CN106892562A - A kind of Ce that sandwich-like is prepared with the tape casting:The method of YAG microcrystalline glass - Google Patents
A kind of Ce that sandwich-like is prepared with the tape casting:The method of YAG microcrystalline glass Download PDFInfo
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- CN106892562A CN106892562A CN201611216180.2A CN201611216180A CN106892562A CN 106892562 A CN106892562 A CN 106892562A CN 201611216180 A CN201611216180 A CN 201611216180A CN 106892562 A CN106892562 A CN 106892562A
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- Prior art keywords
- sandwich
- glass
- yag
- tape casting
- microcrystalline glass
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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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
-
- 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
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
- C03C27/10—Joining glass to glass by processes other than fusing with the aid of adhesive specially adapted for that purpose
-
- 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 with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
Abstract
A kind of Ce that sandwich-like is prepared with the tape casting:The method of YAG microcrystalline glass, comprises the following steps:(1) frit is made up of following effective materials, and the content of each effective material is expressed as with molar fraction:ZnO 10 20%, Sb2O35 17%, TeO225 40%, Li2O 6 13%, K2O 10 15%, Ce:YAG fluorescent powder 5 20%;After frit is sufficiently mixed, grinding, by compound and distilled water hybrid modulation into mixed slurry;(2) by mixed slurry on the casting machine even application thickness be 0.1 0.5mm and the white glass piece that matches with dimension of light source, shape on;(3) the white glass piece that will be coated is dried 69 hours in 200 300 DEG C, the white glass piece of same shape, size is covered after moisture evaporation on batch mixing top layer, in the glass intermediate plate of sandwich-like in 600 800 DEG C of heat preservation sinterings 14 hours, the Ce that room temperature forms the sandwich-like that thickness is 0.4 1.5mm is subsequently cooled to:YAG microcrystalline glass.The present invention fires obtained the preferable sandwich-like devitrified glass of photoelectric parameter at relatively low temperature.
Description
Technical field
The present invention relates to a kind of Ce of sandwich-like:The preparation method of YAG microcrystalline glass, the microcrystalline glass can be direct
It is packaged with light source and is matched, Simplified flowsheet, cost-effective, achievable industrial mass production.
Background technology
White light LEDs as the solid light source of new generation for progressively substituting incandescent lamp, fluorescent lamp and high-voltage gas discharging light,
Because its luminous efficiency is high, long lifespan, energy-saving and environmental protection the advantages of, it is shown that huge market potential and application prospect.Current commercial
The white light LEDs of change be mainly be the combination by blue light for InGaN chip and yellow fluorescent powder come what is realized, its operation principle is exactly
The blue light components that InGaN chips send are absorbed by yellow fluorescent powder, and the fluorescent material being excited sends gold-tinted, and unabsorbed indigo plant
Light is then combined through the gold-tinted that phosphor powder layer and fluorescent material send, so as to obtain white light.It is glimmering using silica gel or resin parcel at present
Light powder is packaged, and because phosphor material powder is close to chip pyrotoxin, chip temperature rises high-heating radiation and can reduce fluorescent material performance,
Simultaneously because heat radiation and shortwave radiation can accelerate, and encapsulating material is aging to pass it through rate reduction, these problems can cause the LED longevity
Life shortening, light efficiency decline, color coordinate drift etc..Additionally, fluorescent material is the problems such as skewness, refractive index are mismatched in silica gel
Equally can also influence the optical property of LED.
Although the commercialized development of LED has been passed by over half a century, the particularly invention of InGaN blue chips accelerates
Solid-state devices realizes the possibility of white light LEDs.The business white light LEDs for wrapping up fluorescent powder packaging with resin or silica gel at present are present
Poor, the higher thermal coefficient of expansion of heat conductivility, relatively low thermally and chemically stability the problems such as, greatly limit its indoors according to
Application on the great power LEDs such as bright, headlight for vehicles.Ce:The solid fluorescences such as YAG devitrified glasses, single crystal fluorescent material, fluorescence ceramics
Material because hard, heat-resisting, humidity, it is corrosion-resistant the advantages of, in the side such as heat endurance, life-span, luminous efficiency for improving white light LEDs
Face obtains some progress, is just causing extensive concern and the research of domestic and foreign scholars.Particularly Ce:YAG devitrified glasses are glimmering compared with monocrystalline
The preparation cost low (relatively low firing temperature, less energy consumption) of luminescent material and fluorescence ceramics, cycle is short, technology are simple, right
Prepare has potential application value and broader development empty without epoxy resin, long lifespan, powerful white light LED part
Between, studying it has practical meaning and value.Current Ce:YAG devitrified glasses it has not proved as commercialization.
Use Ce:The white light LEDs of YAG devitrified glasses encapsulation and the Ce of epoxy resin parcel:YAG fluorescent powder is compared, with the longevity
The advantages of life is long, light efficiency is high, thermal conductivity is good, mechanical strength is good.Use Ce at present:YAG devitrified glasses are used as solid fluorescent material
Patent for white light LEDs is as follows:" low-melting-point fluorescent glass for white light LED and preparation method thereof (China Patent No. CN
101643315B) ", " it is used for white light LEDs Ce:YAG devitrified glasses and preparation method thereof (China Patent No. CN
103183473A) ", " a kind of Ce:YAG devitrified glasses and its application (the China Patent No. CN in white light LEDs
104529166A) ", " a kind of transparent Ce:YAG devitrified glasses and its application (the China Patent No. CN in white light LEDs
104529170A) ", " the enhanced Ce of a kind of metal:YAG devitrified glasses and preparation method thereof (China Patent No. CN
103319092A)”.They are all by Ce:YAG crystallite phases are uniformly inlayed and form Ce in glass:YAG devitrified glasses.It is public
The Ce for opening:The method for packing of YAG devitrified glasses be all after the fluorescent glass dicing that will be prepared again with LED chip light source phase
Matching, this method for packing optimizes the packaging technology of market mainstream LED to a certain extent, but still there is shortcoming.Such as
The heat radiation produced after fluorescent glass and chip directly contact can reduce fluorescent material performance, and the fluorescent glass prepared is bulk
Shape, it is difficult to cutting processing, and the difficult recycling of leftover pieces cut, cause the wasting of resources, limit it industrially big
Large-scale production, prolongs and has hindered Ce:The process of YAG devitrified glass market business.
The tape casting is used as a kind of process for producing, the at present extensive use in the industries such as ceramics, plastics, glass.
The preparation technology that sandwich-like microcrystalline glass of different shapes improves devitrified glass is prepared using the tape casting, can effectively be solved
Current pure Ce:YAG devitrified glass directly contacts chip, it is difficult to cut, wastes leftover pieces and match difficulty etc. with different size light source and ask
Topic.In consideration of it, the Ce of sandwich-like:YAG microcrystalline glass is highly suitable as a kind of new fluorescent material.It is presently disclosed
Document and patent, are not involved with using the Ce of sandwich-like:YAG microcrystalline glass is glimmering as the solid-state of high-power LED encapsulation
Luminescent material.Microcrystalline glass is prepared by the tape casting simplify operation, cost-effective, achievable high-volume, large scale, Multiple Shape
Industrialized production.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of material component is unique, transparency is high, optics
The sandwich-like Ce of excellent performance:The preparation method of YAG microcrystalline glass, the method achieve sandwich-like sheet glass and founds temperature
The low, preparation method of degree is simple, sheet glass of different shapes is directly matched with light source, can industrially realize wanting for mass production
Ask, its product has the advantages that physicochemical properties stabilization, luminous efficiency high, high homogeneity, long lifespan, thermal conductivity are high.
The present invention can be achieved by the following technical programs:
A kind of Ce that sandwich-like is prepared with the tape casting:The method of YAG microcrystalline glass, comprises the following steps:
(1) mixed slurry modulation:Frit is made up of following effective materials:ZnO、Sb2O3、TeO2、Li2O、K20 and Ce:
YAG fluorescent powder;Counted with the total mole number of frit as 100%, the content of each effective material is expressed as with molar fraction:
After frit is sufficiently mixed in mortar, is ground, by compound and distilled water with mass ratio 1:0.05-0.2
Hybrid modulation is into mixed slurry;
(2) curtain coating of mixed slurry:By mixed slurry on casting machine even application thickness be 0.1-0.5mm and with light
On the white glass piece that Source size, shape match, the suspended degree of mixed slurry and the speed and blade of curtain coating are controlled as needed
Thickness;
(3) drying and firing of sandwich-like microcrystalline glass:The white glass piece that will be coated is placed in 200-300 DEG C of vacuum
In drying box, dry 6-9 hours, the white glass piece of same shape, size is covered after moisture evaporation on batch mixing top layer, in sandwich
The glass intermediate plate of shape is sintered in being put in Muffle furnace, and the temperature for setting Muffle furnace is 600-800 DEG C, 1-4 hours is incubated, then with stove
It is the Ce of the sandwich-like of 0.4-1.5mm to naturally cool to room temperature and form thickness:YAG microcrystalline glass.
Further, ZnO content is preferably 10-20mol%, more preferably 12-16mol%.
Further, Sb2O3Content is preferably 10-25mol%, more preferably 15-23mol%.
Further, Te20 content is preferably 25-40mol%, more preferably 32-40mol%.
Further, Li20 content is preferably 6-13mol%, more preferably 6-8mol%.
Further, K20 content is preferably 10-15mol%, more preferably 12-13mol%.
Further, Ce:YAG fluorescent powder content is preferably 5-20mol%, more preferably 12-20mol%.
Further, the transmitance of the white glass piece for being used must must roll over more than 90%, refractive index close to laminated glass matrix
Penetrate rate or Ce:The refractive index of YAG fluorescent powder, reduces light loss;And its softening point temperature must be higher than 800 DEG C, be maintained at 600-
Mechanical strength during 800 DEG C of sintered glasses, the preferred K9 of white glass, sodium calcium silicon, sodium calcium lead glass, the preferred 0.3- of this white glass thickness
0.5mm。
Further, to keep mixed slurry to be coated in the uniformity of blank glass surface, the speed for being cast blade can pass through
Casting apparatus regulate and control, preferably 0.02-0.05m/s, more preferably 0.04m/s.
Further, the thickness of curtain coating blade can be controlled by adjusting micrometer caliper on blade, be lighted to keep stronger
Preferable adsorption strength between intensity and devitrified glass and two white glass pieces, blade thickness is preferably 0.1-0.5mm, more preferably
0.2-0.3mm。
Sandwich-like microcrystalline glass prepared by the present invention can directly match encapsulation with light source, prepare white light LEDs.
Compared with the encapsulation technology of existing white light LEDs, the beneficial effects of the present invention are:The present invention is set by sandwich style
Count fluorescent material Ce:YAG devitrified glasses are encapsulated in sandwich interlayer, by the blade thickness and regulation Ce that control curtain coating:
The composition of YAG devitrified glasses makes it be fired into the preferable sandwich devitrified glass of photoelectric parameter at relatively low temperature, tool
There is following advantage:
(1) this configuration reduces main flow LED fluorescent powder and the directly contact of blue chip, the use of white light LEDs is extended
Life-span.
(2) Ce of the invention:The composition of YAG devitrified glasses causes that it has compared with low melting point, and devitrified glass matrix
Refractive index is approached with the refractive index of fluorescent material.
(3) present invention prepares the sandwich-like microcrystalline glass of different shapes matched with light source, without cutting, directly
Encapsulation, has saved cost, has simplified technique.Sandwich-like devitrified glass prepared by the present invention can on a large scale be used for industrial metaplasia
Produce.
Brief description of the drawings
The present invention is described in further details with reference to different accompanying drawings and example, but is in no way limiting of the present invention.
Accompanying drawing 1 is the wafer illustraton of model of sandwich-like microcrystalline glass prepared by the tape casting of embodiment 1.
Accompanying drawing 2 is that the structural representation of sandwich-like devitrified glass wafer model encapsulation prepared by the tape casting of embodiment 1 is bowed
View.
Accompanying drawing 3 is the square model figure of sandwich-like microcrystalline glass prepared by the tape casting of embodiment 2.
Accompanying drawing 4 is the structural representation top view of sandwich-like microcrystalline glass square package prepared by the tape casting of embodiment 2.
Specific embodiment
The present invention is described in further detail with specific implementation below in conjunction with the accompanying drawings, but is in no way limiting of the present invention.
The Ce that the embodiment of the present invention is used:YAG fluorescent powder manufacturer is Jiangmen City Keheng Industry Co., Ltd, type
Number:L-552.
Embodiment 1:
By analytically pure ZnO, Sb2O3, Te20, Li20, K2O, Ce:YAG, by 12ZnO:17Sb2O3:37Te20:6Li20:
13K2O:15Ce:It is placed in agate mortar after the proportioning accurate weighing of YAG fluorescent powder (mol ratio), mixes in agate mortar and grind
The compound obtained after mill is with distilled water according to 94:6 mass are evenly coated in Φ 50*3mm than hybrid modulation into slurry with casting machine
On the K9 wafer sheet glass of size, spiral micrometer sets the thickness that 0.2mm is curtain coating blade, the speed control of curtain coating and is
0.04m/s, is dried 6 hours in 200 DEG C of vacuum drying chambers, and cooling is taken out, and the K9 wafers of Φ 50*3mm are covered on batch mixing top layer
Sheet glass, is put in after being heated to 650 DEG C in resistance furnace in the glass intermediate plate of sandwich-like and is incubated 1 hour, then cools to the furnace
20 DEG C form the devitrified glass wafer model piece that transparent low melting point, thickness reach 72% sandwich-like for 6.2mm, transmitance
(accompanying drawing 1).As shown in figure 1, devitrified glass 1 is uniformly clipped between white glass piece 2, the microcrystalline glass is in interlayer sandwich-like
Model.
Devitrified glass wafer model piece (accompanying drawing 1) of low melting point sandwich-like prepared by the tape casting is matched with light source and carried out
The structural representation top view of encapsulation such as accompanying drawing 2.In the model, the interlayer sandwich-like microcrystalline glass 4 for preparing is covered in light
White-light LED encapsulation test is carried out on source (blue chip) 3, light efficiency has reached 112.8lm/W, and colour temperature is 5216K, and colour rendering index is
74.2。
Embodiment 2:
By analytically pure ZnO, Sb2O3, Te20, Li20, K2O, Ce:YAG, by 16ZnO:15Sb2O3:35Te20:6Li20:
13K2O:15
Ce:It is placed in agate mortar after the proportioning accurate weighing of YAG fluorescent powder (mol ratio), mixes in agate mortar and grind
The compound obtained after mill is with distilled water according to 94:6 mass are evenly coated in 50* than hybrid modulation into slurry with casting machine
On the square K9 white glasses piece of 50mm, spiral micrometer sets the thickness that 0.3mm is curtain coating blade, the speed control of curtain coating and is
0.04m/s.Dried 6 hours in 200 DEG C of vacuum drying chambers, cooling to be taken out be directly placed into resistance furnace after cover plate and is heated to 620
1 hour is incubated after DEG C, 20 DEG C is then cooled to the furnace and is formed transparent low melting point, thickness for 6.3mm, transmitance reach the three of 69%
The devitrified glass square plate (accompanying drawing 3) of Mingzhi's shape.As shown in figure 3, devitrified glass 1 is uniformly clipped between white glass piece 2, this is micro-
Crystal glass piece is in the model of interlayer sandwich-like.
Such as accompanying drawing 4, the sandwich-like devitrified glass square plate 4 for preparing is covered in above blue chip 3, as described above, enters
Row encapsulation is no longer repeated.Test light efficiency is 119.5lm/W, and colour temperature is 5450K, and colour rendering index is 71.6.
Claims (6)
1. it is a kind of with the tape casting prepare sandwich-like Ce:The method of YAG microcrystalline glass, comprises the following steps:
(1) mixed slurry modulation:Frit is made up of following effective materials:ZnO、Sb2O3、TeO2、Li2O、K20 and Ce:YAG
Fluorescent material;Counted with the total mole number of frit as 100%, the content of each effective material is expressed as with molar fraction:
After frit is sufficiently mixed in mortar, is ground, by compound and distilled water with mass ratio 1:0.05-0.2 mixes
It is modulated into mixed slurry;
(2) curtain coating of mixed slurry:By mixed slurry on casting machine even application thickness be 0.1-0.5mm and with light source chi
On the white glass piece that very little, shape matches;
(3) drying and firing of sandwich-like microcrystalline glass:The white glass piece that will be coated is placed in 200-300 DEG C of vacuum drying
In case, dry 6-9 hours, the white glass piece of same shape, size is covered after moisture evaporation on batch mixing top layer, in sandwich-like
Glass intermediate plate is sintered in being put in Muffle furnace, and the temperature for setting Muffle furnace is 600-800 DEG C, 1-4 hours is incubated, then with stove nature
It is the Ce of the sandwich-like of 0.4-1.5mm to be cooled to room temperature and form thickness:YAG microcrystalline glass.
2. the Ce of sandwich-like is prepared with the tape casting as claimed in claim 1:The method of YAG microcrystalline glass, its feature exists
In:The content of each effective material is expressed as with molar fraction:
3. the Ce of sandwich-like is prepared with the tape casting as claimed in claim 1:The method of YAG microcrystalline glass, its feature exists
In:The content of each effective material is expressed as with molar fraction:
4. as described in one of claims 1 to 3 with the tape casting prepare sandwich-like Ce:The method of YAG microcrystalline glass, its
It is characterised by:The transmitance of the white glass piece for being used must more than 90%, refractive index must close to laminated glass matrix refractive index or
Person Ce:The refractive index of YAG fluorescent powder, and its softening point temperature must be higher than 800 DEG C.
5. the Ce of sandwich-like is prepared with the tape casting as claimed in claim 4:The method of YAG microcrystalline glass, its feature exists
In:White glass is K9, sodium calcium silicon or sodium calcium lead glass.
6. as described in one of claims 1 to 3 with the tape casting prepare sandwich-like Ce:The method of YAG microcrystalline glass, its
It is characterised by:The speed for being cast blade is 0.02-0.05m/s, and blade thickness is 0.1-0.5mm.
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Cited By (7)
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CN107721203A (en) * | 2017-10-27 | 2018-02-23 | 温州大学 | A kind of fluorescent glass-ceramics and preparation method thereof |
CN107799645A (en) * | 2017-09-29 | 2018-03-13 | 温州大学 | A kind of sandwich style titanate fluorescent glass film and preparation method thereof |
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 |
CN107936968A (en) * | 2017-10-27 | 2018-04-20 | 温州大学 | Mn:The preparation method of YAG fluorescent powder, Mn:YAG interlayer fluorescent glass and its preparation method and application |
CN108281535A (en) * | 2018-02-02 | 2018-07-13 | 温州大学 | Composite fluorescence laminated glass and preparation method thereof and the application on white light LEDs |
CN108329914A (en) * | 2018-04-17 | 2018-07-27 | 温州大学 | A kind of preparation method of fluorescent crystal particle |
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CN105523715A (en) * | 2015-06-18 | 2016-04-27 | 温州大学 | Low-melting point transparent fluorescent glass and its preparation method and use in white light LED |
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Cited By (10)
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CN107799645A (en) * | 2017-09-29 | 2018-03-13 | 温州大学 | A kind of sandwich style titanate fluorescent glass film and preparation method thereof |
CN107721203A (en) * | 2017-10-27 | 2018-02-23 | 温州大学 | A kind of fluorescent glass-ceramics and preparation method thereof |
CN107936968A (en) * | 2017-10-27 | 2018-04-20 | 温州大学 | Mn:The preparation method of YAG fluorescent powder, Mn:YAG interlayer fluorescent glass and its preparation method and application |
CN107936968B (en) * | 2017-10-27 | 2020-11-17 | 温州大学 | Mn: YAG fluorescent powder preparation method, Mn: YAG (yttrium aluminum garnet) sandwich fluorescent glass as well as preparation method and application thereof |
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 |
CN107892487B (en) * | 2017-11-01 | 2020-02-18 | 上海应用技术大学 | Preparation method of remote fluorescent sheet based on low-melting-point borosilicate glass powder |
CN107804974B (en) * | 2017-11-01 | 2020-02-21 | 上海应用技术大学 | Preparation method of remote fluorescent sheet based on low-melting-point lead-free glass powder |
CN108281535A (en) * | 2018-02-02 | 2018-07-13 | 温州大学 | Composite fluorescence laminated glass and preparation method thereof and the application on white light LEDs |
CN108329914A (en) * | 2018-04-17 | 2018-07-27 | 温州大学 | A kind of preparation method of fluorescent crystal particle |
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