CN107686243A - A kind of preparation method of low-melting-point fluorescent glass - Google Patents
A kind of preparation method of low-melting-point fluorescent glass Download PDFInfo
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- CN107686243A CN107686243A CN201710648484.4A CN201710648484A CN107686243A CN 107686243 A CN107686243 A CN 107686243A CN 201710648484 A CN201710648484 A CN 201710648484A CN 107686243 A CN107686243 A CN 107686243A
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- 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
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/04—Opacifiers, e.g. fluorides or phosphates; Pigments
Abstract
The invention discloses a kind of preparation method of low-melting-point fluorescent glass, belong to glass material preparation field, it is characterised in that by the optimization design to glass ingredient, propose one kind (NaPO3)6‑NaF‑CaO‑B2O3‑Sb2O3‑Li2O ZnO low-melting glass systems, and propose specific preparation process：（1）First prepare low melting point bare glass；（2）Then the yttrium-aluminium-garnet structure yellow fluorescent powder of commercialization is mixed with this glass powder with low melting point again among being placed in alumina crucible, and is formed by a firing.It is provided by the invention prepare fluorescent glass component cost it is cheap, operating procedure simple and fast, it is heat-resist, machining property is excellent, it is and low with energy consumption, chemical stability is excellent, solution is provided to solving the problems such as high power LED device light decay, color temperature shift, is expected to break through the limitation that conventional fluorescent powder is brought.
Description
Technical field
The invention belongs to glass material preparing technical field, more particularly to a kind of preparation method of low-melting-point fluorescent glass.
Background technology
As the continuous research and development to white light LEDs, its luminous efficiency, optical property have been continuously available improvement, have made white light
LED turns into a kind of new all solid state lighting source.Current most white light LEDs are mainly by conventional fluorescent powder such as commercialization
Yttrium-aluminium-garnet structure yellow fluorescent powder（Ce：YAG）It is coated in LED chip with silica gel or epoxy resin, but makes for a long time
With the meeting aging of silica gel afterwards, light-emitting phosphor strength retrogression, photochromic deviation is shown as, color and luster is deteriorated, and influences the LED component life-span.
Fluorescent glass will be combined to form between fluorescent material and glass at present, be to solve the best selection of conventional LED package.With existing ring
Oxygen resin-encapsulated LED is compared, and fluorescent glass has the advantages of following unique：(1) suppress the aging of encapsulation, improve the life-span；(2)
Heat resistance and water-resistance are improved；(3) great power LED can be prepared, high current is supported, realizes high brightness.Therefore, fluorescence glass
Glass provides the direction of human future lighting source, and the research and development of fluorescent glass material are to solving high power LED device light decay, colour temperature
The problems such as drift, provides a new solution, is expected to break through the limitation that conventional fluorescent powder is brought.But fluorescent glass
Research also face a series of problems, one is exactly the too high problem of temperature of burning glass, secondly being commercial yttroalumite pomegranate
Stone structure yellow fluorescent powder（Ce：YAG）Reaction problem between glass matrix.Solve the two problems at present mainly to find
One kind has inert low-melting glass component.It so both can effectively prevent the yttrium-aluminium-garnet structure yellow fluorescent powder of commercialization
Reaction between glass matrix, the temperature for firing fluorescent glass can also be greatly reduced, so as to preferably save the energy.Cut
Only so far, low-melting glass concentrates on TeO2Glass system is studied（Lin, Z., et al., A chromaticity-
tunable garnet-based phosphor-in-glass color converter applicable in w-LED.
Journal of the European Ceramic Society, 2016. 36(7): p. 1723-1729.；Lin, Z.,
et al., Highly thermal-stable warm w-LED based on Ce:YAG PiG stacked with a
red phosphor layer. Journal of Alloys and Compounds, 2015. 649: p. 661-665.）,
But TeO2Cost it is too high, it is difficult to realize commercialization, but other glass system firing temperatures are all higher, do not meet the present age
The low-carbon life advocated, therefore need to develop a kind of fluorescence glass for not only reducing and firing fluorescent glass temperature but also reducing production cost
Glass preparation method.
The content of the invention
The purpose of the present invention is to propose to a kind of component of low-melting-point fluorescent glass for white light LEDs and by rational
The method that Technology for Heating Processing prepares fluorescent glass, the cost of its glass ingredient is cheap, operating procedure simple and fast, heat-resist,
Machining property is excellent, and low with energy consumption, and chemical stability is excellent to wait clear superiority.
The concrete technical scheme of the present invention comprises the following steps：
（1）Be first according to low-melting glass raw material components proportioning, by Muffle furnace, first sintering prepares bare glass block, and by its
Bare glass powder is broken into, the low-melting glass raw material components are (NaPO3)6-NaF-CaO-B2O3-Sb2O3-Li2O-ZnO；
（2）Then again by the yellow fluorescent powder of commercial yttrium-aluminium-garnet structure（Ce：YAG）Mixed with this low melting point bare glass powder rearmounted
Among alumina crucible；（3）Be subsequently placed into Muffle furnace progress fluorescent glass firing, taken out at 730 DEG C pour into it is made of copper
Die for molding；（4）With mould is incubated into 2h-4h at a temperature of 200 DEG C -400 DEG C of baking oven；（5）Baking oven power supply is finally closed,
Mould is taken out after being cooled to room temperature, obtains the fluorescent glass of low melting point.
In the low-melting glass raw material components, calgon, sodium fluoride, calcium oxide, diboron trioxide, three oxidations two
Antimony, lithia, the molar fraction ratio that feeds intake of zinc oxide are respectively：10%-20%；30%-45%；0-10%；35%-50%；0-10%；0-
10%；0-10%.
It is described to add commercial yttrium-aluminium-garnet structure yellow fluorescent powder（Ce：YAG）Quality be glass ingredient gross mass point
Several 1wt%-5wt%.
The bare glass sintering procedure is the control heating-up time, is 20min- from the heating-up time used in room temperature to 200 DEG C
40min, 20min-30min is incubated at 200 DEG C, then reaches 750 DEG C with 100min-160min and be incubated 30-60min, finally existed
Rapid cooling forms bare glass block among mould made of copper is poured into 750 DEG C of high temperature taking-ups.
The glass powder and commercial yttrium-aluminium-garnet structure yellow fluorescent powder（Ce：YAG）Mixing is to be fully ground 30-
40min, form mixed powder.
The fluorescent glass sintering procedure is is 20min-40min from the heating-up time used in room temperature to 200 DEG C, at 200 DEG C
20min-30min is incubated, then reaches 730 DEG C of insulation 5min-30min with 60min-150min.
The technique effect of the present invention is with advantage：
The preparation method of fluorescent glass of the present invention, new low-melting glass system is proposed, has prepared transparent eutectic
Glass powder after the bare glass of point and grinding can be fired into fluorescent glass after being mixed with yellow fluorescent powder, and control commercial yttrium
Aluminium garnet structure yellow fluorescent powder（Ce：YAG）With the chemical reaction of glass matrix between the two, ensure yellow fluorescence powder particles
Chemical stability in glass matrix, solution party is provided to solving the problems such as high power LED device light decay, color temperature shift
Case.It is of the present invention fire bare glass each component show inertia at high temperature, not with the yellow of yttrium-aluminium-garnet structure
Fluorescent material（Ce：YAG）Reacted between particle and the fluorescent powder grain into glass matrix remains in that integrality, not shadow
Ring its luminescent properties.
The method of the invention prepares the low-melting-point fluorescent glass of function admirable and firing temperature of the present invention exists
730 DEG C -750 DEG C, whole process energy consumption is low.With raw material components TeO2Glass system is compared, and it is each that the present invention prepares bare glass
The cost of raw material components is cheap, and for the price of each raw material components, the cost of material of each component of the present invention is relative to TeO2Glass
Glass system cost of material reduces 54%, and preparation technology is simply easily operated, and the heat-resisting water-resistance of fluorescent glass is good, whole mistake
Journey energy consumption is low, is adapted to popularization and application.
Brief description of the drawings
Fig. 1 is the transmitance figure that the present invention prepares bare glass.
Fig. 2 prepares the yellow fluorescent powder of fluorescent glass and commercial yttrium-aluminium-garnet structure and the X of bare glass for the present invention
X ray diffraction comparison diagram.
The fluorescent glass that Fig. 3 has been prepared for the present invention excites collection of illustrative plates.
Fig. 4 is the transmitting collection of illustrative plates of fluorescent glass prepared by the present invention.
Fig. 5 is the scanning electron microscope sem figure of fluorescent glass of the present invention.
Embodiment
Below by way of case study on implementation, the present invention is further elaborated.
Embodiment 1
(1) low melting point bare glass is prepared：
(the NaPO of low-melting glass component 14% is weighed with counter balance3)6-44%NaF-3%CaO-35%B2O3-2%Sb2O3-2%Li2O
（It is molar fraction）, then load weighted each component is put into mortar and ground uniformly, milling time 30min, grind
Is fitted into after finishing in the alumina crucible cleaned up, is placed in sintering among Muffle furnace, sintering process is from room temperature to 200
Heating-up time used in DEG C is 30min, and 20min is incubated at 200 DEG C, then reaches 750 DEG C with 130min and be incubated 30min, is finally existed
Rapid cooling forms bare glass block among mould is poured into 750 DEG C of high temperature taking-ups, you can obtains low-melting glass.
(2) fluorescent glass is prepared：
The low melting point bare glass baked is broken into required glass powder, and with 0.4g commercialization yttrium-aluminium-garnet structures
Yellow fluorescent powder（Ce：YAG）, milling time 30min after drying for standby uniform by mortar grinder.The powder mixed is taken,
It is fitted into the alumina crucible cleaned up, is placed in sintering in Muffle furnace, preparation technology is from liter used in room temperature to 200 DEG C
The warm time is 40min, and 30min is incubated at 200 DEG C, then reaches 730 DEG C of insulation 20min with 120min, finally at a temperature of 730 DEG C
Fluorescent glass is poured among copper-made mould and is molded, then by the copper-made mould containing fluorescent glass in an oven with 300 DEG C of guarantors
Warm 3h, baking oven power supply is finally closed, mould is taken out after being cooled to room temperature, you can obtain fluorescent glass.
Embodiment 2
(1) low melting point bare glass is prepared：
(the NaPO of low-melting glass component 11% is weighed with counter balance3)6-35%NaF-6%CaO-37%B2O3-3%Sb2O3-2%
Li2O-6%ZnO（It is molar fraction）, then load weighted each component is put into mortar and ground uniformly, milling time is
40min, grinding are fitted into the alumina crucible cleaned up after finishing, are placed in sintering among Muffle furnace, sintering process
To be 30min from the heating-up time used in room temperature to 200 DEG C, 10min is incubated at 200 DEG C, then reach 750 DEG C with 120min and be incubated
30min, finally rapid cooling forms bare glass block among 750 DEG C of high temperature take out and pour into mould, you can obtains low-melting glass.
(2) fluorescent glass is prepared：
The low melting point bare glass baked is broken into required glass powder, and with 0.3g commercialization yttrium-aluminium-garnet structures
Yellow fluorescent powder（Ce：YAG）, milling time 40min after drying for standby uniform by mortar grinder.The powder mixed is taken,
It is fitted into the alumina crucible cleaned up, is placed in sintering in Muffle furnace, preparation technology is from liter used in room temperature to 200 DEG C
The warm time is 30min, and 20min is incubated at 200 DEG C, then reaches 730 DEG C of insulation 10min with 80min, finally at a temperature of 730 DEG C
Fluorescent glass is poured among copper-made mould and is molded, then by the copper-made mould containing fluorescent glass in an oven with 250 DEG C of guarantors
Warm 3h, baking oven power supply is finally closed, mould is taken out after being cooled to room temperature, you can obtain fluorescent glass.
Embodiment 3
(1) low melting point bare glass is prepared：
(the NaPO of low-melting glass component 15% is weighed with counter balance3)6-38%NaF-4%CaO-35%B2O3-3%Sb2O3-2%
Li2O-3%ZnO（It is molar fraction）, then load weighted each component is put into mortar and ground uniformly, milling time is
35min, grinding are fitted into the alumina crucible cleaned up after finishing, are placed in sintering among Muffle furnace, sintering process
To be 35min from the heating-up time used in room temperature to 200 DEG C, 15min is incubated at 200 DEG C, then reach 750 DEG C with 140min and be incubated
20min, finally rapid cooling forms bare glass block among 750 DEG C of high temperature take out and pour into mould, you can obtains low-melting glass.
(2) fluorescent glass is prepared：
The low melting point bare glass baked is broken into required glass powder, and with 0.2g commercialization yttrium-aluminium-garnet structures
Yellow fluorescent powder（Ce：YAG）, milling time 35min after drying for standby uniform by mortar grinder.The powder mixed is taken,
It is fitted into the alumina crucible cleaned up, is placed in sintering in Muffle furnace, preparation technology is from liter used in room temperature to 200 DEG C
The warm time is 35min, and 15min is incubated at 200 DEG C, then reaches 730 DEG C of insulation 15min with 120min, finally at a temperature of 730 DEG C
Fluorescent glass is poured among copper-made mould and is molded, then by the copper-made mould containing fluorescent glass in an oven with 300 DEG C of guarantors
Warm 3h, baking oven power supply is finally closed, mould is taken out after being cooled to room temperature, you can obtain fluorescent glass.
The optics bare glass transparency obtained by embodiment 1 is good, is learnt from Fig. 1 transmittance curve, and its transmitance is high
Up to 84%.Resulting fluorescent glass can excite the Ce in fluorescent glass through blue light caused by blue light exciter：YAG particles produce
Raw gold-tinted and with the interphase interaction of blue light so as to form white light, therefore LED component can be made.In Fig. 2 X-ray diffractogram
In, diffraction maximum occur the characteristic peak of YAG phases and with YAG standard specimens, PDF cards match it is fine, illustrate Ce：YAG fluorescent powder
Mix among the glass matrix.Ce is demonstrated by 345nm3+4f-5d1Energy level excites transition, is demonstrated by 467nm
Ce3+4f-5d2Energy level excites transition（As shown in Figure 3）.Ce is demonstrated by 551nm3+Transmitting characteristic peak（Such as Fig. 4 institutes
Show）.From scanning electron microscope sem figure（Fig. 5）It can be observed how Ce：YAG fluorescent powder is distributed among glass matrix and Ce：YAG particles
It is complete in glass matrix, do not reacted between glass ingredient matrix, so as to ensure Ce：YAG particle chemical stabilities, hair
Luminous intensity is basically unchanged.
Claims (6)
1. a kind of preparation method of low-melting-point fluorescent glass, it is characterised in that specifically preparation process is：（1）It is first according to eutectic
Point glass components proportioning, by Muffle furnace, first sintering prepares bare glass block, and is broken into bare glass powder, institute
It is (NaPO to state low-melting glass raw material components3)6-NaF-CaO-B2O3-Sb2O3-Li2O-ZnO；（2）Then again by commercial yttrium aluminium
The yellow fluorescent powder of garnet structure is placed among alumina crucible after being mixed with this low melting point bare glass powder；（3）Then put
Enter progress fluorescent glass firing in Muffle furnace, taken out at 730 DEG C and pour into die for molding made of copper；（4）With mould existed
2h-4h is incubated at a temperature of 200 DEG C -400 DEG C of baking oven；（5）Baking oven power supply is finally closed, mould is taken out after being cooled to room temperature, is obtained
The fluorescent glass of low melting point.
2. the preparation method of the low-melting-point fluorescent glass according to claim 1, it is characterised in that the low melting point glass
In glass raw material components, the throwing of calgon, sodium fluoride, calcium oxide, diboron trioxide, antimony oxide, lithia, zinc oxide
Expect that molar fraction ratio is respectively：10%-20%；30%-45%；0-10%；35%-50%；0-10%；0-10%；0-10%.
3. the preparation method of low-melting-point fluorescent glass according to claim 1, it is characterised in that described to add commercial yttrium
The quality of aluminium garnet structure yellow fluorescent powder is the 1wt%-5wt% of glass ingredient total mass fraction.
4. the preparation method of the low-melting-point fluorescent glass according to claim 1, it is characterised in that the bare glass burns
Process processed is the control heating-up time, is 20min-40min from the heating-up time used in room temperature to 200 DEG C, and 20min- is incubated at 200 DEG C
30min, then reach 750 DEG C with 100min-160min and be incubated 30-60min, finally poured into 750 DEG C of high temperature taking-ups made of copper
Rapid cooling forms bare glass block among mould.
5. the preparation method of the low-melting-point fluorescent glass according to claim 1 or 3, it is characterised in that the glass dust
It is to be fully ground 30-40min that body mixes with commercial yttrium-aluminium-garnet structure yellow fluorescent powder, forms mixed powder.
6. the preparation method of the low-melting-point fluorescent glass according to claim 1, it is characterised in that the fluorescent glass
Sintering procedure is incubated 20min-30min to be 20min-40min from the heating-up time used in room temperature to 200 DEG C, at 200 DEG C, then uses
60min-150min reaches 730 DEG C of insulation 5min-30min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111253073A (en) * | 2020-01-21 | 2020-06-09 | 徐州凹凸光电科技有限公司 | Method for preparing gadolinium-aluminum-garnet-based white-light glass ceramic by adopting sol-gel method |
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| CN102745893A (en) * | 2012-06-20 | 2012-10-24 | 武汉理工大学 | Composite phosphor luminescent glass and preparation method for same |
| CN103043908A (en) * | 2013-01-11 | 2013-04-17 | 华南师范大学 | Novel fluorescent glass and preparation method thereof |
| CN103539359A (en) * | 2013-09-27 | 2014-01-29 | 南京邮电大学 | Rare earth doped fluoride micro-nano crystal-fluorophosphate glass composite material and preparation method thereof |
| CN106587641A (en) * | 2016-12-01 | 2017-04-26 | 天津理工大学 | Low-melting-point glass powder and laser-illumination glass ceramic made from low-melting-point glass powder |
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2017
- 2017-08-01 CN CN201710648484.4A patent/CN107686243B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5043112A (en) * | 1973-08-22 | 1975-04-18 | ||
| CN102464450A (en) * | 2011-07-01 | 2012-05-23 | 华东理工大学 | Green and energy-saving fluorescent powder/glass compound luminous material and preparation method thereof |
| CN102745893A (en) * | 2012-06-20 | 2012-10-24 | 武汉理工大学 | Composite phosphor luminescent glass and preparation method for same |
| CN103043908A (en) * | 2013-01-11 | 2013-04-17 | 华南师范大学 | Novel fluorescent glass and preparation method thereof |
| CN103539359A (en) * | 2013-09-27 | 2014-01-29 | 南京邮电大学 | Rare earth doped fluoride micro-nano crystal-fluorophosphate glass composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111253073A (en) * | 2020-01-21 | 2020-06-09 | 徐州凹凸光电科技有限公司 | Method for preparing gadolinium-aluminum-garnet-based white-light glass ceramic by adopting sol-gel method |
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