CN103864302A - Glass phosphor and preparation method thereof - Google Patents
Glass phosphor and preparation method thereof Download PDFInfo
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- CN103864302A CN103864302A CN201410131214.2A CN201410131214A CN103864302A CN 103864302 A CN103864302 A CN 103864302A CN 201410131214 A CN201410131214 A CN 201410131214A CN 103864302 A CN103864302 A CN 103864302A
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- 239000011521 glass Substances 0.000 title claims abstract description 105
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000002844 melting Methods 0.000 claims abstract description 14
- 230000008018 melting Effects 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims description 45
- 230000004927 fusion Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 13
- 238000005245 sintering Methods 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 5
- 239000011324 bead Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000006060 molten glass Substances 0.000 abstract 2
- 230000002411 adverse Effects 0.000 abstract 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 14
- 229910010413 TiO 2 Inorganic materials 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 229910052697 platinum Inorganic materials 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000004806 packaging method and process Methods 0.000 description 6
- 239000003292 glue Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 239000012752 auxiliary agent Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- 238000004134 energy conservation Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000005304 joining Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 239000012745 toughening agent Substances 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000001748 luminescence spectrum Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
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- Led Device Packages (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention relates to a glass phosphor preparation method and a glass phosphor prepared by the method. The preparation method comprises the following steps: 1) melting the glass beads with refractive index of more than 1.8 into molten glass; and 2) adding phosphor powder into the molten glass while stirring evenly, and then, cooling for molding. According to the preparation method, the glass beads with refractive index of more than 1.8 and the phosphor powder are used as raw materials, moreover, the phosphor powder is added after the glass beads are melted according to the preparation steps, and then, the mixture is stirred evenly and cooled for molding, thus, the aims of high lighting effect and high energy-saving efficiency of LED devices are realized, adverse effects on the phosphor powder in a high temperature sintering process are avoided effectively, the whole preparation technical process is simple and easy to operate, the production efficiency is high, the production cost is low, various types of products can be prepared and the products are wide in range of application.
Description
Technical field
The present invention relates to glass and glass preparation technology, is a kind of glass fluor and preparation method thereof specifically, and this glass fluor is mainly used in LED encapsulation and application, can improve the light efficiency of LED product.
Background technology
Along with the development day by day of LED lighting engineering, LED light fixture is more and more applied to various occasions, also more and more higher for the requirement of LED light source.The LED light source of common poor efficiency has been difficult to meet the requirement in market, and the research and development of high efficiency LED light source are imperative.
White-light LED encapsulation adopts blue chip excitated fluorescent powder more at present, forms white light.Conventional coating method is that fluorescent material is mixed with fluorescent glue (epoxy resin, silica gel or silicone resin), is coated in chip surface.Due to specific refractory power lower (the n < 1.6) conventionally of fluorescent glue, reduce light extraction efficiency, be difficult to realize the high light efficiency of LED.And, the direct contact chip of fluorescent glue and fluorescent material, the heat that chip produces is delivered to fluorescent material and fluorescent glue, and along with the rising of temperature, the quantum yield of fluorescent material lowers gradually, makes the decay of LED luminous efficiency.Sumita company of Germany adopts fluorescent glass packaging LED module, lights 10000 as a child rear brightness and do not fail in 85 DEG C of environment, slightly rise on the contrary, and common LED package module (adopting fluorescent material glue-line) brightness has under the same conditions reduced by 20%.
If notification number is CN103011614A, the patent that name is called " a kind of fluorescent glass sheet and preparation method thereof " discloses a kind of preparation method of glass flourescent sheet, this patent is by applying the low temperature glass pulp layer containing fluorescent material at glass substrate surface, the component of described low temperature glass pulp layer comprises cryogenic glass powder, fluorescent material, toughener, tackiness agent and dispersion agent, after low-temperature sintering (800 DEG C), form the glass flourescent sheet that a kind of specific refractory power is 1.4-1.6, for the encapsulation of high power device, improve the reliability of light source.
But still there is following defect in above-mentioned glass flourescent sheet:
1, specific refractory power 1.4-1.6 is still lower, be difficult to realize the high light efficiency of LED device, and this glass flourescent sheet is made up of the fluorescent glass layer on glass substrate and surface thereof, glass substrate is different with the specific refractory power of fluorescent glass layer, light losing will cause bright dipping time, reduce the light efficiency of LED device, be therefore difficult to meet market to the high light efficiency of LED, high energy-conservation demand;
2, preparation technology is still very complicated, comprise the cleaning step of glass substrate, glass paste step, coating step and the sintering step that preparation contains fluorescent material, production efficiency is relatively low, and in coating procedure, also need strictly to control coating thickness between 50 microns～500 microns, production difficulty is large, equipment and manually having high input, is unfavorable for large-scale production;
3, in the time that preparation contains the glass paste of fluorescent material, need to add multiple auxiliary agent as toughener, tackiness agent and dispersion agent, objectively extend the production cycle, improve production cost;
4, produce and damage in the crystalline phase (crystalline structure) of avoiding high-temperature sintering process (being greater than 1000 DEG C) to fluorescent material, affect in the luminous efficiency problem of fluorescent material thereby make fluorescent material lose fluorescent characteristic, the method adopting is to use cryogenic glass powder (second-order transition temperature is lower than 800 DEG C) instead, therefore above-mentioned preparation method can only be applicable to cryogenic glass powder, narrow application range, product performance are limited.
Summary of the invention
In order to overcome the defect of above-mentioned prior art, technical problem to be solved by this invention is to provide glass fluor of a kind of high refractive index and preparation method thereof, to solve current fluorescent glue and glass flourescent sheet specific refractory power is low, be difficult to realize a difficult problem for LED packaging and the high light efficiency of LED light fixture.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A kind of glass fluor preparation method, comprises the following steps:
1) selecting specific refractory power is that more than 1.8 glass microballon is melt into glass paste;
2) to add fluorescent material in glass paste and stir after cooling forming.
The present invention compared with prior art, has the following advantages:
1, the glass fluor specific refractory power preparing can be up to 1.8-2.0, approach with the specific refractory power of LED chip, and be single layer structure, what do not have that prior art causes because the specific refractory power of multiple glazing is different goes out light loss problem, has realized the high light efficiency of LED device, high energy-conservation object;
2, preparation technology is simple to operation, has improved production efficiency, has reduced production difficulty, suitability for scale production;
3, the glass paste containing fluorescent material without preparation, without adding other auxiliary agents, when preparation, directly fluorescent material is added the glass microballon of melting to stir, greatly shorten the production cycle, reduce production costs, and realized the consistence of product chromaticity coordinates, make in the poor 4SDCM of being controlled at of color tolerance;
4, the present invention is first melten glass microballon, add again fluorescent material, then cooling forming after stirring, churning time can be controlled in very short scope, compared to existing technology by fluorescent material, glass powder and multiple auxiliary agent are first mixed into after slurry the way of sintering again, the fluorescent material place time is at high temperature short, the crystalline phase extent of damage is little, therefore effectively avoided the detrimentally affect of high-temperature sintering process to fluorescent material, make the glass microballon of different glass transition temperature all can utilize preparation method of the present invention to make the glass fluor of high light efficiency, be particularly useful for the glass microballon that second-order transition temperature is greater than 1000 DEG C, performance categories and the range of application of product are expanded.
Brief description of the drawings
Figure 1 shows that fluorescent glass sheet of the present invention encapsulates the color-division test report of the LED package module obtaining.
Figure 2 shows that the color-division test report of common LED package module.
Embodiment
The key distinction of the present invention and prior art is: adopting specific refractory power is that more than 1.8 glass microballon and fluorescent material are as raw material, and preparation process is for first will adding fluorescent material again after glass microballon melting, then cooling forming after stirring, the high light efficiency of LED device, high energy-conservation object are not only realized, and effectively avoided the detrimentally affect of high-temperature sintering process to fluorescent material, and whole preparation process is simple to operation, and production efficiency is high, production cost is low, product category and applied widely.
Concrete, glass fluor preparation method of the present invention, comprises the following steps:
1) selecting specific refractory power is that more than 1.8 glass microballon is melt into glass paste;
2) to add fluorescent material in glass paste and stir after cooling forming.
In above-mentioned preparation method, the glass microballon of existing known specific refractory power more than 1.8 all can be applied to the present invention, melt temperature can be determined according to the second-order transition temperature of the glass microballon of specifically selecting, and is generally greater than 100～200 DEG C of left and right of second-order transition temperature; Fusion time can determine according to the concrete consumption of glass microballon and melting situation, and general consumption is more, and the required fusion time is longer, to ensure that the abundant melting of glass microballon is as the criterion.Preferably, the present invention adopts TiO
2-BaO-SiO
2-AlO
3the glass microballon of system, this glass microballon has been reported in existing document: " research of high-refraction glass bead and application ", author: Peng Cheng, the building materials world, the 30th the 2nd phase of volume in 2009.The specific refractory power of this glass microballon is 1.8-2.0, TiO
2with the mol ratio of BaO be 0.70-0.85, melt temperature is 1000-1200 DEG C, the fusion time is 30-90 minute.For fear of introducing impurity, described glass microballon is preferably placed in platinum crucible melting.
In above-mentioned preparation method, described fluorescent material can be monochromatic fluorescent material, also can be the mixture of multicolor phosphor or multiple fluorescent material, be preferably the combination of YAG yellow fluorescent powder or YAG yellow fluorescent powder and red fluorescence powder or the combination of green emitting phosphor and red fluorescence powder.The consumption of fluorescent material can require to determine according to actual formula and product performance, is preferably 10～60wt% of glass microballon consumption.The joining day of fluorescent material is preferably controlled in 5s, to reduce as far as possible the fluorescent material place time at high temperature, reduces the crystalline phase extent of damage.Before joining in glass paste, can open in advance whipping device stirs glass paste, in whipping process, keep the temperature-resistant of glass paste, then join in glass paste disposable fluorescent material, control churning time in 5s, fluorescent material is mixed with glass paste, then pour cooling forming in mould into.In order to improve forming quality of products, mould can be in advance by preheating, and preheating temperature equals melt temperature or lower than in 100 DEG C of melt temperatures, process of cooling can be naturally cooling or force cooling.
In above-mentioned preparation method; because fluorescent material is not with glass microballon melting; therefore the fluorescent material place time is at high temperature short; not only the crystalline phase extent of damage is little; and light emitting ionic in fluorescent material is also difficult for being oxidated or reduced, in preparation process, without passing into the inert protective gas such as nitrogen, production technique and production unit are further simplified; the process of having exempted gas recovery processing, reduces production costs.
By describing technology contents of the present invention, structural attitude in detail, being realized object and effect, be explained in detail below in conjunction with embodiment.
Embodiment 1
1) choose the TiO that specific refractory power is 1.8-2.0
2-BaO-SiO
2-AlO
3the glass microballon of system, its TiO
2with the mol ratio of BaO be 0.70-0.85, be placed in platinum crucible melting at 1000-1200 DEG C and be incubated after 30 minutes;
2) ratio that is the 10wt% of glass microballon consumption according to the consumption of fluorescent material takes YAG yellow fluorescent powder, disposablely joins in the glass paste that step 1) obtains and stirs, and then pours cooling forming in mould into.
Embodiment 2
1) choose the TiO that specific refractory power is 1.8-2.0
2-BaO-SiO
2-AlO
3the glass microballon of system, its TiO
2with the mol ratio of BaO be 0.70-0.85, be placed in platinum crucible melting at 1000-1200 DEG C and be incubated after 60 minutes;
2) ratio that is the 30wt% of glass microballon consumption according to the consumption of fluorescent material takes the mixture of YAG yellow fluorescent powder and red fluorescence powder, join in the glass paste that step 1) obtains and stir, then pour cooling forming in preheated mould into, preheating temperature is 1000-1200 DEG C.
Embodiment 3
1) choose the TiO that specific refractory power is 1.8-2.0
2-BaO-SiO
2-AlO
3the glass microballon of system, its TiO
2with the mol ratio of BaO be 0.70-0.85, be placed in platinum crucible melting at 1000-1200 DEG C and be incubated after 90 minutes;
2) ratio that is the 60wt% of glass microballon consumption according to the consumption of fluorescent material takes the mixture of green emitting phosphor and red fluorescence powder, join in the glass paste that step 1) obtains and stir, then pour cooling forming in preheated mould into, preheating temperature is 1000-1200 DEG C.
Embodiment 4
1) choose the TiO that specific refractory power is 1.8-2.0
2-BaO-SiO
2-AlO
3the glass microballon of system, its TiO
2with the mol ratio of BaO be 0.70-0.85, be placed in platinum crucible melting 60 minutes at 1000-1200 DEG C, then open and stir and be incubated;
2) ratio that is the 60wt% of glass microballon consumption according to the consumption of fluorescent material takes YAG yellow fluorescent powder, in 5s, join in the glass paste that step 1) obtains and stir, churning time is controlled in 5s, then pour naturally cooling moulding in preheated mould into, preheating temperature is 1000-1200 DEG C.
Embodiment 5
1) choose the TiO that specific refractory power is 1.8-2.0
2-BaO-SiO
2-AlO
3the glass microballon of system, its TiO
2with the mol ratio of BaO be 0.70-0.85, be placed in platinum crucible melting at 1000-1200 DEG C and stir and be incubated after 30 minutes;
2) ratio that is the 10wt% of glass microballon consumption according to the consumption of fluorescent material takes YAG yellow fluorescent powder, disposablely in 5s join in the glass paste that step 1) obtains and stir, churning time is controlled in 5s, then pour cooling forming in mould into, preheating temperature is 1000-1200 DEG C.
Embodiment 6
1) choose the TiO that specific refractory power is 1.8-2.0
2-BaO-SiO
2-AlO
3the glass microballon of system, its TiO
2with the mol ratio of BaO be 0.70-0.85, be placed in platinum crucible melting at 1000-1200 DEG C and stir and be incubated after 90 minutes;
2) ratio that is the 30wt% of glass microballon consumption according to the consumption of fluorescent material takes the mixture of green emitting phosphor and red fluorescence powder, disposablely in 5s join in the glass paste that step 1) obtains and stir, churning time is controlled in 5s, then pour cooling forming in mould into, preheating temperature is 1000-1200 DEG C.
Color-division test
By preparation-obtained above-described embodiment 1～6 glass fluor, for packaging LED module, the LED package module obtaining is tested by ZWL-3900G integration packaging (COB) LED color-division test macro, and test report as shown in Figure 1.
Common LED package module (silica gel, epoxy resin or the silicone resin that is 1.51 by specific refractory power be mixed and made into fluorescent powder colloid with fluorescent material after packaging LED module) the same ZWL-3900G of employing integration packaging (COB) LED color-division test macro is tested, and test report as shown in Figure 2.
Analyzed from Fig. 1 and Fig. 2, it is in full accord that fluorescent glass sheet of the present invention encapsulates the luminescence spectrum of the LED package module that obtains and common LED package module, and fluorescent glass sheet of the present invention encapsulates the optical throughput of the LED package module obtaining and can reach 150lm, the optical throughput of common LED package module is only 120lm left and right.
X-ray diffraction analysis (XRD) analyze show, glass fluor of the present invention has retained the original crystalline phase of fluorescent material well.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes specification sheets of the present invention and accompanying drawing content to do; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (7)
1. a glass fluor preparation method, is characterized in that, comprises the following steps:
1) selecting specific refractory power is that more than 1.8 glass microballon is melt into glass paste;
2) to add fluorescent material in glass paste and stir after cooling forming.
2. glass fluor preparation method according to claim 1, is characterized in that: described glass microballon is TiO
2-BaO-SiO
2-AlO
3the glass microballon of system, specific refractory power is 1.8-2.0.
3. glass fluor preparation method according to claim 2, is characterized in that: the TiO in described glass microballon
2with the mol ratio of BaO be 0.70-0.85.
4. glass fluor preparation method according to claim 2, is characterized in that: the melting at 1000-1200 DEG C of described glass microballon, the fusion time is 30-90 minute.
5. glass fluor preparation method according to claim 1, is characterized in that: the consumption of described fluorescent material is 10～60wt% of glass microballon consumption.
6. glass fluor preparation method according to claim 1, is characterized in that: described fluorescent material is the combination of YAG yellow fluorescent powder or YAG yellow fluorescent powder and red fluorescence powder or the combination of green emitting phosphor and red fluorescence powder.
7. one kind according to the preparation-obtained glass fluor of glass fluor preparation method described in claim 1 to 6 any one.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190237638A1 (en) | 2016-07-26 | 2019-08-01 | Cree, Inc. | Light emitting diodes, components and related methods |
| US11024785B2 (en) | 2018-05-25 | 2021-06-01 | Creeled, Inc. | Light-emitting diode packages |
| US11101411B2 (en) | 2019-06-26 | 2021-08-24 | Creeled, Inc. | Solid-state light emitting devices including light emitting diodes in package structures |
| US11233183B2 (en) | 2018-08-31 | 2022-01-25 | Creeled, Inc. | Light-emitting diodes, light-emitting diode arrays and related devices |
| US11335833B2 (en) | 2018-08-31 | 2022-05-17 | Creeled, Inc. | Light-emitting diodes, light-emitting diode arrays and related devices |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723586A (en) * | 2009-11-30 | 2010-06-09 | 浙江大学 | Fluorescent powder/glass complex applied to semiconductor lighting and preparation method thereof |
| CN101864127A (en) * | 2010-06-29 | 2010-10-20 | 彩虹集团公司 | Long-afterglow fluorescent powder sizing agent |
-
2014
- 2014-04-02 CN CN201410131214.2A patent/CN103864302B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723586A (en) * | 2009-11-30 | 2010-06-09 | 浙江大学 | Fluorescent powder/glass complex applied to semiconductor lighting and preparation method thereof |
| CN101864127A (en) * | 2010-06-29 | 2010-10-20 | 彩虹集团公司 | Long-afterglow fluorescent powder sizing agent |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190237638A1 (en) | 2016-07-26 | 2019-08-01 | Cree, Inc. | Light emitting diodes, components and related methods |
| US10879435B2 (en) | 2016-07-26 | 2020-12-29 | Cree, Inc. | Light emitting diodes, components and related methods |
| US10964858B2 (en) | 2016-07-26 | 2021-03-30 | Cree, Inc. | Light emitting diodes, components and related methods |
| US11024785B2 (en) | 2018-05-25 | 2021-06-01 | Creeled, Inc. | Light-emitting diode packages |
| US11121298B2 (en) | 2018-05-25 | 2021-09-14 | Creeled, Inc. | Light-emitting diode packages with individually controllable light-emitting diode chips |
| US11233183B2 (en) | 2018-08-31 | 2022-01-25 | Creeled, Inc. | Light-emitting diodes, light-emitting diode arrays and related devices |
| US11335833B2 (en) | 2018-08-31 | 2022-05-17 | Creeled, Inc. | Light-emitting diodes, light-emitting diode arrays and related devices |
| US11101411B2 (en) | 2019-06-26 | 2021-08-24 | Creeled, Inc. | Solid-state light emitting devices including light emitting diodes in package structures |
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| CN103864302B (en) | 2016-06-01 |
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