for removing, thereby has increased the content of impurity in the prepared powder, influence the body colour of luminescent powder and luminosity etc., so Sol-gel technology does not also form industrialization so far.
Hydrothermal method (Hydrothermal Process) also is emerging in recent years synthetic method.This method (Takamori T, DavidL.D.Controlled nucleation for hydrothermal growth of yttrium-aluminum garnetpowders[J] .American Ceramic Society Bulletin, 1986,65 (9): 1282-1286) mainly be meant in the pressurized vessel of sealing, with water (or other fluids) as solvent, preparation and a kind of method of research material under high temperature, highly compressed condition.Studies show that (Zhang Xudong. preparation and the sign [D] of the synthetic and stupalith of YAG powder. Shandong University's doctorate paper, 2004.): it is even that the employing hydrothermal method has been synthesized particle size, well-crystallized's YAG fluorescent material.At first prepare non-crystalline state oxyhydroxide as the hydro-thermal reaction presoma with the precipitator method, then respectively to presoma heat-treat, mechanical mill is handled and introduce a small amount of YAG crystal seed, carry out hydro-thermal reaction under certain condition, induce nucleation density by changing inner sporadic nucleation and outside, to reach the temperature and the even grain size of control YAG nucleation and growth.With the synthetic YAG of hydrothermal method, though can obtain good dispersity, the uniformed powder of particle shape and controllable size at a lower temperature by controlling some factor, but because of needs high pressure and long reaction time (about 100MPa, 15h), to equipment and operational requirement height, this has also limited its application.
Spray pyrolysis is to adopt spray pyrolysis to prepare the process of material.(Y.C.Kang such as Kang.Y.C, I.W.Lenggoro, S.B.Park, K.Okuyama.Photoluminescence characteristics of YAG:Tbphosphor particles with spherical morphology and non-aggregation[J] .Journal of Physics andChemistry of Solids, 1999.60 (11): 1855-1858.) report, can prepare spheric with spray pyrolysis does not have the YAG:Tb of reunion (Ce) fluorescent material.This even-grained globe-type luminescence body helps obtaining higher tap density and reduces the twinkler scattering to improve the high resolving power and the luminous efficiency of twinkler.They also find to change the concentration of precursor solution simultaneously, and particle size also changes thereupon.When concentration from 0.03molL
-1Increase to 1molL
-1The time, granularity then increases to 1.2 μ m from 0.4 μ m.The shortcoming that spray pyrolysis exists is that it is hollow having many in the ultrafine particle that generates, and component is inhomogeneous.
Though solid-phase synthesis is commercialization, there are shortcomings such as high energy consumption, unstable product quality, other several method is not industrialization as yet all.Therefore, seek a kind of less energy-consumption, short period, synthetic product has good luminous performance and dispersed new synthesis process, will effectively promote the development of luminescent material industry.
Polyacrylamide-gel is to be made of the polymer of three-dimensional net structure and the medium that is filled in the macromolecular chain gap.Medium is a liquid generally speaking, therefore, polyacrylamide-gel can be regarded as the polymer three-dimensional network has comprised the expander of liquid (colloidal sol).Chemically crosslinked makes macromolecular chain intersegmental with covalently cross-linked, and this cross-link bond is very firm, makes polymer only swelling take place and can not dissolve.Usually add linking agent and carry out polymerization when synthetic macromolecule, perhaps reacting to each other by functional group in line style or the branching type macromolecular chain forms this covalent crosslink.In high-molecular gel, macromolecule network wraps solution, does not allow liquid flow out, and has played the effect of container, thereby the ion that is dissolved in the liquid can be disperseed well, has kept the primary proportioning, has reduced reunion.Water in the polyacrylamide-gel has several existences, and near the water macromolecule network has very strong interaction with network; And from the far water of network, show and the same character of ortho-water, be called free water (Gu Xuerong, Zhu Yuping. gel chemistry [M]. Beijing: Chemical Industry Press, 2005).
Polymer-network gel method (polyacrylamide method) is that P.Odier is at YBa
2Cu
3O
7A kind of novel method of using in the preparation of powder, its requirement to raw material is very simple, inorganic salt solution gets final product (A.Douy, P.Odier.The polyacrylamide gel:A novel route to ceramic and glassy oxide powders[J] .Materials Research Bulletin, 1989,24 (9): 1119-1126; Li Qiang, high Lian .YAG:Ce is given birth in tight east
3+The preparation of micro mist and spectrum property [J]. Journal of Inorganic Materials, 1997,12 (4): 575-578.).It is traditional solid phase method and novel ceramic molding---gel injection molding and forming technology (Gelcasting) combines and a kind of novel powder preparing technology that produces.This method is applied to the preparation of YAG:Ce fluorescent material, can avoids using expensive alkoxide to do raw material.What is more important since in gelation process formed macromolecule network the touch opportunity of metal ion is reduced, thereby reduced the generation of reuniting, can obtain little, the finely dispersed powder of particle size.
Summary of the invention
The object of the present invention is to provide a kind ofly to prepare the method for rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder, to obtain a kind of low reunion, little, the well behaved fluorescent material of particle size with network gel.
The present invention includes following steps:
1) preparation of metal ion solution: yttrium oxide powder is dissolved it with the excessive vitriol oil, mix being made into metal ion solution again with cerous nitrate and aluminum nitrate solution, wherein in molar ratio, control Y
3+: Ce
3+: Al
3+=2.94: 0.06: 5;
2) regulator solution pH value: in the metal ion solution that step 1) prepares, add NH
4HCO
3, the pH value of control metal ion solution is 3～5;
3) preparation of gel: in step 2) add acrylamide monomer, lattice reagent and initiator in the solution of gained, get wet gel after the polymerization;
4) the wet gel oven dry that step 3) is obtained gets xerogel;
5) with the xerogel pre-burning of step 4) gained, get preburning powder;
6) in the preburning powder of step 5) gained, add fusing assistant, get rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder after the calcining.
In step 3), described lattice reagent can adopt N, N '-methylene-bisacrylamide etc., and described initiator can adopt ammonium persulphate etc.; Described polymeric temperature can be 60～90 ℃, and the polymeric time can be 1～3h.
In step 4), the temperature of described oven dry can be 70～90 ℃.
In step 5), described xerogel pre-burning preferably rises to 650～750 ℃ with xerogel with the temperature rise rate of 1～5 ℃/min, and constant temperature 100～400min.
In step 6), described fusing assistant can adopt BaF
2And H
3BO
3, press mass ratio, BaF
2: H
3BO
3Be preferably 1: 1, described incinerating temperature can be 800～1300 ℃, preferably insulation after the calcining, and the time of insulation can be 100～400min.
Advantage of the present invention is: colloid chemistry and gel chemistry are introduced fluorescent material preparation technology, make each raw material particle position relative fixed, avoided occurring the phenomenon of uneven components in last calcination process.By polymer-network gel method, in the time of 1000 ℃, just can form pure YAG phase, this is than using low about 600 ℃ of traditional high-temperature solid phase reaction method.In the present invention, be incubated the different time down, can both form comparatively perfect YAG phase, and the difference of microscopic appearance be little between them at 1100 ℃.Along with holding time prolonging, excite with the relative intensity of emmission spectrum and improve, sample is not observed other dephasigns after adding solubility promoter, can improve the relative luminous intensity of fluorescent material simultaneously.In addition, add two kinds of solubility promoter (BaF
2And H
3BO
3) relative luminous intensity than only adding a kind of solubility promoter BaF
2Want high.
The present invention is containing metal ion Y
3+, Ce
3+And Al
3+Solution in, by the synthetic precursor of polymer-network gel method, calcining has at last obtained fluorescent material.In this process, reduced the reunion of powder greatly, obtain functional, tiny and uniform particle, and greatly reduced calcining temperature.
Embodiment
Embodiment 1
1) preparation of metal ion solution: take by weighing a certain amount of yttrium oxide powder, it is dissolved, mix being made into metal ion solution again with cerous nitrate and aluminum nitrate solution, (down together) wherein in molar ratio, control Y with the excessive vitriol oil
3+: Ce
3+: Al
3+=2.94: 0.06: 5.
2) regulator solution pH value: in the solution that step 1 prepares, add NH
4HCO
3The pH value of control metal ion solution is 3.
3) solution adds acrylamide monomer the preparation of gel: in step 2), N, and N '-methylene-bisacrylamide lattice reagent and ammonium persulfate initiator, controlled temperature obtains gel at 60 ℃ of polymerization 2h.
4) wet gel that step 3) is obtained 60 ℃ of oven dry moisture in air dry oven obtain xerogel.
5) xerogel of step 4) gained is risen to 700 ℃ with the heat-up rate of 1 ℃/min, and constant temperature 100min, preburning powder obtained.
6) two kinds of fusing assistant (BaF will be added in the preburning powder reducing atmosphere of step 5) gained
2+ H
3BO
3, 1: 1) and calcining, the control calcining temperature is incubated then at 800 ℃, and soaking time is controlled at 100min;
7) particle that the YAG:Ce fluorescent material particle diameter that makes is about 70nm accounts for 80% of total granularity, its colour rendering index Ra=56.5, fluorescent material can effectively be excited by blue light (460nm) and near-ultraviolet light (330nm-350nm), during with the excited by visible light of 460nm, can realize the VISIBLE LIGHT EMISSION of wavelength 565.6nm, relative intensity Y/Y0=5.300 has very high chemical stability and spectrum thermostability.
Embodiment 2
Raw material and technological process are with embodiment 1.The proportioning of metal ion is Y in the metal ion solution
3+: Ce
3+: Al
3+=2.94: 0.06: 5, add NH
4HCO
3The pH value of regulator solution is 4, the preparing gel controlled temperature is that 60 ℃ of polymerization times are 2.5h, the wet gel bake out temperature is 70 ℃, xerogel rises to 650 ℃ with the heat-up rate of 2 ℃/min, constant temperature 200min, the temperature of calcining preburning powder is 900 ℃, soaking time is 200min, the particle that the YAG:Ce fluorescent material particle diameter that makes is about 80nm accounts for 85% of total granularity,, its colour rendering index Ra=56.5, relative intensity Y/Y0=5.300, fluorescent material can (330～350nm) effectively excite, and during with the excited by visible light of 460nm, can realize that wavelength is the VISIBLE LIGHT EMISSION of 568nm by blue light (460nm) and near-ultraviolet light.
Embodiment 3
Raw material and technological process are with embodiment 1.The proportioning of metal ion is Y in the metal ion solution
3+: Ce
3+: Al
3+=2.94: 0.06: 5, add NH
4HCO
3The pH value of regulator solution is 5, the preparing gel controlled temperature is that 60 ℃ of polymerization times are 1h, the wet gel bake out temperature is 80 ℃, xerogel rises to 680 ℃ with the heat-up rate of 3 ℃/min, constant temperature 200min, the temperature of calcining preburning powder is 1000 ℃, soaking time is 300min, the particle that the YAG:Ce fluorescent material particle diameter that makes is about 90nm accounts for 90% of total granularity, its colour rendering index Ra=81, relative intensity Y/Y0=5.300, fluorescent material can (330～350nm) effectively excite by blue light (460nm) and near-ultraviolet light, during with the excited by visible light of 460nm, can realize that wavelength is the VISIBLE LIGHT EMISSION of 527nm.
Embodiment 4
Raw material and technological process are with embodiment 1.The proportioning of metal ion is Y in the metal ion solution
3+: Ce
3+: Al
3+=2.94: 0.06: 5, add NH
4HCO
3The pH value of regulator solution is 4, the preparing gel controlled temperature is that 60 ℃ of polymerization times are 3h, the wet gel bake out temperature is 90 ℃, xerogel rises to 750 ℃ with the heat-up rate of 4 ℃/min, constant temperature 200min, the temperature of calcining preburning powder is 1100 ℃, soaking time is 400min, the particle that the YAG:Ce fluorescent material particle diameter that makes is about 130nm accounts for 75% of total granularity, its colour rendering index Ra=65, and relative intensity can reach, relative brightness Y/Y0=5.300, fluorescent material can (330～350nm) effectively excite, and during with the excited by visible light of 460nm, can realize that wavelength is the VISIBLE LIGHT EMISSION of 558nm by blue light (460nm) and near-ultraviolet light.
Embodiment 5
Raw material and technological process are with embodiment 1.The proportioning of metal ion is Y in the metal ion solution
3+: Ce
3+: Al
3+=2.94: 0.06: 5, add NH
4HCO
3The pH value of regulator solution is 4, the preparing gel controlled temperature is that 60 ℃ of polymerization times are 2h, the wet gel bake out temperature is 80 ℃, xerogel rises to 720 ℃ with the heat-up rate of 5 ℃/min, constant temperature 200min, the temperature of calcining preburning powder is 1200 ℃, soaking time is 200min, the YAG:Ce fluorescent material particle diameter that makes is about the 100nm particle and accounts for 85% of total granularity, its colour rendering index Ra=62, and relative intensity can reach, relative brightness Y/Y0=5.300, fluorescent material can (330～350nm) effectively excite, and during with the excited by visible light of 460nm, can realize that wavelength is the VISIBLE LIGHT EMISSION of 532nm by blue light (460nm) and near-ultraviolet light.
Embodiment 6
Raw material and technological process are with embodiment 1.The proportioning of metal ion is Y in the metal ion solution
3+: Ce
3+: Al
3+=2.94: 0.06: 5, add NH
4HCO
3The pH value of regulator solution is 4, the preparing gel controlled temperature is that 60 ℃ of polymerization times are 1.5h, the wet gel bake out temperature is 80 ℃, xerogel rises to 730 ℃ with the heat-up rate of 2 ℃/min, constant temperature 200min, the temperature of calcining preburning powder is 1300 ℃, soaking time is 200min, the particle that the YAG:Ce fluorescent material particle diameter that makes is about 110nm accounts for 80% of total granularity, its colour rendering index Ra=70, and relative intensity can reach, relative brightness Y/Y0=5.300, fluorescent material can (330～350nm) effectively excite, and during with the excited by visible light of 460nm, can realize that wavelength is the VISIBLE LIGHT EMISSION of 518nm by blue light (460nm) and near-ultraviolet light.
Claims (9)
1. prepare the method for rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder with network gel, it is characterized in that may further comprise the steps:
1) preparation of metal ion solution: yttrium oxide powder is dissolved it with the excessive vitriol oil, mix being made into metal ion solution again with cerous nitrate and aluminum nitrate solution, wherein in molar ratio, control Y
3+: Ce
3+: Al
3+=2.94: 0.06: 5;
2) regulator solution pH value: in the metal ion solution that step 1) prepares, add NH
4HCO
3, the pH value of control metal ion solution is 3～5;
3) preparation of gel: in step 2) add acrylamide monomer, lattice reagent and initiator in the solution of gained, get wet gel after the polymerization;
4) the wet gel oven dry that step 3) is obtained gets xerogel;
5) with the xerogel pre-burning of step 4) gained, get preburning powder;
6) in the preburning powder of step 5) gained, add fusing assistant, get rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder after the calcining.
2. as claimed in claim 1ly prepare the method for rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder, it is characterized in that in step 3) described lattice reagent is N, N '-methylene-bisacrylamide with network gel.
3. as claimed in claim 1ly prepare the method for rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder, it is characterized in that in step 3) described initiator is an ammonium persulphate with network gel.
4. as claimed in claim 1ly prepare the method for rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder with network gel, it is characterized in that in step 3) described polymeric temperature is 60～90 ℃, the polymeric time is 1～3h.
5. as claimed in claim 1ly prepare the method for rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder, it is characterized in that in step 4) the temperature of described oven dry is 70～90 ℃ with network gel.
6. the method for preparing rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder with network gel as claimed in claim 1, it is characterized in that in step 5), described xerogel pre-burning is that xerogel is risen to 650～750 ℃ with the temperature rise rate of 1～5 ℃/min, and constant temperature 100～400min.
7. as claimed in claim 1ly prepare the method for rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder, it is characterized in that in step 6) described fusing assistant is BaF with network gel
2And H
3BO
3, press mass ratio, BaF
2: H
3BO
3It is 1: 1.
8. as claimed in claim 1ly prepare the method for rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder, it is characterized in that in step 6) described incinerating temperature is 800～1300 ℃ with network gel.
9. describedly prepare the method for rare-earth cerium ion doped yttrium aluminum garnet fluorescent powder as claim 1 or 8, it is characterized in that in step 6) with network gel, described calcining back insulation, the time of insulation is 100～400min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344806A (en) * | 2011-07-20 | 2012-02-08 | 太原理工大学 | Preparation method of white-light phosphor |
| RU2503754C1 (en) * | 2012-08-06 | 2014-01-10 | Федеральное Государственное Унитарное Предприятие "Государственный Ордена Трудового Красного Знамени Научно-Исследовательский Институт Химических Реактивов И Особо Чистых Химических Веществ" Министерства Образования И Науки Российской Федерации | Method of producing yttrium aluminium garnet alloyed with rare earth elements |
| CN107986630A (en) * | 2017-11-30 | 2018-05-04 | 华南协同创新研究院 | A kind of preparation method of nano-bioactive glass powder |
| CN112592064A (en) * | 2020-12-15 | 2021-04-02 | 新沂市锡沂高新材料产业技术研究院有限公司 | YAG microcrystalline glass and preparation method thereof |
| CN116103040A (en) * | 2023-02-10 | 2023-05-12 | 华北水利水电大学 | Preparation method of nano luminescent material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344806A (en) * | 2011-07-20 | 2012-02-08 | 太原理工大学 | Preparation method of white-light phosphor |
| CN102344806B (en) * | 2011-07-20 | 2013-11-27 | 太原理工大学 | Preparation method of white-light phosphor |
| RU2503754C1 (en) * | 2012-08-06 | 2014-01-10 | Федеральное Государственное Унитарное Предприятие "Государственный Ордена Трудового Красного Знамени Научно-Исследовательский Институт Химических Реактивов И Особо Чистых Химических Веществ" Министерства Образования И Науки Российской Федерации | Method of producing yttrium aluminium garnet alloyed with rare earth elements |
| CN107986630A (en) * | 2017-11-30 | 2018-05-04 | 华南协同创新研究院 | A kind of preparation method of nano-bioactive glass powder |
| CN112592064A (en) * | 2020-12-15 | 2021-04-02 | 新沂市锡沂高新材料产业技术研究院有限公司 | YAG microcrystalline glass and preparation method thereof |
| CN112592064B (en) * | 2020-12-15 | 2022-06-07 | 新沂市锡沂高新材料产业技术研究院有限公司 | YAG microcrystalline glass and preparation method thereof |
| CN116103040A (en) * | 2023-02-10 | 2023-05-12 | 华北水利水电大学 | Preparation method of nano luminescent material |
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