CN109437590A - A kind of preparation method of the glass fluorescent plate for warm white LED - Google Patents
A kind of preparation method of the glass fluorescent plate for warm white LED Download PDFInfo
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- CN109437590A CN109437590A CN201811388400.9A CN201811388400A CN109437590A CN 109437590 A CN109437590 A CN 109437590A CN 201811388400 A CN201811388400 A CN 201811388400A CN 109437590 A CN109437590 A CN 109437590A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/0883—Arsenides; Nitrides; Phosphides
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7734—Aluminates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7774—Aluminates
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/23—Mixtures
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/119—Deposition methods from solutions or suspensions by printing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/13—Deposition methods from melts
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
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- Inorganic Chemistry (AREA)
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- Geochemistry & Mineralogy (AREA)
- Glass Compositions (AREA)
Abstract
The present invention provides a kind of preparation methods of glass fluorescent plate for warm white LED.The glass fluorescent plate is the glaze layer that one layer of evenly dispersed fluorescent powder is fired by glaze in transparent glass substrate；Fluorescent powder removes Ce3+:Y3Al5O12Outside, Eu is added2+:Sr3SiO5、Eu2+:Sr2Si5N8One or both of；Glaze layer constituent content (mol%) are as follows: 35~50P2O5, 0~10B2O3, 30~50ZnO, 0~20RxO, RxO is one or more of alkaline earth, alkali metal oxide.The present invention also provides the preparation methods of the glass fluorescent plate, and the cost of material is low, and simple process is suitable for large-scale production.Glass fluorescent plate of the invention blue light excitation under can emit orange light, combine with blue light generate warm white, thus can development and application in building blue chip excite warm white LED.
Description
Technical field
The present invention relates to solid luminescent material fields, can realize that orange light is sent out under blue light excitation more particularly, to one kind
The preparation method for the glass fluorescent plate penetrated.
Background technique
Currently, most commercialization white light LEDs are by blue light for InGaN chip and Ce3+:Y3Al5O12Fluorescent powder packaging is one
Made of rising, fluorescent powder is scattered in silica gel and is coated on chip.Blue light a part that InGaN chip issues is inhaled by fluorescent powder
It receives, makes it be excited to issue yellow light, the yellow light that unabsorbed blue light and fluorescent powder issue, which mixes, just obtains white light.Due to silicon
The thermal conductivity and chemical stability of glue are poor, are easy to happen aging, yellow under the hot environment of high-power die irradiation, cause
LED colour cast, the serious curtailment service life of LED component.Further, since the missing of feux rouges, the white light exhibition for causing device to issue
Existing higher colour temperature and relatively low colour rendering index.Therefore, it researches and develops one kind and can effectively be excited by blue chip, adjustable color, Gao Xian
Colour index, high heat conductance, high physicochemical stability glass fluorescent plate to substitute fluorescent powder/silica gel fluorescence conversion layer, be in the world
Develop the newest direction of white light for illumination LED technology.Compared with conventional device, is encapsulated using glass fluorescent plate, be not only omitted
The preparation of fluorescent powder and packaging plastic and coating processes, improve the efficiency of white light encapsulation, and improve the uniformity of fluorescent powder
And thermal stability, so as to improve the luminous mass and reliability of device.
By Commercial optical powder microcrystalline dispersion into low-melting-point glass matrix, it has also become acquisition has excellent performance grinding for glass fluorescent plate
Study carefully hot spot.There are mainly three types of preparation methods: (1) tabletting sintering process, such as report (Chung W.et al, Optics Lett.,
2012,37(15):3276-3278；Tsai C.et al, Opt.Mater.Express, 2014,4 (1): 121-128 etc.) institute
It states, a certain proportion of fluorescent powder and low-melting-point glass powder is pressed into thin slice after evenly mixing, then press the heat treatment side of ceramic post sintering
Formula obtains glass fluorescent plate；This method is simple and fast, avoids erosion of the glass metal to fluorescent powder to a certain extent, but product is saturating
Lightness is poor, and inside is easy some holes of residual, and needs to grind, could be used to encapsulate after polishing, and process costs are very high.
(2) melt supercooled method such as reports (Wang Y.et al, Laser Photonics Rev., 2014,8 (1): 158-164；
Xiang W.et al,CrystEngComm,2015,17(37):7079-7085；Patent CN103183473A etc.) it is described, by one
After evenly mixing, melten glass powder simultaneously keeps fluorescent powder solid-state to the fluorescent powder and low-melting-point glass powder of certainty ratio, then infuses melt
Mold forming obtains glass fluorescent plate after annealed processing；This method acquisition product transparency is high, consistency is high, but fluorescent powder
Easy to be big by glass melt erosion, consumption, product needs to cut, grind, could be used to encapsulate after polishing, and process costs are very high.
(3) film sintering process such as reports (Liu S.et al, Opt.Lett., 2013,38 (13): 2240-2243；Patent
CN103189326A；CN104428256A；CN103011614A etc.) it is described, by a certain proportion of fluorescent powder, glass powder and organic
Solvent is coated on transparent glass substrate after evenly mixing, and solvent volatilization, glass powder are melted (fluorescent powder holding through Overheating Treatment
Solid-state) and obtain glass fluorescent plate；The cost of material is low for this method, simple process, strong applicability, is suitable for large-scale production, product
Transparency is high, and luminescent properties are excellent, are the technologies of preparing for most having application prospect.But in the above-mentioned report using film sintering process
In, the design of the component of low-melting-point glass is unreasonable, containing to the unfavorable PbO of environment, to the Bi of luminescence queenching effect2O3Or glass is molten
Temperature height processed.The invention proposes a kind of based on the new glass fluorescent plate of glaze component formula and preparation method thereof, and material is saturating
Lightness is high, and luminescent properties are excellent；Orange light is issued under the excitation of 465nm blue light, is that one kind is excellent, can be applied to warm white
The novel solid luminescent material of LED.
Summary of the invention
The present invention for overcome the deficiencies in the prior art, proposes a kind of orange smooth glass based on new glaze component formula
Fluorescent plate has transparent glass substrate, and it is 20~100 μm, evenly dispersed fluorescent powder crystal grain that one side surface, which is fired by glaze a layer thickness,
Glass luminescent layer.Spectrum test the result shows that, glass fluorescent plate 465nm blue light excitation under issue bright orange light, with
It can produce warm white light emitting after commercial blue chip combination.
The preparation method of glass fluorescent plate of the present invention, comprising the following steps:
(1) constituent content (mol%) of glass glaze are as follows: 35~50P2O5；0~10B2O3；30~50ZnO；0~20RO；
0~20R2O；The RO is one of ZnO, MgO, CaO, SrO, BaO or a variety of, R2O is Li2O、Na2O、K2One of O or
It is a variety of.Weighed powder material is fully ground and is uniformly placed in corundum crucible, be put into Muffle furnace and be heated to 1000~
1~2 hour is kept the temperature after 1200 DEG C to be allowed to melt, and then glass melt is taken out and is quickly poured into copper mold or cold water and obtain glass
Presoma.
(2) it after step (1) forerunner's glass obtained being crushed, ground, crosses standard screen screening and obtains partial size less than 5 μm
Glass powder；Then glass powder and fluorescent powder are mixed simultaneously for 1:0.05~0.2 with fluorescent powder mass ratio according to glass powder quality
Grind 10~15 minutes obtained mixed powders；Then based on by mixed powder and organic solvent mass ratio for 1:0.8, by mixed powder be placed in by
In the organic solvent that 85wt% terpinol, 5wt% ethyl cellulose, 10wt% lauric acid form, it is sufficiently stirred 1~2 hour and makes
Obtain glass ink.Wherein, the fluorescent powder removes Ce3+:Y3Al5O12Outside bloom, Eu is added2+:Sr3SiO5Orange powder, Eu2+:Sr2Si5N8
One or both of rouge and powder.
(3) step (2) resulting glass ink is coated in 0.5~3.0mm by silk-screen printing or casting molding processes
On the clean transparent glass substrate of thickness, formed the uniform glass paste bed of material of 40~140 μ m thicks, be subsequently placed in Muffle furnace in
400 DEG C of heat treatment, 1 hour removing organic matter, then be warming up to 520~560 DEG C and be heat-treated 0.5~1 hour, make low-melting-point glass glaze
Bond vitrified obtains glass fluorescent plate on the glass substrate.
Glass fluorescent plate preparation process of the invention is simple, low in cost, nontoxic and pollution-free, has good calorifics and change
Learn stability and excellent optical characteristics, can development and application in the warm white LED of building blue chip excitation.
Detailed description of the invention
Fig. 1 is fluorescence spectra of the 1 glass fluorescent plate of embodiment under the excitation of 465 nano wave lengths.
Specific embodiment
The present invention will be further illustrated in the following examples, but there is no limit to the present invention.
Embodiment 1:
By analytically pure NH4H2PO4、ZnO、Li2CO3、Na2CO3、K2CO3Powder, by 35P2O5: 50ZnO:5Li2CO3:
5Na2CO3: 5K2CO3(mol%) proportion accurate weighing is placed in agate mortar, is mixed and is ground and is uniformly placed on corundum crucible
In, be put into Muffle furnace and be heated to 1200 DEG C of heat preservations and be allowed to melt for 1 hour, then melt is taken out and be quickly poured into mold at
Type obtains blocky forerunner's glass.Glass powder quality 20% is added in the agate mortar after grinding uniformly in forerunner's glass breaking
Ce3+:Y3Al5O12/Eu2+:Sr3SiO5Fluorescent powder, grinding are placed in a beaker after ten minutes, add mixed powder quality 80%
Organic solvent, stirring are allowed to uniformly mixed in 1 hour.By the glass ink of acquisition by screen-printing deposition with a thickness of 1mm's
It cleans on glass slide, forms the glass paste bed of material of about 40 μ m thicks, be then placed in Muffle furnace and remove within heat treatment 1 hour for 400 DEG C
Organic matter, then be warming up to 560 DEG C and be heat-treated 0.5 hour, make glass glaze bond vitrified on glass slide, obtains glass fluorescent plate
After the cutting of glass fluorescent plate, its Emission at Room Temperature spectrum is measured with FLS920 Fluorescence Spectrometer.It is excited in 465 nano blue lights
Under, there is the orange light emitting (as shown in Figure 1) that central wavelength is 580 nanometers.By 465 nano blue lights of glass fluorescent plate and business
Chip coupling, the capable of emitting bright warm white under blue light excitation.
Embodiment 2:
By analytically pure NH4H2PO4、ZnO、H3BO3、BaCO3、Na2CO3、K2CO3Powder, by 40P2O5: 30ZnO:10B2O3:
10BaCO3: 5Na2CO3: 5K2CO3(mol%) proportion accurate weighing is placed in agate mortar, is mixed and is ground and is uniformly placed on
In corundum crucible, it is put into Muffle furnace and is heated to 1000 DEG C of heat preservations and is allowed to melt for 1 hour, then melt is taken out and is quickly poured into
Die for molding obtains blocky forerunner's glass.Glass powder is added in the agate mortar after grinding uniformly in forerunner's glass breaking
The Ce of quality 5%3+:Y3Al5O12/Eu2+:Sr2Si5N8Fluorescent powder, grinding are placed in a beaker after ten minutes, add mixing silty
The organic solvent of amount 80%, stirring are allowed to uniformly mixed in 1 hour.By the glass ink of acquisition by screen-printing deposition in thickness
To form the glass paste bed of material of about 140 μ m thicks on the cleaning glass slide of 1mm, it is then placed in 400 DEG C of heat treatment 1 in Muffle furnace
Hour removes organic matter, then is warming up to 520 DEG C and is heat-treated 0.5 hour, makes glass glaze bond vitrified on glass slide, obtains glass
Glass fluorescent plate.
Embodiment 3:
By analytically pure NH4H2PO4、ZnO、H3BO3、CaCO3、Li2CO3、Na2CO3Powder, by 35P2O5: 40ZnO:5B2O3:
5CaO:10Li2CO3: 5Na2CO3(mol%) proportion accurate weighing is placed in agate mortar, is mixed and is ground and is uniformly placed on
In corundum crucible, it is put into Muffle furnace and is heated to 1100 DEG C of heat preservations and is allowed to melt for 1 hour, then melt is taken out and is quickly poured into
Graininess forerunner's glass is obtained in cold water.Glass powder quality is added in the agate mortar after grinding uniformly in forerunner's glass breaking
15% Ce3+:Y3Al5O12/Eu2+:Sr3SiO5/Eu2+:Sr2Si5N8Fluorescent powder, grinding are placed in a beaker after ten minutes, add
The organic solvent of mixed powder quality 80%, stirring are allowed to uniformly mixed in 2 hours.The glass ink of acquisition is brushed by screen printing
It overlays on the cleaning glass slide with a thickness of 1mm, forms the glass paste bed of material of about 60 μ m thicks, be then placed in Muffle furnace 400 DEG C
It is heat-treated 1 hour removing organic matter, then is warming up to 540 DEG C and is heat-treated 1 hour, makes glass glaze bond vitrified on glass slide,
Obtain glass fluorescent plate.
Claims (1)
1. a kind of preparation method of the glass fluorescent plate for warm white LED, comprising the following steps:
(1) constituent content (mol%) of glass glaze are as follows: 35~50P2O5；0~10B2O3；30~50ZnO；0~10RO；10~
20R2O；The RO is one of ZnO, MgO, CaO, SrO, BaO or a variety of, R2O is Li2O、Na2O、K2One of O or more
Kind, weighed powder material is fully ground in the agate mortar and is uniformly placed in corundum crucible, is put into Muffle furnace and adds
Heat is allowed to melt to keeping the temperature 1~2 hour after 1000~1200 DEG C, then takes out glass melt and is quickly poured into copper mold or cold
Glass presoma is obtained in water；
(2) it after step (1) forerunner's glass obtained being crushed, ground, crosses standard screen screening and obtains glass of the partial size less than 5 μm
Glass powder；Then glass powder and fluorescent powder are mixed and is ground for 1:0.05~0.2 with fluorescent powder mass ratio according to glass powder quality
10~15 minutes obtained mixed powders；Then based on by mixed powder and organic solvent mass ratio for 1:1.6, by mixed powder be placed in by
In the organic solvent that 85wt% terpinol, 5wt% ethyl cellulose, 10wt% lauric acid form, it is sufficiently stirred 1~2 hour and makes
Obtain glass ink, wherein the fluorescent powder removes Ce3+:Y3Al5O12Outside bloom, Eu is added2+:Sr3SiO5Orange powder, Eu2+:Sr2Si5N8
One or both of rouge and powder；
(3) step (2) resulting glass ink is coated in 0.5~3.0mm thickness by silk-screen printing or casting molding processes
Clean transparent glass substrate on, formed the uniform glass paste bed of material of 40~140 μ m thicks, be then placed in resistance furnace 400 DEG C
It is heat-treated 1 hour removing organic matter, then is warming up to 520~560 DEG C and is heat-treated 0.5~1 hour, keeps the melting of low-melting-point glass glaze viscous
Knot obtains glass fluorescent plate on the glass substrate.
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| CN201811388400.9A CN109437590A (en) | 2018-11-21 | 2018-11-21 | A kind of preparation method of the glass fluorescent plate for warm white LED |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109988557A (en) * | 2019-04-28 | 2019-07-09 | 大连工业大学 | A kind of novel solid green CsPbBr3The preparation method of quantum dot crystallite luminescent material |
| CN111675492A (en) * | 2020-05-21 | 2020-09-18 | 中国计量大学 | High-color-rendering-property mixed fluorescent glass film for laser, preparation method thereof and thickness pre-screening method |
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| CN102730975A (en) * | 2012-06-20 | 2012-10-17 | 武汉理工大学 | Glass-ceramic and preparation method thereof |
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| CN107804974A (en) * | 2017-11-01 | 2018-03-16 | 上海应用技术大学 | A kind of preparation method of the remote fluorescence piece based on low-melting point lead-less glasses powder |
| CN107892487A (en) * | 2017-11-01 | 2018-04-10 | 上海应用技术大学 | A kind of preparation method of the remote fluorescence piece based on low melting point borosilicate glass powder |
| CN108529893A (en) * | 2018-05-08 | 2018-09-14 | 上海应用技术大学 | A kind of preparation method of high-capacity LED fluorescent glass film |
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2018
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109988557A (en) * | 2019-04-28 | 2019-07-09 | 大连工业大学 | A kind of novel solid green CsPbBr3The preparation method of quantum dot crystallite luminescent material |
| CN111675492A (en) * | 2020-05-21 | 2020-09-18 | 中国计量大学 | High-color-rendering-property mixed fluorescent glass film for laser, preparation method thereof and thickness pre-screening method |
| CN111675492B (en) * | 2020-05-21 | 2022-05-27 | 中国计量大学 | High-color-rendering-performance mixed fluorescent glass film for laser, preparation method thereof and thickness pre-screening method |
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