CN103864302B - A kind of glass fluor and its preparation method - Google Patents
A kind of glass fluor and its preparation method Download PDFInfo
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- CN103864302B CN103864302B CN201410131214.2A CN201410131214A CN103864302B CN 103864302 B CN103864302 B CN 103864302B CN 201410131214 A CN201410131214 A CN 201410131214A CN 103864302 B CN103864302 B CN 103864302B
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- 239000011521 glass Substances 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 50
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 238000002844 melting Methods 0.000 claims abstract description 14
- 230000008018 melting Effects 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims description 21
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 11
- 230000004927 fusion Effects 0.000 claims description 4
- 238000005304 joining Methods 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 229910052593 corundum Inorganic materials 0.000 claims 1
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 12
- 238000005245 sintering Methods 0.000 abstract description 5
- 238000004134 energy conservation Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 14
- 238000005516 engineering process Methods 0.000 description 8
- 229910052697 platinum Inorganic materials 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- 238000000576 coating method Methods 0.000 description 5
- 238000005538 encapsulation Methods 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000000203 mixture 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
- 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
- 230000001795 light effect Effects 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
- 239000011324 bead Substances 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
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011835 investigation Methods 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
- 230000001681 protective effect Effects 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
Abstract
The present invention relates to the preparation method of a kind of glass fluor and the glass fluor prepared by the method, described preparation method comprises the following steps: 1) select specific refractory power be more than 1.8 glass microballon be melt into glass paste; 2) in glass paste, add fluorescent material and stir evenly cooling forming afterwards. The present invention by adopt specific refractory power be more than 1.8 glass microballon and fluorescent material as raw material, and preparation process is for first adding fluorescent material again after glass microballon melting, then cooling forming after evenly is stirred, not only achieve LED component specular removal, high energy-conservation object, and effectively prevent high-temperature sintering process to the detrimentally affect of fluorescent material, whole preparation process is simple to operation, production efficiency height, production cost is low, product category and applied widely.
Description
Technical field
The present invention relates to glass and glass technology of preparing, be a kind of glass fluor and its preparation method specifically, this glass fluor is mainly used in LED and application, can improve the light effect of LED product.
Background technology
Along with the development day by day of LED illumination technology, what LED lamp was got more and more is applied to various occasion, and the requirement for LED/light source is also more and more higher. 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.
The encapsulation of current white light LEDs adopts blue chip excitated fluorescent powder, forms white light. Conventional coating method is mixed with fluorescent glue (epoxy resin, silica gel or silicone resin) by fluorescent material, is coated in chip surface. Due to the specific refractory power usual lower (n < 1.6) of fluorescent glue, reduce light extraction efficiency, it is difficult to realize the specular removal of LED. And, fluorescent glue directly contacts chip with fluorescent material, and 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 so that LED luminous efficiency decays. Sumita company of Germany adopts fluorescent glass packaging LED module, light in 85 DEG C of environment 10000 as a child after brightness do not fail, slightly rise on the contrary, and typical LED packages module (adopt fluorescent material glue-line) luminance-reduction 20% under the same conditions.
If notification number is CN103011614A, name is called the preparation method that patent discloses a kind of glass flourescent sheet of " a kind of fluorescent glass sheet and its preparation method ", this patent by containing the low temperature glass pulp layer of fluorescent material in glass substrate surface coating, the component of described low temperature glass pulp layer comprises cryogenic glass powder, fluorescent material, toughener, tackiness agent and dispersion agent, the glass flourescent sheet that a kind of specific refractory power is 1.4-1.6 is formed after low-temperature sintering (800 DEG C), for the encapsulation of high power device, it is to increase 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, it is difficult to realize the specular removal of LED component, 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 during bright dipping will be caused, reduce the light effect of LED component, therefore, it is difficult to meet market to LED specular removal, high energy-conservation demand;
2, preparation technology is still very complicated, comprise the cleaning step of glass substrate, prepare the glass paste step, coating step and the sintering step that contain fluorescent material, production efficiency is relatively low, and coating procedure also needs strictly control coating thickness between 50 microns��500 microns, production difficulty is big, equipment and manually having high input, is unfavorable for large-scale production;
3, when preparing containing the glass paste of fluorescent material, it is necessary to add multiple auxiliary agent such as toughener, tackiness agent and dispersion agent, objectively extend the production cycle, it is to increase production cost;
4, high-temperature sintering process (being greater than 1000 DEG C) is being avoided to produce to damage to the crystalline phase (crystalline structure) of fluorescent material, fluorescent material is made to lose fluorescent characteristic thus affect in the luminous efficiency problem of fluorescent material, the method adopted uses 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 and its preparation method of a kind of high refractive index, low to solve current fluorescent glue and glass flourescent sheet specific refractory power, it is difficult to realize LED device and a difficult problem for LED lamp specular removal.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A kind of glass phosphor preparation method, comprises the following steps:
1) select specific refractory power be more than 1.8 glass microballon be melt into glass paste;
2) in glass paste, add fluorescent material and stir evenly cooling forming afterwards.
The present invention compared with prior art, has the following advantages:
1, the glass fluor specific refractory power prepared can up to 1.8-2.0, close 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, it is achieved that LED component specular removal, high energy-conservation object;
2, preparation technology is simple to operation, it is to increase production efficiency, reduces production difficulty, suitability for scale production;
3, the glass paste of fluorescent material is contained without the need to preparation, without the need to adding other auxiliary agents, the glass microballon that fluorescent material directly adds during preparation melting stirs evenly, substantially reduce the production cycle, reduce production cost, and achieve the consistence of product chromaticity coordinates, make color tolerance control within 4SDCM;
4, the present invention is the first micro-pearl of melten glass, add fluorescent material again, then cooling forming after evenly is stirred, churning time can be controlled in very short scope, by fluorescent material in compared to existing technology, the way that glass powder and multiple auxiliary agent sinter after being first mixed into slurry again, the fluorescent material place time at high temperature is short, the crystalline phase extent of damage is little, therefore effectively prevent high-temperature sintering process to the detrimentally affect of fluorescent material, make the glass microballon of different glass transition temperature all can utilize the glass fluor of the obtained specular removal of preparation method of the present invention, it is particularly useful for the glass microballon that second-order transition temperature is greater than 1000 DEG C, expand performance categories and the range of application of product.
Accompanying drawing explanation
Fig. 1 show the color-division test report of the LED module that fluorescent glass sheet of the present invention encapsulation obtains.
Fig. 2 show the color-division test report of typical LED packages module.
Embodiment
The key distinction of the present invention and prior art is: adopt specific refractory power be more than 1.8 glass microballon and fluorescent material as raw material, and preparation process is for first adding fluorescent material again after glass microballon melting, then cooling forming after evenly is stirred, not only achieve LED component specular removal, high energy-conservation object, and effectively prevent high-temperature sintering process to the detrimentally affect of fluorescent material, whole preparation process is simple to operation, production efficiency height, production cost is low, product category and applied widely.
Concrete, the glass phosphor preparation method of the present invention, comprises the following steps:
1) select specific refractory power be more than 1.8 glass microballon be melt into glass paste;
2) in glass paste, add fluorescent material and stir evenly cooling forming afterwards.
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 specifically selected, and is generally greater than about 100��200 DEG C 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 many, and the required fusion time is more long, to ensure that the abundant melting of glass microballon is as the criterion. Preferably, the present invention adopts TiO2-BaO-SiO2-AlO3The glass microballon of system, this glass microballon has been reported in existing document: " investigation and application of high-refraction glass bead ", author: Peng Cheng, the building materials world, the 30th volume the 2nd phase in 2009. The specific refractory power of this glass microballon is 1.8-2.0, TiO2Being 0.70-0.85 with the mol ratio of BaO, melt temperature is 1000-1200 DEG C, and the fusion time is 30-90 minute. In order to avoid 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, it can also be multicolor phosphor or the mixture of multiple fluorescent material, it is preferable to the combination of the combination of YAG yellow fluorescent powder or YAG yellow fluorescent powder and red fluorescence powder or green emitting phosphor and red fluorescence powder. The consumption of fluorescent material can require according to actual formula and product performance and determine, it is preferable to 10��60wt% of glass microballon consumption. The joining day of fluorescent material preferably controls within 5s, to reduce the fluorescent material place time at high temperature as far as possible, reduces the crystalline phase extent of damage. Before joining in glass paste, whipping device can be opened in advance to be stirred by glass paste, whipping process keeps the temperature-resistant of glass paste, then join in glass paste by disposable for fluorescent material, control churning time is within 5s, fluorescent material is mixed with glass paste, then pours cooling forming in mould into. In order to improve forming quality of products, mould can pass through preheating in advance, and preheating temperature equals melt temperature or lower than within melt temperature 100 DEG C, process of cooling can be naturally cooling or force cooling.
In above-mentioned preparation method; owing to fluorescent material is not with glass microballon melting; therefore fluorescent material place time at high temperature is short; not only the crystalline phase extent of damage is little; and the light emitting ionic in fluorescent material is also not easily oxidated or reduced, without the need to leading to into inert protective gas such as nitrogen in preparation process, further simplify production technique and production unit; eliminate the process of gas recovery process, reduce production cost.
By technology contents, the structural attitude of the present invention being described in detail, is realized object and effect, it is explained in detail below in conjunction with enforcement mode.
Embodiment 1
1) TiO that specific refractory power is 1.8-2.0 is chosen2-BaO-SiO2-AlO3The glass microballon of system, its TiO2It is 0.70-0.85 with the mol ratio of BaO, it is placed in platinum crucible melting at 1000-1200 DEG C and is incubated after 30 minutes;
2) it is that the ratio of 10wt% of glass microballon consumption takes YAG yellow fluorescent powder according to the consumption of fluorescent material, disposable join in the glass paste that step 1) obtains and stir evenly, then pour cooling forming in mould into.
Embodiment 2
1) TiO that specific refractory power is 1.8-2.0 is chosen2-BaO-SiO2-AlO3The glass microballon of system, its TiO2It is 0.70-0.85 with the mol ratio of BaO, it is placed in platinum crucible melting at 1000-1200 DEG C and is incubated after 60 minutes;
2) according to the consumption of fluorescent material it is the mixture that the ratio of 30wt% of glass microballon consumption takes YAG yellow fluorescent powder and red fluorescence powder, join in the glass paste that step 1) obtains and stir evenly, then pouring cooling forming in preheated mould into, preheating temperature is 1000-1200 DEG C.
Embodiment 3
1) TiO that specific refractory power is 1.8-2.0 is chosen2-BaO-SiO2-AlO3The glass microballon of system, its TiO2It is 0.70-0.85 with the mol ratio of BaO, it is placed in platinum crucible melting at 1000-1200 DEG C and is incubated after 90 minutes;
2) according to the consumption of fluorescent material it is the mixture that the ratio of 60wt% of glass microballon consumption takes green emitting phosphor and red fluorescence powder, join and the glass paste that step 1) obtains stirs evenly, then pouring cooling forming in preheated mould into, preheating temperature is 1000-1200 DEG C.
Embodiment 4
1) TiO that specific refractory power is 1.8-2.0 is chosen2-BaO-SiO2-AlO3The glass microballon of system, its TiO2It is 0.70-0.85 with the mol ratio of BaO, it is placed in platinum crucible melting 60 minutes at 1000-1200 DEG C, then open and stir and be incubated;
2) it is that the ratio of 60wt% of glass microballon consumption takes YAG yellow fluorescent powder according to the consumption of fluorescent material, join in the glass paste that step 1) obtains in 5s and stir evenly, churning time controls within 5s, then pouring naturally cooling in preheated mould into shaping, preheating temperature is 1000-1200 DEG C.
Embodiment 5
1) TiO that specific refractory power is 1.8-2.0 is chosen2-BaO-SiO2-AlO3The glass microballon of system, its TiO2It is 0.70-0.85 with the mol ratio of BaO, it is placed in platinum crucible melting at 1000-1200 DEG C and stirs after 30 minutes and be incubated;
2) it is that the ratio of 10wt% of glass microballon consumption takes YAG yellow fluorescent powder according to the consumption of fluorescent material, disposable in 5s join in the glass paste that step 1) obtains and stir evenly, churning time controls within 5s, then pouring cooling forming in mould into, preheating temperature is 1000-1200 DEG C.
Embodiment 6
1) TiO that specific refractory power is 1.8-2.0 is chosen2-BaO-SiO2-AlO3The glass microballon of system, its TiO2It is 0.70-0.85 with the mol ratio of BaO, it is placed in platinum crucible melting at 1000-1200 DEG C and stirs after 90 minutes and be incubated;
2) according to the consumption of fluorescent material it is the mixture that the ratio of 30wt% of glass microballon consumption takes green emitting phosphor and red fluorescence powder, disposable in 5s join in the glass paste that step 1) obtains and stir evenly, churning time controls within 5s, then pouring cooling forming in mould into, preheating temperature is 1000-1200 DEG C.
Color-division is tested
Preparation-obtained for above-described embodiment 1��6 glass fluor is used for packaging LED module, and the LED module obtained is tested by ZWL-3900G integration packaging (COB) LED color-division test macro, and test report is as shown in Figure 1.
By typical LED packages module (with specific refractory power be 1.51 silica gel, epoxy resin or silicone resin be mixed and made into packaging LED module after fluorescent powder colloid with fluorescent material) same employing ZWL-3900G integration packaging (COB) LED color-division test macro tests, test report is as shown in Figure 2.
Analyze from Fig. 1 and Fig. 2, the luminescence spectrum of the LED module that fluorescent glass sheet of the present invention encapsulation obtains and typical LED packages module is completely the same, and the optical throughput of the LED module that fluorescent glass sheet of the present invention encapsulation obtains can reach 150lm, the optical throughput of typical LED packages module is only about 120lm.
X-ray diffraction analysis (XRD) is analyzed and is shown, the glass fluor of the present invention remains the original crystalline phase of fluorescent material well.
The foregoing is only embodiments of the invention; not thereby the patent scope of the present invention is limited; every utilize specification sheets of the present invention and accompanying drawing content to do equivalent structure or equivalence flow process conversion; or directly or indirectly it is used in other relevant technical fields, all it is included in the scope of patent protection of the present invention with reason.
Claims (4)
1. a glass phosphor preparation method, it is characterised in that, comprise the following steps:
1) selecting specific refractory power to be that the glass microballon of 1.8-2.0 is melt into glass paste, described glass microballon is TiO2-BaO-SiO2-Al2O3The glass microballon of system, the TiO in described glass microballon2It is 0.70-0.85 with the mol ratio of BaO;
2) in glass paste, add fluorescent material and stir evenly cooling forming afterwards; The consumption of described fluorescent material is 10��60wt% of glass microballon consumption; The joining day of described fluorescent material is less than 5s.
2. glass phosphor preparation method according to claim 1, it is characterised in that: the melting at 1000-1200 DEG C of described glass microballon, the fusion time is 30-90 minute.
3. glass phosphor preparation method according to claim 1, it is characterised 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.
4. the preparation-obtained glass fluor of glass phosphor preparation method according to claims 1 to 3 any one.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US10290777B2 (en) | 2016-07-26 | 2019-05-14 | Cree, Inc. | Light emitting diodes, components and related methods |
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| US11121298B2 (en) | 2018-05-25 | 2021-09-14 | Creeled, Inc. | Light-emitting diode packages with individually controllable light-emitting diode chips |
| US11335833B2 (en) | 2018-08-31 | 2022-05-17 | Creeled, Inc. | Light-emitting diodes, light-emitting diode arrays and related devices |
| US11233183B2 (en) | 2018-08-31 | 2022-01-25 | 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 |
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 |
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| 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 (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10290777B2 (en) | 2016-07-26 | 2019-05-14 | Cree, Inc. | Light emitting diodes, components and related methods |
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