CN105198224A - Ce:YAG glass ceramic as well as preparation method and application thereof - Google Patents
Ce:YAG glass ceramic as well as preparation method and application thereof Download PDFInfo
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- CN105198224A CN105198224A CN201510571101.9A CN201510571101A CN105198224A CN 105198224 A CN105198224 A CN 105198224A CN 201510571101 A CN201510571101 A CN 201510571101A CN 105198224 A CN105198224 A CN 105198224A
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Abstract
The invention discloses Ce:YAG glass ceramic as well as a preparation method and an application thereof. The Ce:YAG glass ceramic is prepared by active ingredients SiO2, B2O3, PbO, ZnO and Ce: YAG fluorescent powder, and on the basis of the SiO2, B2O3, PbO and ZnO, the content of each active ingredient is as follows (by molar fraction or mass fraction): 2 to 20 percent of SiO2, 10 to 35 percent of B2O3, 20 to 50 percent of PbO, 5 to 15 percent of ZnO and 2 to 10 percent of Ce:YAG fluorescent powder. According to the prepared Ce: YAG glass ceramic, the Ce: YAG microcrystal particles are uniformly distributed in the glass, so that the Ce:YAG glass ceramic has advantages of high transparency, low cost, excellent optical performance and the like. The invention also provides an application of the Ce:YAG glass ceramic in preparing a white-light LED (light emitting diode) device. By adopting the Ce:YAG glass ceramic, the sealing structure of the white-light LED device can be optimized, the process is simplified, and the lighting effect is improved.
Description
(1) technical field
The present invention relates to a kind of Ce:YAG devitrified glass and preparation method thereof and the application in white light LEDs, belong to LED fluorescent material technical field.
(2) background technology
White light LEDs has that volume is little, thermal value is low, current consumption is little, the life-span is long, speed of response is fast, environmental protection, planar package, easy exploiting can become the advantages such as frivolous small and exquisite product, be described as by surmount incandescent light, luminescent lamp " forth generation lighting source ", application prospect is very wide.At present, white-light LED fluorescence material is mainly based on amorphous fluorescent material, and commercialization white light LEDs product forms white light for Developing mainstream with chip and phosphor combination, and fluorescent material to be mixed in epoxy resin and to be coated on InGaN chip.Its principle of work is by blue light for InGaN chip and phosphor combination (or other array mode), the blue light components that InGaN chip sends is absorbed by fluorescent material, it is made to be excited to send gold-tinted, and the yellow light mix that unabsorbed blue light and fluorescent material send, just produce white light.But, due to epoxy resin thermal conductivity and chemical stability poor, easily aging, yellow is there is under the hot environment that high-power die is irradiated, cause LED colour cast, in addition, the specific refractory power (n=1.45-1.55) that the specific refractory power (n=1.83) that Ce:YAG microcrystal grain is high is low with epoxy resin/silica gel is not mated, and light scattering loss will be caused higher lower with light extraction efficiency, the work-ing life of serious curtailment LED component.Therefore, high, the chemically stable novel solid luminescent material of research and development thermal conductivity is the up-to-date direction developing White light LED technology in the world.
Devitrified glass (being also called glass-ceramic), by the parent glass of specific composition, a class obtained by controlling crystallizing in heat-processed contains the polycrystalline solids material of a large amount of crystallite phase and glassy phase, it combines the advantage of crystal and glass material, existing glass material preparation method is simple, thermostability and the high advantage of chemical stability, there is again the polycrystalline feature of pottery, compared with epoxy resin, its thermal conductivity is much bigger, become the type material of a class uniqueness, in addition, devitrified glass is also easily processed into tabular or hollow bulb-shaped directly overlays on chip, therefore, can be used for substituting conventional fluorescent material and build novel white-light LED (avoiding using epoxy resin or silica gel).Compared with conventional LED device, this new device has the remarkable advantage of photochromic stable, long service life.
And the common method preparing devitrified glass has two kinds: one first forms forerunner's glass to heat-treat again, from glass basis, crystallization separates out crystallite; Another kind directly Ce:YAG fluorescent material and low melting glass mixing low temp co-sintering is formed devitrified glass.
Adopt first method Application and preparation in the patent of the devitrified glass of white light LEDs, as:
Wenzhou University is to the Chinese invention patent CN102040337B of people's applications such as Wei Dong, " rare-earth-dopping yttrium aluminum garnet microcrystal glass material and the application in white light LEDs thereof ", in this patent, crystalline phase contained by devitrified glass is Ce:YAG, simultaneously, this microcrystal glass material has the outstanding advantages such as excitation-emission efficiency is high, physical and chemical performance stable, thermal conductivity is high, is applied to white light LEDs.
The PCT publication number of Nippon Electric Glass Co., Ltd and Kyoto University's co-applications is the patent " fluorescent substance and LED " of WO2005/097938A1, also the devitrified glass containing Ce:YAG crystalline phase is disclosed in this patent, but because glass basis component is mainly sieve and silica-sesquioxide, material transparent is poor, the reasons such as the high temperature crystallization crystallite lattice imperfection (rise optical quenching central role) of separating out is more, cause its luminous efficiency not high (see SetsuhisaTanabeetal, " YAGglass-ceramicphosphorforwhiteLED (II): luminescencecharacteristics ", ProcofSPIE, 2005, Vol.5941, 594112).
And adopt second method Application and preparation in the patent of the devitrified glass of white light LEDs, as:
The Chinese invention patent CN101643315B of Wuhan University of Technology's application, " low-melting-point fluorescent glass for white light LED and preparation method thereof ", discloses the preparation method of the low-melting-point fluorescent glass containing Ce:YAG crystalline phase in this patent, glass basis component is SiO
2-Al
2o
3-B
2o
3-CaO-ZnO-Na
2o-MgO.This material transparent is poor, and luminescent properties is also bad.
The Chinese invention patent CN103183473A that Chinese Academy of Sciences's Fujian thing structure is applied for, " the Ce:YAG devitrified glass and preparation method thereof for white light LEDs ", which discloses the method preparing Ce:YAG fluorescent glass.By by commercial micron order Ce:YAG fluorescent material and the mode of low melting glass mixing congruent melting, realize the controlled synthesis of fluorescent glass material.The low-melting-point fluorescent glass of this invention sends bright gold-tinted under 465nm is blue-light excited, and its maximum quantum efficiency can reach 94%, can produce white light emission after itself and commercial blue chip being combined.
In brief, the disclosed patent of invention for the devitrified glass being applied to white light LEDs has both at home and abroad so far, but it is unreasonable mainly due to Material composition design, the specific refractory power that the specific refractory power that Ce:YAG microcrystal grain is high is low with host glass is not mated, cause the transparency of devitrified glass low, poor optical properties; Meanwhile, preparation technology's more complicated of devitrified glass, glass melting temperature is higher, and energy consumption is larger.
The present invention proposes a kind of based on the Ce:YAG devitrified glass and preparation method thereof of new component formula for white light LEDs, and the method preparation technology is simple, less energy consumption, cost are low, with short production cycle.This low melting point Ce:YAG devitrified glass is packaged into white light LED part, and photoelectric properties are good, and under 20mA drive current, luminous efficiency is up to 133.34lm/W.
(3) summary of the invention
Technical problem to be solved by this invention is to provide a kind of Ce:YAG devitrified glass and preparation method thereof and the application in white light LEDs, the preparation method of described Ce:YAG devitrified glass achieves the requirement that preparation technology is simple, less energy consumption, cost are low, be easy to mass production, this Ce:YAG devitrified glass fusing point is low, excellent in optical properties, transparency are high, bright gold-tinted is sent under 460nm is blue-light excited, be applied to white light LEDs, White-light LED package structure can be optimized, reduce costs, improve white light LEDs light efficiency.
The present invention's adopted technical scheme that solves the problem is as follows:
A kind of Ce:YAG devitrified glass, it is by effective material SiO
2, B
2o
3, PbO, ZnO and Ce:YAG fluorescent material prepares, based on SiO
2, B
2o
3, PbO and ZnO, the content of each effective material is expressed as follows with molar fraction or massfraction: SiO
22-10mol%, B
2o
310-35mol%; PbO20-50mol%, ZnO5-15mol%, Ce:YAG fluorescent material 2 ~ 10wt%.
Further, SiO
2content is preferably 4-10mol%, is more preferably 5-8mol%.
Further, B
2o
3content is preferably 20-35mol%, is more preferably 30-35mol%.
Further, PbO content is preferably 30-50mol%, is more preferably 40-50mol%.
Further, ZnO content is preferably 10-15mol%, is more preferably 10-13mol%.
Further, Ce:YAG fluorescent material content is preferably 4 ~ 10wt%, is more preferably 4 ~ 7wt%.
Further, described effective material B
2o
3with H
3bO
3form add, all the other raw materials all add with above-mentioned oxide form.
The invention provides the preparation method of described Ce:YAG devitrified glass, by after all raw materials are carried out proportioning weighing by certain molar fraction, mixed grinding, and then prepared by a step sintering synthesis method, its preparation method specifically comprises frit mixing, frit melted and cooling process three steps:
(1) frit mixing: by raw material SiO
2, H
3bO
3, after PbO, ZnO, Ce:YAG fluorescent material weighs by a certain percentage, be then placed in mortar and fully mix, grind, then pour in corundum crucible;
(2) frit melted: to be inserted in retort furnace by glass mixture and sinter, the temperature arranging retort furnace is 600-800 DEG C, obtains melten glass material after insulation 1-4h;
(3) frit cooling: melten glass material being poured into temperature is on the pig mold of 300-500 DEG C, then be placed in retort furnace to carry out annealing to eliminate internal stress, in glass transformation temperature Tg temperature 2-4h, then naturally cool to 20 DEG C with stove, prepare Ce:YAG devitrified glass.
The transition temperature Tg of Ce:YAG devitrified glass of the present invention can be low to moderate about 350 DEG C.
The shape of the Ce:YAG devitrified glass prepared by the present invention can be plane, concave surface, convex surface, and can carry out, cut, grind, polishing.
Present invention also offers the application of described Ce:YAG devitrified glass in white light LED part preparation, the encapsulating structure of white light LED part can be optimized, Simplified flowsheet, improve light efficiency.
Compared with prior art, beneficial effect of the present invention is:
(1) the present invention passes through with PbO-B
2o
3-SiO
2-ZnO, as host glass system, adjusts PbO/SiO
2molar ratio, glass is mated mutually with the specific refractory power of fluorescent material, and meanwhile, the melt temperature that ZnO effectively can reduce glass at high temperature decomposes sex change, B to prevent Ce:YAG fluorescent material
2o
3as glass network control agent, SiO
2as glass-former, be conducive to obtain fusing point low, transparency is high, the Ce:YAG devitrified glass of excellent in optical properties;
(2) preparation method of Ce:YAG devitrified glass in the present invention, do not need the host glass first preparing low melting point, more do not need to sinter mixing with fluorescent material after host glass pulverizing, its glass transition temp is low again, thus preparation technology can be simplified, effective save energy.
(3) the Ce:YAG devitrified glass obtained by the present invention, Ce:YAG microcrystal grain is evenly distributed in glass, has the advantages such as transparency is high, cost is low, excellent in optical properties.
(4) accompanying drawing explanation
Fig. 1 is the pictorial diagram of the Ce:YAG devitrified glass of embodiment 1.
Fig. 2 is the Ce:YAG fluorescent material of embodiment 1 and the XRD figure spectrum of Ce:YAG devitrified glass.
Fig. 3 is the exciting light spectrogram of the Ce:YAG devitrified glass of embodiment 1.
Fig. 4 is the utilizing emitted light spectrogram of the Ce:YAG devitrified glass of embodiment 1.
Fig. 5 is the utilizing emitted light spectrogram of the Ce:YAG devitrified glass of embodiment 2.
Fig. 6 is the utilizing emitted light spectrogram of the Ce:YAG devitrified glass of embodiment 3.
Fig. 7 is the luminous photo of sample after the Ce:YAG devitrified glass wafer of embodiment 2 is coupled with blue chip.
(5) embodiment
With specific embodiment, technical scheme of the present invention is described further below, but protection scope of the present invention is not limited thereto:
Embodiment 1:
By analytically pure SiO
2, H
3bO
3, PbO, ZnO, Ce:YAG fluorescent material, by 8mol%SiO
2, 35mol%B
2o
3, 46mol%PbO, 11mol%ZnO, 5wt%Ce:YAG fluorescent material proportioning accurate weighing be placed in agate mortar, in agate mortar, mixed grinding is evenly placed in corundum crucible, then put into after resistance furnace is heated to 650 DEG C and be incubated 1h, then, being taken out and pour temperature fast into by glass melt is on the pig mold of 400 DEG C, annealing with being placed in retort furnace, in 350 DEG C of insulation 2h, finally cooling to 20 DEG C with the furnace and forming transparent Ce:YAG devitrified glass.
Thing phase and spectral quality test are carried out to the transparent Ce:YAG devitrified glass of preparation, its XRD figure as shown in Figure 2, the XRD diffraction peak of fluorescent glass sample all conforms to the main diffraction peak of the standard card of YAG crystalline phase, illustrates that Ce:YAG powder has been dispersed in glass medium, without other impurity phase; And the fluorescent glass emmission spectrum excited by 460nm wavelength as shown in Figure 3, emission peak wavelength is positioned at 538nm.Fluorescent glass is coupled with 460nm blue chip, bright white light can be sent down blue-light excited.Under the electric current of 20mA excites, luminous efficiency can reach 126lm/W.
Embodiment 2:
By analytically pure SiO
2, H
3bO
3, PbO, ZnO, Ce:YAG fluorescent material, by 7mol%SiO
2, 35mol%B
2o
3, 47mol%PbO, 11mol%ZnO, 5wt%Ce:YAG fluorescent material proportioning accurate weighing be placed in agate mortar, in agate mortar, mixed grinding is evenly placed in corundum crucible, then put into after resistance furnace is heated to 700 DEG C and be incubated 1h, then, being taken out and pour temperature fast into by glass melt is on the pig mold of 400 DEG C, annealing with being placed in retort furnace, in 350 DEG C of insulation 2h, finally cooling to 20 DEG C with the furnace and forming transparent Ce:YAG devitrified glass.
Transparent Ce:YAG devitrified glass is coupled with 460nm blue chip, bright white light can be sent down blue-light excited.Excited by 460nm wavelength, emission peak wavelength is positioned at 538nm, and under the electric current of 20mA excites, luminous efficiency can reach 133lm/W.
Embodiment 3:
By analytically pure SiO
2, H
3bO
3, PbO, ZnO, Ce:YAG fluorescent material, by 6mol%SiO
2, 35mol%B
2o
3, 48mol%PbO, 11mol%ZnO, 5wt%Ce:YAG fluorescent material proportioning accurate weighing be placed in agate mortar, in agate mortar, mixed grinding is evenly placed in corundum crucible, then put into after resistance furnace is heated to 750 DEG C and be incubated 1h, then, being taken out and pour temperature fast into by glass melt is on the pig mold of 400 DEG C, annealing with being placed in retort furnace, in 350 DEG C of insulation 2h, finally cooling to 20 DEG C with the furnace and forming transparent Ce:YAG devitrified glass.
Transparent Ce:YAG devitrified glass is coupled with 460nm blue chip, bright white light can be sent down blue-light excited.Excited by 460nm wavelength, emission peak wavelength is positioned at 538nm, and under the electric current of 20mA excites, luminous efficiency can reach 124lm/W.
Claims (6)
1. a Ce:YAG devitrified glass, it is by effective material SiO
2, B
2o
3, PbO, ZnO and Ce:YAG fluorescent material prepares, based on SiO
2, B
2o
3, PbO and ZnO, the content of each effective material is expressed as follows with molar fraction or massfraction: SiO
22-10mol%, B
2o
310-35mol%; PbO20-50mol%, ZnO5-15mol%, Ce:YAG fluorescent material 2 ~ 10wt%.
2. Ce:YAG devitrified glass as claimed in claim 1, is characterized in that: the content of each effective material is expressed as follows with molar fraction or massfraction: SiO
24-10mol%, B
2o
320-35mol%; PbO30-50mol%, ZnO10-15mol%, Ce:YAG fluorescent material 4 ~ 10wt%.
3. Ce:YAG devitrified glass as claimed in claim 1, is characterized in that: the content of each effective material is expressed as follows with molar fraction or massfraction: SiO
25-8mol%, B
2o
330-35mol%; PbO40-50mol%, ZnO10-13mol%, Ce:YAG fluorescent material 4 ~ 7wt%.
4. the Ce:YAG devitrified glass as described in one of claims 1 to 3, is characterized in that: described effective material B
2o
3with H
3bO
3form add.
5. a preparation method for Ce:YAG devitrified glass as claimed in claim 1, specifically comprises frit mixing, frit melted and cooling process three steps:
(1) frit mixing: by raw material SiO
2, H
3bO
3, after PbO, ZnO, Ce:YAG fluorescent material weighs by a certain percentage, be then placed in mortar and fully mix, grind, then pour in corundum crucible;
(2) frit melted: to be inserted in retort furnace by glass mixture and sinter, the temperature arranging retort furnace is 600-800 DEG C, obtains melten glass material after insulation 1-4h;
(3) frit cooling: melten glass material being poured into temperature is on the pig mold of 300-500 DEG C, then be placed in retort furnace to carry out annealing to eliminate internal stress, in glass transformation temperature Tg temperature 2-4h, then naturally cool to 20 DEG C with stove, prepare Ce:YAG devitrified glass.
6. the application of Ce:YAG devitrified glass as claimed in claim 1 in white light LED part preparation.
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CN104556703A (en) * | 2015-01-04 | 2015-04-29 | 华东理工大学 | Preparation method for lead oxide-doped yttrium aluminum garnet glass ceramic for white light LED |
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CN110156326B (en) * | 2018-02-11 | 2021-11-26 | 天津理工大学 | Fluorescent glass ceramic based on low-melting-point glass powder and preparation method thereof |
CN109111120A (en) * | 2018-10-26 | 2019-01-01 | 浙江工业大学 | A kind of warm white LED is with can spontaneous crystallization fluorescent glass-ceramics and preparation method thereof |
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CN109516694B (en) * | 2018-11-07 | 2021-11-30 | 深圳市齐尚光科技有限公司 | Fluorescent glass, preparation method thereof and light-emitting device |
CN110117160A (en) * | 2019-05-10 | 2019-08-13 | 福建江夏学院 | A kind of devitrified glass and its preparation method and application |
CN110117160B (en) * | 2019-05-10 | 2021-12-07 | 福建江夏学院 | Microcrystalline glass and preparation method and application thereof |
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CN112979169A (en) * | 2020-10-14 | 2021-06-18 | 温州大学 | One kind of Ce: YAGG composite glass material and preparation and application thereof |
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