CN103469298A - Growth method of cerium-doped yttrium aluminium garnet single crystal by adopting kyropoulos method and high-temperature furnace - Google Patents
Growth method of cerium-doped yttrium aluminium garnet single crystal by adopting kyropoulos method and high-temperature furnace Download PDFInfo
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- CN103469298A CN103469298A CN2013103698326A CN201310369832A CN103469298A CN 103469298 A CN103469298 A CN 103469298A CN 2013103698326 A CN2013103698326 A CN 2013103698326A CN 201310369832 A CN201310369832 A CN 201310369832A CN 103469298 A CN103469298 A CN 103469298A
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Abstract
The invention discloses a growth method of a cerium-doped yttrium aluminium garnet single crystal by adopting a kyropoulos method and a high-temperature furnace. The single crystal can be applicable to the field of white-light LEDs. The chemical formula of the single crystal is (Y1-x-mAxCem)3(A11-yBy)5O12, wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, m is more than or equal to 0 and less than or equal to 0.05, A is one of Lu, Tb, Pr, La, Gd and Sm, and B is one of Ga, Ti, Mn, Cr and Zr. The growth process of the crystal comprises the following steps: preparing materials; mixing materials; pressing materials; sintering materials; performing vacuum pumping for a furnace body; increasing heating power at the velocity of 1.5 to 4KW/h until raw materials are fused; performing heat preservation for several hours; dropping seed crystals so as to enable the seed crystals to be positioned 5 to 10 mm above a melt liquid level; performing crystal transformation, and keeping the revolving speed at 2 to 15t/min; dropping the seed crystals again so as to enable the lower ends of the seed crystals to be contacted with melt; starting seeding and shouldering; adjusting the heating power appropriately, so that crystal growth is completed; adjusting the heating power and dropping temperature; performing in-situ annealing at the temperature of 1500 DEG C; then adjusting the heat power again until the temperature in the furnace drops to indoor temperature; opening the furnace and taking the crystal out of the furnace.
Description
Technical field
The present invention relates to LED and manufacture field, relate in particular to a kind of method of kyropoulos growth cerium-doped yttrium aluminum garnet single crystal fluorescent material.
Background technology
LED is a kind of solid-state semiconducter device, and it can be electric energy conversion directly luminous energy.With traditional incandescent light, luminescent lamp, compare, white light LEDs has the advantages such as current consumption is little, luminous efficiency is high, long service life, energy-conserving and environment-protective, not only in the normal lighting field, is widely used, and has entered the demonstration field.At present, the technology of obtaining white light LEDs can be divided into two large classes: (1) adopts three kinds of LED chips of emission red, green, blue coloured light line to mix; (2) adopt monochromatic (blue light or ultraviolet) LED chip to excite the gold-tinted fluorescent material.White light LEDs is mainly to utilize the cerium-doped yttrium aluminum garnet fluorescent powder of blue-light LED chip and Yellow light-emitting low temperature in conjunction with obtaining at present.
White light LEDs for the gold-tinted fluorescent powder packaging, because fluorescent material is close to chip, the chip temperature rising can directly cause the light-emitting phosphor Efficiency Decreasing, and the heat that chip distributes simultaneously and short-wave radiation can make the packaged material accelerated deterioration cause transmitance to descend, and shorten the life-span of white light LEDs.In addition, fluorescent material is skewness in colloid, is prone to the inconsistent problem of white light quality of white light LED part.And yttrium-aluminum garnet single crystal compares fluorescent material and have the advantages such as excitation-emission efficiency is high, Heat stability is good, thermal conductivity is high, physical strength good, optical homogeneity is good, be suitable as very much the equivalent material of conventional fluorescent powder.
Traditional cerium-doped yttrium aluminum garnet method for monocrystal growth is mainly crystal pulling method and warm terraced method.Crystal pulling method is most widely used at present, but the method there are the following problems in actual applications: 1) crystalline size is restricted, and it is 3～4 inches that crystal pulling method only can grow diameter usually, the crystal that length is about 200mm; 2) matter crystal internal defect is more, easily produces more dislocation and bubble.The crystal that Chinese Academy of Sciences's Shanghai ray machine has adopted warm terraced method to grow more than diameter 100mm, but also there are some defects in this method: and 1) crystal of warm terraced method growth directly contacts with sidewall of crucible, causes the crystals internal stress bigger than normal, easily cracking; 2) warm terraced method adopts graphite heater, and in process of growth, carbon atom can enter crystal lattices in a large number, forms impurity, affects the crystal optics quality.
Summary of the invention
The technical problem to be solved in the present invention is to provide and a kind ofly can overcomes the prior art defect, realizes growth method and the growing apparatus of the yttrium-aluminum garnet single crystal fluorescent material of large size, low cost, defect is few, optical quality is high cerium (rare earth) doping.
For addressing the above problem, the method for a kind of kyropoulos growth cerium-doped yttrium aluminum garnet monocrystalline of the present invention comprises the following steps:
1) raw material is carried out to the weighing proportioning according to the mol ratio in following chemical formula, mix, be pressed into cake, high temperature sintering, put into crucible;
Chemical formula: (Y
1-x-ma
xce
m)
3(Al
1-yb
y)
5o
12
0≤x≤1，0≤y≤1，0≤m≤0.05
Wherein A is a kind of in Lu, Tb, Pr, La, Gd, Sm; B is a kind of in Ga, Ti, Mn, Cr, Zr;
2) put into seed crystal, regulate seed rod, make seed crystal be positioned at the crucible geometric centre;
3) body of heater is evacuated to 5 * 10
-3pa～8 * 10
-3pa, then start heating with the speed of 1.5～4KW/h, until raw material all melts, then is incubated 2～8 hours, makes in melt temperature distribution everywhere tend towards stability;
4) slow decreasing seed crystal, make it drop to the above 5～10mm of melt liquid level, opens crystalline substance and turn, and maintains rotating speed 2～15r/min, and the decline seed crystal makes its lower end in contact melt;
5) carry out seeding, shouldering, the speed of shouldering stage with 0.1～1mm/h lifts seed rod, and the while is with the rate reduction heating power of 1～20W/h; After shouldering finishes, stop lifting, with the rate reduction heating power of 5～40W/h, make crystal maintain a stable speed of growth, when crystal weight stops increasing, complete process of growth;
6) regulate the speed slow decreasing of heating power with 20～80W/h, in stove, during temperature to 1500 ℃, constant temperature carries out in-situ annealing to crystal in 8～12 hours, again regulates afterwards heating power and descends with 80～150W/h speed, until in stove, temperature is reduced to room temperature; Maintain 10～20 hours at room temperature state, then crystal is taken out in blow-on.
In described step 1, the temperature that sinters piece into is 1200 ℃, and sintering time is 12h.
A kind of High Temperature Furnaces Heating Apparatus, comprise body of heater, bell, is provided with crucible in body of heater, and crucible is arranged on pallet, and the crucible periphery is heating element, and heating element is provided with radiation shield outward, and radiation shield is outward thermal insulation layer; The bell upper end is provided with seed rod, seed rod connecting electronic scale and lifting device.
Described heating element is tungsten cage heating element.
The method of kyropoulos growth cerium-doped yttrium aluminum garnet monocrystalline of the present invention compared with prior art, has the following advantages:
1) the method can grow large-sized cerium-doped yttrium aluminum garnet monocrystalline, and maximum weight is more than 20 kilograms, and raw material availability is greater than 85%, can significantly reduce costs;
2) crystal does not contact crucible in process of growth and after the growth end, can effectively reduce crystal stress and reduce the pollution that crucible causes;
3) after seeding finishes, realize static growth, disturbance is little, can effectively reduce the defects such as dislocation;
4) adopt tungsten cage heating element, under vacuum environment, also without any volatilization, guaranteed the clean of growing environment, avoid the pollution of crystal.
The accompanying drawing explanation
Fig. 1 is for the structural representation of the High Temperature Furnaces Heating Apparatus of crystal growth in the present invention;
Relative energy distribution curve when the crystal that Fig. 2 is embodiment 1 growth excites with blue-ray LED;
The printing opacity spectrum of the crystal that Fig. 3 is embodiment 2 growths.
Embodiment
In order to make those skilled in the art person understand better technical solution of the present invention, below in conjunction with drawings and embodiments, the present invention is described in further detail.
A kind of High Temperature Furnaces Heating Apparatus of the present invention, for the cerium-doped yttrium aluminum garnet single crystal fluorescent material of growing by kyropoulos, comprise furnace wall 9, bell 7, be provided with crucible 5 in described body of heater, crucible 5 is arranged on pallet 8, and in crucible 5, for generating crystal 4, crucible 5 peripheries are tungsten cage heating element 6, tungsten cage heating element 6 is outer is provided with radiation shield 3, and radiation shield is outward thermal insulation layer 2; The bell upper end is provided with seed rod 1, seed rod 1 connecting electronic scale and lifting device.
Embodiment mono-:
According to chemical formula (Y
1-mce
m)
3al
5o
12(m=0.01) Raw Y
2o
3, Al
2o
3, CeO
2the mol ratio of powder is carried out the weighing proportioning, and gross weight 15Kg mixes, briquetting, and 1200 ℃ of sintering, the time is 12h; Put into crucible after sintering; The dress seed crystal, regulate seed rod, makes seed crystal be positioned at the crucible geometric centre; Body of heater is evacuated to 6 * 10
-3pa, the speed increase heating power with 3.5KW/h, until raw material all melts, then be incubated 2 hours; The slow decreasing seed crystal, make it drop to the above 5mm of melt liquid level, opens crystalline substance and turn, and maintains rotating speed 2r/min, and the decline seed crystal makes its lower end in contact melt; Suitably regulate heating power, control seed end shape and size, complete the seeding process; Speed with 0.3mm/h lifts seed rod, with the rate reduction heating power of 15W/h, after growing into needed diameter, stops lifting, and slowly reduces rotating speed simultaneously, to finally stopping the rotation; With the rate reduction heating power of 30W/h, make crystal in the stable growth state afterwards, when crystal weight stops increasing, complete process of growth; Regulate the speed slow decreasing of heating power with 30W/h, in stove, temperature is in the time of 1500 ℃, and constant temperature carries out in-situ annealing to crystal in 8 hours, again regulates afterwards heating power and descends with 80W/h speed, until in stove, temperature is reduced to room temperature, after room temperature state maintains 10 hours, crystal is taken out in blow-on.Obtain the crystal yellow transparent, profile is complete, and quality is better.
Embodiment bis-:
According to chemical formula (Y
1-mce
m)
3al
5o
12(m=0.005) Raw Y
2o
3, Al
2o
3, CeO
2the mol ratio of powder is carried out the weighing proportioning, and gross weight 18Kg mixes, briquetting, and 1200 ℃ of sintering, the time is 12h; Put into crucible after sintering; The dress seed crystal, regulate seed rod, makes seed crystal be positioned at the crucible geometric centre; Body of heater is evacuated to 5 * 10
-3pa, the speed increase heating power with 1.5KW/h, until raw material all melts, then be incubated 8 hours; The slow decreasing seed crystal, make it drop to the above 7mm of melt liquid level, opens crystalline substance and turn, and maintains rotating speed 9r/min, and the decline seed crystal makes its lower end in contact melt; Suitably regulate heating power, control seed end shape and size, complete the seeding process; Speed with 0.1mm/h lifts seed rod, with the rate reduction heating power of 1W/h, after growing into needed diameter, stops lifting, and slowly reduces rotating speed simultaneously, to finally stopping the rotation, completes the shouldering process; With the rate reduction heating power of 40W/h, make crystal in the stable growth state afterwards, when crystal weight stops increasing, complete process of growth; Regulate the speed slow decreasing of heating power with 20W/h, in stove, temperature is in the time of 1500 ℃, constant temperature carries out in-situ annealing to crystal in 10 hours, again regulating afterwards heating power descends with 150W/h speed, until in stove, temperature is reduced to room temperature, after room temperature state maintains 12 hours, crystal is taken out in blow-on.Obtain the crystal yellow transparent, profile is complete, and quality is better.
Embodiment tri-:
According to chemical formula (Y
0.99ce
0.01)
3(Al
0.998mn
0.002)
5o
12raw material Y
2o
3, Al
2o
3, CeO
2the mol ratio of powder is carried out the weighing proportioning, and gross weight 22Kg mixes, briquetting, and 1200 ℃ of sintering, the time is 12h; Put into crucible after sintering; The dress seed crystal, regulate seed rod, makes seed crystal be positioned at the crucible geometric centre; Body of heater is evacuated to 8 * 10
-3pa, the speed increase heating power with 4KW/h, until raw material all melts, then be incubated 4 hours; The slow decreasing seed crystal, make it drop to the above 10mm of melt liquid level, opens crystalline substance and turn, and maintains rotating speed 15r/min, and the decline seed crystal makes its lower end in contact melt; Suitably regulate heating power, control seed end shape and size, complete the seeding process; Speed with 1mm/h lifts seed rod, with the rate reduction heating power of 20W/h, after growing into needed diameter, stops lifting, and slowly reduces rotating speed simultaneously, to finally stopping the rotation; With the rate reduction heating power of 5W/h, make crystal in the stable growth state afterwards, when crystal weight stops increasing, complete process of growth; Regulate the speed slow decreasing of heating power with 80W/h, in stove, temperature is in the time of 1500 ℃, constant temperature carries out in-situ annealing to crystal in 12 hours, again regulating afterwards heating power descends with 100W/h speed, until in stove, temperature is reduced to room temperature, after room temperature state maintains 20 hours, crystal is taken out in blow-on.Obtain the inclined to one side yellow-green colour of crystal, transparent complete, quality is better.
Claims (4)
1. the method for kyropoulos growth cerium-doped yttrium aluminum garnet monocrystalline comprises the following steps:
1) raw material is carried out to the weighing proportioning according to the mol ratio in following chemical formula, mix, be pressed into cake, high temperature sintering, put into crucible;
Chemical formula: (Y
1-x-ma
xce
m)
3(Al
1-yb
y)
5o
12
0≤x≤1，0≤y≤1，0≤m≤0.05
Wherein A is a kind of in Lu, Tb, Pr, La, Gd, Sm; B is a kind of in Ga, Ti, Mn, Cr, Zr;
2) put into seed crystal, regulate seed rod, make seed crystal be positioned at the crucible geometric centre;
3) body of heater is evacuated to 5 * 10
-3pa～8 * 10
-3pa, then start heating with the speed of 1.5～4KW/h, until raw material all melts, then is incubated 2～8 hours, makes in melt temperature distribution everywhere tend towards stability;
4) slow decreasing seed crystal, make it drop to the above 5～10mm of melt liquid level, opens crystalline substance and turn, and maintains rotating speed 2～15r/min, and the decline seed crystal makes its lower end in contact melt;
5) carry out seeding, shouldering, the speed of shouldering stage with 0.1～1mm/h lifts seed rod, and the while is with the rate reduction heating power of 1～20W/h; After shouldering finishes, stop lifting, with the rate reduction heating power of 5～40W/h, make crystal maintain a stable speed of growth, when crystal weight stops increasing, complete process of growth;
6) regulate the speed slow decreasing of heating power with 20～80W/h, in stove, during temperature to 1500 ℃, constant temperature carries out in-situ annealing to crystal in 8～12 hours, again regulates afterwards heating power and descends with 80～150W/h speed, until in stove, temperature is reduced to room temperature; Maintain 10～20 hours at room temperature state, then crystal is taken out in blow-on.
2. the method for kyropoulos as claimed in claim 1 growth cerium-doped yttrium aluminum garnet monocrystalline, it is characterized in that: in described step 1, the temperature that sinters piece into is 1200 ℃, and sintering time is 12h.
3. a High Temperature Furnaces Heating Apparatus, for the cerium-doped yttrium aluminum garnet monocrystalline as claimed in claim 1 of growing, is characterized in that: comprise body of heater, bell, be provided with crucible in body of heater, crucible is arranged on pallet, and the crucible periphery is heating element, heating element is provided with radiation shield outward, and radiation shield is outward thermal insulation layer; The bell upper end is provided with seed rod, seed rod connecting electronic scale and lifting device.
4. High Temperature Furnaces Heating Apparatus as claimed in claim 3, it is characterized in that: described heating element is tungsten cage heating element.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105283526A (en) * | 2013-10-23 | 2016-01-27 | 株式会社光波 | Single crystal phosphor, phosphor-containing member and light emitting device |
| CN105483818A (en) * | 2015-12-25 | 2016-04-13 | 邢台晶龙电子材料有限公司 | M2 type monocrystalline silicon shouldering method |
| CN105803516A (en) * | 2015-01-20 | 2016-07-27 | 丰田自动车株式会社 | Single crystal production apparatus |
| JPWO2019181618A1 (en) * | 2018-03-23 | 2021-03-25 | Tdk株式会社 | Fluorescent material and light source device |
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| JPWO2019181618A1 (en) * | 2018-03-23 | 2021-03-25 | Tdk株式会社 | Fluorescent material and light source device |
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Application publication date: 20131225 |