CN103215646A - Novel production method of c-orientation sapphire single crystal - Google Patents
Novel production method of c-orientation sapphire single crystal Download PDFInfo
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- CN103215646A CN103215646A CN2013101129265A CN201310112926A CN103215646A CN 103215646 A CN103215646 A CN 103215646A CN 2013101129265 A CN2013101129265 A CN 2013101129265A CN 201310112926 A CN201310112926 A CN 201310112926A CN 103215646 A CN103215646 A CN 103215646A
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Abstract
The invention discloses a novel production method of a c-orientation sapphire single crystal. The novel production method comprises the following steps of: placing c-orientation sapphire seed crystals in the seed crystal groove of a crucible; filling high-purity aluminum oxide raw materials; vacuumizing and subsequently heating to completely melt the aluminum oxide raw materials and partially melt the seed crystals; slowly cooling at a speed of 0.01-10DEG C/h; controlling a solid-liquid interface to a plane having a certain angle with a c-surface; annealing at a cooling speed of 2-50 DEG C/h after the growth of the crystals is ended; and cooling to the room temperature and subsequently taking the crystal out. According to the invention, by adopting a method for deviating a crucible symmetry axis, a heater symmetry axis and a lateral reflecting screen symmetry axis, the solid-liquid interface in the growth process of the sapphire single crystal is a plane having a certain angle with the c-surface, and the material utilization rate of grown c-orientation crystal ingots can be greatly improved in comparison with the material utilization rate of a-orientation crystal ingots; and compared with the traditional growth method of the c-orientation crystal ingots, the crystal quality of the crystal ingots can be improved and the distortions of crystal boundaries and crystal lattices normally occurring during the growth of the c-orientation crystal ingots can be reduced.
Description
Technical field
The present invention relates to the Sapphire Crystal Growth technical field, relate in particular to a kind of new method for producing of c orientation sapphire single-crystal.
Background technology
Sapphire (Sapphire) is a kind of aluminum oxide (α-Al
2O
3) monocrystalline, be called corundum again, crystal has excellent optical property, mechanical property and chemical stability, the intensity height, hardness is big, anti-washes away, can under near 2000 ℃ of pyritous mal-conditions, work, thereby be widely used in the window material of infrared military installation, satellite spatial technology, high intensity laser beam.Its unique crystalline network, excellent mechanical property, good thermal property make sapphire crystal become the semi-conductor GaN/Al of practical application
2O
3Photodiode (LED), ideal substrate materials such as large-scale integrated circuit SOI and SOS and superconducting nano structural membrane.In recent years, along with development of modern science and technology, new requirement is proposed constantly for size, the quality of sapphire crystal material.For example, American National natural science fund committee is as LIGO(Laser Interferometer Gravitational Wave Observatory) sapphire crystal used of beam splitting lens in the works, crystalline size: ￠ 350 * 120mm, optical homogeneity: △ n＜2 * 10
-7, low light level uptake factor (1064nm): 10
-6/ cm; The window material of infrared imaging detection equipment, lowest calibre are ￠ 150mm, the service band transmitance〉80%.In addition, consideration based on process redundancy in the actual course of processing and saturating ripple direction, the sapphire single-crystal base substrate must have certain physical dimension can satisfy above-mentioned requirements, so low-cost, growing large-size sapphire single-crystal has become the current urgent task that faces in high quality.
The c surface sapphire substrate is having a wide range of applications aspect the making GaN base LED.At present kyropoulos growth a axial cylindrical shape sapphire crystal ingots that adopt are drawn rod and can be obtained c to crystal bar more along the side, obtain the c surface sapphire substrate after the slice processing, but this method sapphire utilization ratio is lower; Growth c orientation sapphire can be drawn rod from the crystal ingot top, this has improved greatly and excellent rate, but owing to sapphire along c to when growth plastic zone, solid-liquid interface place slippage easily takes place produces a large amount of dislocations, dislocation is gathered also can form crystal boundary, so c is slow and defect concentration is high to the speed of growth than a to growth.
C adopts crystal pulling method to carry out c to growth to the sapphire crystal ingot more at present, Kyocera company, the Sino-U.S. silicon wafer goods limited-liability company of Taiwan, the Chongqing tetrad sapphire company limited of Japan have all realized 4 inches sapphire Czochralski growns, but dislocation desity is up to 104/cm
-2, and further increased in size is comparatively difficult.Korea S STC Corporation adopts the VHGF method, and a carries out c to drawing rod then to growth rectangular parallelepiped sapphire, can only accomplish 6 inches at present, because this method is comparatively special to the thermal field requirement, the thermal field design is the more bottleneck of large-size sapphire of growing.
Yunnan aquamaine Science and Technology Ltd. adopts falling crucible method to realize 6 inches c to sapphire growth, but this method can't overcome the difficulty that c exists to growing sapphire.U.S. ARC Energy company has also adopted similar method, its crucible bottom adopts the helium cooling, can prevent the seed crystal fusing of crucible bottom like this, change molten intravital temperature field simultaneously, solid-liquid interface when making crystal growth is protruding in melt, this moment the solid-liquid interface place the plastic zone suffered be shearing stress along solid-liquid interface, and this moment, solid-liquid interface no longer was the c face, therefore be difficult for slippage takes place, the falling crucible method that this method is more simple can obtain higher crystal mass.But the speed of growth is slow, and less to the variable range of solid-liquid interface and c face angulation.
Therefore, at above-mentioned technical problem, be necessary to provide a kind of method that can high quality c oriented growth sapphire single-crystal, to overcome above-mentioned defective.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of new method for producing of c orientation sapphire single-crystal, defectives such as the crystal boundary that is prone in the elimination c orientation Sapphire Crystal Growth process, lattice distortion, thus realize that high quality c is orientated the growth of sapphire single-crystal.
For achieving the above object, the invention provides following technical scheme:
Core design thought of the present invention is, by the angle of change solid-liquid interface and c axle, thereby avoids translation gliding in the long brilliant process, and then obtains high-quality target product.
The new method for producing of c orientation sapphire single-crystal of the present invention specifically may further comprise the steps:
In the seed slot of crucible, place c orientation sapphire seed crystal, fill the high purity aluminium oxide raw material, vacuumize post-heating, alumina raw material is all melted, the seed crystal partial melting is slowly lowered the temperature with the speed of 0.01 ℃/h～10 ℃/h, and solid-liquid interface is controlled to be and c face plane at an angle, treat that crystal growth finishes the rate of temperature fall annealing of back with 2 ℃/h～50 ℃/h, take out crystal after being cooled to room temperature.
Concrete, three symmetry axis by crucible, well heater, lateral reflection screen do not overlap solid-liquid interface are tilted, thereby solid-liquid interface is controlled to be and c face plane at an angle.
Further, the radiation shield by placing a truncated cone-shaped on the crucible top is to reduce the radial symmetry gradient of crystal and melt, and making solid-liquid interface is a plane; And/or to make well heater be the big truncated conical shape of the little lower ending opening of upper end open to increase axial-temperature gradient; And/or make lateral reflection screen for the big truncated conical shape of the little lower ending opening of upper end open increasing axial-temperature gradient, thereby solid-liquid interface is controlled to be and c face plane at an angle.
Preferably, described vacuum is meant the enclosed environment that 5Pa is following.
Preferably, the described well heater that adds thermal recovery is birdcage shape, netted tubular tungsten well heater or tubular graphite heater.
Further, described heater diameter is 100mm～2000mm, highly is 100mm～3000mm.
Preferably, the angle between described solid-liquid interface normal and the crucible symmetry axis is 0～80 °.
Preferably, described crucible is tungsten crucible, molybdenum crucible, miramint crucible or iridium crucible.
Further, described crucible bottom form be in the right angle, fillet or chamfering form.
Preferably, described c orientation sapphire seed crystal diameter is 10mm～60mm, highly is 10mm～100mm, and described seed slot diameter is 10mm～60mm, and the degree of depth is 2mm～20mm.
Preferably, described high purity aluminium oxide raw material is preferably from Al
2O
3Powder, Al
2O
3Biscuit, granular Al
2O
3And any one or two or more combinations in the sapphire broken grain.
From technique scheme as can be seen, the present invention has adopted the method that crucible symmetry axis, well heater symmetry axis, lateral reflection screen symmetry axis are departed from, make in the Sapphire Crystal Growth process solid-liquid interface be a plane and with the c face at an angle, the c of growth can improve the material use efficiency of crystal ingot greatly to crystal ingot than a to crystal ingot; More traditional c promptly reduces growth c to normal crystal boundary and the lattice distortion that occurs of crystal ingot to the crystal mass that the crystal ingot growth method can improve crystal ingot.
Description of drawings
In order to be illustrated more clearly in the technical scheme in the embodiment of the invention, the accompanying drawing of required use is done to introduce simply in will describing embodiment below, apparently, accompanying drawing relevant of the present invention in describing below only is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the synoptic diagram that adopts the inventive method growth c orientation sapphire single-crystal, and wherein, Fig. 1 a is a sectional view, and Fig. 1 b is a vertical view;
Fig. 2 is the synoptic diagram that the present invention adopts the big truncated conical shape well heater growth c orientation sapphire single-crystal of the little lower ending opening of upper end open;
Fig. 3 is the synoptic diagram that the present invention adopts the big truncated conical shape lateral reflection screen growth c orientation sapphire single-crystal of the little lower ending opening of end opening;
More than assembly and Reference numeral thereof among each figure be respectively: well heater 1, crucible 2, alumina melt 3, solid-liquid interface 4, sapphire crystal 5, seed slot 21, helium tube 6.
Embodiment
As previously mentioned, many defectives at prior art, this case contriver is intended to propose a kind of new method for producing of c orientation sapphire single-crystal, this method mainly comprise place seed crystal (seed crystal is put into crucible bottom), feed, vacuumize, start helium, add the thermalization material, crystal growth, cooling annealing and operation such as come out of the stove.
More specifically, aforementioned technological process is as follows:
(1) places seed crystal: c is orientated in the seed slot that seed crystal is placed on crucible;
(2) charging: the high purity aluminium oxide raw material is put into crucible, close bell;
(3) vacuumize: start vacuum system, preferably furnace chamber pressure is evacuated to below the 5Pa;
(4) start helium: start helium cooling system, regulate helium gas flow;
(5) add the thermalization material: start heating system and heat up, begin fusing until high purity aluminium oxide, with the position of tungsten tipped probe detection solid-liquid interface, the control temperature rise rate makes the seed crystal partial melting;
(6) crystal growth: slowly cooling cooperation change helium gas flow control solid-liquid interface is a normal and crucible symmetry axis direction plane at an angle, until the whole crystallizations of all melts;
(7) cooling annealing: progressively improve rate of temperature fall and make crystal be cooled to room temperature;
(8) come out of the stove: treat to open bell taking-up crystal after temperature is reduced to room temperature.
Particularly, described crucible can be selected from but be not limited to tungsten crucible, molybdenum crucible, miramint crucible, iridium crucible etc., and the crucible bottom form can be selected from but be not limited to right angle, fillet, chamfering form.
Described high purity aluminium oxide raw material can be selected from but be not limited to Al
2O
3Powder, Al
2O
3Biscuit, granular Al
2O
3And the sapphire broken grain etc.
Described c orientation sapphire seed crystal diameter is 10mm～60mm, highly is 10mm～100mm.
It is circulation power that described helium cooling system preferably adopts helium compressor, and helium adopts water coolant to cool off.Certainly, those skilled in the art also can adopt other the various refrigerating units or the cooling structure of commonly seeing according to the needs of practical application, as long as it can reach the purpose that the temperature of seed crystal is controlled.
The material of described well heater can be selected from but be not limited to graphite, tungsten, and form can be selected from but be not limited to sheet, bar-shaped and netted.
Below in conjunction with the accompanying drawing in the embodiment of the invention, the technical scheme in the embodiment of the invention is described in detail, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, the every other embodiment that those of ordinary skills are obtained under the prerequisite of not making creative work belongs to the scope of protection of the invention.
Adopt the thermal field shown in the accompanying drawing 1 to carry out the growth of c orientation sapphire single-crystal.
Three symmetry axis by crucible, well heater, lateral reflection screen do not overlap solid-liquid interface are tilted, thereby solid-liquid interface is controlled to be and c face plane at an angle, and its technological process is specific as follows:
(1) places seed crystal: c is orientated in the seed slot that seed crystal is placed on crucible;
(2) charging: 20～100kg high purity aluminium oxide raw material is put into crucible, close bell, start cooling water recirculation system;
(3) vacuumize: start vacuum system, furnace chamber pressure is evacuated to 4Pa;
(4) start helium: start helium cooling system, the adjusting helium gas flow is 40～100slm, and seed crystal melts fully in the preventing material process;
(5) add the thermalization material: start heating system and heat up, begin fusing, survey the position of solid-liquid interface, (0.5 ℃/h～500 ℃/h) make the seed crystal partial melting of control temperature rise rates with tungsten tipped probe until high purity aluminium oxide;
(6) crystal growth: slowly cooling, 0.01 ℃/h of rate of temperature fall～10 ℃/h, cooperate to change helium gas flow control solid-liquid interface and be a normal and the crucible symmetry axis direction plane of (angle between solid-liquid interface normal and the crucible symmetry axis is 0～80 °) at an angle, until the whole crystallizations of all melts;
(7) cooling annealing: progressively improve (2 ℃/h～50 ℃/h) make crystal be cooled to room temperature of rate of temperature fall;
(8) come out of the stove: treat to open bell taking-up crystal after temperature is reduced to room temperature.
Adopt the thermal field shown in the accompanying drawing 2 to carry out the growth of c orientation sapphire single-crystal.
Three symmetry axis by crucible, well heater, lateral reflection screen do not overlap solid-liquid interface are tilted, radiation shield by placing a truncated cone-shaped on the crucible top is to reduce the radial symmetry gradient of crystal and melt, making solid-liquid interface is a plane, making well heater is that the big truncated conical shape of the little lower ending opening of upper end open is to increase axial-temperature gradient, thereby solid-liquid interface is controlled to be and c face plane at an angle, and its technological process is specific as follows:
(1) places seed crystal: c is orientated in the seed slot that seed crystal is placed on crucible;
(2) charging: 20～100kg high purity aluminium oxide raw material is put into crucible, close bell, start cooling water recirculation system;
(3) vacuumize: start vacuum system, furnace chamber pressure is evacuated to 4Pa;
(4) start helium: start helium cooling system, the adjusting helium gas flow is 40～100slm, and seed crystal melts fully in the preventing material process;
(5) add the thermalization material: start heating system and heat up, begin fusing, survey the position of solid-liquid interface, (0.5 ℃/h～500 ℃/h) make the seed crystal partial melting of control temperature rise rates with tungsten tipped probe until high purity aluminium oxide;
(6) crystal growth: slowly cooling, 0.01 ℃/h of rate of temperature fall～10 ℃/h, cooperate to change helium gas flow control solid-liquid interface and be a normal and the crucible symmetry axis direction plane of (angle between solid-liquid interface normal and the crucible symmetry axis is 0～80 °) at an angle, until the whole crystallizations of all melts;
(7) cooling annealing: progressively improve (2 ℃/h～50 ℃/h) make crystal be cooled to room temperature of rate of temperature fall;
(8) come out of the stove: treat to open bell taking-up crystal after temperature is reduced to room temperature.
Adopt the thermal field shown in the accompanying drawing 3 to carry out the growth of c orientation sapphire single-crystal.
Three symmetry axis by crucible, well heater, lateral reflection screen do not overlap solid-liquid interface are tilted, radiation shield by placing a truncated cone-shaped on the crucible top is to reduce the radial symmetry gradient of crystal and melt, making solid-liquid interface is a plane, making the lateral reflection screen is that the big truncated conical shape of the little lower ending opening of upper end open is to increase axial-temperature gradient, thereby solid-liquid interface is controlled to be and c face plane at an angle, and its technological process is specific as follows:
(1) places seed crystal: c is orientated in the seed slot that seed crystal is placed on crucible;
(2) charging: 20～100kg high purity aluminium oxide raw material is put into crucible, close bell, start cooling water recirculation system;
(3) vacuumize: start vacuum system, furnace chamber pressure is evacuated to 4Pa;
(4) start helium: start helium cooling system, the adjusting helium gas flow is 40～100slm, and seed crystal melts fully in the preventing material process;
(5) add the thermalization material: start heating system and heat up, begin fusing, survey the position of solid-liquid interface, (0.5 ℃/h～500 ℃/h) make the seed crystal partial melting of control temperature rise rates with tungsten tipped probe until high purity aluminium oxide;
(6) crystal growth: slowly cooling, 0.01 ℃/h of rate of temperature fall～10 ℃/h, cooperate to change helium gas flow control solid-liquid interface and be a normal and the crucible symmetry axis direction plane of (angle between solid-liquid interface normal and the crucible symmetry axis is 0～80 °) at an angle, until the whole crystallizations of all melts;
(7) cooling annealing: progressively improve (2 ℃/h～50 ℃/h) make crystal be cooled to room temperature of rate of temperature fall;
(8) come out of the stove: treat to open bell taking-up crystal after temperature is reduced to room temperature.
In sum, the present invention is by changing the angle of solid-liquid interface and c axle, thereby avoid translation gliding in the long brilliant process, and then obtain high-quality target product, the present invention has adopted the method that crucible symmetry axis, well heater symmetry axis, lateral reflection screen symmetry axis are departed from, make in the c orientation Sapphire Crystal Growth process solid-liquid interface be a plane and with the c face at an angle, can effectively avoid the slippage in the c axle sapphire growth process like this, thereby reduce generation of defects such as dislocation, crystal boundary in the long brilliant process.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and under the situation that does not deviate from spirit of the present invention or essential characteristic, can realize the present invention with other specific form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims rather than above-mentioned explanation, therefore is intended to include in the present invention dropping on the implication that is equal to important document of claim and all changes in the scope.Any Reference numeral in the claim should be considered as limit related claim.
In addition, be to be understood that, though this specification sheets is described according to embodiment, but be not that each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets only is for clarity sake, those skilled in the art should make specification sheets as a whole, and the technical scheme among each embodiment also can form other embodiments that it will be appreciated by those skilled in the art that through appropriate combination.
Claims (10)
1. the new method for producing of a c orientation sapphire single-crystal is characterized in that, comprises the steps:
In the seed slot of crucible, place c orientation sapphire seed crystal, fill the high purity aluminium oxide raw material, vacuumize post-heating, alumina raw material is all melted, the seed crystal partial melting is slowly lowered the temperature with the speed of 0.01 ℃/h～10 ℃/h, and solid-liquid interface is controlled to be and c face plane at an angle, treat that crystal growth finishes the rate of temperature fall annealing of back with 2 ℃/h～50 ℃/h, take out crystal after being cooled to room temperature.
2. production method according to claim 1 is characterized in that: three symmetry axis by crucible, well heater, lateral reflection screen do not overlap solid-liquid interface are tilted, thereby solid-liquid interface is controlled to be and c face plane at an angle.
3. production method according to claim 2 is characterized in that: the radiation shield by placing a truncated cone-shaped on the crucible top is to reduce the radial symmetry gradient of crystal and melt, and making solid-liquid interface is a plane; And/or to make well heater be the big truncated conical shape of the little lower ending opening of upper end open to increase axial-temperature gradient; And/or make lateral reflection screen for the big truncated conical shape of the little lower ending opening of upper end open increasing axial-temperature gradient, thereby solid-liquid interface is controlled to be and c face plane at an angle.
4. production method according to claim 1 is characterized in that: described vacuum is meant the enclosed environment that 5Pa is following.
5. production method according to claim 1 is characterized in that: the described well heater that adds thermal recovery is birdcage shape, netted tubular tungsten well heater or tubular graphite heater.
6. production method according to claim 5 is characterized in that: described heater diameter is 100mm～2000mm, highly is 100mm～3000mm.
7. production method according to claim 1 is characterized in that: the angle between described solid-liquid interface normal and the crucible symmetry axis is 0～80 °.
8. production method according to claim 5 is characterized in that: described crucible is tungsten crucible, molybdenum crucible, miramint crucible or iridium crucible, described crucible bottom form be in the right angle, fillet or chamfering form.
9. production method according to claim 5 is characterized in that: described c orientation sapphire seed crystal diameter is 10mm～60mm, highly is 10mm～100mm, and described seed slot diameter is 10mm～60mm, and the degree of depth is 2mm～20mm.
10. production method according to claim 5 is characterized in that: described high purity aluminium oxide raw material is preferably from Al
2O
3Powder, Al
2O
3Biscuit, granular Al
2O
3And any one or two or more combinations in the sapphire broken grain.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104120487A (en) * | 2013-08-23 | 2014-10-29 | 江苏中电振华晶体技术有限公司 | Growth method and growth equipment of platelike sapphire crystals |
| CN105088331A (en) * | 2015-08-26 | 2015-11-25 | 哈尔滨工业大学 | Small-corner crucible for growing sapphire single crystal in C- direction |
| CN105185896A (en) * | 2015-06-18 | 2015-12-23 | 江苏苏创光学器材有限公司 | Sapphire LED filament production method |
| CN105185877A (en) * | 2015-06-18 | 2015-12-23 | 江苏苏创光学器材有限公司 | Sapphire LED filament preparation method |
| CN105297130A (en) * | 2014-06-03 | 2016-02-03 | 长春理工大学 | Method and device for orientated growth of fluoride crystals by bridgman method |
| CN105369345A (en) * | 2015-12-03 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Crucible and preparation method for preparing sapphire single crystals |
| CN105648520A (en) * | 2016-03-18 | 2016-06-08 | 江苏中电振华晶体技术有限公司 | Seed crystal capable of reinforcing seeding temperature signals and seeding method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104120487A (en) * | 2013-08-23 | 2014-10-29 | 江苏中电振华晶体技术有限公司 | Growth method and growth equipment of platelike sapphire crystals |
| CN105297130A (en) * | 2014-06-03 | 2016-02-03 | 长春理工大学 | Method and device for orientated growth of fluoride crystals by bridgman method |
| CN105185896A (en) * | 2015-06-18 | 2015-12-23 | 江苏苏创光学器材有限公司 | Sapphire LED filament production method |
| CN105185877A (en) * | 2015-06-18 | 2015-12-23 | 江苏苏创光学器材有限公司 | Sapphire LED filament preparation method |
| CN105088331A (en) * | 2015-08-26 | 2015-11-25 | 哈尔滨工业大学 | Small-corner crucible for growing sapphire single crystal in C- direction |
| CN105088331B (en) * | 2015-08-26 | 2017-10-13 | 哈尔滨工业大学 | A kind of C is to growing sapphire monocrystalline with small angle crucible |
| CN105369345A (en) * | 2015-12-03 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Crucible and preparation method for preparing sapphire single crystals |
| CN105369345B (en) * | 2015-12-03 | 2018-01-26 | 河南西格马晶体科技有限公司 | A kind of crucible and preparation method for being used to prepare sapphire monocrystal |
| CN105648520A (en) * | 2016-03-18 | 2016-06-08 | 江苏中电振华晶体技术有限公司 | Seed crystal capable of reinforcing seeding temperature signals and seeding method thereof |
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Application publication date: 20130724 |