CN104609848B - A kind of compound phase crystalline ceramics changed for white-light LED fluorescence and preparation method thereof - Google Patents
A kind of compound phase crystalline ceramics changed for white-light LED fluorescence and preparation method thereof Download PDFInfo
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Abstract
A kind of compound phase crystalline ceramics changed for white-light LED fluorescence and preparation method thereof, the compound phase crystalline ceramics is by the first phase (CexPryY1‑x‑y)3(CrzAl1‑z)5O12Crystalline phase and the second phase Al2O3Crystalline phase is constituted, wherein x, and y and z span are respectively：0.0001≤x≤0.01,0≤y≤0.01,0≤z≤0.01 and the second phase Al2O3Fixing fabric structure between 0.1% the 30% of cumulative volume.The compound phase transparent fluorescent ceramic is excited using blue-ray LED, the blue light of gold-tinted, feux rouges and transmission that ceramics are produced is into high-quality white light, with high luminous efficiency, colour rendering index and physical and chemical performance stabilization, low cost and other advantages.
Description
Technical field
The present invention relates to fluorescent ceramic material, particularly a kind of compound phase crystalline ceramics changed for white-light LED fluorescence
And preparation method thereof.
Background technology
In recent years, be widely used using the light-emitting device of semiconductor light emitting, particularly high efficiency blue light emitting diode with
And the semiconductor white light illumination device based on blue light is successfully developed, the more known CCFL of this light-emitting device, incandescent lamp
Deng light-emitting device, there is high-luminous-efficiency, small volume, low power consumption, low cost, therefore can come as energy-efficient light source
Use.
Existing white light-emitting diodes light-emitting device, is mainly developed by complementary color principle.Sent out by semiconductor luminous assembly
Go out blue light, toward after fluorophor incidence, phosphor portion, which absorbs blue light and is converted to gold-tinted, to be sent, and blue light is mixed with gold-tinted while entering
When entering human eye, people is then felt as white light.Presently commercially available yellow fluorophor is generally powder, and high molecular bonding is needed when it is encapsulated
Agent, but will directly affect luminous efficiency with the increase adhesive aging of use time.Therefore how to extend light-emitting device makes
Reach with the life-span and simultaneously that briliancy is lifted, as one of existing phosphor technology developing focus.
Ce:YAG transparent fluorescent ceramics have the thermal conductivity and heat endurance more much higher than silica gel, can be declined with anti-light, reduce
Scattering loss, and with mechanical properties such as higher hardness, extend the service life of white light LEDs, with higher economy effect
Benefit.At present, in the world the well-known mechanism such as Philip Luminleds companies, Osram companies and Kyoto Univ Japan from
The research of thing this respect.Wherein, Philip Luminleds developed using ceramic fluorescent material heavy-power LED product-
Lumiramic LUXEONa LED, its technological core is exactly ceramic fluorescent plate (Lumiramic) combination film flip-chip
(Thin Film Flip Chip, TFFC).The colour temperature change of white light LEDs can be reduced to original 1/4 by the technology, be changed significantly
It has been apt to the uneven phenomenon of colour temperature between each LED, has also improved the stability of brightness and spectrum.Representational achievement in research：1、
Publication No. CN101080823A Chinese invention patent application, applicant Ube Industries, Ltd, this patent describes light
Transducing structure and the light-emitting device that make use of the light transducing structure, the light transducing structure mentioned in it are a kind of solidifications
Body is by α-Al2O3Crystalline phase and the Y that work is assigned with cerium3Al5O12Formed by crystalline phase is dimensionally mutually tangled, its preparation method needs height
Unidirectional solidification after temperature melting, and gained ceramics are almost opaque.2nd, Lu shen, Yang Li, and Qing Huang,
“Ultrafast fabrication of solid phosphor based white light emitting diodes:
From powder synthesis to devices”Appl.Phys.Lett.103,2(2013).Elaborate in the publication
One kind prepares Ce using SPS sintering:YAG and MgAl2O4The method of composite ceramics fluorophor.
The content of the invention
It is an object of the invention to provide compound phase crystalline ceramics changed for white-light LED fluorescence and preparation method thereof,
The compound phase ceramics are excited using blue-ray LED, the gold-tinted and feux rouges and the blue light of transmission that ceramics are produced are into white light, with hair
Light efficiency is high, colour rendering index is high, physical and chemical performance is stable, low cost and other advantages.
Technical scheme proposed by the present invention is：
A kind of compound phase ceramics changed for white-light LED fluorescence, feature is the compound phase crystalline ceramics by the first phase
(CexPryY1-x-y)3(CrzAl1-z)5O12Crystalline phase and the second phase Al2O3Crystalline phase is constituted, wherein x, and y and z span are respectively：
The fixing fabric structure of 0.0001≤x≤0.01,0≤y≤0.01,0≤z≤0.01 and the second phase the 0.1%-30% of cumulative volume it
Between.This is a kind of fluorescent transparent ceramics that can improve light-emitting phosphor efficiency and colour rendering index.
The preparation method of described compound phase crystalline ceramics, comprises the following steps：
1. the parameter x, y and z of compound phase crystalline ceramics are selected and second bulk volume fraction is mutually accounted for, using yittrium oxide
(Y2O3), aluminum oxide (Al2O3), cerium oxide (CeO2), praseodymium oxide (Pr6O11), chromium oxide (Cr2O3) it is raw material, selective oxidation magnesium
(MgO), the one or more in tetraethyl orthosilicate (TEOS) and polyethylene glycol (PEG) are transparent according to compound phase as additive
Ceramic chemical composition configures ceramic powder raw material；
2. prepare ceramic powder by ball-milling medium of absolute ethyl alcohol or deionized water with wet ball grinding again, powder through drying,
Sieving, tabletting, then more than 150MPa isostatic cool pressings formation ceramic body is imposed to it；
3. described ceramic body is put into vacuum sintering furnace and sintered, obtain crystalline ceramics；
4. the thin slice of thickness needed for described crystalline ceramics is cut into, that is, obtain for answering that white-light LED fluorescence is changed
Close phase crystalline ceramics.
When described crystalline ceramics base substrate is sintered in vacuum sintering furnace, vacuum is better than 10-2Pa, sintered heat insulating temperature is
1650~1780 DEG C, the sintered heat insulating time is 1~24 hour.
The technique effect of the present invention：
1) fluorescence transformational structure of the invention is mainly with the second phase Al2O3Crystalline phase is uniformly distributed in the first phase with graininess
(CexPryY1-x-y)3(CrzAl1-z)5O12In crystalline phase, its preparation method is solid reaction process, it is not necessary to melted, and preparation temperature is relative
Lower, the gained ceramics transparency preferably, and due to introducing Pr and (or) Cr energy transfer red emission, greatly improved multiple
The luminous colour rendering index of phase crystalline ceramics and spectral qualities are closed, are more suitable for room lighting.
2) (Ce is obtained using solid phase reaction vacuum-sinteringxPryY1-x-y)3(CrzAl1-z)5O12With Al2O3The transparent pottery of mixing
Porcelain fluorophor, test result indicates that containing Al2O3Compound phase fluorescence ceramics ratio contain MgAl2O4Compound phase fluorescence ceramics it is luminous
It is more efficient, and due to introducing Pr and (or) Cr energy transfer red emission so that color developing is more preferable.
3) effectively solve to run into the development of current white light LEDs because the encapsulating material aging coloring containing organic principle causes
Light decay, spectrum stability it is not ideal enough, the problems such as luminous efficiency of fluorescent material declines with the rise of LED temperature.
Brief description of the drawings
Fig. 1 is the structural representation of compound phase fluorescence ceramics of the present invention
Fig. 2 is principle of luminosity figure of the compound phase fluorescence ceramics of the present invention in the case where blue light is excited
Symbol description
1 first phase (CexPryY1-x-y)3(CrzAl1-z)5O12；2 second phase Al2O3；3 mixing high-quality white lights；4
(CexPryY1-x-y)3(CrzAl1-z)5O12With Al2O3Compound phase crystalline ceramics fluorophor；5InGaN/GaN base blue-ray LEDs.
Embodiment
With reference to embodiment, the invention will be further described, but should not be limited the scope of the invention with this.
Fig. 1 is the structural representation of compound phase fluorescence ceramics of the present invention, as illustrated, a kind of turn for white-light LED fluorescence
The compound phase crystalline ceramics changed is by the first phase (CexPryY1-x-y)3(CrzAl1-z)5O12Crystalline phase 1 and the second phase Al2O3Crystalline phase 2 is constituted,
Wherein x, y and z span is respectively：0.0001≤x≤0.01,0≤y≤0.01,0≤z≤0.01 and the body of the second phase
Product control is between the 0.1%-30% of cumulative volume.
Compound phase crystalline ceramics fluorescent material is in the case where InGaN/GaN base blue-ray LEDs are excited, (CexPryY1-x-y)3
(CrzAl1-z)5O12Ce in phase3+Excite and send gold-tinted and Pr3+And Cr3+Send feux rouges.Gold-tinted can be by changing with red light intensity
Become the thickness and Ce therein of compound phase crystalline ceramics3+、Pr3+And Cr3+Ion concentration is adjusted.
During Fig. 2 is principle of luminosity figure of the compound phase crystalline ceramics of the present invention in the case where blue light is excited, the compound phase crystalline ceramics
Ce3+Gold-tinted, the Pr sent in the case where blue light is excited3+And (or) Cr3+What the feux rouges and InGaN/GaN sent was sent is not inhaled
The blue light of receipts obtains high-quality white light.
The present invention doping concentration and crystalline ceramics thickness by optimizing active ions etc. obtain gentle colour temperature, Gao Xian
The compound phase fluorescent material of colour index and optical quenching temperature occurred frequently.
The preparation method of compound phase crystalline ceramics of the present invention is：
Using yittrium oxide (Y2O3), aluminum oxide (Al2O3), cerium oxide (CeO2), praseodymium oxide (Pr6O11), chromium oxide (Cr2O3)
For raw material, one or more of in selective oxidation magnesium (MgO), tetraethyl orthosilicate (TEOS) and polyethylene glycol (PEG) are used as addition
Agent, by the first phase (CexPryY1-x-y)3(CrzAl1-z)5O12Wherein x, y and z span is respectively：0.0001≤x≤
0.01,0≤y≤0.01,0≤z≤0.01 and the second phase Al2O3Fixing fabric structure is between the 0.1%-30% of cumulative volume, simultaneously
Add appropriate and appropriate additive.Powder material has been configured, then has been situated between with wet ball grinding using absolute ethyl alcohol or deionized water as ball milling
Matter prepares ceramic powder, and powder is through drying, sieving, tabletting；More than 150MPa isostatic cool pressings are imposed to it afterwards into base substrate；Then put
Enter and sinter some hours in vacuum at a certain temperature, obtain ceramics, resulting fluorescent ceramic material is cut into required thickness
Degree, obtains composite transparent ceramic as shown in Figure 1.
Embodiment 1
Using yittrium oxide (Y2O3), aluminum oxide (Al2O3), cerium oxide (CeO2), praseodymium oxide (Pr6O11), chromium oxide (Cr2O3)
Additive is used as raw material, and magnesia (MgO), polyethylene glycol (PEG) and tetraethyl orthosilicate (TEOS).First phase in dispensing
(CexPryY1-x-y)3(CrzAl1-z)5O12(x=0.001, y=0, z=0.001) and the second phase alumina (Al2O3) volume
Control is the 10% of cumulative volume, and magnesia (MgO) addition is the 0.1% of gross mass, and polyethylene glycol (PEG) addition is total matter
The 1% of amount, tetraethyl orthosilicate (TEOS) addition is the first phase (CexPryY1-x-y)3(CrzAl1-z)5O12The 0.4% of quality, is pressed
The compositing formula has configured powder material, then in the method for wet ball grinding and prepares ceramic powder by ball-milling medium of absolute ethyl alcohol
Material, powder is through drying, sieving, tabletting；200MPa isostatic cool pressings formation base substrate is imposed to it again, is then placed in vacuum sintering furnace
In 1700 DEG C of vacuums 10-3Sintered 24 hours under the conditions of Pa, obtain (CexPryY1-x-y)3(CrzAl1-z)5O12With Al2O3Compound phase
Fluorescent transparent ceramics, 0.44 mm of thickness is cut into by resulting ceramic material, obtains white light compound phase fluorescent transparent pottery
Porcelain.
Embodiment 2
Using yittrium oxide (Y2O3), aluminum oxide (Al2O3), cerium oxide (CeO2), praseodymium oxide (Pr6O11), chromium oxide (Cr2O3)
Additive is used as raw material, and magnesia (MgO) and tetraethyl orthosilicate (TEOS).First phase (Ce in dispensingxPryY1-x-y)3
(CrzAl1-z)5O12(x=0.001, y=0.001, z=0) and the second phase alumina (Al2O3) fixing fabric structure in cumulative volume
10%, magnesia (MgO) addition be gross mass 0.1%, tetraethyl orthosilicate (TEOS) addition be the first phase
(CexPryY1-x-y)3(CrzAl1-z)5O12The 0.4% of quality, powder material has been configured by the compositing formula, then with wet ball grinding
Method simultaneously prepares ceramic powder by ball-milling medium of absolute ethyl alcohol, and powder is through drying, sieving, tabletting；200MPa is imposed to it again
Isostatic cool pressing formation base substrate, is then placed in vacuum sintering furnace in 1700 DEG C of vacuums 10-3Sinter 24 hours, obtain under the conditions of Pa
(CexPryY1-x-y)3(CrzAl1-z)5O12With Al2O3Compound phase fluorescent transparent ceramics, 0.44 is cut into by resulting ceramic material
Mm of thickness, obtains white light compound phase fluorescent transparent ceramics.
Embodiment 3
Using yittrium oxide (Y2O3), aluminum oxide (Al2O3), cerium oxide (CeO2), praseodymium oxide (Pr6O11), chromium oxide (Cr2O3)
Additive is used as raw material, and magnesia (MgO) and polyethylene glycol (PEG).First phase (Ce in dispensingxPryY1-x-y)3
(CrzAl1-z)5O12(x=0.002, y=0.001, z=0.001) and the second phase alumina (Al2O3) fixing fabric structure total
The 20% of volume, magnesia (MgO) addition is the 0.1% of gross mass, and polyethylene glycol (PEG) addition is the 1% of gross mass,
Powder material has been configured by the compositing formula, then in the method for wet ball grinding and has prepared ceramic powder by ball-milling medium of absolute ethyl alcohol
Material, powder is through drying, sieving, tabletting；200MPa isostatic cool pressings formation base substrate is imposed to it again, is then placed in vacuum sintering furnace
In 1700 DEG C of vacuums 10-3Sintered 24 hours under the conditions of Pa, obtain (CexPryY1-x-y)3(CrzAl1-z)5O12With Al2O3Compound phase
Fluorescent transparent ceramics, 0.45 mm of thickness is cut into by resulting ceramic material, obtains white light compound phase fluorescent transparent pottery
Porcelain.
Embodiment 4
Using yittrium oxide (Y2O3), aluminum oxide (Al2O3), cerium oxide (CeO2), praseodymium oxide (Pr6O11), chromium oxide (Cr2O3)
Additive is used as raw material, and tetraethyl orthosilicate (TEOS) and polyethylene glycol (PEG).First phase (Ce in dispensingxPryY1-x-y)3
(CrzAl1-z)5O12(x=0.002, y=0.001, z=0.001) and the second phase alumina (Al2O3) fixing fabric structure total
The 20% of volume, polyethylene glycol (PEG) addition is the 1% of gross mass, and tetraethyl orthosilicate (TEOS) addition is the first phase
(CexPryY1-x-y)3(CrzAl1-z)5O12The 0.4% of quality, powder material has been configured by the compositing formula, then with wet ball grinding
Method simultaneously prepares ceramic powder by ball-milling medium of deionized water, and powder is through drying, sieving, tabletting；200MPa is imposed to it again
Isostatic cool pressing formation base substrate, is then placed in vacuum sintering furnace in 1700 DEG C of vacuums 10-3Sinter 24 hours, obtain under the conditions of Pa
(CexPryY1-x-y)3(CrzAl1-z)5O12With Al2O3Compound phase fluorescent transparent ceramics, 0.45 is cut into by resulting ceramic material
Mm of thickness, obtains white light compound phase fluorescent transparent ceramics.
Embodiment 5
Using yittrium oxide (Y2O3), aluminum oxide (Al2O3), cerium oxide (CeO2), praseodymium oxide (Pr6O11), chromium oxide (Cr2O3)
For raw material, using magnesia (MgO) as additive, by the first phase (CexPryY1-x-y)3(CrzAl1-z)5O12(x=0.002, y=
0.001, z=0.001) and the second phase alumina (Al2O3) fixing fabric structure in the 20% of cumulative volume, and magnesia (MgO)
Addition is the 0.1% of gross mass, and powder material has been configured by the compositing formula, then in the method for wet ball grinding and with anhydrous second
Alcohol is that ball-milling medium prepares ceramic powder, and powder is through drying, sieving, tabletting；200MPa isostatic cool pressings formation base is imposed to it again
Body, is then placed in vacuum sintering furnace and is sintered 10 hours at 1650 DEG C, then lower 1450 DEG C of hot pressed sinterings of 100MPa 10 hours.Most
High (the Ce of consistency is obtained afterwardsxPryY1-x-y)3(CrzAl1-z)5O12With Al2O3Compound phase fluorescent transparent ceramics, by resulting pottery
Ceramic material carries out cutting into 0.45 mm of thickness, obtains white light compound phase fluorescent transparent ceramics.
Claims (4)
1. a kind of compound phase crystalline ceramics changed for white-light LED fluorescence, it is characterised in that the compound phase crystalline ceramics is by the
One phase (CexPryY1-x-y)3(CrzAl1-z)5O12Crystalline phase and the second phase Al2O3Crystalline phase is constituted, the second phase Al2O3It is uniform with graininess
It is distributed in the first phase (CexPryY1-x-y)3(CrzAl1-z)5O12In host material, wherein x, y and z span is respectively：
0.0001≤x≤0.01,0≤y≤0.01,0≤z≤0.01, and the second phase fixing fabric structure cumulative volume 0.1%-30%
Between.
2. the preparation method of the compound phase crystalline ceramics described in claim 1, it is characterised in that this method comprises the following steps：
1. the parameter x, y and z and the second phase volume percentage of the total volume of compound phase crystalline ceramics are selected, using yittrium oxide
Y2O3, aluminium oxide Al2O3, cerium oxide CeO2, praseodymium oxide Pr6O11With chromium oxide Cr2O3For raw material, with magnesia MgO, polyethylene glycol
One or more weigh ceramics as additive according to compound phase crystalline ceramics chemical composition in PEG and tetraethyl orthosilicate TEOS
Powder material；
2. prepare ceramic powder by ball-milling medium of absolute ethyl alcohol or deionized water with wet ball grinding again, powder through drying, sieving,
Tabletting, then more than 150MPa isostatic cool pressings formation ceramic body is imposed to it；
3. described ceramic body is put into vacuum sintering furnace and sintered, obtain crystalline ceramics；
4. the thin slice of thickness needed for described ceramics are cut into, that is, obtain the transparent pottery of compound phase changed for white-light LED fluorescence
Porcelain.
3. the preparation method of compound phase crystalline ceramics according to claim 2, it is characterised in that described ceramic body exists
When being sintered in vacuum sintering furnace, vacuum is better than 10-2Pa, sintered heat insulating temperature is 1650~1780 DEG C, sintered heat insulating time
For 1~24 hour.
4. the preparation method of compound phase crystalline ceramics according to claim 2, it is characterised in that described magnesia MgO,
One or more are as additive in polyethylene glycol PEG and tetraethyl orthosilicate TEOS, and the control of magnesia MgO additions is gross mass
0%-0.3%, polyethylene glycol PEG additions control for gross mass 0%-1.5%, tetraethyl orthosilicate TEOS additions control
For the first phase (CexPryY1-x-y)3(CrzAl1-z)5O12The 0%-0.4% of quality.
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| CN107651955A (en) * | 2017-10-23 | 2018-02-02 | 苏州创思得新材料有限公司 | A kind of complex phase crystalline ceramics of White-light LED illumination and preparation method thereof |
| CN109896843A (en) * | 2017-12-07 | 2019-06-18 | 上海航空电器有限公司 | Complex phase ceramic array, preparation method and light supply apparatus for laser lighting |
| 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 |
| CN110423109A (en) * | 2019-09-02 | 2019-11-08 | 谢琳祥 | A kind of ceramic formula, preparation method, ceramic tube and ceramic tube application method |
| JP7445949B2 (en) | 2019-09-05 | 2024-03-08 | Ｏｒｂｒａｙ株式会社 | ceramic composite |
| WO2021045077A1 (en) * | 2019-09-05 | 2021-03-11 | アダマンド並木精密宝石株式会社 | Ceramic composite |
| CN111875370B (en) * | 2020-07-07 | 2023-05-09 | 中国科学院上海光学精密机械研究所 | Composite crystalline phase fluorescent ceramic for blue light LED or LD excitation and preparation method thereof |
| CN113461417A (en) * | 2021-06-29 | 2021-10-01 | 南通大学 | Fluorescent ceramic processed by femtosecond laser texturing technology |
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| CN1738781A (en) * | 2003-01-20 | 2006-02-22 | 宇部兴产株式会社 | Ceramic composite material for optical conversion and use thereof |
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| CN102173825A (en) * | 2011-01-28 | 2011-09-07 | 中国科学院上海光学精密机械研究所 | Sintering aid for yttrium aluminum garnet-based fluorescent transparent ceramic and using method thereof |
| CN103956421A (en) * | 2014-04-22 | 2014-07-30 | 中国科学院上海光学精密机械研究所 | LED lamp based on transparent fluorescent ceramics |
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| CN101284733A (en) * | 2007-04-10 | 2008-10-15 | 中国科学院上海硅酸盐研究所 | Yttrium aluminium garnet and yttria double crystal transparent ceramic and method for making same |
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