CN106800371B - A kind of high thermal conductivity coefficient borosilicate fluorescent glass material and preparation method thereof - Google Patents
A kind of high thermal conductivity coefficient borosilicate fluorescent glass material and preparation method thereof Download PDFInfo
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- CN106800371B CN106800371B CN201710060625.0A CN201710060625A CN106800371B CN 106800371 B CN106800371 B CN 106800371B CN 201710060625 A CN201710060625 A CN 201710060625A CN 106800371 B CN106800371 B CN 106800371B
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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
- 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
- C03C3/07—Glass compositions containing silica with less than 40% silica by weight containing lead
- C03C3/072—Glass compositions containing silica with less than 40% silica by weight containing lead containing boron
- C03C3/074—Glass compositions containing silica with less than 40% silica by weight containing lead containing boron containing zinc
Abstract
The invention discloses a kind of high thermal conductivity coefficient borosilicate fluorescent glass, are prepared by host glass powder and Ce:YAG fluorescent powder, and host glass powder is by 0-15mol%SiO2、20‑55mol%B2O3、10‑50mol%ZnO、0‑15mol%TiO2、5‑20mol%Na2O、0‑5mol%Li2O composition, the doping of Ce:YAG fluorescent powder are the 1-10wt% of host glass powder total weight.The preparation method of above-mentioned fluorescent glass is additionally provided, this fluorescent glass piece has the advantage that thermal conductivity is high, thermal stability is good as the fluorescence transition material of white light LEDs.The problems such as compared to the packing forms of traditional silica gel and epoxy resin, the present invention has environmental stability good, declines there is no aging, yellow, color with light efficiency reduction, is particularly suitable in some high-capacity LED lighting devices.
Description
Technical field
The invention belongs to materialogy fields, are related to a kind of LED encapsulation technology, specifically a kind of high thermal conductivity coefficient borosilicate
Hydrochlorate fluorescent glass material and preparation method thereof.
Background technique
LED light source has that the service life is long, low energy consumption, the remarkable advantages such as pollution-free, high-efficient, small in size, is illuminating and is showing
Field has broad application prospects, and meets the developing direction of future light source.
The LED packing forms of mainstream are to be mixed using transparent organic silicon glue with Ce:YAG fluorescent powder at present, are then existed
Dispensing is carried out on InGaN blue chip.Current this encapsulation mode is continued working due to the presence of organic silica gel in light source
In the case of, chip fever will lead to the organic matter yellow being adhered to above, and aging then causes chromaticity coordinates elegant and light decay, shadow
The luminous efficiency and service life of LED light source are rung.Especially for the high-power LED light source of watt grade, the work electricity of chip
Stream is 300mA or more, generates heat serious in the case where working long hours, accelerates the aging of organic silica gel, shorten light source life.
Fluorescent glass is a kind of material of effective solution LED light fever.LED fluorescence conversion glass material has been done largely both at home and abroad
Research, current most commonly used preparation method is to prepare host glass first, and then milling prepares fluorescence with fluorescent powder co-sintering
Glass block.Current related fluorescent glass patent is concentrated mainly on the composition and technology of preparing of fluorescent glass.It is both domestic and external
Technical specialist successively develops the glass systems such as phosphate, borophosphate, borosilicate, aluminium borate, tellurate.Fluorescence
The technology of preparing of piece generally uses two-step method, first step synthetic substrate glass, and the glass making techniques of use include water quenching, melt
Melt method, sol-gal process and chemical vapor deposition etc..The preparation of second step fluorescent glass piece, the technology of preparing used is co-sintering
Method, silk screen print method, the tape casting, cladding process etc..
Summary of the invention
For above-mentioned technical problem in the prior art, the present invention provides a kind of high thermal conductivity coefficient borosilicate fluorescence glass
Glass material and preparation method thereof, described this high thermal conductivity coefficient borosilicate fluorescent glass material and preparation method thereof will solve
Since heat dissipation problem causes chromaticity coordinates elegant and light decay after LED encapsulation in the prior art, the luminous efficiency of LED light source is affected
And the technical issues of service life.
It is glimmering by host glass powder and Ce:YAG the present invention provides a kind of high thermal conductivity coefficient borosilicate fluorescent glass material
Light powder is prepared, and the host glass powder is prepared by the raw material of following molar percentage:
The doping of Ce:YAG fluorescent powder is the 1-10wt% of host glass powder total weight
The present invention also provides a kind of preparation methods of above-mentioned high thermal conductivity coefficient borosilicate fluorescent glass material, including
Following steps:
1) each reactive material is weighed according to molar percentage, is fully ground after above-mentioned each reactive material is mixed, then mixes
It closes uniform；
2) ground mixture is put into corundum crucible, is subsequently placed in 1050~1100 DEG C of temperature range of Si-Mo rod
Carry out melted in electric furnace, fusing time is 15~40min, is poured into distilled water at room temperature after raw material melt clarify completely
Water quenching is carried out, drying is milled to partial size between 40~50 μm, obtains host glass powder；
3) the host glass powder prepared is mixed with Ce:YAG fluorescent powder, the doping of Ce:YAG fluorescent powder is
The 1-10wt% of host glass powder total weight, mixed powder is placed in Muffle furnace and is fired, firing temperature be 500~
600 DEG C, the firing time is 20~30 minutes, high thermal conductivity coefficient borosilicate fluorescent glass material.
Further, the thermal conductivity of the high thermal conductivity coefficient borosilicate fluorescent glass material is in 1.23W/m/K-
1.35W/m/K。
Further, the chromaticity coordinate of the high thermal conductivity coefficient borosilicate fluorescent glass material can be according to fluorescence glass
The thickness of glass piece is adjusted.
The present invention prepares fluorescence bulk glass by two-step method, carries out various concentration after selected host glass composition
YAG fluorescent powder doping, obtains a series of borosilicate fluorescent glass of concentration proportionings.Glass is in glassy yellow, opaque, mechanical
Intensity is high, optical property is uniform, and physicochemical properties are stablized, and thermal conductivity is in 1.23W/m/K-1.35W/m/K.In 450nm wavelength
Excitation optical pumping under, obtain 550nm yellow light output, with InGaN blue chip fasten after issue white light.
The present invention, can be according to the thickness of fluorescent glass piece and the content of fluorescent powder while keeping preferable thermal conductivity
To adjust the position of luminous spectrum.Also there is preferable chemical stability and mechanical strength, avoid phosphate glass it is easily moist and
The lower defect of tellurate glass mechanical strength, it is practical, especially in high-capacity LED lighting area.
The present invention prepares presoma host glass material using high-temperature melting method by composition design, then total using low temperature
Sintering process prepares fluorescent glass piece.Combine the encapsulation of fluorescent glass piece and blue chip and generates white light, according to glass thickness with
Fluorescence Spectra is adjusted in phosphor concentration.Fluorescent glass used in the present invention both ensure that its conduct by well-designed
The good physicochemical stability of Pyrex and mechanical performance, and thermal conductivity with higher and optical uniformity.Ce3+: YAG fluorescence
Powder is as in the doping centre of luminescence.
The present invention is compared with prior art, and technological progress is significant.Fluorescence of this fluorescent glass piece as white light LEDs
Transition material has thermal conductivity height (1.35Wm-1·K-1) advantages such as thermal stability is good.Compared to traditional silica gel and asphalt mixtures modified by epoxy resin
The packing forms of rouge, the fluorescent glass piece have environmental stability it is good, there is no aging, yellow, color decline with light efficiency reduce etc. ask
Topic, is particularly suitable in some high-capacity LED lighting devices.Fluorescent glass prepared by the present invention according to using mold shape not
With different shapes can be made, it is easily assembled to, is directly bonded with blue chip, be easily formed large-scale production.
Detailed description of the invention
Fig. 1 is the fluorescence spectrum that embodiment 4# blue light obtained excites fluorescent glass.
Fig. 2 is the cie color coordinate of embodiment 4# fluorescence spectrum obtained.
Specific embodiment
The glass ingredient of 12 specific embodiments of LED encapsulation borosilicate fluorescent glass of the present invention is as shown in table 1:
Table 1: the host glass powder formula of specific 12 embodiments
Embodiment 1:
For composition as shown in 4# in table 1, specific preparation process is as follows:
According to the molar percentage that 4# glass in table 1 forms, the weight respectively formed accordingly is calculated, weighs each raw material simultaneously
It is uniformly mixed；Mixture is put into corundum crucible and is melted in 1050 DEG C~1100 DEG C of Elema electric furnace, after being completely melt
Clarification 15 minutes, will be in the distilled water of the glass metal casting of melting at room temperature；Moved into rapidly after slightly cooling in drying box into
Row drying is pulverized after dry, d50At 12 μm or so.Glass powder and Ce:YAG fluorescent powder are mixed according to mass ratio 20:1
It is placed in 580 DEG C of Muffle furnace and is sintered after even, the polishing of sample cutting and grinding is taken out after 15 minutes, in case follow-up test.
To the glass, test result is as follows:
Sample is processed into Φ=15mm, the sheet glass of h=2mm and polishing are tested under the blue light pumping of 450nm wavelength
Its fluorescence spectrum.The electroluminescence spectrum of LED encapsulation borosilicate glass flourescent sheet of the present invention is as shown in Figure 1.Experiment shows glass
Glass be in glassy yellow, opaque, optical property is uniform, excellent in physical and chemical performance, 450nm wavelength it is laser diode-pumped under
Very wide yellow fluorescence transmitting can be obtained.Its chromaticity coordinate figure is as shown in Figure 2.
Embodiment 2:
For composition as shown in 7# in table 1, specific preparation process is as follows:
According to the molar percentage that 7# glass in table 1 forms, the weight respectively formed accordingly is calculated, weighs each raw material simultaneously
It is uniformly mixed；Mixture is put into corundum crucible and is melted in 1050 DEG C~1100 DEG C of Elema electric furnace, after being completely melt
Clarification 15 minutes, will be in the distilled water of the glass metal casting of melting at room temperature；Moved into rapidly after slightly cooling in drying box into
Row drying is pulverized after dry, d50At 12 μm or so.Glass powder and Ce:YAG fluorescent powder are mixed according to mass ratio 20:1
It is placed in 580 DEG C of Muffle furnace and is sintered after even, the polishing of sample cutting and grinding is taken out after 15 minutes, in case follow-up test.
To the glass, test result is as follows:
Sample is processed into Φ=15mm, the sheet glass of h=2mm and polishing are tested under the blue light pumping of 450nm wavelength
Its fluorescence spectrum.Experiment shows glass in glassy yellow, and opaque, optical property is uniform, excellent in physical and chemical performance, in 450nm
The laser diode-pumped of wavelength lower can obtain very wide yellow fluorescence transmitting.
Embodiment 3:
For composition as shown in 11# in table 1, specific preparation process is as follows:
According to the molar percentage that 11# glass in table 1 forms, the weight respectively formed accordingly is calculated, each raw material is weighed
And it is uniformly mixed；Mixture is put into corundum crucible and is melted in 1050 DEG C~1100 DEG C of Elema electric furnace, is completely melt
It clarifies 15 minutes afterwards, it will be in the distilled water of the glass metal casting of melting at room temperature；It is moved into drying box rapidly after slightly cooling down
It is dried, pulverizes after dry, d50At 12 μm or so.Glass powder and Ce:YAG fluorescent powder are mixed according to mass ratio 15:1
It is placed in 580 DEG C of Muffle furnace and is sintered after uniformly, the polishing of sample cutting and grinding is taken out after 15 minutes, in case follow-up test.
To the glass, test result is as follows:
Sample is processed into Φ=15mm, the sheet glass of h=2mm and polishing are tested under the blue light pumping of 450nm wavelength
Its fluorescence spectrum.Experiment shows glass in glassy yellow, and opaque, optical property is uniform, excellent in physical and chemical performance, in 450nm
The laser diode-pumped of wavelength lower can obtain very wide yellow fluorescence transmitting.
Embodiment 4:
For composition as shown in 4# in table 1, specific preparation process is as follows:
According to the molar percentage that 4# glass in table 1 forms, the weight respectively formed accordingly is calculated, weighs each raw material simultaneously
It is uniformly mixed；Mixture is put into corundum crucible and is melted in 1050 DEG C~1100 DEG C of Elema electric furnace, after being completely melt
Clarification 15 minutes, will be in the distilled water of the glass metal casting of melting at room temperature；Moved into rapidly after slightly cooling in drying box into
Row drying is pulverized after dry, d50At 12 μm or so.Glass powder and Ce:YAG fluorescent powder are mixed according to mass ratio 15:1
It is placed in 580 DEG C of Muffle furnace and is sintered after even, the polishing of sample cutting and grinding is taken out after 15 minutes, in case follow-up test.
To the glass, test result is as follows:
Sample is processed into Φ=15mm, the sheet glass of h=2mm and polishing are tested under the blue light pumping of 450nm wavelength
Its fluorescence spectrum.Experiment shows glass in glassy yellow, and opaque, optical property is uniform, excellent in physical and chemical performance, in 450nm
The laser diode-pumped of wavelength lower can obtain very wide yellow fluorescence transmitting.
Embodiment 5:
For composition as shown in 4# in table 1, specific preparation process is as follows:
According to the molar percentage that 4# glass in table 1 forms, the weight respectively formed accordingly is calculated, weighs each raw material simultaneously
It is uniformly mixed；Mixture is put into corundum crucible and is melted in 1050 DEG C~1100 DEG C of Elema electric furnace, after being completely melt
Clarification 15 minutes, will be in the distilled water of the glass metal casting of melting at room temperature；Moved into rapidly after slightly cooling in drying box into
Row drying is pulverized after dry, d50At 12 μm or so.Glass powder and Ce:YAG fluorescent powder are mixed according to mass ratio 10:1
It is placed in 620 DEG C of Muffle furnace and is sintered after even, the polishing of sample cutting and grinding is taken out after 15 minutes, in case follow-up test.
Claims (2)
1. a kind of high thermal conductivity coefficient borosilicate fluorescent glass material, it is characterised in that: by host glass and Ce:YAG fluorescent powder
It is prepared, the host glass is prepared by the raw material of following molar percentage:
The doping of the Ce:YAG fluorescent powder is the 1-10wt% of host glass powder total weight；
A kind of preparation method of above-mentioned high thermal conductivity coefficient borosilicate fluorescent glass material, includes the following steps:
1) each reactive material is weighed according to molar percentage, is fully ground after above-mentioned each reactive material is mixed, then mixing is equal
It is even；
2) ground mixture is put into corundum crucible, is subsequently placed in 1050~1100 DEG C of temperature range of silicon molybdenum rod furnace
In carry out melted, fusing time is 15~40min, is poured into distilled water at room temperature and carries out after raw material melt clarify completely
Water quenching, drying are milled to partial size between 40~50 μm, obtain host glass powder；
3) the host glass powder prepared is mixed with Ce:YAG fluorescent powder, the doping of Ce:YAG fluorescent powder is matrix
Mixed powder is placed in Muffle furnace and is fired by the 1-10wt% of glass powder total weight, and firing temperature is 500~600
DEG C, the firing time is 20~30 minutes, obtains high thermal conductivity coefficient borosilicate fluorescent glass material, the high thermal conductivity coefficient boron
The thermal conductivity of silicate fluorescent glass material is in 1.23W/m/K-1.35W/m/K.
2. a kind of high thermal conductivity coefficient borosilicate fluorescent glass material prepared according to claim 1, it is characterised in that: institute
The chromaticity coordinate for the high thermal conductivity coefficient borosilicate fluorescent glass material stated can be adjusted according to the thickness of fluorescent glass piece.
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| CN107365070A (en) * | 2017-09-13 | 2017-11-21 | 上海应用技术大学 | A kind of white light LEDs red green composite fluorescence glass and preparation method thereof |
| CN107879640A (en) * | 2017-11-01 | 2018-04-06 | 上海应用技术大学 | A kind of preparation method of the remote fluorescence piece based on borate glass powder |
| CN107879623B (en) * | 2017-11-20 | 2021-12-21 | 上海应用技术大学 | Red luminescent glass ceramic for white light LED and preparation method thereof |
| CN109830587A (en) * | 2019-01-10 | 2019-05-31 | 徐煜 | A kind of full angle shines and the led lighting source production method of single side encapsulation |
| CN110395913B (en) * | 2019-08-08 | 2022-02-25 | 上海应用技术大学 | Preparation method of fluorescent glass with layered arrangement structure for full-spectrum LED |
| CN110818248B (en) * | 2019-11-22 | 2022-05-27 | 广州光联电子科技有限公司 | High-thermal-conductivity and high-refractive-index fluorescent glass layer and preparation method thereof |
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| CN101643315B (en) * | 2009-08-10 | 2012-02-08 | 武汉理工大学 | Low-melting-point fluorescent glass for white light LED and preparation method thereof |
| JP6398351B2 (en) * | 2013-07-25 | 2018-10-03 | セントラル硝子株式会社 | Phosphor dispersed glass |
| CN105621886A (en) * | 2014-11-26 | 2016-06-01 | 中央硝子株式会社 | Phosphor-dispersed glass |
| CN105399325B (en) * | 2015-04-17 | 2018-06-22 | 苏州工业园区晶冠瓷材料科技有限公司 | For the Ce of white light LEDs：YAG fluorescent glass and preparation method thereof |
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