CN104177078A - Ce:YAG based transparent ceramic being used for fluorescence conversion of white LED and containing Lu and preparation method thereof - Google Patents
Ce:YAG based transparent ceramic being used for fluorescence conversion of white LED and containing Lu and preparation method thereof Download PDFInfo
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- CN104177078A CN104177078A CN201410342569.6A CN201410342569A CN104177078A CN 104177078 A CN104177078 A CN 104177078A CN 201410342569 A CN201410342569 A CN 201410342569A CN 104177078 A CN104177078 A CN 104177078A
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Abstract
The invention relates to a transparent fluorescent ceramic material and in particular relates to a Ce:YAG based transparent ceramic being used for fluorescence conversion of a white laser diode (hereinafter referred to as LED) and containing Lu and a preparation method thereof. The chemical formula of the transparent ceramic is MgAl<2>O<4>-(Ce<x>Lu<y>Y<1-x-y>)<3>Al<5>O<12>. The transparent ceramic can be directly used as a packaging material to replace traditional organic polymers or silica gel packaging materials, and compared with existing transparent ceramics, has lower and stable color temperature, excellent luminous efficiency, obviously improved color rendering index and quite high stability and optical attenuation resistance; therefore the transparent ceramic has satisfactory service life.
Description
Technical field
The present invention relates to transparent fluorescent ceramic material, particularly a kind of Ce:YAG base transparent ceramic containing Lu for the conversion of white light laser diode (being designated hereinafter simply as LED) fluorescence and preparation method thereof, this crystalline ceramics is by MgAl
2o
4-(Ce
xlu
yy
1-x-y)
3al
5o
12form.
Background technology
White light LEDs is since coming out, because of its have the advantages such as energy-efficient, environmental protection, life-span be long be described as be after incandescent light, luminescent lamp, gas discharge lamp the 4th generation lighting source, be widely used in the fields such as mobile phone, digital camera, family or outdoor lighting.It is predicted, the ratio that LED illumination accounts for conventional lighting field will reach 50% in 2015, will reach 80%, and become global topmost lighting system to the year two thousand twenty, and whole white light LEDs market just will reach the market scale of 20,400,000,000 U.S. dollars in 2014.
Having realized now business-like white-light LED encapsulation technology is that Ce:YAG yellow fluorescent powder is dispersed in epoxy resin or layer of silica gel to fix blue chip, reduce the air pore between chip and powder simultaneously, but epoxy resin or silica gel are macromolecule organics, the heat dispersion of these organic polymer packaged materials is poor, the blue chip of LED is under persistent fever, its temperature can raise, particularly high power LED device encapsulation, not only fluorescent powder grain is along with the rising luminous efficiency of temperature declines, and there is chemical reaction in organic polymer packaged material in the time that temperature raises, cause the organic transmitance after aging to decline, cause LED device, especially the light decay outstanding problem of high power LED device, seriously reduce its work-ing life.Even, because heat dispersion is poor, can cause the thermal quenching phenomenon of Ce:YAG fluorescent material.
The problems referred to above that occur based on current white light LEDs, researchist starts to research and develop the crystalline ceramics with high stability as fluorescence conversion and packaged material.
And Ce:YAG transparent fluorescent ceramic has the thermal conductivity more much higher than silica gel and thermostability, can anti-lightly decline, reduce scattering loss, and there is the mechanical properties such as higher hardness, extend the work-ing life of white light LEDs, there is higher economic benefit.At present, the well-known mechanism such as Philip Luminleds company, Osram company and Kyoto Univ Japan is all being engaged in the research of this respect in the world.Wherein, Philip Luminleds has developed the heavy-power LED product-Lumiramic LUXEONa LED that uses ceramic fluorescent material, its technological core is exactly ceramic fluorescent plate (Lumiramic) combination film flip-chip (Thin Film Flip Chip, TFFC).This technology can change the colour temperature of white light LEDs and be reduced to originally 1/4, has greatly improved the phenomenon of colour temperature inequality between each LED, has also improved the stability of brightness and spectrum.
Domestic aspect, has also carried out many research work about Ce:YAG transparent fluorescent ceramic, and such as He Feilong etc. are at " the novel MgAl of white light LEDs
2o
4the luminescent properties of/Ce:YAG crystalline ceramics " middle proposition, MgAl
2o
4/ Ce:YAG crystalline ceramics and blue-light LED chip are packaged into white light LEDs, and under 35mA drives, light efficiency reaches 133.47lmW
-1, its colour temperature stability will be better than the white light LEDs of traditional YAG:Ce fluorescent powder packaging, the life-span of obviously having improved white light LEDs far away.
Although for example CN102832328A discloses a kind of fluorescence ceramics that consists of polycrystalline Re:YAG, wherein rare earth element Re is selected from Ce, Eu, Er, Nd, Tb, Sm, Tm, Dy or Yb, doping is 0.005 to 10wt%, after but it has only investigated light source igniting 30 minutes, the luminous efficiency of source of described fluorescence ceramics, and impact on colour temperature.
But when current Ce-YAG base transparent fluorescent ceramic directly substitutes organic polymer or silica gel as packaged material, while also existing high temperature to use for a long time, luminous efficiency there will be obvious decline, thereby work-ing life still cannot be satisfactory.
Summary of the invention
The object of the present invention is to provide a kind of crystalline ceramics for white-light LED fluorescence conversion and preparation method thereof, this crystalline ceramics can directly substitute traditional organic polymer or silica type packaged material as packaged material, it is with respect to existing crystalline ceramics, there is lower and stable colour temperature, excellent luminous efficiency, the colour rendering index significantly improving, very high stability and the anti-light performance that declines, thereby there is gratifying work-ing life.
The present inventor, by arduous test, studies for a long time, and the technical scheme of proposition is as follows:
For the Ce:YAG base transparent ceramic containing Lu of white-light LED fluorescence conversion, it is characterized in that by its chemical constitution be MgAl
2o
4/ (Ce
xlu
yy
1-x-y)
3al
5o
12, wherein the span of x and y is respectively: 0.001≤x≤0.03; 0.001≤y≤0.03; In the gross weight of crystalline ceramics, MgAl
2o
4quality percentage composition be about 55%-95%.
Wherein the span of x is preferably: 0.008≤x≤0.02, more preferably 0.013≤x≤0.015; The span of y is preferably: 0.008≤y≤0.02, more preferably 0.016≤y≤0.018.
Wherein in the gross weight of crystalline ceramics, MgAl
2o
4quality percentage composition be preferably about 65%-85%, more preferably 70%-80%, most preferably is 74-76%.
1. the preparation method of described crystalline ceramics, comprise the following steps: to react and obtain metal alkoxide according to required ratio and Virahol taking metallic aluminium, magnesium as raw material, then pass through underpressure distillation, in baking oven, dries, and high-temperature roasting 2-4 hour, obtains nanometer MgAl
2o
4powder;
2. adopt yttrium oxide (Y
2o
3), aluminum oxide (Al
2o
3), Praseodymium trioxide (Pr
2o
3), lutecium oxide (Lu
2o
3), cerium oxide (CeO
2) be raw material, configure the powder raw material of each component by the chemical constitution of crystalline ceramics, then taking dehydrated alcohol or deionized water as medium, carry out ground and mixed powder raw material with wet ball grinding, until the median size of powder raw material is less than 0.5 micron, then add the nanometer MgAl of aequum
2o
4powder, continues ball milling until mix;
3. mixed powder raw material drying, sieve, compressing tablet, then it is imposed to the above isostatic cool pressing of 150MPa, described pressure is preferably 200-400MPa, thereby is pressed into ceramic body;
4. described ceramic body is put into vacuum sintering furnace or hot-pressed sintering furnace sintering, obtained the crystalline ceramics that thickness is about 0.2-0.3mm;
5. alternatively by crystalline ceramics surface finish.
Described crystalline ceramics base substrate is in vacuum sintering furnace when sintering, and sintered heat insulating temperature is 1680~1750 DEG C, and the sintered heat insulating time is 2~24 hours.
Described crystalline ceramics base substrate is in described hot-pressed sintering furnace when sintering, and applied pressure is 15~40MPa, and sintered heat insulating temperature is 1500~1700 DEG C, and the sintered heat insulating time is 2~10 hours.
Technique effect of the present invention:
Crystalline ceramics of the present invention, the heat dispersion that can effectively solve organic polymer packaged material is poor, easily aging, high temperature or short wavelength light be according to lower easy to change, luminous efficiency reduces gradually, work-ing life is poor technical problem.Its effect be mainly following some:
Crystalline ceramics of the present invention, its colour temperature is lower, be located substantially in the scope of 3200-4000K, thereby the white light obtaining is comparatively soft, can avoid because colour temperature is compared with high " dazzle " phenomenon producing; And its colour temperature is comparatively stable, when Injection Current is in the time that 100-350mA changes, its colour temperature changing value is only 10K.
When crystalline ceramics of the present invention is used as white-light LED encapsulation material, luminous efficiency can reach 145.32-168.78lm/W.
Crystalline ceramics of the present invention, its colour rendering index is 80.1-92.3, far above existing crystalline ceramics.
Crystalline ceramics of the present invention, there is very high stability and the anti-light performance that declines, after the aging resistance test of 3000h, relative light intensity by the white light LEDs of its encapsulation is not decayed substantially, and the decay of 13% left and right has just appearred in the relative light intensity of the white light LEDs of traditional way encapsulation after 800h.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but should not limit the scope of the invention with this.
Embodiment 1
React and obtain metal alkoxide according to required ratio and Virahol taking metallic aluminium, magnesium as raw material, then pass through underpressure distillation, in baking oven, dry, high-temperature roasting 3 hours, obtains the nanometer MgAl of 75g
2o
4powder.Adopt yttrium oxide (Y
2o
3), aluminum oxide (Al
2o
3), lutecium oxide (Lu
2o
3),, cerium oxide (CeO
2) be raw material, by (Ce
0.001lu
0.001y
0.998)
3al
5o
12chemical constitution configure powder material 25g, then carry out ground and mixed powder raw material taking dehydrated alcohol as medium with wet ball grinding, until the median size of powder raw material is 0.4 micron.Then add nanometer MgAl
2o
4powder, continues ball milling until mix.Mixed powder drying, sieve, compressing tablet; Again it is imposed respectively to 200MPa isostatic cool pressing and become base substrate, put into vacuum sintering furnace sintering 20 hours at 1700 DEG C, acquisition thickness is 0.3mm, MgAl
2o
4the quality percentage composition MgAl that is 75%
2o
4/ (Ce
0.001lu
0.001y
0.998)
3al
5o
12transparent fluorescent ceramic, by obtained crystalline ceramics surface finish processing.
Then described crystalline ceramics is combined with InGaN blue-light LED chip, is packaged into white light LED part.
At room temperature, pass into 350mA constant-current driving, its performance index are as shown in table 1.
Embodiment 2
Adopt the mode identical with embodiment 1 prepare and test MgAl
2o
4/ (Ce
0.03lu
0.03y
0.94)
3al
5o
12transparent fluorescent ceramic.
Embodiment 3
Adopt the mode identical with embodiment 1 prepare and test MgAl
2o
4/ (Ce
0.01lu
0.01y
0.98)
3al
5o
12transparent fluorescent ceramic.
Embodiment 4
Adopt the mode identical with embodiment 1 prepare and test MgAl
2o
4/ (Ce
0.014lu
0.017y
0.969)
3al
5o
12transparent fluorescent ceramic.
Embodiment 5
Except nanometer MgAl
2o
4the addition of powder is 55g, and the total amount of other powder raw material is outside 45g, and other condition is with embodiment 4, prepares and tests MgAl
2o
4the quality percentage composition MgAl that is 55%
2o
4/ (Ce
0.014lu
0.017y
0.969)
3al
5o
12transparent fluorescent ceramic.
Embodiment 6
Except nanometer MgAl
2o
4the addition of powder is 95g, and the total amount of other powder raw material is outside 5g, and other condition is with embodiment 4, prepares and tests MgAl
2o
4the quality percentage composition MgAl that is 95%
2o
4/ (Ce
0.014lu
0.017y
0.969)
3al
5o
12transparent fluorescent ceramic.
Embodiment 7
Except nanometer MgAl
2o
4the addition of powder is 85g, and the total amount of other powder raw material is outside 15g, and other condition is with embodiment 4, prepares and tests MgAl
2o
4the quality percentage composition MgAl that is 85%
2o
4/ (Ce
0.014lu
0.017y
0.969)
3al
5o
12transparent fluorescent ceramic.
Embodiment 8
Except nanometer MgAl
2o
4the addition of powder is 65g, and the total amount of other powder raw material is outside 35g, and other condition is with embodiment 4, prepares and tests MgAl
2o
4the quality percentage composition MgAl that is 65%
2o
4/ (Ce
0.014lu
0.017y
0.969)
3al
5o
12transparent fluorescent ceramic.
Comparative example 1
Except with gadolinium sesquioxide (Gd
2o
3) alternative lutecium oxide (Lu
2o
3) outside, other condition is with embodiment 4, prepares and tests MgAl
2o
4the quality percentage composition MgAl that is 75%
2o
4/ (Ce
0.014gd
0.017y
0.969)
3al
5o
12transparent fluorescent ceramic.
Comparative example 2
Except with Samarium trioxide (Sm
2o
3) alternative lutecium oxide (Lu
2o
3) outside, other condition is with embodiment 4, prepares and tests MgAl
2o
4the quality percentage composition MgAl that is 75%
2o
4/ (Ce
0.014sm
0.017y
0.969)
3al
5o
12transparent fluorescent ceramic.
Comparative example 3
Except with Neodymium trioxide (Nd
2o
3) alternative lutecium oxide (Lu
2o
3) outside, other condition is with embodiment 4, prepares and tests MgAl
2o
4the quality percentage composition MgAl that is 75%
2o
4/ (Ce
0.014nd
0.017y
0.969)
3al
5o
12transparent fluorescent ceramic.
Comparative example 4
Except with europium sesquioxide (Eu
2o
3) and ytterbium oxide (Yb
2o
3) alternative lutecium oxide (Lu
2o
3) outside, other condition is with embodiment 4, prepares and tests MgAl
2o
4the quality percentage composition MgAl that is 75%
2o
4/ (Ce
0.014eu
0.0004yb
0.0166y
0.969)
3al
5o
12transparent fluorescent ceramic.
Comparative example 5
Except not adding lutecium oxide (Lu
2o
3) outside, other condition is with embodiment 4, prepares and tests MgAl
2o
4the quality percentage composition MgAl that is 75%
2o
4/ (Ce
0.031y
0.969)
3al
5o
12transparent fluorescent ceramic.
Comparative example 6
To mix organosilicon (conventional package mode) by the product YAG:Ce of Ying Temei company of U.S. fluorescent material (model is YAG-04) and encapsulate, according to the test condition of embodiment 1, its performance be tested.
Table 1 test-results
Experiment shows, obtained for example luminous efficiency, colour rendering index, the anti-light performance that declines of the present invention is very superior, and unexpected.
Claims (6)
1. for the Ce:YAG base transparent ceramic containing Lu of white-light LED fluorescence conversion, it is characterized in that by its chemical constitution be MgAl
2o
4/ (Ce
xlu
yy
1-x-y)
3al
5o
12, wherein the span of x and y is respectively: 0.001≤x≤0.03; 0.001≤y≤0.03; In the gross weight of crystalline ceramics, MgAl
2o
4quality percentage composition be about 55%-95%.
2. crystalline ceramics claimed in claim 1, is characterized in that the span of x and y is respectively: 0.008≤x≤0.02,0.008≤y≤0.02; In the gross weight of crystalline ceramics, MgAl
2o
4quality percentage composition be about 65%-85%.
3. crystalline ceramics claimed in claim 1, is characterized in that the span of x and y is respectively: 0.013≤x≤0.015,0.016≤y≤0.018; In the gross weight of crystalline ceramics, MgAl
2o
4quality percentage composition be about 70%-80%.
4. the preparation method of crystalline ceramics claimed in claim 1, is characterized in that the method comprises the following steps:
1. react and obtain metal alkoxide according to required ratio and Virahol taking metallic aluminium, magnesium as raw material, then pass through underpressure distillation, in baking oven, dry, high-temperature roasting 2-4 hour, obtains nanometer MgAl
2o
4powder;
2. adopt yttrium oxide (Y
2o
3), aluminum oxide (Al
2o
3), lutecium oxide (Lu
2o
3), cerium oxide (CeO
2) be raw material, configure the powder raw material of each component by the chemical constitution of crystalline ceramics, then taking dehydrated alcohol or deionized water as medium, carry out ground and mixed powder raw material with wet ball grinding, until the median size of powder raw material is less than 0.5 micron, then add the nanometer MgAl of aequum
2o
4powder, continues ball milling until mix;
3. mixed powder raw material drying, sieve, compressing tablet, thereby then it imposed to the above isostatic cool pressing of 150MPa be pressed into ceramic body;
4. described ceramic body is put into vacuum sintering furnace or hot-pressed sintering furnace sintering, obtained the crystalline ceramics that thickness is about 0.2-0.3mm;
5. alternatively by crystalline ceramics surface finish.
5. the preparation method of composite transparent ceramic according to claim 2, is characterized in that described crystalline ceramics base substrate is in vacuum sintering furnace when sintering, and sintered heat insulating temperature is 1680~1750 DEG C, and the sintered heat insulating time is 2~24 hours.
6. the preparation method of composite transparent ceramic according to claim 2, it is characterized in that described crystalline ceramics base substrate is in described hot-pressed sintering furnace when sintering, applied pressure is 15~40MPa, and sintered heat insulating temperature is 1500~1700 DEG C, and the sintered heat insulating time is 2~10 hours.
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CN111285683A (en) * | 2018-12-07 | 2020-06-16 | 上海航空电器有限公司 | High-stability fluorescent ceramic for high-power laser illumination and preparation method thereof |
CN111875370A (en) * | 2020-07-07 | 2020-11-03 | 中国科学院上海光学精密机械研究所 | Composite crystalline phase fluorescent ceramic for excitation of blue light LED or LD and preparation method thereof |
CN112159220A (en) * | 2020-09-24 | 2021-01-01 | 徐州凹凸光电科技有限公司 | High-thermal-stability high-quantum-efficiency fluorescent ceramic for white light LED/LD and preparation method thereof |
CN112661512A (en) * | 2020-12-23 | 2021-04-16 | 新沂市锡沂高新材料产业技术研究院有限公司 | Method for densification of fluorescent powder and yttrium oxide ceramic at room temperature |
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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CN111285683A (en) * | 2018-12-07 | 2020-06-16 | 上海航空电器有限公司 | High-stability fluorescent ceramic for high-power laser illumination and preparation method thereof |
CN109437900A (en) * | 2018-12-12 | 2019-03-08 | 中国科学院宁波材料技术与工程研究所 | A kind of fluorescence ceramics block, preparation method and its application in laser lighting |
CN111875370A (en) * | 2020-07-07 | 2020-11-03 | 中国科学院上海光学精密机械研究所 | Composite crystalline phase fluorescent ceramic for excitation of blue light LED or LD and preparation method thereof |
CN112159220A (en) * | 2020-09-24 | 2021-01-01 | 徐州凹凸光电科技有限公司 | High-thermal-stability high-quantum-efficiency fluorescent ceramic for white light LED/LD and preparation method thereof |
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 |
CN112661512A (en) * | 2020-12-23 | 2021-04-16 | 新沂市锡沂高新材料产业技术研究院有限公司 | Method for densification of fluorescent powder and yttrium oxide ceramic at room temperature |
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