CN103059860A - Manganese-doped yttrium aluminium garnet monocrystal material and application for same - Google Patents
Manganese-doped yttrium aluminium garnet monocrystal material and application for same Download PDFInfo
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- CN103059860A CN103059860A CN2012103453413A CN201210345341A CN103059860A CN 103059860 A CN103059860 A CN 103059860A CN 2012103453413 A CN2012103453413 A CN 2012103453413A CN 201210345341 A CN201210345341 A CN 201210345341A CN 103059860 A CN103059860 A CN 103059860A
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Abstract
The invention discloses a manganese-doped yttrium aluminium garnet monocrystal material and an application for the same. The chemical composition expression of the manganese-doped yttrium aluminium garnet monocrystal material is Y3-yAl5-xO12: Mnx, Cey, wherein the value of x ranges from 0.01 to 0.12, and the value of y ranges from 0 to 0.1; and the manganese-doped yttrium aluminium garnet monocrystal material is prepared via a melt direct-pull method. The monocrystal material disclosed by the invention has the characteristics of being low in colour temperature, wide in wave spectrum, high in luminous intensity and the like; and the comprehensive photoelectric property of a white-light LED (light-emitting diode) device can be improved.
Description
Technical field
The present invention relates to transition element doped novel monocrystal material and application thereof, particularly a kind of manganese doped yttrium aluminium garnet monocrystal material and application thereof.
Background technology
The LED fluorescent material is hot topic and the advanced subject of current research, present stage commercialization white light LEDs product is take chip and phosphor combination as Developing mainstream, but improving luminous efficiency, improves color developing, increasing the service life and the aspect such as high-power use meets with bottleneck.Be accompanied by the growing lighting demand of people, preparation high-level efficiency, high color rendering index (CRI), low colour temperature, powerful fluorescent material for white light LED will have very important significance.
The people such as T.Ludziejewski in 1997 have studied the Ce:YAG crystal of different cerium doping contents and have drawn the optimum doping concentration (" Investigation of some scintillation properties of YAG:Ce crystals " is published in Nuclear Instruments and Methods in Physics Research A398 (1997) 287-294) of cerium ion in the scintillation crystal; Patent CN101894900A openly utilizes the YAG monocrystalline as the substrate material of white light LEDs.At present, there are some researches show and on the basis of doped Ce ion, to have mixed altogether other rare earth ion, improved light efficiency and the spectral emissions scope of YAG fluorescent material.Patent CN102168307A has narrated the Pr that grows from high-temperature fusant, Tb, Sm, the method for Dy and Ce ion doping hundred million aluminum carbuncle crystals; Patent CN101899710A discloses the preparation method of cerium and ytterbium ion codoped Yttrium aluminium garnet laser crystal.For red emission, commonly used have rare earth ions such as Pr, Eu, Sm, the luminous of them caused by the 4f-4f transition, characteristics are that the position of glow peak is not affected by matrix, but also exist the feature glow peak narrower, halfwidth is little, and the shortcoming that the glow peak wavelength is short is not ideal enough to the increase effect of red composition in the spectrum.
Transition element manganese is a kind of chemical element that enriches valence state that has, Mn ion (the 2+ of different valence state, 3+, 4+) has the different characteristics of luminescences, the Mn ion is in some matrix, can produce the broadband emission that is positioned at the ruddiness zone, the Mn ion is applied to fluorescent material as luminescence center and has been reported.Patent CN102337134A has related to a kind of white light LEDs is mixed hundred million aluminium garnet fluorescent material altogether with the manganese cerium preparation method.By the glow peak red shift that mixing of Mn ion can make YAG:Ce fluorescent material, peak width at half height enlarges, and has improved the color developing of fluorescent material in the white light LEDs.Yet still there is certain defective in fluorescent material at aspects such as stability, aging, homogeneities, has limited its application and development at white light LEDs especially great power LED.The human Czochralski growns such as W xiang in 2012 the manganese cerium mix altogether hundred million aluminum carbuncle crystals and carried out annealing experiment, the Mn ion is+4 valencys in the prepared crystal, the main glow peak position though light efficiency promotes to some extent after the annealing, fails significantly to increase the red composition in the emmission spectrum at 530nm.
Existing wafer prepares the technology of white light LEDs to be compared with fluorescent powder packaging, has the problem that colour temperature is high, colour rendering index is low.It is that white light LEDs further develops difficult point and the emphasis that needs solution with wafer that ruddiness lacks.Manganese of the present invention hundred million aluminum carbuncle crystals that mix utilize transmission ofenergy mechanism between rare earth ion cerium and the mn ion, adopt blue-light excited, effectively overcome the ruddiness shortage problem that the cerium yttrium aluminum garnet prepares white light LEDs, promote the comprehensive photoelectric properties that wafer prepares white light LEDs.
Summary of the invention
Primary and foremost purpose of the present invention is to provide a kind of manganese doped yttrium aluminum garnet monocrystal material, and this monocrystal material has the characteristics such as colour temperature is low, wave spectrum is wide, luminous intensity is large, can improve the comprehensive photoelectric properties of white light LED part.
Second purpose of the present invention be with described manganese doped yttrium aluminum garnet monocrystal material as fluorescent material for the preparation of white light LED part.
The below does technical scheme of the present invention and specifies.
The invention provides a kind of manganese doped yttrium aluminum garnet monocrystal material, it is characterized in that the chemical constitution expression of described manganese doped yttrium aluminum garnet monocrystal material is: Y
3-yAl
5-xO
12: Mn
x, Ce
y, wherein the span of x is 0.01≤x≤0.12, the span of y is 0≤y≤0.1; Described manganese doped yttrium aluminum garnet monocrystal material is by the preparation of melt vertical pulling method, and the preparation method comprises the steps:
1. with raw material Y
2O
3, Al
2O
3, CeO
2, MnO
2Or Y
2O
3, Al
2O
3, MnO
2By the accurate weighing of chemical constitution, mix rear briquetting, in 1100-1300 ℃ of pre-burning 12-24h; Wherein guarantee raw material Y
2O
3, Al
2O
3Purity 〉=99.99%, CeO
2, MnO
2Purity 〉=99.9%;
2. the product after the pre-burning and seed crystal are transferred in the crystal furnace, are evacuated to 10 after the sealing
-2-10
-4Pa passes into inert protective gas when furnace temperature arrives 1000-1300 ℃, continue to be warming up to design temperature, and described design temperature is in 1700-2000 ℃ scope; After the furnace temperature of crystal furnace reaches design temperature, be incubated 1-3 hour, make raw material fusing by the regulating stove bore temperature, roasting seed crystal is through process pulling growth manganese doped yttrium aluminum garnet monocrystalline such as inoculation, shouldering, isometrical, endings;
3. after crystal growth finishes, with the speed slow cooling of 20-80 ℃/h, take out crystal after being down to room temperature, obtain manganese doped yttrium aluminum garnet monocrystal material.
Preferably, the span of x is 0.01≤x≤0.08, and the span of y is 0≤y≤0.06.
The preparation method of manganese doped yttrium aluminum garnet crystalline material of the present invention adopts the melt vertical pulling method, and equipment therefor is Frequency Induction Heating pull-type single crystal growing furnace.
In the described step (2), crystal growth direction is＜111〉direction.
In the described step (2), inert protective gas is preferably purity greater than 99% Ar or N
2
In the described step (2), preferably set temperature in 1800-1900 ℃ scope.
Manganese doped yttrium aluminum garnet crystalline material of the present invention has the strongest fluorescent orange to send blue-light excited lower about 588 nanometers, is the glow peak of bivalent manganese herein through looking into, and as seen in crystal, mn ion mainly exists with bivalent manganese.Mix altogether hundred million aluminium garnet monocrystalline with previous tetravalence manganese cerium and compare, manganese doped yttrium aluminum garnet monocrystal material of the present invention has a series of outstanding advantages, sees Table 1:
The comparison that table 1 manganese doped yttrium aluminum garnet of the present invention monocrystalline and existing manganese cerium are mixed monocrystalline altogether
Manganese doped yttrium aluminum garnet monocrystal material of the present invention can be used as fluorescent material for the preparation of in the white light LED part, monocrystal material can be directly after the operations such as cutting, polishing and the blue chip spiral-lock for the preparation of white light LED part, light efficiency＞50lm/W after encapsulation.
(1) compares with existing fluorescent material for white light LED, manganese doped yttrium aluminum garnet monocrystal material of the present invention utilizes the energy level pass through mechanism between cerium ion and mn ion, adopt blue-light excited, increased the blood orange light emission of Mn ion on the basis of emission gold-tinted, have the characteristics such as colour temperature is low, wave spectrum is wide, luminous intensity is large, can improve the comprehensive photoelectric properties of white light LED part.；
(2) the present invention can realize that by the ratio of allotment rare earth element ce and transition element Mn the luminous wave band of monocrystal material is tuning;
(3) the present invention compares than prior art, and the material purity of employing decreases, and the monocrystalline performance of preparation is more good, and technique is more easy without annealing process, has certain advantage towards suitability for industrialized production at economic aspect.
Description of drawings
Fig. 1 is the abosrption spectrogram of the manganese cerium co-doped yttrium aluminium garnet monocrystalline of embodiment 1.
Fig. 2 is the exciting light spectrogram of the manganese cerium co-doped yttrium aluminium garnet monocrystalline of embodiment 1.
Fig. 3 is the spectrum relative energy scatter chart of the manganese cerium co-doped yttrium aluminium garnet monocrystalline of embodiment 2.
Fig. 4 is the utilizing emitted light spectrogram of the manganese cerium co-doped yttrium aluminium garnet monocrystalline of embodiment 3.
Fig. 5 be the manganese cerium co-doped yttrium aluminium garnet monocrystalline of embodiment 4 at electrical parameter 3V, 350mA, the CIE chromaticity diagram of test gained under 150 ℃ of conditions, the chromaticity coordinates of its white light that is near the mark (0.33,0.33).
Embodiment
Below by embodiment the present invention is done to describe in further detail, but limit the present invention absolutely not.
Embodiment 1.
According to chemical constitution expression Y
2.964Al
4.952O
12: Mn
0.048, Ce
0.036(x=0.048, y=0.036) takes by weighing the Y of purity 〉=99.99%
2O
3, Al
2O
3, CeO
2, MnO
2Raw material grinds and mixes, and briquetting is transferred in the Medium frequency induction single crystal growing furnace together with seed crystal behind 1200 ℃ of pre-burning 24h, and tightness system was evacuated to 10 after shove charge was finished
-4Pa, when furnace temperature arrives 1400 ℃, pass into purity greater than 99% nitrogen, be warming up to 1800 ℃ in that this atmosphere relaying is continuous, be incubated 2 hours, until raw materials melt, pass through again the process pulling growth bivalent manganese doped yttrium aluminum garnet monocrystalline such as inoculation, shouldering, isometrical, ending by the regulating stove bore temperature.Crystal growth direction is＜111〉direction, and after growth finished, to room temperature, cooling finished to obtain manganese cerium co-doped yttrium aluminium garnet monocrystalline with the speed slow cooling of 20 ℃/h.The crystal entire body takes on a red color, transparent complete flawless, and quality is better.The absorption of gained monocrystalline and exciting light spectrogram are as depicted in figs. 1 and 2.
Embodiment 2.
According to chemical constitution expression Y
2.94Al
4.96O
12: Mn
0.04, Ce
0.06(x=0.04, y=0.06) takes by weighing the Y of purity 〉=99.99%
2O
3, Al
2O
3, CeO
2, MnO
2Raw material grinds and mixes, and briquetting is transferred in the Medium frequency induction single crystal growing furnace behind 1100 ℃ of pre-burning 12h, and tightness system was evacuated to 10 after shove charge was finished
-4Pa, when furnace temperature arrives 1400 ℃, pass into purity greater than 99% nitrogen, be warming up to 1850 ℃ in that this atmosphere relaying is continuous, be incubated 2 hours, until raw materials melt, pass through again the process pulling growth bivalent manganese doped yttrium aluminum garnet monocrystalline such as inoculation, shouldering, isometrical, ending by the regulating stove bore temperature.Crystal growth direction is＜111〉direction, and after growth finished, to room temperature, cooling finished to obtain manganese cerium co-doped yttrium aluminium garnet monocrystalline with the speed slow cooling of 20 ℃/h.The crystal entire body takes on a red color, transparent complete flawless, and quality is better.The spectrum relative energy scatter chart of gained monocrystalline cuts this monocrystalline gained wafer and rated output and is the blue chip coupling of 1W and make white light LEDs as shown in Figure 3, and colour temperature is 4870K.
Embodiment 3.
According to chemical constitution expression Y
2.94Al
4.92O
12: Mn
0.08, Ce
0.06(x=0.08, y=0.06) takes by weighing the Y of purity 〉=99.99%
2O
3, Al
2O
3, CeO
2, MnO
2Raw material grinds and mixes, and briquetting is transferred in the Medium frequency induction single crystal growing furnace behind 1200 ℃ of pre-burning 12h, and tightness system was evacuated to 10 after shove charge was finished
-4Pa, when furnace temperature arrives 1400 ℃, pass into purity greater than 99% nitrogen, be warming up to 1900 ℃ in that this atmosphere relaying is continuous, be incubated 1 hour, until raw materials melt, pass through again the process pulling growth bivalent manganese doped yttrium aluminum garnet monocrystalline such as inoculation, shouldering, isometrical, ending by the regulating stove bore temperature.Crystal growth direction is＜111〉direction, and after growth finished, to room temperature, cooling finished to obtain manganese cerium co-doped yttrium aluminium garnet monocrystalline with the speed slow cooling of 25 ℃/h.Crystal upper part takes on a red color transparent, and it is orange translucent that lower part is, the complete flawless of entire body, and quality is better.The utilizing emitted light spectrogram of obtained monocrystalline as shown in Figure 4.
Embodiment 4.
According to chemical constitution expression Y
2.94Al
4.88O
12: Mn
0.12, Ce
0.06(x=0.12, y=0.06) takes by weighing the Y of purity 〉=99.99%
2O
3, Al
2O
3, CeO
2, MnO
2Raw material grinds and mixes, and briquetting is transferred in the Medium frequency induction single crystal growing furnace behind 1300 ℃ of pre-burning 15h, and tightness system was evacuated to 10 after shove charge was finished
-2Pa, when furnace temperature arrives 1400 ℃, pass into purity greater than 99% argon gas, in this atmosphere, be heated to 1900 ℃, be incubated 3 hours, until raw materials melt, pass through again the process pulling growth bivalent manganese doped yttrium aluminum garnet monocrystalline such as inoculation, shouldering, isometrical, ending by the regulating stove bore temperature.Crystal growth direction is＜111〉direction, and after growth finished, to room temperature, cooling finished to obtain manganese cerium co-doped yttrium aluminium garnet monocrystalline with the speed slow cooling of 25 ℃/h.Part is darkorange on the crystal, and lower part is the national defence look, the complete flawless of entire body, and quality is better.Prepared monocrystalline is at electrical parameter 3V, 350mA, and the CIE chromaticity diagram of test gained is as shown in Figure 5 under 150 ℃ of conditions.
Embodiment 5.
According to chemical constitution expression Y
3Al
4.96O
12: Mn
0.04(x=0.04) take by weighing the Y of purity 〉=99.99%
2O
3, Al
2O
3, MnO
2Raw material grinds and mixes, and briquetting is transferred in the Medium frequency induction single crystal growing furnace together with seed crystal behind 1200 ℃ of pre-burning 24h, and tightness system was evacuated to 10 after shove charge was finished
-4Pa, when furnace temperature arrives 1300 ℃, pass into purity greater than 99% nitrogen, be warming up to 1800 ℃ in that this atmosphere relaying is continuous, be incubated 2 hours, until raw materials melt, pass through again the process pulling growth bivalent manganese doped yttrium aluminum garnet monocrystalline such as inoculation, shouldering, isometrical, ending by the regulating stove bore temperature.Crystal growth direction is＜111〉direction, and after growth finished, to room temperature, cooling finished to obtain manganese list doped yttrium aluminum garnet monocrystalline with the speed slow cooling of 20 ℃/h.Crystal entire body pinkiness, transparent complete flawless, quality is better.
Claims (6)
1. a manganese doped yttrium aluminum garnet monocrystal material is characterized in that the chemical constitution expression of described manganese doped yttrium aluminum garnet monocrystal material is: Y
3-yAl
5-xO
12: Mn
x, Ce
y, wherein the span of x is 0.01≤x≤0.12, the span of y is 0≤y≤0.1; Described manganese doped yttrium aluminum garnet monocrystal material is by the preparation of melt vertical pulling method, and the preparation method comprises the steps:
1. with raw material Y
2O
3, Al
2O
3, CeO
2, MnO
2Or Y
2O
3, Al
2O
3, MnO
2By the accurate weighing of chemical constitution, mix rear briquetting, in 1100-1300 ℃ of pre-burning 12-24h; Wherein guarantee raw material Y
2O
3, Al
2O
3Purity 〉=99.99%, CeO
2, MnO
2Purity 〉=99.9%;
2. the product after the pre-burning and seed crystal are transferred in the crystal furnace, are evacuated to 10 after the sealing
-2-10
-4Pa passes into inert protective gas when furnace temperature arrives 1000-1300 ℃, continue to be warming up to design temperature, and described design temperature is in 1700-2000 ℃ scope; After the furnace temperature of crystal furnace reaches design temperature, be incubated 1-3 hour, make raw material fusing by the regulating stove bore temperature, roasting seed crystal is through process pulling growth manganese doped yttrium aluminum garnet monocrystalline such as inoculation, shouldering, isometrical, endings;
3. after crystal growth finishes, with the speed slow cooling of 20-80 ℃/h, take out crystal after being down to room temperature, obtain manganese doped yttrium aluminum garnet monocrystal material.
2. manganese doped yttrium aluminum garnet monocrystal material as claimed in claim 1, it is characterized in that: the span of x is 0.01≤x≤0.08, the span of y is 0≤y≤0.06.
3. by claim 1 or 2 described manganese doped yttrium aluminum garnet monocrystal materials, it is characterized in that crystal growth direction is＜111〉direction.
4. by claim 1 or 2 described manganese doped yttrium aluminum garnet monocrystal materials, it is characterized in that described inert protective gas is purity greater than 99% Ar or N
2
5. by claim 1 or 2 described manganese doped yttrium aluminum garnet monocrystal materials, it is characterized in that preferred design temperature is in 1800-1900 ℃ scope.
6. by the application of manganese doped yttrium aluminum garnet monocrystal material claimed in claim 1 as fluorescent material and blue chip coupling preparation white light LED part.
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Cited By (7)
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|---|---|---|---|---|
| CN103469298A (en) * | 2013-08-22 | 2013-12-25 | 昆山开威电子有限公司 | Growth method of cerium-doped yttrium aluminium garnet single crystal by adopting kyropoulos method and high-temperature furnace |
| CN104357899A (en) * | 2014-11-21 | 2015-02-18 | 中国电子科技集团公司第二十六研究所 | Kyropoulos method-based preparation method of large-size Yb-YAG laser crystals |
| CN105331364A (en) * | 2015-10-12 | 2016-02-17 | 杭州电子科技大学 | YAG:Mn red phosphor, preparation method and applications thereof |
| CZ307024B6 (en) * | 2014-05-05 | 2017-11-22 | Crytur, Spol.S R.O. | A light source |
| CN107541780A (en) * | 2016-06-29 | 2018-01-05 | 安徽中科镭泰激光科技有限公司 | Garnet matrix colour jewel and its growing method |
| CN111205081A (en) * | 2020-01-21 | 2020-05-29 | 徐州凹凸光电科技有限公司 | Single-structure type low-color-temperature high-color-rendering-index fluorescent ceramic and preparation method and application thereof |
| CN112266239A (en) * | 2020-10-19 | 2021-01-26 | 徐州凹凸光电科技有限公司 | High-thermal-stability high-color-rendering-index fluorescent ceramic for white light LED/LD and preparation method thereof |
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| CN103469298A (en) * | 2013-08-22 | 2013-12-25 | 昆山开威电子有限公司 | Growth method of cerium-doped yttrium aluminium garnet single crystal by adopting kyropoulos method and high-temperature furnace |
| CZ307024B6 (en) * | 2014-05-05 | 2017-11-22 | Crytur, Spol.S R.O. | A light source |
| CN104357899A (en) * | 2014-11-21 | 2015-02-18 | 中国电子科技集团公司第二十六研究所 | Kyropoulos method-based preparation method of large-size Yb-YAG laser crystals |
| CN105331364A (en) * | 2015-10-12 | 2016-02-17 | 杭州电子科技大学 | YAG:Mn red phosphor, preparation method and applications thereof |
| CN105331364B (en) * | 2015-10-12 | 2017-09-05 | 杭州电子科技大学 | A kind of YAG：Mn red fluorescence powders with and its preparation method and application |
| CN107541780A (en) * | 2016-06-29 | 2018-01-05 | 安徽中科镭泰激光科技有限公司 | Garnet matrix colour jewel and its growing method |
| CN111205081A (en) * | 2020-01-21 | 2020-05-29 | 徐州凹凸光电科技有限公司 | Single-structure type low-color-temperature high-color-rendering-index fluorescent ceramic and preparation method and application thereof |
| CN112266239A (en) * | 2020-10-19 | 2021-01-26 | 徐州凹凸光电科技有限公司 | High-thermal-stability high-color-rendering-index fluorescent ceramic for white light LED/LD and preparation method thereof |
| CN112266239B (en) * | 2020-10-19 | 2022-11-25 | 徐州凹凸光电科技有限公司 | High-thermal-stability high-color-rendering-index fluorescent ceramic for white light LED/LD and preparation method thereof |
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