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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- 239000011521 glass Substances 0.000 title claims abstract description 122
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 36
- 238000002844 melting Methods 0.000 claims abstract description 27
- 239000002223 garnet Substances 0.000 claims abstract description 16
- 230000008018 melting Effects 0.000 claims abstract description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000010304 firing Methods 0.000 claims abstract description 7
- 239000004615 ingredient Substances 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 8
- 239000011787 zinc oxide Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 241001460678 Napo <wasp> Species 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 230000005496 eutectics Effects 0.000 claims description 2
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 239000011775 sodium fluoride Substances 0.000 claims description 2
- 235000013024 sodium fluoride Nutrition 0.000 claims description 2
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 2
- 229910000410 antimony oxide Inorganic materials 0.000 claims 1
- 239000000428 dust Substances 0.000 claims 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 abstract description 2
- 238000003754 machining Methods 0.000 abstract description 2
- 238000011017 operating method Methods 0.000 abstract description 2
- 238000005457 optimization Methods 0.000 abstract 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 15
- 239000011159 matrix material Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 6
- 238000003801 milling Methods 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 229910003069 TeO2 Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 241000219991 Lythraceae Species 0.000 description 1
- 235000014360 Punica granatum Nutrition 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
- Glass Compositions (AREA)
- Led Device Packages (AREA)
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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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 |
Citations (6)
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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 |
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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Patent Citations (6)
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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 |
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 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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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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