CN103964834A - Composite fluorescent transparent ceramic used for white-light LED and adopting garnet structure - Google Patents

Composite fluorescent transparent ceramic used for white-light LED and adopting garnet structure Download PDF

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CN103964834A
CN103964834A CN201410055010.5A CN201410055010A CN103964834A CN 103964834 A CN103964834 A CN 103964834A CN 201410055010 A CN201410055010 A CN 201410055010A CN 103964834 A CN103964834 A CN 103964834A
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composite
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white light
ceramics
transparent ceramic
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张红卫
陈剑
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Abstract

The invention relates to the field of transparent fluorescent ceramics of LEDs, and discloses a composite fluorescent transparent ceramic used for a white-light LED and adopting a garnet structure. The composite fluorescent transparent ceramic is prepared through tape casting and vacuum sintering; and the chemical composition of the transparent ceramic comprises N transparent ceramic phosphors or non-phosphor components with different LED light emitting properties, wherein N is larger than or equal to 2. The prepared composite fluorescent transparent ceramic is simple in structure, the packaging process is simplified, the white-light LED has high luminous efficacy, high color rendering index, high quantum efficiency and excellent temperature quenching performance, and the composite fluorescent transparent ceramic can be used for packaging various white-light LED devices.

Description

A kind of composite fluorescence crystalline ceramics body of the garnet type structure for white light LEDs
Technical field
The present invention relates to LED transparent fluorescent ceramic field, particularly relate to a kind of for high light efficiency white light LEDs composite transparent fluorescence ceramics structure.
Background technology
White light LEDs has Small Solid, and instantaneous starting and fast-response (μ s) are energy-conservation, life-span is long, and many advantages such as green high-efficient, are widely used in various buildings and Landscape Lighting, automotive lighting, medical and various portable lightings etc., developed into the 4th generation new lighting source.The white light LEDs technology use the most at present, technology being the most ripe is that GaN base blue chip adds yellow fluorescent powder (cerium-doped yttrium aluminum garnet, Ce:Y 3al 5o 12) technology, it is to excite blue light by GaN chip, the blue-light excited Ce:Y of part 3al 5o 12fluorescent material produces gold-tinted, and gold-tinted and remaining blue light form white light.
White light LEDs is fluorescent material and resin or silica gel to be mixed after forming phosphor gel to be bonded on chip in when encapsulation.Yet this type of LED is encapsulated in research process, exist an outstanding problem: poor heat stability.Resinous material long-term exposure is under hot environment or uv irradiation, and transparency degradation, produces serious aging, has greatly shortened the life-span of white light LEDs; Although the performance of silica gel is better than resin, along with temperature raises, silica gel built-in thermal stress strengthens, and causes specific refractory power to reduce, and affects light efficiency and the light distribution of LED; The quantum yield of fluorescent material can reduce due to temperature quenching effect, and higher temperature also can be accelerated the aging of fluorescent material.
Adopt Ce:YAG transparent fluorescent ceramic to substitute " Ce:YAG fluorescent material+silica gel ", can effectively address the above problem.Fluorescence crystalline ceramics good heat conductivity, not only can resist light decay, reduces scattering of light, can also improve the stability of brightness and spectrum.At present, the well-known mechanism such as Philip Luminleds company, Kyoto Univ Japan is all being engaged in the research of this respect in the world.Yet ceramic fluorescent material also exists some shortcomings.In fluorescence spectrum in Ce:YAG, lack ruddiness composition, make the white light colour temperature that obtains after mixing with GaN blue chip higher, the disappearance of ruddiness also makes the colour rendering index of LED lower.Address this problem, can make Ce by doped rare earth element in fluorescence ceramics material 3+the emission peak of emission peak red shift or introducing red spectral band improves.But the new problem that the fluorescence ceramics materials of many doping bring out is that interaction between different dopant ions, energy transfer etc. are comparatively complicated, and luminous efficiency is had to negative impact.Composite fluorescence crystalline ceramics can solve this problem, and the rare earth ion between its different piece can not influence each other.
CN102531564A, CN102501478A, CN102249660A all discloses a kind of white LEDs composite transparent ceramic and preparation method thereof, this composite structure fluorescence ceramics is to consist of by side is bonding upper strata crystalline ceramics and lower floor's crystalline ceramics, described composite transparent ceramic be Ce:YAG ceramic plate respectively with Eu3+, Pr3+, compound the obtaining of YAG of Cr3+ doping.By the doping of different rare earths, increased ruddiness composition in LED spectrum, improved colour rendering index and gentle colour temperature.The problem that exists of this kind of method be: upper and lower two-layer ceramic sheet exists certain thickness air casing between interface, causes the to a certain degree loss of amount of light, and luminous efficiency is reduced.
Summary of the invention
The object of the present invention is to provide for high light efficiency white light LEDs composite transparent fluorescence ceramics structure, to overcome the deficiencies in the prior art, obtain the white light LEDs of high light efficiency, high color rendering index (CRI), high-quantum efficiency and good temperature cancellation performance.
The preparation method of transparent fluorescent ceramic structure of the present invention, comprises that raw material weighing, ball milling are mixed, sieve powder, dry-pressing formed, cold isostatic compaction, degreasing, vacuum sintering, anneal, plane lapping, polishing, and each technological process is characterised in that:
(1) raw material weighing:
By (Ce xy 1-x-kre k) 3al 5o 12stoichiometric ratio weigh commercially available purity at more than 99.9% Y2O3 powder, Al 2o 3powder, CeO 2powder, Re 2o 3powder, and add a certain amount of sintering aid, binding agent, softening agent, dispersion agent; Wherein, 0≤x≤0.05,0≤k≤1, Re is Lu 3+, La 3+, Gd 3+, Pr 3+, Sm 3+, Eu 3+in a kind of.
(2) ball milling hybrid technique:
Adopt planetary ball mill to mix 2～48 hours.Ball-milling medium is comprised of liquid medium and abrading-ball, and liquid medium is deionized water or alcohols, or the liquid being mixed by a certain percentage by both; Abrading-ball adopts a kind of in alumina balls, agate ball, ball grinder to adopt a kind of in oxidation aluminium pot, agate tank.Raw material: ball: mass ratio=1 of liquid medium: (2～5): (0.5～3).Drum's speed of rotation is 200～500rpm.
(3) casting molding processes:
1. by the slurry mixing de-bubble 10～60min in defoaming machine, wherein powder solid content is 50%～70%, the fluorescence ceramics powder of N kind (N >=2) different chemical component injects successively casting machine and carries out curtain coating, the cast layer thickness obtaining is 0.1mm～2.0mm, it is 1～20 layer that the cast layer of chemical composition of the same race is used the number of plies, and the order that stacks of the cast layer of different chemical component is not limit; How much patterns of cast layer comprise circle, square, rhombus, trilateral, Polygons etc.The cast layer of several different chemical components is stacked into compound cast sheet, is positioned over dry pressing die set and is incubated 5h～12h at 110 ℃～150 ℃ temperature;
2. the axial unidirectional pressuring method adopting in dry-pressing process, pressure is 15～40Mpa, the dwell time is 0.5～5min;
3. the biscuit after dry-pressing is after vacuum packaging, cold isostatic compaction under the pressure of 150～300Mpa, and the dwell time is 1～10min;
(4) degreasing process: pack crucible and sample into vacuum oven, adopt 0.1～10 ℃/min to be warmed up to the organic decomposition temperature of interpolation, insulation for some time, size per sample and organic kind and molecular weight determine soaking time; Utilize vacuum atmosphere or oxygen atmosphere to carry out binder removal.(5) vacuum sintering, annealing process:
Biscuit after degreasing is put into vacuum oven and is carried out sintering, 1500～1900 ℃ of sintering ranges, and size per sample, sintering time is 0.5～120 hour.After sintering under 1100～1500 ℃ of oxygen atmospheres anneal.
(6) finally the transparent fluorescent ceramic of vacuum sintering is carried out to plane lapping and polished finish.
According to technique of the present invention, can prepare the white light LEDs transparent fluorescent ceramic of high light efficiency, high color rendering index (CRI), high-quantum efficiency and good temperature cancellation performance.
Accompanying drawing explanation
Fig. 1 is the structural representation of composite transparent fluorescence ceramics of the present invention
Fig. 2 is the transmitance figure of embodiment 4 composite transparent fluorescence ceramics
Fig. 3 is the spectrogram of embodiment 4 composite transparent fluorescence ceramics
Embodiment
Below in conjunction with example, the invention will be further described, but should not limit the scope of the invention with this.
As shown in Figure 1, this composite transparent fluorescence ceramics is divided into two or more parts to the structure of composite transparent fluorescence ceramics of the present invention, and in figure, the chemical constitution of composite transparent fluorescence ceramics body different piece is (Ce xy 1-x-kre k) 3al 5o 12, wherein, 0≤x≤0.03,0≤k≤0.2, Re is Lu 3+, La 3+, Gd 3+, Pr 3+, Sm 3+, Eu 3+in a kind of.This composite transparent fluorescence ceramics is by flow casting molding, and vacuum sintering prepares.
Embodiment 1:
By (Ce 0.1%y 99.9%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, CeO 2powder raw material, another by (Ce 0.1%sm 0.2%y 99.7%) 3al 5o 12chemical constitution weighs CeO 2powder, α-Al 2o 3powder, Y 2o 3powder, Sm 2o 3powder.Two class mixed powders all add the TEOS of 0.1200g, the PVB of 0.5400g puts into high-purity agate jar, adds high-purity agate ball of 80g, dehydrated alcohol 12g, after ball milling 20h, pour successively de-bubble 20min in defoaming machine into, then by casting machine curtain coating, obtain the cast layer of 600 microns.By (the Ce preparing 0.1%sm 0.2%y 99.7%) 3al 5o 12(Ce 0.1%y 99.9%) 3al 5o 12each ten layers of composite ceramics cast layer that is stacked into 20 layers of cast layer, pack 110 ℃ of insulation 10h in dry pressing die set into, force together not stratified whole composite ceramics powder agglomates, isostatic cool pressing under 200Mpa with forcing spindle unidirectional adding of 20Mpa.By the sintered sample in a vacuum of the biscuit after degreasing, temperature rise rate is: 10 ℃/min, sintering temperature is 1800 ℃, sintering time 15h.After polishing, obtaining thickness of sample is 2.20mm, and wherein upper and lower two portions thickness is 1.10mm.Visible light transmissivity can reach 83%.
The prepared crystalline ceramics white light LEDs of the present embodiment is under 20mA constant-current driving, and 450nm blue chip excites the LED that obtains inclined to one side gold-tinted.Its performance index are as follows:
Light efficiency: 181lm/W
Quantum yield: 94.6%
Colour rendering index: 71
Colour temperature: 6500K.
Embodiment 2:
Get (Ce 0.1%y 99.9%) 3al 5o 12six layers of cast layer, (Ce 0.1%sm 0.2%y 99.7%) 3al 5o 12six layers of parts, after polishing, obtaining thickness of sample is 1.30mm, wherein (Ce 0.1%y 99.9%) 3al 5o 12segment thickness is 0.65mm, (Ce 0.1%sm 0.2%y 99.7%) 3al 5o 12segment thickness is 0.65mm.Other condition, with embodiment 1, obtains composite transparent fluorescence ceramics, and its visible light transmissivity is 83.2%.
The prepared crystalline ceramics white light LEDs of the present embodiment is under 20mA constant-current driving, and 450nm blue chip excites the LED that obtains white light, and its performance index are as follows:
Light efficiency: 135lm/W
Quantum yield: 95.2%
Colour rendering index: 79
Colour temperature: 5700K.
Embodiment 3:
By (Ce 0.1%y 99.9%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, CeO 2powder raw material, another by (Ce 0.1%gd 5%y 94.9%) 3al 5o 12chemical constitution weighs CeO 2powder, α-Al 2o 3powder, Y 2o 3powder, Gd 2o 3powder.Sintering temperature is 1825 ℃, soaking time 25h, and other condition, with embodiment 2, obtains composite transparent fluorescence ceramics, and its visible light transmissivity is 82.7%.
The prepared crystalline ceramics white light LEDs of the present embodiment is under 20mA constant-current driving, and 450nm blue chip excites the LED that obtains white light, and its performance index are as follows:
Light efficiency: 134lm/W
Quantum yield: 94.9%
Colour rendering index: 80
Colour temperature: 5600K.
Embodiment 4:
By (Ce 0.1%y 89.9%gd 5%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, CeO 2powder, Gd 4o 7powder raw material, another by (Ce 0.1%pr 0.2%y 99.7%) 3al 5o 12chemical constitution weighs CeO 2powder, α-Al 2o 3powder, Y 2o 3powder, Pr 6o 11powder.Other condition, with embodiment 2, obtains composite transparent fluorescence ceramics,
Its visible light transmissivity is 833%.
The prepared crystalline ceramics white light LEDs of the present embodiment is under 20mA constant-current driving, and 450nm blue chip excites the LED that obtains white light, and as shown in the figure, its performance index are as follows for its spectral power distribution figure:
Light efficiency: 138lm/W
Quantum yield: 96.0%
Colour rendering index: 86
Colour temperature: 4500K.
Embodiment 5:
By (Ce 0.1%y 99.9%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, CeO 2powder raw material, by (Ce 0.1%y 89.9%gd 5%) 3al 5o 12chemical constitution weighs α-Al 2o 3powder, Y 2o 3powder, CeO 2powder, Gd 4o 7powder raw material, another by (Ce 0.1%pr 0.2%y 99.7%) 3al 5o 12chemical constitution weighs CeO 2powder, α-Al 2o 3powder, Y 2o 3powder, Pr 6o 11powder.Other condition, with embodiment 2, obtains the composite transparent fluorescence ceramics of three kinds of chemical constitutions, and its visible light transmissivity is 83.3%.
The prepared crystalline ceramics white light LEDs of the present embodiment is under 20mA constant-current driving, and 450nm blue chip excites the LED that obtains white light, and its performance index are as follows:
Light efficiency: 131lm/W
Quantum yield: 94.0%
Colour rendering index: 84
Colour temperature: 4000K.

Claims (7)

1. for high light efficiency white light LEDs composite transparent fluorescence ceramics, prepare for one kind, comprise the steps:
1) by (Ce xy 1-xre k) 3Al 5o 12the stoichiometric ratio of (0≤x≤0.05,0≤k≤1) weighs more than 99.9% Y of commercially available purity 2o 3powder, Al 2o 3powder, CeO 2powder, Re 2o 3powder, and add a certain amount of sintering aid, binding agent, softening agent, dispersion agent;
2) by step 1) described powder and additive ball milling in planetary ball mill;
3) by step 2) the described slurry froth in vacuum mixing, different chemical component slurry injects successively casting machine and carries out flow casting molding;
4) by step 3) described several different chemical components, the cast layer of different thickness are stacked into compound cast sheet, and be placed in the Bidirectional-pressure mould of heating and be incubated several minutes;
5) by step 4) described compound cast sheet forces together with dry-pressing formed machine is dry the compound curtain coating biscuit that there is no demixing phenomenon, then the static pressure 100-200MPa moulding composite ceramics biscuit such as pass through;
6) by step 5) the composite ceramics biscuit of described moulding carries out degreasing;
7) last, by step 6) described composite ceramics biscuit carries out vacuum sintering, anneal, obtains target product.
2. by claimed in claim 1 for high light efficiency white light LEDs composite transparent fluorescence ceramics preparation method, it is characterized in that: described Re 2o 3powder raw material adopts Gd 4o 7, La 2o 3, Pr 6o 11, Sm 2o 3, Eu 2o 3, Lu 2o 3in one or several rare earth powders.
3. by claimed in claim 1 for high light efficiency white light LEDs composite transparent fluorescence ceramics preparation method, it is characterized in that: the curtain coating thin layer of composite fluorescence crystalline ceramics is obtained through flow casting molding by the slurry of N kind (N >=2) different chemical component.
4. by claimed in claim 1, for high light efficiency white light LEDs composite transparent fluorescence ceramics preparation method, it is characterized in that: the curtain coating number of plies of chemical composition of the same race is 1～20 layer, can comprise pure YAG ceramic layer, the order that stacks of cast layer is not limit.
5. by claimed in claim 1 for high light efficiency white light LEDs composite transparent fluorescence ceramics preparation method, it is characterized in that: according to design needs, prepare how much patterns of cast layer that composite fluorescence crystalline ceramics uses and comprise circle, square, rhombus, trilateral, Polygons different shapes.
6. by claimed in claim 1 for high light efficiency white light LEDs composite transparent fluorescence ceramics preparation method, it is characterized in that: thoroughly do away with design needs, in N kind cast layer material (N >=2), can comprise non-fluorescent material, as pure YAG stupalith.
7. by claimed in claim 1 for high light efficiency white light LEDs composite transparent fluorescence ceramics preparation method, it is characterized in that: prepared transparent fluorescent ceramic package white light LEDs, under 20mA constant-current driving, 450nm blue chip excites the LED that obtains white light, its performance index can reach light efficiency: 1381m/W, quantum yield: 96.0%, colour rendering index: 86, colour temperature: 4500K.
CN201410055010.5A 2014-02-18 2014-02-18 Composite fluorescent transparent ceramic used for white-light LED and adopting garnet structure Pending CN103964834A (en)

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CN104725052A (en) * 2014-12-18 2015-06-24 徐州市江苏师范大学激光科技有限公司 Preparation method of multilayer composite structured transparent ceramic
CN104803670A (en) * 2015-04-10 2015-07-29 中国科学院宁波材料技术与工程研究所 Scintillation ceramic for double-layer detector and preparation method of scintillation ceramic
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WO2018097003A1 (en) * 2016-11-25 2018-05-31 大電株式会社 Fluorescent substance for vacuum ultraviolet excitation, luminescent element, and light-emitting device
CN109336582A (en) * 2018-09-30 2019-02-15 汪阳 A kind of composite construction fluorescence ceramics and preparation method thereof for white light LEDs
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CN109896853A (en) * 2017-12-11 2019-06-18 上海航空电器有限公司 With more low-expansion ceramic composite, preparation method and light supply apparatus
CN111018512A (en) * 2019-12-30 2020-04-17 江苏师范大学 Preparation method of high-luminous-efficiency and high-color-rendering-index fluorescent ceramic with gradient refractive index structure
CN111393166A (en) * 2020-03-27 2020-07-10 徐州凹凸光电科技有限公司 High-thermal-stability fluorescent ceramic for white light L ED/L D and preparation method thereof
CN112094110A (en) * 2020-10-15 2020-12-18 贵州赛义光电科技有限公司 Al (aluminum)2O3-YAG:Ce3+Preparation method of complex phase fluorescent ceramic
CN113024252A (en) * 2019-12-09 2021-06-25 上海航空电器有限公司 Hierarchical pore structure ceramic phosphor for white light laser illumination and preparation method thereof
CN113979739A (en) * 2021-10-27 2022-01-28 中国科学院上海硅酸盐研究所 Composite fluorescent ceramic, preparation method and luminescent device
CN114477989A (en) * 2020-11-11 2022-05-13 中国科学院福建物质结构研究所 Graphene-modified green-light transparent ceramic material and preparation method and application thereof
CN115386374A (en) * 2022-09-07 2022-11-25 包头稀土研究院 Rare earth doped fluorescent material and preparation method and application thereof
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CN104725052A (en) * 2014-12-18 2015-06-24 徐州市江苏师范大学激光科技有限公司 Preparation method of multilayer composite structured transparent ceramic
CN104803670A (en) * 2015-04-10 2015-07-29 中国科学院宁波材料技术与工程研究所 Scintillation ceramic for double-layer detector and preparation method of scintillation ceramic
CN105906328A (en) * 2016-04-22 2016-08-31 横店集团浙江英洛华电子有限公司 Alumina fluorescence ceramic material, and preparation method and application thereof
WO2018097003A1 (en) * 2016-11-25 2018-05-31 大電株式会社 Fluorescent substance for vacuum ultraviolet excitation, luminescent element, and light-emitting device
JP2018083912A (en) * 2016-11-25 2018-05-31 大電株式会社 Vacuum ultraviolet-excited phosphor, light-emitting element, and light emitting device
CN109838763B (en) * 2017-09-13 2021-04-30 深圳光峰科技股份有限公司 Wavelength conversion device and preparation method thereof
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CN111018512A (en) * 2019-12-30 2020-04-17 江苏师范大学 Preparation method of high-luminous-efficiency and high-color-rendering-index fluorescent ceramic with gradient refractive index structure
CN111018512B (en) * 2019-12-30 2022-03-08 江苏师范大学 Preparation method of high-luminous-efficiency and high-color-rendering-index fluorescent ceramic with gradient refractive index structure
CN111393166A (en) * 2020-03-27 2020-07-10 徐州凹凸光电科技有限公司 High-thermal-stability fluorescent ceramic for white light L ED/L D and preparation method thereof
CN112094110A (en) * 2020-10-15 2020-12-18 贵州赛义光电科技有限公司 Al (aluminum)2O3-YAG:Ce3+Preparation method of complex phase fluorescent ceramic
CN114477989A (en) * 2020-11-11 2022-05-13 中国科学院福建物质结构研究所 Graphene-modified green-light transparent ceramic material and preparation method and application thereof
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Application publication date: 20140806