CN106800371A - 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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- CN106800371A CN106800371A CN201710060625.0A CN201710060625A CN106800371A CN 106800371 A CN106800371 A CN 106800371A CN 201710060625 A CN201710060625 A CN 201710060625A CN 106800371 A CN106800371 A CN 106800371A
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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
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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
- 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
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Abstract
The invention discloses a kind of high thermal conductivity coefficient borosilicate fluorescent glass, by host glass powder and Ce：YAG fluorescent material is prepared from, and host glass powder is by 0 15mol%SiO2、20‑55mol%B2O3、10‑50mol%ZnO、0‑15mol%TiO2、5‑20mol%Na2O、0‑5mol%Li2O is constituted, Ce：The doping of YAG fluorescent powder is 1 10wt% of host glass powder gross weight.The preparation method of above-mentioned fluorescent glass is additionally provided, this fluorescent glass piece has the advantage that thermal conductivity is high, heat endurance is good as the fluorescence transition material of white light LEDs.Compared to the packing forms of traditional silica gel and epoxy resin, the present invention has environmental stability good, is declined the problems such as being reduced with light efficiency in the absence of aging, yellow, color, is particularly suited in some high-capacity LED lighting devices.
Description
Technical field
The invention belongs to materialogy field, it is related to a kind of LED encapsulation technologies, specifically a kind of high thermal conductivity coefficient borosilicate
Hydrochlorate fluorescent glass material and preparation method thereof.
Background technology
LED light source has the remarkable advantages such as low, pollution-free long lifespan, energy consumption, efficiency high, small volume, is illuminating and is showing
Field has broad application prospects, and meets the developing direction of future light source.
The LED packing forms of current main flow are using transparent organic silicon glue and Ce：YAG fluorescent powder is mixed, Ran Hou
Dispensing is carried out on InGaN blue chips.Current this encapsulation mode due to the presence of organic silica gel, in light source continuous firing
In the case of, chip heating can cause to adhere to superincumbent organic matter yellow, aging, then cause 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 level, the work electricity of its chip
It is more than 300mA to flow, and is generated heat in the case of working long hours serious, accelerates the aging of organic silica gel, shortens light source life.
Fluorescent glass is a kind of effective material for solving LED heating.Substantial amounts of has been done to LED fluorescence conversion glass material both at home and abroad
Research, is at present to prepare host glass first using most preparation methods, and then milling prepares fluorescence with fluorescent material co-sintering
Glass block.Current relevant 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 typically uses two-step method, and first step synthetic substrate glass, 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 for using is co-sintering
Method, silk screen print method, the tape casting, cladding process etc..
The content of the invention
For above-mentioned technical problem of the prior art, the 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 be solved
Because heat dissipation problem causes chromaticity coordinates elegant and light decay after LED encapsulation of the prior art, the luminous efficiency of LED light source is have impact on
With the technical problem of service life.
The invention provides a kind of high thermal conductivity coefficient borosilicate fluorescent glass material, by host glass powder and Ce：YAG is glimmering
Light powder is prepared from, and described host glass powder is prepared from by the raw material of following molar percentage：
Ce：The doping of YAG fluorescent powder is the 1-10wt% of host glass powder gross weight
Present invention also offers a kind of preparation method 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 mixed
Close uniform；
2) ground compound is put into corundum crucible, is subsequently placed in the Si-Mo rod of 1050~1100 DEG C of temperature range
Founded in electric furnace, fusing time is 15~40min, be poured into after raw material melts clarification completely in distilled water at room temperature
Water quenching is carried out, drying is milled to particle diameter between 40~50 μm, obtains host glass powder；
3) the host glass powder and Ce that will be prepared：YAG fluorescent powder is mixed, Ce：The doping of YAG fluorescent powder is
The 1-10wt% of host glass powder gross 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 described high thermal conductivity coefficient borosilicate fluorescent glass material is in 1.23W/m/K-
1.35W/m/K。
Further, the chromaticity coordinate of described 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, and various concentrations are carried out after selected host glass composition
YAG fluorescent powder is adulterated, and obtains a series of borosilicate fluorescent glass of concentration proportionings.Glass is in glassy yellow, opaque, machinery
Intensity is high, optical property is uniform, physicochemical properties stabilization, and thermal conductivity is in 1.23W/m/K-1.35W/m/K.In 450nm wavelength
Excite optical pumping under, obtain the gold-tinted output of 550nm, send white light after being fastened with InGaN blue chips.
The present invention, can be according to the thickness of fluorescent glass piece and the content of fluorescent material while preferable thermal conductivity is kept
To adjust the position of luminous spectrum.Also there is preferable chemical stability and mechanical strength, it is to avoid phosphate glass it is easily moist and
The relatively low defect of tellurate glass mechanical strength, it is practical, especially in high-capacity LED lighting field.
The present invention prepares presoma host glass material by constituting design using high-temperature melting method, is then total to using low temperature
Sintering process prepares fluorescent glass piece.By fluorescent glass piece and blue chip encapsulation combine generation white light, according to glass thickness with
Phosphor concentration is adjusted to fluorescence Spectra.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 with thermal conductivity and optical uniformity higher.Ce3+：YAG fluorescence
Powder is used as in the doping centre of luminescence.
The present invention is compared with prior art, and its technological progress is significant.This fluorescent glass piece as white light LEDs fluorescence
Transition material has thermal conductivity (1.35Wm high-1·K-1) advantage such as heat endurance is good.Compared to traditional silica gel and asphalt mixtures modified by epoxy resin
The packing forms of fat, the fluorescent glass piece has environmental stability good, in the absence of aging, yellow, color decline with light efficiency reduction etc. ask
Topic, is particularly suited in some high-capacity LED lighting devices.The present invention prepare fluorescent glass according to using mold shape not
It is same to be made different shapes, it is easy to assemble, directly fitted with blue chip, it is easy to form large-scale production.
Brief description of the drawings
Fig. 1 is excited the fluorescence spectrum of fluorescent glass by blue light that embodiment 4# is obtained.
The cie color coordinate of the fluorescence spectrum that Fig. 2 is obtained by embodiment 4#.
Specific embodiment
LED encapsulation of the present invention is as shown in table 1 with the glass ingredient of 12 specific embodiments of borosilicate fluorescent glass：
Table 1：The host glass powder formula of specific 12 embodiments
Embodiment 1:
Composition is as shown in 4# in table 1, and specific preparation process is as follows：
According to the molar percentage that 4# glass in table 1 is constituted, the weight of corresponding each composition is calculated, weigh each raw material simultaneously
It is well mixed；Compound 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, in the glass metal cast that will be melted distilled water at room temperature；Enter in rapid immigration drying box after slightly cooling down
Row drying, pulverizes after drying, d50At 12 μm or so.By glass dust and Ce：YAG fluorescent powder is according to mass ratio 20:1 mixing is equal
Sintering in 580 DEG C of Muffle furnace is positioned over after even, the polishing of sample cutting and grinding is taken out after 15 minutes, in case follow-up test.
Test result to the glass is as follows：
Sample is processed into Φ=15mm, the sheet glass of h=2mm is simultaneously polished, is tested under the blue light pumping of 450nm wavelength
Its fluorescence spectrum.LED encapsulation of the present invention is as shown in Figure 1 with the electroluminescence spectrum of borosilicate glass flourescent sheet.Experiment shows, glass
Glass is in glassy yellow, opaque, and optical property is uniform, excellent in physical and chemical performance, 450nm wavelength it is laser diode-pumped under
Yellow fluorescence transmitting very wide can be obtained.Its chromaticity coordinate figure is as shown in Figure 2.
Embodiment 2:
Composition is as shown in 7# in table 1, and specific preparation process is as follows：
According to the molar percentage that 7# glass in table 1 is constituted, the weight of corresponding each composition is calculated, weigh each raw material simultaneously
It is well mixed；Compound 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, in the glass metal cast that will be melted distilled water at room temperature；Enter in rapid immigration drying box after slightly cooling down
Row drying, pulverizes after drying, d50At 12 μm or so.By glass dust and Ce：YAG fluorescent powder is according to mass ratio 20:1 mixing is equal
Sintering in 580 DEG C of Muffle furnace is positioned over after even, the polishing of sample cutting and grinding is taken out after 15 minutes, in case follow-up test.
Test result to the glass is as follows：
Sample is processed into Φ=15mm, the sheet glass of h=2mm is simultaneously polished, is tested under the blue light pumping of 450nm wavelength
Its fluorescence spectrum.Experiment shows that glass is in glassy yellow, opaque, and optical property is uniform, excellent in physical and chemical performance, in 450nm
The laser diode-pumped lower of wavelength can obtain yellow fluorescence transmitting very wide.
Embodiment 3:
Composition is as shown in 11# in table 1, and specific preparation process is as follows：
According to the molar percentage that 11# glass in table 1 is constituted, the weight of corresponding each composition is calculated, weigh each raw material
And be well mixed；Compound is put into corundum crucible and is melted in 1050 DEG C~1100 DEG C of Elema electric furnace, be completely melt
Clarify 15 minutes afterwards, in the glass metal cast that will be melted distilled water at room temperature；After slightly cooling down in rapid immigration drying box
It is dried, is pulverized after drying, d50At 12 μm or so.By glass dust and Ce：YAG fluorescent powder is according to mass ratio 15:1 mixing
Sintering in 580 DEG C of Muffle furnace is positioned over after uniform, the polishing of sample cutting and grinding is taken out after 15 minutes, in case follow-up test.
Test result to the glass is as follows：
Sample is processed into Φ=15mm, the sheet glass of h=2mm is simultaneously polished, is tested under the blue light pumping of 450nm wavelength
Its fluorescence spectrum.Experiment shows that glass is in glassy yellow, opaque, and optical property is uniform, excellent in physical and chemical performance, in 450nm
The laser diode-pumped lower of wavelength can obtain yellow fluorescence transmitting very wide.
Embodiment 4:
Composition is as shown in 4# in table 1, and specific preparation process is as follows：
According to the molar percentage that 4# glass in table 1 is constituted, the weight of corresponding each composition is calculated, weigh each raw material simultaneously
It is well mixed；Compound 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, in the glass metal cast that will be melted distilled water at room temperature；Enter in rapid immigration drying box after slightly cooling down
Row drying, pulverizes after drying, d50At 12 μm or so.By glass dust and Ce：YAG fluorescent powder is according to mass ratio 15:1 mixing is equal
Sintering in 580 DEG C of Muffle furnace is positioned over after even, the polishing of sample cutting and grinding is taken out after 15 minutes, in case follow-up test.
Test result to the glass is as follows：
Sample is processed into Φ=15mm, the sheet glass of h=2mm is simultaneously polished, is tested under the blue light pumping of 450nm wavelength
Its fluorescence spectrum.Experiment shows that glass is in glassy yellow, opaque, and optical property is uniform, excellent in physical and chemical performance, in 450nm
The laser diode-pumped lower of wavelength can obtain yellow fluorescence transmitting very wide.
Embodiment 5:
Composition is as shown in 4# in table 1, and specific preparation process is as follows：
According to the molar percentage that 4# glass in table 1 is constituted, the weight of corresponding each composition is calculated, weigh each raw material simultaneously
It is well mixed；Compound 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, in the glass metal cast that will be melted distilled water at room temperature；Enter in rapid immigration drying box after slightly cooling down
Row drying, pulverizes after drying, d50At 12 μm or so.By glass dust and Ce：YAG fluorescent powder is according to mass ratio 10:1 mixing is equal
Sintering in 620 DEG C of Muffle furnace is positioned over after even, the polishing of sample cutting and grinding is taken out after 15 minutes, in case follow-up test.
Claims (4)
1. a kind of high thermal conductivity coefficient borosilicate fluorescent glass material, it is characterised in that：By host glass powder and Ce：YAG fluorescence
Powder is prepared from, and described host glass powder is prepared from by the raw material of following molar percentage：
SiO20-15%；
B2O320-55%；
ZnO 10-40%；
TiO20-15%；
Na2O 5-20%；
Li2O 0-5%；
Described Ce：The doping of YAG fluorescent powder is the 1-10wt% of host glass powder gross weight.
2. the preparation method of a kind of high thermal conductivity coefficient borosilicate fluorescent glass material described in claim 1, it is characterised in that
Comprise 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 mix equal
It is even；
2）Ground compound is put into corundum crucible, the silicon molybdenum rod furnace of 1050 ~ 1100 DEG C of temperature range is subsequently placed in
In founded, fusing time is 15 ~ 40min, is carried out in the distilled water for being poured at room temperature after raw material melts clarification completely
Water quenching, drying is milled to particle diameter between 40 ~ 50 μm, obtains host glass powder；
3）The host glass powder and Ce that will be prepared：YAG fluorescent material is mixed, Ce：The doping of YAG fluorescent powder is base
The 1-10wt% of matter glass dust gross weight, mixed powder is placed in Muffle furnace and is fired, and firing temperature is 500 ~ 600
DEG C, the firing time is 20 ~ 30 minutes, high thermal conductivity coefficient borosilicate fluorescent glass material.
3. a kind of fluorescence conversion glass for being prepared according to claim 1, it is characterised in that：Described high thermal conductivity coefficient
The thermal conductivity of borosilicate fluorescent glass material is in 1.23W/m/K-1.35 W/m/K.
4. a kind of fluorescence conversion glass for being prepared according to claim 1, it is characterised in that：Described high thermal conductivity coefficient
The chromaticity coordinate of borosilicate fluorescent glass material can be adjusted according to the thickness of fluorescent glass piece.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107879623A (en) * | 2017-11-20 | 2018-04-06 | 上海应用技术大学 | A kind of white light LEDs emitting red light glass ceramics 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 |
| CN110395913A (en) * | 2019-08-08 | 2019-11-01 | 上海应用技术大学 | A kind of preparation method of the layer-stepping arrangement architecture fluorescent glass for full-spectrum LED |
| CN110818248A (en) * | 2019-11-22 | 2020-02-21 | 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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| CN105121375A (en) * | 2013-07-25 | 2015-12-02 | 中央硝子株式会社 | Phosphor-dispersed glass |
| CN105399325A (en) * | 2015-04-17 | 2016-03-16 | 苏州工业园区晶冠瓷材料科技有限公司 | Ce:YAG fluorescent glass for white-light LED and preparation method of Ce:YAG fluorescent glass |
| CN105621886A (en) * | 2014-11-26 | 2016-06-01 | 中央硝子株式会社 | Phosphor-dispersed glass |
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| CN101643315A (en) * | 2009-08-10 | 2010-02-10 | 武汉理工大学 | Low-melting-point fluorescent glass for white light LED and preparation method thereof |
| CN105121375A (en) * | 2013-07-25 | 2015-12-02 | 中央硝子株式会社 | Phosphor-dispersed glass |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107879623A (en) * | 2017-11-20 | 2018-04-06 | 上海应用技术大学 | A kind of white light LEDs emitting red light glass ceramics 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 |
| CN110395913A (en) * | 2019-08-08 | 2019-11-01 | 上海应用技术大学 | A kind of preparation method of the layer-stepping arrangement architecture fluorescent glass for full-spectrum LED |
| 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 |
| CN110818248A (en) * | 2019-11-22 | 2020-02-21 | 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 |
| 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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