CN107352795A - A kind of full-inorganic low temperature fluorescent glass material and preparation method thereof - Google Patents
A kind of full-inorganic low temperature fluorescent glass material and preparation method thereof Download PDFInfo
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- CN107352795A CN107352795A CN201710698432.8A CN201710698432A CN107352795A CN 107352795 A CN107352795 A CN 107352795A CN 201710698432 A CN201710698432 A CN 201710698432A CN 107352795 A CN107352795 A CN 107352795A
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- 239000011521 glass Substances 0.000 title claims abstract description 82
- 239000000463 material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 26
- 238000000576 coating method Methods 0.000 claims abstract description 26
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 15
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000919 ceramic Substances 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 21
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 19
- 238000005245 sintering Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 7
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000003698 laser cutting Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 238000010257 thawing Methods 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 abstract description 13
- 229920000647 polyepoxide Polymers 0.000 abstract description 13
- 238000005516 engineering process Methods 0.000 abstract description 8
- 238000005538 encapsulation Methods 0.000 abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 5
- 239000003063 flame retardant Substances 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 239000010703 silicon Substances 0.000 abstract description 5
- 230000032683 aging Effects 0.000 abstract description 3
- 238000005286 illumination Methods 0.000 abstract description 3
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 230000003247 decreasing effect Effects 0.000 description 6
- 230000009477 glass transition Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 230000000171 quenching effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 241001062009 Indigofera Species 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000011222 crystalline ceramic Substances 0.000 description 2
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007500 overflow downdraw method Methods 0.000 description 2
- 206010009232 Clang associations Diseases 0.000 description 1
- 241001025261 Neoraja caerulea Species 0.000 description 1
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000006025 fining agent Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010345 tape casting Methods 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
-
- 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
-
- 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
- H01L33/507—Wavelength conversion elements the elements being in intimate contact with parts other than the semiconductor body or integrated with parts other than the semiconductor body
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Led Device Packages (AREA)
- Glass Compositions (AREA)
Abstract
The present invention provides a kind of full-inorganic low temperature fluorescent glass material and preparation method thereof.By mole, including：30‑48% Bi2O3、30‑45%ZnO、10‑25% B2O3、0‑1% Sb2O3、0‑1% NaNO3.Low temperature fluorescent glass coating is replaced epoxy resin or organosilicon fluoresent coating to prepare white light LEDs by the present invention, with very strong novelty and challenge, encapsulation technology generally used now is not only overturned, can also solve thermo-labile caused by current epoxy resin or organosilicon fluoresent coating, it is not fire-retardant, it is easy to aging, not the shortcomings that UV resistant irradiation etc., and because low temperature fluorescent glass material compares epoxy resin or organic silicon coating with more preferably heat conductivility, low temperature fluorescent glass coating is more suitable for being used for small size, high current, the preparation and application of illumination level LED light source.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of full-inorganic low temperature fluorescent glass material and preparation method thereof.
Background technology
Large power white light LED light source is mainly produced in a manner of " blue chip+yellow fluorescent powder " at present.It is substantially all and adopts
Mixed with epoxy resin or organosilicon with fluorescent material, apply or be wrapped in the surrounding of blue chip, form epoxy resin or organic
Luminescence from silicon coating.
The content of the invention
Based on this, the present invention provides a kind of full-inorganic low temperature fluorescent glass material, by mole, including：30-48%
Bi2O3, 30-45%ZnO, 10-25%B2O3, 0-1%Sb2O3, 0-1%NaNO3。
The present invention use above technical scheme, the advantage is that, ZnO can reduce glass glass transition temperature,
Bi2O3To form the main component of glass network structure, B2O3The melting effect of glass can be improved, it helps reduce glass
Glass transition temperature, Sb2O3For fining agent, NaNO3For defoamer；Epoxy resin is replaced using low temperature fluorescent glass coating
Or organosilicon fluoresent coating prepares white light LEDs and has not only overturned encapsulation technology generally used now, moreover it is possible to solves current epoxy resin
Or the shortcomings of thermo-labile, not fire-retardant, easy to aging, UV resistant does not irradiate caused by organosilicon fluoresent coating, and due to low
Warm fluorescent glass coating has more preferably heat conductivility compared to epoxy resin or organic silicon coating, and low temperature fluorescent glass coating is more
It is adapted for use in the preparation and application of small size, high current, illumination level LED light source.Prepared using low temperature fluorescent glass coating new
Type white LED light source will have the advantages that heat-resisting, fire-retardant, uvioresistant irradiates, moreover it is possible to which significantly simplification uses white light LEDs as light
The design of the light fixture in source, reduce the manufacturing cost of light fixture.
Accordingly, a kind of method for preparing full-inorganic low temperature fluorescent glass material, including following steps：
Step A：By above-mentioned load weighted raw material Bi2O3、ZnO、B2O3、Sb2O3、NaNO3Put platinum after being sufficiently mixed into
Melt in crucible and in electric furnace；The glass metal of melting is poured into mould and cooled down, annealing in electric furnace is then put into again and obtains
The glass needed；
Step B：By glass grinds, with Ce：YAG fluorescent powder grinding is uniform, and blade coating is stripped in spraying after mixing adhesive
On the ceramic substrate of agent,
Step C：Low-melting-point fluorescent glass piece is removed by ceramic substrate in muffle furnace after sinter molding, uses ceramic laser
Cutting machine is cut to various sizes, and LED illuminating modules are then packaged into blue chip, then carries out luminescent properties to it
Test.
Preferably, the Ce：It is 8%-20% that YAG fluorescent powder, which accounts for all material quality percentages,.
Preferably, in the step A, the temperature of electric furnace is 800 DEG C -1000 DEG C；Thawing time is 2-3 hours.
Preferably, in the step A, chilling temperature is less than 500 DEG C, and the temperature of annealing is 450 ± 50 DEG C.
Preferably, in the step C, 500 DEG C -600 DEG C of sintering temperature, 2-4 DEG C of heating rate/min, sintering time 0.5-
1h。
2005, NEC glass company was prepared for the devitrified glass ceramics fluorophor of white light LEDs first, due to the material
Material has many advantages of glass and ceramics concurrently, such as heat-resisting, humidity, corrosion-resistant, and good effect is achieved with being encapsulated in LED
Fruit, but its synthesis condition is quite harsh, it is very difficult to realize.The patent report of Dutch PHILIPS Co. in 2008 mixes fluorescent material
In the miscellaneous ceramics to aluminum oxide polycrystal, the doping volumetric concentration of fluorescent material realizes itself and blue-ray LED in 0.01%-20%
Encapsulation.This approach improve LED calorifics and optical property, and by the LED backscattering damage control 5%, but it is relevant white
The numerical value such as light LED light intensity, luminous flux are not revealed.Because the limitation of aluminium oxide ceramics itself crystal structure makes its light transmission rate
It is relatively low, it can only accomplish translucent, this shortcoming have impact on its application in terms of white-light LED fluorescence ceramic package.
Shandong Huaguang Photoelectronic Co., Ltd. of China in 2008 disclose the method that white light LEDs are prepared using YAG crystalline ceramics
Patent, but the patent is not had LED is packaged using the crystalline ceramics that does not form by a firing, and simply application is rear-earth-doped
YAG ceramic powders are coated to LED chip, the problems such as avoiding the yellow light ring brought using epoxy resin etc..Zhongshan University
Soviet Union clanging or clanking sound academician etc. utilize rear-earth-doped YAG single-chips, be packaged with GaN base LED chip, realize the defeated of white light LEDs
Go out, but because the growth cycle of YAG single-chips is longer, cost is high, and the doping of rare earth element is difficult to control, and institute is in this way
It is more difficult to be applied to production.Extensively culvert etc. uses sol-gel technology to South China Normal University's photoelectron material with technical research institute's model, leads to
Cross incorporation YAG:Ce fluorescent material prepares glass fluorophor, and uses it for the encapsulation of white light LEDs, and this method still uses fluorescence
Powder under matrix liquid with adulterating, it cannot be guaranteed that uniform doping.
Wuhan University of Technology Cheng Jin trees in 2010 etc. propose a kind of low-melting-point fluorescent glass for white light LED and preparation method thereof
(Chinese invention patent CN200910063528.2), the preparation method of use are to prepare low-melting glass with fusion method first,
Glass powder with low melting point is mixed with fluorescent material again, low-melting-point fluorescent glass is obtained after sintered.Prepared low melting point fluorescence glass
Glass has good luminescent properties and excellent stability.The low-melting-point fluorescent glass powder prepared by fusion method can be with hot pressing
Shaping prepares variously-shaped fluorescent glass, can also be with it such as the method described by patent of invention CN201210187387.7
The mixing of its slurry is coated on other substrate surfaces, sintered formation fluorescence membrane, can also directly by glass powder with low melting point with it is glimmering
Light powder and the mixing of other slurries are coated on other substrate surfaces, sintered formation fluorescence membrane.Relevant report and patent have China
Patent of invention CN201310030220.4,201210228419.3,201210294570.7,201210492751.0,
201210125776.7,201210488706.3,201210199171.2 etc..
No matter variously-shaped fluorescence ceramics or fluorescent glass are formed into, or low-melting-point fluorescent glass powder or mixed with glimmering
The glass powder with low melting point of light powder is coated on other base materials, and it is it to re-sinter and to form the common feature of low-melting-point fluorescent glass film
Belong to long-distance fluorescent powder technology, i.e., fluorescence coating is away from blue-light LED chip.Described fluorescence ceramics, fluorescent glass or eutectic
Point fluorescent glass film does not occur directly to contact with blue-light LED chip.That is, described low-melting-point fluorescent glass
Film is coated on the outer cover of lamp, or, described fluorescence ceramics or fluorescent glass are fabricated to the outer cover of lamp, including lamp in itself
Bubble, fluorescent tube or lampshade panel etc., turn into a part for light fixture component.
It is of different sizes because the outer hood shape of all kinds of lamps differs, and glomeration or tubulose is often presented, using high temperature sintering
The cost that fluorescence ceramics and the mode of low temperature clinkering prepare fluorescent lamp bulb, fluorescent tube or lamp plate is very high, and versatility is very poor.Sinter shape
Into ceramic base bulb, fluorescent tube, lamp plate and the other components of light fixture combination it is also highly difficult, waterproof and dampproof poor performance, assembly technology
Complexity, cost are high.Manufactured light fixture also belongs to glassware, frangible, easily splits, transport and in-convenience in use.So far batch has been there is no
The practicality product of production emerges.
Low temperature fluorescent glass coating is replaced epoxy resin or organosilicon fluoresent coating to prepare white light LEDs by the present invention, is had
Very strong novelty and challenge, has not only overturned encapsulation technology generally used now, moreover it is possible to solves current epoxy resin or organic
The shortcomings of thermo-labile, not fire-retardant, easy to aging, UV resistant does not irradiate caused by luminescence from silicon coating, and due to low temperature fluorescence
Glass coating compared to epoxy resin or organic silicon coating there is more preferably heat conductivility, low temperature fluorescent glass coating to be more suitable for
For the preparation and application of small size, high current, illumination level LED light source, current foreign countries there is no correlation technique and product to issue.Can
With expection, using the heat-resisting of low temperature fluorescent glass coating preparation, fire-retardant, uvioresistant irradiation, novel white-light LED light source will enter one
Step expands the application field of white LED light source, moreover it is possible to which significantly simplification uses design of the white light LEDs as the light fixture of light source, reduces
The manufacturing cost of light fixture.
Embodiment
The preferably embodiment of the present invention is described in further detail below：
Embodiment 1
1) mole percent as shared by each component weighs raw material 44%Bi2O3, 36%ZnO, 20%B2O3And quality is
Said mixture gross mass is respectively 0.5% Sb2O3、NaNO3；
2) by above-mentioned load weighted raw material Bi2O3、ZnO、B2O3、Sb2O3、NaNO3Put platinum crucible after being sufficiently mixed into
It is interior and melt 3 hours in 900 DEG C of electric furnace in electric furnace；The glass metal of melting is poured into less than 500 DEG C is cooled in mould,
Then the glass for being annealed to room temperature in 450 ± 50 DEG C in electric furnace and being needed is put into again；
3) by glass grinds, according to certain mass ratio and Ce：YAG fluorescent powder is ground uniformly in agate mortar, mixing
Blade coating sinters, 500-600 DEG C of sintering temperature on the ceramic substrate of spraying releasing agent under protective atmosphere after adhesive, heats up
4 DEG C/min of speed, sintering time 0.5h, then carries out annealing cooling, produces low-melting-point fluorescent glass for white light LED.Using DSC
The glass transition temperature that tester measures product is 375 DEG C；
4) low-melting-point fluorescent glass piece is removed, various sizes is cut to ceramic laser cutting machine, then with indigo plant
Optical chip is packaged into LED illuminating modules, then carries out luminescent properties test to it.
Table 1
| YAG contents | Sintering temperature | Luminous efficiency | |
| Case 1 | 10% | 500℃ | 101lm/W |
| Case 2 | 10% | 550℃ | 118lm/W |
| Case 3 | 10% | 600℃ | 98lm/W |
| Case 4 | 13% | 500℃ | 108lm/W |
| Case 5 | 13% | 550℃ | 124lm/W |
| Case 6 | 13% | 600℃ | 104lm/W |
| Case 7 | 16% | 500℃ | 99lm/W |
| Case 8 | 16% | 550℃ | 111lm/W |
| Case 9 | 16% | 600℃ | 91lm/W |
As can be seen from Table 1 as the rise of sintering temperature, the luminous efficiency of fluorescent glass first raise, at 550 DEG C most
Height, when temperature continues to rise to 600 DEG C, luminous efficiency is remarkably decreased；Equally, with the rise of phosphor concentration, fluorescence glass
Glass luminous efficiency rise, the highest at 13%, when phosphor concentration continues to rise to 16%, luminous efficiency because there occurs
Concentration quenching effect and be remarkably decreased.Can be seen that fluorescence powder content from above-mentioned example is 13%, and 0.5h systems are sintered at 550 DEG C
Standby fluorescent glass encapsulating material best results, highest luminous efficiency have reached 124lm/W, close to current market white light LEDs
Luminous efficiency.
Embodiment 2
1) mole percent as shared by each component weighs raw material 30%Bi2O3, 45%ZnO, 25%B2O3；
2) by above-mentioned load weighted raw material Bi2O3、ZnO、B2O3Put into after being sufficiently mixed in platinum crucible and in electric furnace
Melt 2 hours in 800 DEG C of electric furnace；The glass metal of melting is poured into less than 500 DEG C are cooled in mould, then put electricity into again
The glass for being annealed to room temperature in 450 ± 50 DEG C in stove and being needed；
3) by glass grinds, according to certain mass ratio and Ce：YAG fluorescent powder is ground uniformly in agate mortar, mixing
Blade coating sinters, 500-600 DEG C of sintering temperature on the ceramic substrate of spraying releasing agent under protective atmosphere after adhesive, heats up
2 DEG C/min of speed, sintering time 1h, then carries out annealing cooling, produces low-melting-point fluorescent glass for white light LED.Surveyed using DSC
The glass transition temperature that examination instrument measures product is 375 DEG C；
4) low-melting-point fluorescent glass piece is removed, various sizes is cut to ceramic laser cutting machine, then with indigo plant
Optical chip is packaged into LED illuminating modules, then carries out luminescent properties test to it.
Table 2
| YAG contents | Sintering temperature | Luminous efficiency | |
| Case 10 | 10% | 500℃ | 101lm/W |
| Case 11 | 10% | 550℃ | 118lm/W |
| Case 12 | 10% | 600℃ | 98lm/W |
| Case 13 | 13% | 500℃ | 108lm/W |
| Case 14 | 13% | 550℃ | 124lm/W |
| Case 15 | 13% | 600℃ | 104lm/W |
| Case 16 | 16% | 500℃ | 99lm/W |
| Case 17 | 16% | 550℃ | 111lm/W |
| Case 18 | 16% | 600℃ | 91lm/W |
As can be seen from Table 2 as the rise of sintering temperature, the luminous efficiency of fluorescent glass first raise, at 550 DEG C most
Height, when temperature continues to rise to 600 DEG C, luminous efficiency is remarkably decreased；Equally, with the rise of phosphor concentration, fluorescence glass
Glass luminous efficiency rise, the highest at 13%, when phosphor concentration continues to rise to 16%, luminous efficiency because there occurs
Concentration quenching effect and be remarkably decreased.Can be seen that fluorescence powder content from above-mentioned example is 13%, and 0.5h systems are sintered at 550 DEG C
Standby fluorescent glass encapsulating material best results, highest luminous efficiency have reached 124lm/W, close to current market white light LEDs
Luminous efficiency.
Embodiment 3
1) mole percent as shared by each component weighs raw material 48%Bi2O3, 40%ZnO, 10%B2O3And quality is
Said mixture gross mass is respectively 1% Sb2O3、NaNO3；
2) by above-mentioned load weighted raw material Bi2O3、ZnO、B2O3、Sb2O3、NaNO3Put platinum crucible after being sufficiently mixed into
It is interior and melt 3 hours in 1000 DEG C of electric furnace in electric furnace；The glass metal of melting is poured into be cooled in mould 500 DEG C with
Under, then put the glass for being annealed to room temperature in 450 ± 50 DEG C in electric furnace and being needed into again；
3) by glass grinds, according to certain mass ratio and Ce：YAG fluorescent powder is ground uniformly in agate mortar, mixing
Blade coating sinters, 500-600 DEG C of sintering temperature on the ceramic substrate of spraying releasing agent under protective atmosphere after adhesive, heats up
4 DEG C/min of speed, sintering time 0.5h, then carries out annealing cooling, produces low-melting-point fluorescent glass for white light LED.Using DSC
The glass transition temperature that tester measures product is 375 DEG C；
4) low-melting-point fluorescent glass piece is removed, various sizes is cut to ceramic laser cutting machine, then with indigo plant
Optical chip is packaged into LED illuminating modules, then carries out luminescent properties test to it.
Table 3
As can be seen from Table 3 as the rise of sintering temperature, the luminous efficiency of fluorescent glass first raise, at 550 DEG C most
Height, when temperature continues to rise to 600 DEG C, luminous efficiency is remarkably decreased；Equally, with the rise of phosphor concentration, fluorescence glass
Glass luminous efficiency rise, the highest at 13%, when phosphor concentration continues to rise to 16%, luminous efficiency because there occurs
Concentration quenching effect and be remarkably decreased.Can be seen that fluorescence powder content from above-mentioned example is 13%, and 0.5h systems are sintered at 550 DEG C
Standby fluorescent glass encapsulating material best results, highest luminous efficiency have reached 124lm/W, close to current market white light LEDs
Luminous efficiency.
Prepared full-inorganic low temperature fluorescent glass material has the following advantages：
After 1. low temperature fluorescent glass prepares white LED light source, stable luminescence is reliable, reduces temperature quenching effect, solves
The problem of current epoxy resin or organosilicon encapsulating material do not adapt to small size, great power LED internal high temperature, has started one
Individual brand-new white LED light source method for packing.
2nd, innovatively fluorescent glass slurry is applied in the making of full-inorganic white LED light source using knife coating, is
White LED light source makes and provides a kind of brand-new technological process and method.
3rd, realize that " blue chip+inorganic Low fluorescent glass " wafer-level package (CSP-LED) is integrated with lighting.It is luminous
Efficiency can be widely used in small size high current LED chip encapsulation field close to current heavy-power LED product luminous efficiency.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (6)
- A kind of 1. full-inorganic low temperature fluorescent glass material, it is characterised in that by mole, including：30-48% Bi2O3、30- 45%ZnO、10-25% B2O3、0-1% Sb2O3、0-1% NaNO3。
- 2. one kind prepares full-inorganic low temperature fluorescent glass material as claimed in claim 1, it is characterised in that including following Step：Step A：By above-mentioned load weighted raw material Bi2O3、ZnO、B2O3、Sb2O3、NaNO3Put into after being sufficiently mixed in platinum crucible And melt in electric furnace；The glass metal of melting is poured into mould and cooled down, then puts what annealing in electric furnace was needed into again Glass；Step B：By glass grinds, with Ce：YAG fluorescent powder grinding is uniform, and blade coating is in spraying releasing agent after mixing adhesive On ceramic substrate；Step C：Low-melting-point fluorescent glass piece will be removed after ceramic substrate sinter molding, cut with ceramic laser cutting machine Cut, LED illuminating modules are then packaged into blue chip.
- 3. method as claimed in claim 2, it is characterised in that the Ce：YAG fluorescent powder accounts for all material quality percentages 8%-20%。
- 4. method as claimed in claim 2, it is characterised in that in the step A, the temperature of electric furnace is 800 DEG C -1000 DEG C； Thawing time is 1-4 hours.
- 5. method as claimed in claim 2, it is characterised in that in the step A, chilling temperature is less than 500 DEG C, annealing Temperature is 450 ± 50 DEG C.
- 6. method as claimed in claim 2, it is characterised in that in the step C, 500-600 DEG C of sintering temperature, heating rate 2-5 DEG C/min, sintering time 0.5-2h.
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Application publication date: 20171117 |