CN108623153A - A kind of preparation method of remote fluorescence film for high-capacity LED - Google Patents
A kind of preparation method of remote fluorescence film for high-capacity LED Download PDFInfo
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- CN108623153A CN108623153A CN201810431364.3A CN201810431364A CN108623153A CN 108623153 A CN108623153 A CN 108623153A CN 201810431364 A CN201810431364 A CN 201810431364A CN 108623153 A CN108623153 A CN 108623153A
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- glass
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Classifications
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- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/068—Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
-
- 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
- H01L33/505—Wavelength conversion elements characterised by the shape, e.g. plate or foil
-
- 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
- C03C2204/00—Glasses, glazes or enamels with special properties
- C03C2204/08—Glass having a rough surface
Abstract
The present invention provides a kind of preparation methods of the remote fluorescence film for high-capacity LED, first prepare glass powder with low melting point using fusion method, and glass powder and fluorescent powder are disperseed in organic solvent, to be uniformly mixed into fluorescent glass slurry；Fluorescent glass slurry is coated on ground glass substrate with spin coating/screen printing technique, forms one layer of uniform fluorescent film layer, sintering and furnace cooling at low temperature are dried then in vacuum drying oven, the fluorescence membrane is made.Fluorescence membrane preparation process prepared by this method is simple, chemical property and optical property are preferable, in addition the glass substrate of frosting can reduce mirror-reflection, total internal reflection is made to minimize to increase the efficiency of white light output, therefore, compared to flat glass plate, using ground glass be the fluorescence membrane of substrate LED blue chips excitation under, its efficiency increases, and the preparation method is easy regulation and control and realizes white light output, therefore can be applied to field of semiconductor illumination.
Description
Technical field
The invention belongs to materialogy fields, are related to a kind of luminescent material, specifically a kind of for the remote of high-capacity LED
The preparation method of journey fluorescence membrane.
Background technology
Industrialization LED excites Ce by blue InGaN chips at present3+:YAG fluorescent powder realizes white light output.Organic resin/
Silica gel is frequently as encapsulating material, with the increase of electric current, concentrates on temperature on chip and is difficult to disperse, lead to organic packaging materials
Failure, the luminous mass and reliability in turn resulting in LED component reduce.In view of the above problems, studying and being reported at most at present
Solution is full-inorganic remote fluorescence glass material (phosphors-in-glass materials), simple preparation side
Method and good luminescent properties allow the remote fluorescence glass material to have larger potential use value in high-capacity LED, wherein
Remote fluorescence film gradually substitutes fluorescence because of its simpler process, ripe technology of preparing, the more preferably advantages such as performance
Block materials.The remote fluorescence method for manufacturing thin film is to be covered with fluorescent glass layer in glass substrate painting, and this thin-film material can be with
White light output is realized by the thickness etc. for adjusting raw material components, film, and need not be processed by shot blasting.Chinese patent
(CN102442778A) a kind of fluorescent glass and preparation method thereof is disclosed, it is characterised in that be applied to fluorescent glass obtained
When LED chip encapsulates, fluorescent glass is directly coated in by glass micro mist layer using dotting glue method.Still there is coating in the preparation method
In place of the deficiencies of unevenness, organic gel aging, yellow.
Most reports are all based on a series of fluorescence membranes of flat glass substrate preparation at present, but light is in the glass of plane
Visual angle is smaller when glass board transport, and total internal reflection causes significant portion of light loss.
Invention content
For above-mentioned technical problem in the prior art, the present invention provides a kind of remote fluorescences for high-capacity LED
The preparation method of the preparation method of film, this remote fluorescence film for high-capacity LED will solve the prior art
In a series of light of fluorescence membranes that is prepared based on the flat glass substrate visual angle in the glass substrate transmission of plane it is smaller and complete
Internal reflection causes the technical issues of significant portion of light loss.
The present invention provides a kind of preparation methods of the remote fluorescence film for high-capacity LED, include the following steps：
1) one the step of 50~65min prepares glass powder of the fusing point less than 600 DEG C is melted using fusion method at 1200 DEG C,
The mass percent of each component of the glass powder is as follows；
2) in organic solvent by glass powder and fluorescent powder dispersion, be uniformly mixed into fluorescent glass slurry, wherein glass powder,
The mass ratio of fluorescent powder and organic solvent is 20~100：2~6：8~32；
3) with spin coating, either the fluorescent glass slurry of step 2) is coated in ground glass by silk-screen printing or casting technology
On substrate, the transmitance of the ground glass substrate is 80~90%, and refractive index is 1.50~1.84, forms one layer uniformly
Fluorescent film layer dries 1~2h in 150~200 DEG C of vacuum drying ovens and is then sintered 10~30min simultaneously at 540 DEG C~660 DEG C
The fluorescence membrane is made in furnace cooling.
Further, the organic solvent is made of hexamethylene, terpinol, lauric acid and ethyl cellulose, hexamethylene,
The mass ratio of terpinol, lauric acid and ethyl cellulose is 5:10:1:1, the viscosity of the fluorescent glass slurry of preparation is 145~
160cps。
Fluorescence membrane preparation process prepared by the method for the present invention is simple, chemical property and optical property are preferable, frosted in addition
The glass substrate in face can reduce mirror-reflection, minimizing refraction in complete is made therefore to be compared to increase the efficiency of white light output
It is the fluorescence membrane of substrate under the excitation of LED blue chips using ground glass, efficiency increases, and the system in flat glass plate
Preparation Method is easy regulation and control and realizes white light output, therefore can be applied to field of semiconductor illumination.
The present invention is compared with prior art, and technological progress is significant.The present invention is made using the glass substrate of frosting
For the carrier of fluorescence membrane, and the glass plate of frosting is easier to prepare the higher fluorescence of performance with the bonding of fluorescent glass slurry
Thin-film material.The method of the present invention increases white light output quantity, therefore, can effectively improve great power LED luminous mass simultaneously
And enhance its reliability.
Description of the drawings
Fig. 1 is based on rough surface and ultra-clear glasses substrate light transmission path schematic diagram.
Fig. 2 is PL the and PLE spectrum of fluorescence membrane prepared by embodiment 1.
Prepared by 1 embodiment 1 of table is compared using ultra-clear glasses and ground glass as substrate fluorescence film performance.
Specific implementation mode
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated.
Embodiment 1：
1) SiO that will be weighed2, B2O3, ZnO, Na2CO3Its mass percent of raw material is respectively：25%, 42%, 20%,
13%, it is uniformly mixed, glass block, and grounds travel is prepared with fusion method；
2) glass powder and fluorescent powder that quality parts ratio is 20 parts and 6 parts are weighed, powder is dispersed in 8 parts of quality parts ratio
Organic solvent in, be uniformly mixed into viscosity be 145~155cps slurry；
3) 2) screen printing technique of slurry made from is coated on ground glass plate；
4) 3) fluorescence membrane prepared is dried into 1~2h in 150~200 DEG C of vacuum drying ovens, then at 540 DEG C~660 DEG C
10~30min of low-temperature sintering is to get to the remote fluorescence thin-film material.
Further, the organic solvent is made of hexamethylene, terpinol, lauric acid and ethyl cellulose, hexamethylene,
The mass ratio of terpinol, lauric acid and ethyl cellulose is 5:10:1:1, the viscosity of the fluorescent glass slurry of preparation is 145~
160cps。
Fig. 1 is to be based on rough surface and ultra-clear glasses substrate light transmission path schematic diagram.It is scribed by different glass substrates,
When the LED blue chips excitation obtained mixed white light of YAG fluorescent powder passes through glass substrate, in the glass substrate and sky of plane
Total internal reflection is generated between gas, is caused white light output to reduce, by changing the roughness of glass substrate, clearly can effectively be reduced
Light loss, to improve the luminous efficiency of LED.
As shown in Figure 2, based on different substrate of glass, the fluorescent glass film prepared, should under 460nm excitation wavelengths
There is Ce at 550nm in sample3+Characteristic emission peak, and the sample based on frosted substrate its emissive porwer is higher than ultra-clear glasses base
The fluorescence membrane at bottom.As shown in Table 1, which couples with blue chip, when operation electric current is 100mA, with mill
It is 70.43lm/W, colour temperature 5247K, colour rendering index 67.5 that sand glass, which is the film of substrate its photoelectric conversion efficiency,；With ultrawhite
It is 61.94lm/W, colour temperature 5193K, colour rendering index 64.8 that glass, which is the film of substrate its photoelectric conversion efficiency,.By above
Data analysis can illustrate thin as the fluorescence of substrate better than using ultra-thin glass by its performance of the fluorescence membrane of substrate of ground glass
Film, therefore be expected to that high-capacity LED performance can be improved.
Table 1
| Fluorescent glass film | Light efficiency (lm/w) | Colour temperature (K) | It is aobvious to refer to |
| Ultra-clear glasses plate | 61.94 | 5193 | 64.8 |
| Ground glass plate | 70.43 | 5247 | 67.5 |
Embodiment 2：
1) SiO that will be weighed2, B2O3, ZnO, Na2CO3Its mass percent of raw material is respectively：27%, 39%, 20%,
14%, it is uniformly mixed, glass block, and grounds travel is prepared with fusion method；
2) glass powder and fluorescent powder that quality parts ratio is 25 parts and 5 parts are weighed, powder is dispersed in quality parts ratio 8.5
In the organic solvent of part, it is uniformly mixed into the slurry that viscosity is 145~155cps；
3) 2) spin coating technique of slurry made from is coated on ground glass plate；
4) 3) fluorescence membrane prepared is dried into 1~2h in 150~200 DEG C of vacuum drying ovens, then at 540 DEG C~660 DEG C
10~30min of low-temperature sintering is to get to the remote fluorescence thin-film material.
Further, the organic solvent is made of hexamethylene, terpinol, lauric acid and ethyl cellulose, hexamethylene,
The mass ratio of terpinol, lauric acid and ethyl cellulose is 5:10:1:1, the viscosity of the fluorescent glass slurry of preparation is 145~
160cps。
Embodiment 3：
1) SiO that will be weighed2, B2O3, ZnO, Na2CO3Its mass percent of raw material is respectively：30%, 36%, 19%,
15%, it is uniformly mixed, glass block, and grounds travel is prepared with fusion method；
2) glass powder and fluorescent powder that quality parts ratio is 40 parts and 5.5 parts are weighed, powder is dispersed in quality parts ratio
In 10 parts of organic matter, it is uniformly mixed into the slurry that viscosity is 145~155cps；
3) 2) spin coating technique of slurry made from is coated on ground glass plate；
4) 3) fluorescence membrane prepared is dried into 1~2h in 150~200 DEG C of vacuum drying ovens, then at 540 DEG C~660 DEG C
10~30min of low-temperature sintering is to get to the remote fluorescence thin-film material.
Further, the organic solvent is made of hexamethylene, terpinol, lauric acid and ethyl cellulose, hexamethylene,
The mass ratio of terpinol, lauric acid and ethyl cellulose is 5:10:1:1, the viscosity of the fluorescent glass slurry of preparation is 145~
160cps。
Embodiment 4：
1) SiO that will be weighed2, B2O3, ZnO, Na2CO3Its mass percent of raw material is respectively：32%, 34.4%, 18%,
15.6%, it is uniformly mixed, glass block, and grounds travel is prepared with fusion method；
2) glass powder and fluorescent powder that quality parts ratio is 60 parts and 5 parts are weighed, powder is dispersed in quality parts ratio 20
In the organic solvent of part, it is uniformly mixed into the slurry that viscosity is 145~155cps；
3) 2) spin coating technique of slurry made from is coated on ground glass plate；
4) 3) fluorescence membrane prepared is dried into 1~2h in 150~200 DEG C of vacuum drying ovens, then at 540 DEG C~660 DEG C
10~30min of low-temperature sintering is to get to the remote fluorescence thin-film material.
Further, the organic solvent is made of hexamethylene, terpinol, lauric acid and ethyl cellulose, hexamethylene,
The mass ratio of terpinol, lauric acid and ethyl cellulose is 5:10:1:1, the viscosity of the fluorescent glass slurry of preparation is 145~
160cps。
Embodiment 5：
1) SiO that will be weighed2, B2O3, ZnO, Na2CO3Its mass percent of raw material is respectively：35%, 31%, 18%,
16%, it is uniformly mixed, glass block, and grounds travel is prepared with fusion method；
2) glass powder and fluorescent powder that quality parts ratio is 90 parts and 4.5 parts are weighed, powder is dispersed in quality parts ratio
In 30 parts of organic solvent, it is uniformly mixed into the slurry that viscosity is 145~155cps；
3) 2) spin coating technique of slurry made from is coated on ground glass plate；
4) say that the fluorescence membrane 3) prepared dries 1~2h in 150~200 DEG C of vacuum drying ovens, then at 540 DEG C~660 DEG C
10~30min of low-temperature sintering is to get to the remote fluorescence thin-film material.
Further, the organic solvent is made of hexamethylene, terpinol, lauric acid and ethyl cellulose, hexamethylene,
The mass ratio of terpinol, lauric acid and ethyl cellulose is 5:10:1:1, the viscosity of the fluorescent glass slurry of preparation is 145~
160cps。
Claims (2)
1. a kind of preparation method of remote fluorescence film for high-capacity LED, it is characterised in that include the following steps：
1）One 50 ~ 65min is melted at 1200 DEG C using fusion method and prepares the step of fusing point is less than 600 DEG C of glass powder, described
Glass powder each component mass percent it is as follows；
SiO225~35%；
B2O330~42%；
ZnO 17~20%；
Na2O 14~17%；
2）In organic solvent by glass powder and fluorescent powder dispersion, fluorescent glass slurry, wherein glass powder, fluorescence are uniformly mixed into
The mass ratio of powder and organic solvent is 20 ~ 100：2~6：8~32；
3）With spin coating either silk-screen printing or casting technology by step 2）Fluorescent glass slurry be coated in ground glass substrate
On, the transmitance of the ground glass substrate is 80 ~ 90%, and refractive index is 1.50 ~ 1.84, and it is thin to form one layer of uniform fluorescence
Then film layer is dried in vacuum drying oven and is then sintered at low temperature, low-temperature sintering temperature is 540 DEG C~660 DEG C, and sintering 10~
The fluorescence membrane is made in 30min, then furnace cooling.
2. a kind of preparation method of remote fluorescence film for high-capacity LED according to claim 1, feature exist
In：The organic solvent is made of hexamethylene, terpinol, lauric acid and ethyl cellulose, hexamethylene, terpinol, lauric acid
Mass ratio with ethyl cellulose is 5:10:1:1, the viscosity of the fluorescent glass slurry of preparation is 145 ~ 160cps.
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Cited By (4)
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| CN109860377A (en) * | 2018-12-12 | 2019-06-07 | 华中科技大学鄂州工业技术研究院 | Using the white light LEDs and preparation method thereof of burst of ultraviolel |
| CN110041931A (en) * | 2019-04-19 | 2019-07-23 | 中国计量大学 | A kind of near-infrared fluorescent film and preparation method thereof, near-infrared LED |
| CN113860913A (en) * | 2021-11-03 | 2021-12-31 | 武汉高星紫外光电科技有限公司 | High-thermal-conductivity diamond film fluorescent glass and preparation method of semiconductor lighting product thereof |
| CN114133930A (en) * | 2021-12-01 | 2022-03-04 | 上海应用技术大学 | Warm white garnet type fluorescent glass ceramic and preparation method thereof |
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| CN113860913A (en) * | 2021-11-03 | 2021-12-31 | 武汉高星紫外光电科技有限公司 | High-thermal-conductivity diamond film fluorescent glass and preparation method of semiconductor lighting product thereof |
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