CN107721161A - A kind of green fluorescence glass applied to LED encapsulation and preparation method thereof - Google Patents
A kind of green fluorescence glass applied to LED encapsulation and preparation method thereof Download PDFInfo
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- CN107721161A CN107721161A CN201711044829.1A CN201711044829A CN107721161A CN 107721161 A CN107721161 A CN 107721161A CN 201711044829 A CN201711044829 A CN 201711044829A CN 107721161 A CN107721161 A CN 107721161A
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- 239000011521 glass Substances 0.000 title claims abstract description 172
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000005538 encapsulation Methods 0.000 title claims abstract description 16
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000000463 material Substances 0.000 claims abstract description 55
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 239000000146 host glass Substances 0.000 claims abstract description 20
- 238000002844 melting Methods 0.000 claims abstract description 13
- 230000008018 melting Effects 0.000 claims abstract description 13
- 238000010348 incorporation Methods 0.000 claims abstract description 6
- 239000011812 mixed powder Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 37
- 229910052593 corundum Inorganic materials 0.000 claims description 22
- 239000010431 corundum Substances 0.000 claims description 22
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000003287 optical effect Effects 0.000 description 30
- 238000004458 analytical method Methods 0.000 description 18
- 239000011159 matrix material Substances 0.000 description 18
- 229910052751 metal Inorganic materials 0.000 description 18
- 239000002184 metal Substances 0.000 description 18
- 238000004064 recycling Methods 0.000 description 17
- 238000001429 visible spectrum Methods 0.000 description 17
- 239000002994 raw material Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 4
- 230000008878 coupling Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000004075 alteration Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910003069 TeO2 Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 1
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000006025 fining agent Substances 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 235000021384 green leafy vegetables Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 239000013500 performance material Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 1
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/14—Silica-free oxide glass compositions containing boron
- C03C3/15—Silica-free oxide glass compositions containing boron containing rare earths
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- 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
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
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- Computer Hardware Design (AREA)
- Dispersion Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a kind of green fluorescence glass applied to LED encapsulation and preparation method thereof, the green fluorescence glass is made up of host glass and green emitting phosphor, wherein the host glass is made up of effective material of following molar fraction：Bi2O3：10 50mol%, B2O3：30 80mol%, ZnO：5 20mol%, in the green fluorescence glass, the mass fraction of the green emitting phosphor is 1 10wt%.The preparation method includes：Frit mixed melting, green emitting phosphor incorporation, mixed powder co-sintering handle three steps.The green fluorescence glass of the present invention realizes that host glass melt temperature is low, production cost is low, can produce the advantages that high quality LED.
Description
Technical field
The present invention relates to luminescent material and its preparation field, more particularly, to a kind of green fluorescence applied to LED encapsulation
Glass and preparation method thereof.
Background technology
White light LEDs have the advantages that energy-efficient, green, service life is long, turn into forth generation solid-state illumination light source,
With development in recent years, its application has penetrated into the every field of general illumination.And its market great economy, society behind
Benefit so that it is included national strategy plan by countries in the world one after another, and China is also opened in the case where the Department of Science and Technology " 863 " plan is supported
Move " National Semiconductor illuminating engineering ".
At present in mainstream market white light LEDs packaging technology, mainly utilize traditional silica gel and organic resin and fluorescent material
Mix to be packaged, then heated curing molding.It is well known that LED light source also produces amount of heat luminous while,
Temperature around core PN junction is even up to 150 DEG C.During long-time use, some drawbacks can gradually show white light LEDs
It is existing --- aging, the yellow of encapsulating material, the light decay and color drift of white light LEDs.How to solve this problem be development the long-life,
The key of high power white LED technology.For these problems, domestic and international scientist proposes that white light LEDs are sealed with phosphor
The thinking of dress, substitute organic packaging materials such as glass ceramics, fluorescent glass (PiG).Because glass/ceramic inorganic matrix has
Excellent both thermally and chemically stability, by the service life of the more preferable fluorescent material for extending incorporation.Fluorescent material mixes low melting point base
Matter glass and the fluorescent glass being uniformly mixed with less than 800 degree melting conditions are considered as the inorganic encapsulated of excellent performance
Material.
With the development of LED industry, the requirement more and more higher to LED product, the warm white LED of high color rendering index (CRI) also turns into
One hot research direction, thus turn into needs applied to the green fluorescence glass of LED encapsulation.
The Chinese invention patent CN201310010509.X of South China Normal University's application, a kind of entitled " novel fluorescence glass
Glass and preparation method thereof ", fluorescent glass is by P in the document2O5、ZnO、MgO、Na2O、Li2The glass matrix and Ce of O compositions：YAG
Phosphor raw material is made in 600-1000 degree co-sinterings.The preparation temperature of the host glass is too high and complicated components, in preparation
Impurity may be mixed in water quenching cooling and mechanical milling process；And the Na wherein contained2O is easily caused the deliquescence reaction of glass, is unfavorable for
Large-scale production, but Na2O effect is to reduce melting temperature, can not directly remove, otherwise can cause its obtained product
It is unqualified.
The Chinese invention patent CN105523715.A of Wenzhou University's application, a kind of entitled " the transparent fluorescent glass of low melting point
Glass and preparation method thereof and the application in white light LEDs ", fluorescent glass is by B in the document2O3、Bi2O3、TeO2、ZnO、Na2O、
Sb2O3、NaNO3Raw material components and Ce：YAG fluorescent powder is well mixed to be directly incubated 1-4 hours in 500-650 degree, fluorescent glass liquid
It is on 300-500 DEG C of pig mold to pour into temperature, is subsequently placed in Muffle furnace and is annealed, and is protected during glass transformation temperature Tg temperature
Warm 2-4 hours, it is cooled back to room temperature and forms fluorescent glass.The patent prepares fluorescent glass, Step Time by a fusion method
Na that is long, and wherein containing2O is easily caused the deliquescence reaction of glass, and the transparency is bad, but Na2O has reduction melting temperature
Effect, can not directly be removed；In addition, the necessary component Sb as fining agent2O3It is irritant, poisonous oxide, right and wrong
Environmentally friendly composition, and the TeO contained in frit2、Sb2O3It is expensive, it is unfavorable for mass producing.
The content of the invention
The present invention provides a kind of green fluorescence glass and preparation method thereof applied to LED encapsulation, this fluorescent glass with compared with
Few raw material and simple formula have reached the requirement of fluorescent glass, have higher luminescent properties and the transparency, this preparation side
Method has proportioning process simple, pollution-free and be easy to civilian high-quality LED large-scale production, green emitting phosphor in fluorescent glass
There are higher luminescent properties and transparent performance.
Technical scheme is as follows：
A kind of green fluorescence glass applied to LED encapsulation, it is made up of host glass and green emitting phosphor, wherein described
Host glass is made up of effective material of following molar fraction：
Bi2O3：10-50mol%,
B2O3：30-80mol%,
ZnO：5-20mol%,
In the green fluorescence glass, the mass fraction of the green emitting phosphor is 1-10wt%.
Preferably, the effectively material B2O3With H3BO3Form add, remaining effective material is with above-claimed cpd shape
Formula adds.
Preferably, the green emitting phosphor is the yellowish green powder of GaYAG series or the green powder of LuAG.
Preferably, the Bi2O3Molar fraction be 15-30mol%.
Preferably, the B2O3Molar fraction be 55-80mol%.
Preferably, the molar fraction of the ZnO is 5-15mol%.
A kind of preparation method of green fluorescence glass applied to LED encapsulation, the green fluorescence glass is by host glass
It is made with green emitting phosphor, wherein the host glass is made up of effective material of following molar fraction：Bi2O3：10-
50mol%, B2O3：30-80mol%, ZnO：5-20mol%, in the green fluorescence glass, the quality of the green emitting phosphor
Fraction is 1-10wt%；The preparation method includes：Frit mixed melting, green emitting phosphor mix, at mixed powder co-sintering
Manage three steps.
Preferably, the Bi2O3Molar fraction be 15-30mol%.
Preferably, the B2O3Molar fraction be 55-80mol%.
Preferably, the molar fraction of the ZnO is 5-15mol%.
In certain embodiments, the step of frit mixed melting is as follows：Effective material Bi2O3、B2O3, ZnO is by pre-
After fixed molar fraction proportioning is sufficiently mixed, pour into corundum crucible or platinum crucible, then by corundum crucible or platinum crucible
It is positioned in Muffle furnace and is sintered with above-mentioned glass mixed material, the temperature setting of Muffle furnace is 750 DEG C -950 DEG C, insulation
0.5-2 hours, obtain glass solution.
In certain embodiments, the step of green emitting phosphor incorporation is as follows：Glass solution is cooled to room temperature, then
Glass powder is ground into, and crosses 100-300 mesh sieves；The glass powder obtained with grinding mixes with the green emitting phosphor.
In certain embodiments, the step of mixed powder co-sintering processing is as follows：The glass powder and the green
The powder that fluorescent material is mixed to get is placed in Muffle furnace, and temperature range is arranged within 500 DEG C -650 DEG C, and 10-30 takes after minute
Go out, be cooled to room temperature, form fluorescent glass.
In certain embodiments, the green emitting phosphor is the yellowish green powder of GaYAG series or the green powder of LuAG.
Preferably, the effectively material B2O3With H3BO3Form add, remaining effective material is with above-claimed cpd shape
Formula adds；Above-mentioned various raw materials are that analysis is pure.
Preferably, in the step of frit mixed melting, it is 900 DEG C to set sintering temperature, is incubated 2 hours.
Preferably, in the step of walking the green emitting phosphor incorporation, the mesh number of sieving is 200 mesh.
Preferably, in the step of mixed powder co-sintering processing, the glass powder burns altogether with the green emitting phosphor
The temperature of knot is 600 DEG C, and soaking time is 30 minutes.
Compared with prior art, beneficial effects of the present invention are as follows：
(1) host glass of the invention has following advantage：The present invention is with Bi2O3-B2O3- ZnO is used as host glass body
System, wherein ZnO can effectively reduce the melting temperature of host glass, prevent green emitting phosphor from decomposing denaturation at high temperature；B2O3As
Glass network adjusts body, Bi2O3As glass former, under the suitable proportioning that the present invention limits, triple interaction can
Obtain the host glass that fusing point is low, transparency is high；
(2) method provided by the invention for preparing green fluorescence glass, the melting of host glass raw material and incorporation green are glimmering
Co-sintering after light powder extraneous need not provide too high temperature, and preparation process time it is short, without noxious gas emission, realize
Energy-conservation and environmental protection.
Certainly, any product for implementing the present invention it is not absolutely required to reach all the above advantage simultaneously.
Brief description of the drawings
Fig. 1 is the pictorial diagram of green fluorescence glass prepared by the embodiment of the present invention 1；
Fig. 2 is the hair of sample after green fluorescence glass prepared by the embodiment of the present invention 1 couples with blue light for InGaN chip
Radiograph；
Fig. 3 is the spectrogram that green fluorescence glass prepared by the embodiment of the present invention 1 couples with blue light for InGaN chip；
Fig. 4 is the chromaticity diagram after green fluorescence glass prepared by the embodiment of the present invention 1 couples with blue chip；
Fig. 5 is the spectrogram that green fluorescence glass prepared by the embodiment of the present invention 2 couples with blue light for InGaN chip；
Fig. 6 is the spectrogram that green fluorescence glass prepared by the embodiment of the present invention 3 couples with blue light for InGaN chip；
Fig. 7 is the spectrogram that green fluorescence glass prepared by the embodiment of the present invention 8 couples with blue light for InGaN chip；
Fig. 8 is the chromaticity diagram after green fluorescence glass prepared by the embodiment of the present invention 8 couples with blue chip.
Fig. 9 is the transmitance figure for the host glass that the embodiment of the present invention 8 is prepared.
Embodiment
The present invention provides a kind of green fluorescence glass applied to LED encapsulation and preparation method thereof, is especially applicable to white
Light LED encapsulation fields.
Herein, the scope represented by " numerical value to another numerical value ", is that one kind avoids enumerating in the description
The summary representation of all numerical value in the scope.Therefore, the record of a certain special value scope, covers the number range
Interior any number and the relatively fractional value scope defined by any number in the number range, as bright in the description
Text writes out any number and is somebody's turn to do as compared with fractional value scope.
The invention is specifically described with reference to specific embodiment.Following examples will be helpful to that this is expanded on further
Invention, but the invention is not limited in any way.It should be pointed out that to those skilled in the art, do not taking off
On the premise of present inventive concept, various modifications and improvements can be made.These belong to protection scope of the present invention.
Embodiment 1
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, obtains glass after being cooled to room temperature, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 510nm-GaYAG fluorescent material of 9% mass fraction, pass through co-sintering, temperature
Degree is arranged on 600 DEG C, is incubated 30min, is cooled to room temperature and forms green fluorescence glass, as shown in Figure 1.
The luminous photo that GaYAG green fluorescences glass couples with blue chip, bright green glow is sent, as shown in Figure 2.
But because accompanying drawing can not use colour, so it is green that Fig. 1 and Fig. 2, which are changed into not seeing after gray scale,.
Carrying out test using stc-4000 rapid spectrometers and PMS-80 visible Spectra Analysis on Edge Recycling system, can to obtain GaYAG green
Coupling spectrum figure such as Fig. 3 of color fluorescent glass, obtained chromaticity diagram such as Fig. 4.From figure 3, it can be seen that the GaYAG greens of the present invention
The emission peak of fluorescent glass is broadband peak, and most strong launch wavelength is at 511nm；From fig. 4, it can be seen that the present invention
The chromaticity coordinates drop point of GaYAG green fluorescence glass is in green area.
Embodiment 2
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 520nm-GaYAG fluorescent material of 9% mass fraction, pass through co-sintering, temperature
Degree is arranged on 600 DEG C, is incubated 30min, is cooled to room temperature and forms fluorescent glass.
Carrying out test using stc-4000 rapid spectrometers and PMS-80 visible Spectra Analysis on Edge Recycling system, can to obtain GaYAG green
The coupling spectrum figure of color fluorescent glass is as shown in figure 5, visible in figure, centre wavelength in the spectrogram intensity highest in 519nm,
Illustrate 520nm-GaYAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 3
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 525nm-GaYAG fluorescent material of 9% mass fraction, pass through co-sintering, temperature
Degree is arranged on 600 DEG C, is incubated 30min, is cooled to room temperature and forms fluorescent glass.
Carrying out test using stc-4000 rapid spectrometers and PMS-80 visible Spectra Analysis on Edge Recycling system, can to obtain GaYAG green
The coupling spectrum figure of color fluorescent glass is as shown in fig. 6, centre wavelength in spectrogram intensity highest, explanation in 525nm
525nm-GaYAG fluorescent material is in success doped matrix glass in the case of not changing optical property.
Embodiment 4
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 530nm-GaYAG fluorescent material of 9% mass fraction, pass through co-sintering, temperature
Degree is arranged on 600 DEG C, is incubated 30min, is cooled to room temperature and forms the good fluorescent glass of optical property, it is fast by stc-4000
Intensity is most in 529nm for centre wavelength in the spectrogram that fast spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling system is tested to obtain
Height, illustrate 530nm-GaYAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 5
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 535nm-GaYAG fluorescent material of 9% mass fraction, pass through co-sintering, temperature
Degree is arranged on 600 DEG C, is incubated 30min, is cooled to room temperature and forms the good fluorescent glass of optical property, it is fast by stc-4000
Intensity is most in 535nm for centre wavelength in the spectrogram that fast spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling system is tested to obtain
Height, illustrate 535nm-GaYAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 6
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 540nm-GaYAG fluorescent material of 9% mass fraction, pass through co-sintering, temperature
Degree is arranged on 600 DEG C, is incubated 30min, is cooled to room temperature and forms the good fluorescent glass of optical property, it is fast by stc-4000
Intensity is most in 540nm for centre wavelength in the spectrogram that fast spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling system is tested to obtain
Height, illustrate 540nm-GaYAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 7
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 545nm-GaYAG fluorescent material of 9% mass fraction, pass through co-sintering, temperature
Degree is arranged on 600 DEG C, is incubated 30min, is cooled to room temperature and forms the good fluorescent glass of optical property, it is fast by stc-4000
Intensity is most in 546nm for centre wavelength in the spectrogram that fast spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling system is tested to obtain
Height, illustrate 545nm-GaYAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 8
By 15mol%Bi2O3, 80mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, 200 mesh was ground to the glass for being cooled to room temperature
Sieve, takes a certain amount of glass powder to be mixed with the 520nm-LuAG fluorescent material of 9% mass fraction, passes through co-sintering, temperature setting
At 600 DEG C, 30min is incubated, room temperature is cooled to and forms fluorescent glass.Using stc-4000 rapid spectrometers and PMS-80 visible rays
Spectrum analysis system, which carries out test, can obtain coupling spectrum figure such as Fig. 7 of LuAG green fluorescence glass, and obtained chromaticity diagram is as schemed
8.From figure 7 it can be seen that the emission peak of the GaYAGLuAG green fluorescence glass of the present invention is broadband peak, most strong transmitting
Wavelength is at 520nm；From figure 8, it is seen that the chromaticity coordinates drop point of the LuAG green fluorescence glass of the present invention is in green area.From
The host glass transparency that the transmitance figure of the host glass of the present embodiment shown in Fig. 9 can be seen that the present invention is high.
Embodiment 9
By 20mol%Bi2O3, 75mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 525nm-LuAG fluorescent material of 9% mass fraction, pass through co-sintering, temperature
600 DEG C are arranged on, is incubated 30min, room temperature is cooled to and forms the good fluorescent glass of optical property, it is quick by stc-4000
Intensity is most in 525nm for centre wavelength in the spectrogram that spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling systems are tested to obtain
Height, illustrate 525nm-LuAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 10
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 530nm-LuAG fluorescent material of 9% mass fraction, pass through co-sintering, temperature
600 DEG C are arranged on, is incubated 30min, room temperature is cooled to and forms the good fluorescent glass of optical property, it is quick by stc-4000
Intensity is most in 530nm for centre wavelength in the spectrogram that spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling systems are tested to obtain
Height, illustrate 530nm-LuAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 11
By 20mol%Bi2O3, 70mol%B2O3, 10mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 535nm-LuAG fluorescent material of 9% mass fraction, pass through co-sintering, temperature
600 DEG C are arranged on, is incubated 30min, room temperature is cooled to and forms the good fluorescent glass of optical property, it is quick by stc-4000
Intensity is most in 534nm for centre wavelength in the spectrogram that spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling systems are tested to obtain
Height, illustrate 535nm-LuAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 12
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 540nm-LuAG fluorescent material of 9% mass fraction, pass through co-sintering, temperature
600 DEG C are arranged on, is incubated 30min, room temperature is cooled to and forms the good fluorescent glass of optical property, it is quick by stc-4000
Intensity is most in 541nm for centre wavelength in the spectrogram that spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling systems are tested to obtain
Height, illustrate 540nm-LuAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 13
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 545nm-LuAG fluorescent material of 9% mass fraction, pass through co-sintering, temperature
600 DEG C are arranged on, is incubated 30min, room temperature is cooled to and forms the good fluorescent glass of optical property, it is quick by stc-4000
Intensity is most in 546nm for centre wavelength in the spectrogram that spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling systems are tested to obtain
Height, illustrate 545nm-LuAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 14
By 15mol%Bi2O3, 80mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 525nm-GaYAG fluorescent material of 7% mass fraction, pass through co-sintering, temperature
Degree is arranged on 600 DEG C, is incubated 30min, is cooled to room temperature and forms the good fluorescent glass of optical property, it is fast by stc-4000
Intensity is most in 526nm for centre wavelength in the spectrogram that fast spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling system is tested to obtain
Height, illustrate 525nm-LuAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 15
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 525nm-GaYAG fluorescent material of 11% mass fraction, pass through co-sintering, temperature
Degree is arranged on 600 DEG C, is incubated 30min, is cooled to room temperature and forms the good fluorescent glass of optical property, it is fast by stc-4000
Intensity is most in 525nm for centre wavelength in the spectrogram that fast spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling system is tested to obtain
Height, illustrate 525nm-LuAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 16
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 535nm-LuAG fluorescent material of 7% mass fraction, pass through co-sintering, temperature
600 DEG C are arranged on, is incubated 30min, room temperature is cooled to and forms the good fluorescent glass of optical property, it is quick by stc-4000
Intensity is most in 536nm for centre wavelength in the spectrogram that spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling systems are tested to obtain
Height, illustrate 535nm-LuAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 17
By 25mol%Bi2O3, 70mol%B2O3, 5mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 535nm-LuAG fluorescent material of 11% mass fraction, pass through co-sintering, temperature
Degree is arranged on 600 DEG C, is incubated 30min, is cooled to room temperature and forms the good fluorescent glass of optical property, it is fast by stc-4000
Intensity is most in 535nm for centre wavelength in the spectrogram that fast spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling system is tested to obtain
Height, illustrate 535nm-LuAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Embodiment 18
By 30mol%Bi2O3, 55mol%B2O3, 15mol%ZnO weighs by proportioning, it is well mixed after pour into corundum crucible
In, it is put into and is incubated 2 hours in 900 DEG C of Muffle furnace and obtains glass metal, is cooled to room temperature and obtains glass, it was ground
200 mesh sieves, take a certain amount of glass powder to be mixed with the 535nm-LuAG fluorescent material of 11% mass fraction, pass through co-sintering, temperature
Degree is arranged on 600 DEG C, is incubated 30min, is cooled to room temperature and forms the good fluorescent glass of optical property, it is fast by stc-4000
Intensity is most in 535nm for centre wavelength in the spectrogram that fast spectrometer and PMS-80 visible Spectra Analysis on Edge Recycling system is tested to obtain
Height, illustrate 535nm-LuAG fluorescent material in success doped matrix glass in the case of not changing optical property.
Above example has been described in detail to the present invention.It is to be appreciated that the invention is not limited in above-mentioned spy
Determine embodiment, those skilled in the art can make various deformations or amendments within the scope of the claims, and this has no effect on
The substantive content of the present invention.
Under the teaching of the present invention and above-described embodiment, those skilled in the art are easy to it is envisioned that cited by the present invention
Or each raw material enumerated or its equivalent alterations, each processing method or its equivalent alterations can realize the present invention, and each original
The parameter bound value of material and processing method, interval value can realize the present invention, embodiment numerous to list herein.
Claims (10)
- A kind of 1. green fluorescence glass applied to LED encapsulation, it is characterised in that it is made up of host glass and green emitting phosphor, Wherein described host glass is made up of effective material of following molar fraction：Bi2O3：10-50mol%,B2O3：30-80mol%,ZnO：5-20mol%,In the green fluorescence glass, the mass fraction of the green emitting phosphor is 1-10wt%.
- 2. the green fluorescence glass applied to LED encapsulation as claimed in claim 1, it is characterised in that the green emitting phosphor For the yellowish green powder of GaYAG series or the green powder of LuAG.
- 3. the green fluorescence glass applied to LED encapsulation as claimed in claim 1, it is characterised in that the Bi2O3Mole Fraction is 15-30mol%.
- 4. the green fluorescence glass applied to LED encapsulation as claimed in claim 1, it is characterised in that the B2O3Mole point Number is 55-80mol%.
- 5. as claimed in claim 1 applied to LED encapsulation green fluorescence glass, it is characterised in that the ZnO mole point Number is 5-15mol%.
- 6. it is a kind of applied to LED encapsulation green fluorescence glass preparation method, it is characterised in that the green fluorescence glass by Host glass and green emitting phosphor are made, wherein the host glass is made up of effective material of following molar fraction：Bi2O3：10-50mol%,B2O3：30-80mol%,ZnO：5-20mol%,In the green fluorescence glass, the mass fraction of the green emitting phosphor is 1-10wt%.The preparation method includes：Glass Glass material mixed melting, green emitting phosphor incorporation, mixed powder co-sintering handle three steps.
- 7. the preparation method applied to the LED green fluorescence glass encapsulated as claimed in claim 6, it is characterised in that described The step of frit mixed melting, is as follows：Effective material Bi2O3、B2O3, after ZnO is sufficiently mixed by predetermined molar fraction proportioning, Pour into corundum crucible or platinum crucible, corundum crucible or platinum crucible and above-mentioned glass mixed material are then positioned over Muffle It is sintered in stove, the temperature setting of Muffle furnace is 750 DEG C -950 DEG C, is incubated 0.5-2 hours, obtains glass solution.
- 8. the preparation method applied to the LED green fluorescence glass encapsulated as claimed in claim 6, it is characterised in that described The step of green emitting phosphor mixes is as follows：Glass solution is cooled to room temperature, is then ground to glass powder, and cross 100-300 Mesh sieve；The glass powder obtained with grinding mixes with the green emitting phosphor.
- 9. the preparation method applied to the LED green fluorescence glass encapsulated as claimed in claim 6, it is characterised in that described The step of mixed powder co-sintering processing, is as follows：The glass powder is placed in Muffle with the powder that the green emitting phosphor is mixed to get In stove, temperature range is arranged within 500 DEG C -650 DEG C, and 10-30 takes out after minute, naturally cools to room temperature, forms fluorescence glass Glass.
- 10. the preparation method applied to the LED green fluorescence glass encapsulated as claimed in claim 6, it is characterised in that described Green emitting phosphor is the yellowish green powder of GaYAG series or the green powder of LuAG.
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