CN203530480U - Equipment for growing sapphire single crystals - Google Patents
Equipment for growing sapphire single crystals Download PDFInfo
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- CN203530480U CN203530480U CN201320555834.XU CN201320555834U CN203530480U CN 203530480 U CN203530480 U CN 203530480U CN 201320555834 U CN201320555834 U CN 201320555834U CN 203530480 U CN203530480 U CN 203530480U
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- heater
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- pillar stiffener
- cooling
- growing sapphire
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Abstract
The utility model discloses equipment for growing sapphire single crystals. The equipment comprises a furnace body, a vacuum system, a pulling system, a power supply as well as a heating system and a cooling system arranged in the furnace body, wherein the vacuum system is communicated with an inner cavity of the furnace body, and the pulling system is arranged above the furnace body and comprises a pulling power device and a seed rod connected with the pulling power device. The equipment further comprises a control system which is electrically connected with the power supply, the heating system, the cooling system and the pulling system. A heat preserving layer is arranged between the heating system and the furnace body. By adopting the equipment and method of growing sapphire single crystals, the temperature gradient and solid-liquid interface state at the growing leading edge can be effectively regulated so as to avoid bubbles and reduce defect density, so that the high quality sapphire single crystals are obtained.
Description
Technical field
The utility model belongs to crystal preparing technology field, relates to a kind of crystal growth equipment, relates in particular to a kind of equipment of growing sapphire monocrystalline.
Background technology
Sapphire is the monocrystalline form of aluminum oxide (Al2O3), has very wide optics and penetrates band, all has good light transmission from near-ultraviolet light to middle infrared (Mid-IR).Sapphire also has the high velocity of sound, high-temperature resistant, anticorrosive, high rigidity, fusing point high.Due to its good machinery and optical property, sapphire crystal is widely used in the fields such as LED substrate material, infrared facility, the radium-shine eyeglass of high strength.The fast development of semiconductor lighting industry in recent years, has promoted the rapid growth of sapphire demand and the development of crystal technique.
At present, in the world application and research the most widely sapphire crystal growth technology be melting method, comprise crystal pulling, guided mode method, heat-exchanging method and kyropoulos, wherein, kyropoulos crystal growth technique, through the improvement of continuing to optimize of researcher decades, has become one of main stream approach of current production large size sapphire crystal.
In recent years, sapphire is widely used, and aspect window visor and LED substrate, is occupying the huge market share.Therefore, need can stable growth sapphire monocrystal method.The growth of sapphire crystal is carried out in high-temperature vacuum furnace, at the beginning of process of growth, well heater must consume a large amount of electric energy so that the hot conditions higher than crystalline melting point to be provided, make raw material be molten into melt, and the process of growth of sapphire crystal is longer, process control system is complicated, the photoelectric functional monocrystal material of growth of large size high quality, especially high-temp oxide crystal material exists technical barrier, the technology and equipment that different crystal material require is different, wherein relatively more outstanding is problem how accurately to control horizontal thermograde longitudinally and processing unit singularity.
Utility model content
The technical problem that the utility model solves is to provide a kind of equipment of growing sapphire monocrystalline; It is adjusted voltage and is reconciled the temperature of the gas in air-cooling apparatus and the thermograde that flow regulates thermal field by Controlling System, conveniently obtains the needed transverse and longitudinal thermograde of crystal, thereby monocrystalline crystalline size and quality are significantly improved; Research and development and the growing technology difficult problem of large-size high-quality photoelectric functional crystal have been solved.
The technical problem that the utility model solves realizes by the following technical solutions:
The equipment of a kind of growing sapphire monocrystalline of the present utility model, comprises a body of heater, a vacuum system, a handle system, a power supply and the heating system and the cooling system that are arranged at described body of heater; Described vacuum system is communicated with the inner chamber of described body of heater; Described handle system is arranged at the top of described body of heater; Described handle system comprises and lifts power set and lift with described the seed rod that power set is connected; Also comprise a Controlling System, described Controlling System is electrically connected to described power supply, described heating system, described cooling system and described handle system, described heating system comprises a well heater, a crucible and a supporting structure, and described supporting structure comprises a pillar stiffener.
Further improvement of the utility model is, described well heater is cage shape and is arranged at described supporting structure top; Described crucible is arranged in described well heater; Between described well heater and described body of heater, be provided with thermal insulation layer.
Further improvement of the utility model is, described supporting structure also comprises that two are individually fixed in the pallet of described pillar stiffener top and bottom.
Further improvement of the utility model is, described cooling system comprises water cooling loop; In the sidewall of described body of heater or chassis, be provided with described water cooling loop.
Further improvement of the utility model is, described cooling system comprises an air-cooling apparatus, described pillar stiffener hollow, and described air-cooling apparatus is arranged in described pillar stiffener, and the pallet at described pillar stiffener top forms the through hole corresponding with the hollow bulb of described pillar stiffener.
Further improvement of the utility model is, is provided with described water cooling loop in described seed rod.
Further improvement of the utility model is, described vacuum system comprises vacuum device, and described vacuum device is communicated with the cavity of described body of heater by a valve tube; Described vacuum device adopt in mechanical pump, lobe pump, diffusion pump and molecular pump one of or arbitrary combination.
The method of the growing sapphire monocrystalline of the equipment of a kind of growing sapphire monocrystalline of the present utility model, comprises the steps:
A. raw material with device preparation step;
B. by vacuum system, body of heater is vacuumized;
C. by the well heater in heating system, crucible is carried out to heat fused raw material and form melt, described crucible is by the support construction supports that comprises a pillar stiffener;
D. by starting handle system, seed crystal is contacted to melt realization inoculation seeding;
E. utilize Controlling System to control power supply, the voltage that makes well heater reduces gradually with the speed of 30～1000mv/h; And control temperature and the flow of gas in described air-cooling apparatus, make melt crystallize into gradually single crystal along the direction of seed crystal;
F. by described Controlling System, regulate cooling system, single crystal is grown gently by predetermined form.
Further improvement of the utility model is, describedly by well heater, crucible carried out to heat fused raw material and forms melt step and further comprise step:
By well heater, crucible is heated, make the internal temperature of crucible from room temperature, be increased to 2050～2200 ℃ in 8～20 hours;
Be incubated and within 0～10 hour, melt raw material completely.
Further improvement of the utility model is, describedly by described Controlling System, regulates cooling system step further to comprise step:
In single crystal growth process, when the solid-liquid interface of described melt is matrix form, by Controlling System, turn down the gas temperature in air-cooling apparatus, and strengthen gas flow, make the solid-liquid interface of described melt protruding by recessed change;
When the solid-liquid interface of described melt is convex form and its protruding rate surpasses a preset requirement value, by Controlling System, heighten the gas temperature in air-cooling apparatus, and reduce gas flow.
The utility model has been owing to having adopted above technical scheme, makes it have following beneficial effect to be:
By Controlling System, power supply, coordinate with refrigeration equipment, the growth apparatus of the sapphire crystal the utility model proposes, can control air-cooling apparatus in crucible supporting post by Controlling System and regulate thermograde, adjust the form of crystallization forward position solid-liquid interface, eliminate bubble and growth defect, improve single crystal size and quality, make the sapphire single-crystal of growth there is no the defect such as bubble, crackle etc.In method of the present utility model, in single crystal growth process, by adjusting bottom air-cooling apparatus, realize the thermograde of adjusting whole thermal field, improve solid liquid interface morphology, obtain high quality sapphire crystal.
Accompanying drawing explanation
Fig. 1 is the system architecture schematic diagram of the equipment of the utility model growing sapphire monocrystalline;
Fig. 2 is heating system and the heat insulation layer structure schematic diagram of the equipment of the utility model growing sapphire monocrystalline;
Fig. 3 is in the utility model embodiment in crystal growing process, dimpling form solid-liquid interface schematic diagram.
Embodiment
Below in conjunction with specific embodiment, the utility model is described in further detail.
Refer to Fig. 1, the equipment of a kind of growing sapphire monocrystalline of the present utility model, comprises body of heater 7, one vacuum systems 1, a handle system 2, a power supply 6 and the heating system 3 and the cooling system 4 that are arranged at body of heater 7; Vacuum system 1 is communicated with the inner chamber of body of heater 7; Handle system 2 is arranged at the top of body of heater 7; Handle system 2 comprise lift power set 21 and with the seed rod 22 that lifts power set 21 and be connected; Also comprise a Controlling System 5, Controlling System 5 is electrically connected to power supply 6, heating system 3, cooling system 4 and handle system 2.
Refer to Fig. 2, heating system 3 comprises a well heater 31, a crucible 32 and a supporting structure 34, and well heater 31 is cage shape and is arranged at supporting structure 34 tops; Crucible 32 is arranged in well heater 31; Between well heater 31 and body of heater 7, be provided with thermal insulation layer 33.Thermal insulation layer 33 is one or more layers structure.Wherein, supporting structure 34 comprises that a pillar stiffener 341 and two is individually fixed in the pallet 342 of pillar stiffener 341 tops and bottom.
Refer to Fig. 1,2, cooling system 4 comprises water cooling loop; The sidewall of body of heater 7 is provided with water cooling loop, meanwhile, is also provided with water cooling loop in seed rod 22, and seed rod 22 ends are provided with seed chuck.
Cooling system also comprises an air-cooling apparatus 41, pillar stiffener 341 hollows, and air-cooling apparatus 41 is arranged in pillar stiffener 341, and the pallet 342 at pillar stiffener 341 tops forms the through hole corresponding with the hollow bulb of pillar stiffener 341.
Vacuum system 1 comprises vacuum device, and vacuum device is communicated with the cavity of body of heater 7 by a valve tube.Vacuum device can adopt in mechanical pump, lobe pump, diffusion pump and molecular pump one of or arbitrary combination.
The method of a kind of growing sapphire monocrystalline of the present utility model, comprises the steps:
First, raw material and device preparation step, specifically comprise: on the seed chuck of seed rod 22 ends, place seed crystal, and at the Al of 40～100 kilograms of the interior placements of crucible 32
2o
3raw material; Crucible 32 is placed in the cage shape well heater 31 in body of heater 7;
Then, by 1 pair of body of heater 7 of vacuum system, vacuumize;
Then, by the 31 pairs of crucibles of cage shape well heater 32 in heating system 3, carry out heat fused raw material and form melt; Specifically comprise step, by well heater 31 crucibles, heat, make the internal temperature of crucible from room temperature, be increased to 2050～2150 ℃ in 8～20 hours, in the present embodiment, preferably within 8 hours, from room temperature, be increased to 2100 ℃; Crucible 32 is supported by the supporting structure 34 that comprises a pillar stiffener 341.
Insulation is melted raw material in 0-10 hour completely, in the present embodiment, is preferably incubated 4 hours;
Then, by starting handle system 2, seed crystal is contacted to melt realization inoculation seeding;
Then, utilize Controlling System 5 to control power supplys 6, the voltage that makes well heater 31 reduces gradually with the speed of 30-1000mv/h; And control temperature and the flow of the cooling gas such as helium or argon gas in air-cooling apparatus 41, make melt crystallize into gradually single crystal along the direction of seed crystal; Wherein in the present embodiment, preferred voltage reduces gradually with the speed of 600mv/h;
The air-cooling apparatus 41 finally regulating in crucible 32 supported underneath posts 341 by Controlling System 5, makes single crystal grow gently by predetermined form; This method can be adjusted crystal growth angle and solid liquid interface morphology, makes the solid-liquid interface of crystal growth front be the form of dimpling; It specifically comprises step:
In single crystal growth process, when the solid-liquid interface of melt is matrix form, by Controlling System 5, turn down the temperature of the gas in air-cooling apparatus 41, and strengthen gas flow, make the solid-liquid interface of melt protruding by recessed change;
When the solid-liquid interface of melt is convex form and its protruding rate surpasses a preset requirement value, by Controlling System 5, heighten the gas temperature in air-cooling apparatus 41, and reduce gas flow.
In embodiment, in crystal growing process, dimpling form solid-liquid interface schematic diagram refers to Fig. 3, visible by Fig. 3, and the sapphire crystal of dimpling form growth in the present embodiment does not have the defect of bubble, crackle etc., and monocrystalline performance and quality are better.
In addition, the sapphire single-crystal of growth is processed into wafer, in KOH solution, corrodes, measuring unit of display Area defect density is 10-1000EPD/cm2.
Below embodiment has been described in detail the utility model by reference to the accompanying drawings, and those skilled in the art can make many variations example to the utility model according to the above description.Thereby some details in embodiment should not form restriction of the present utility model, the utility model will be usingd scope that appended claims defines as protection domain of the present utility model.
Claims (5)
1. an equipment for growing sapphire monocrystalline, comprises a body of heater, a vacuum system, a handle system, a power supply and the heating system and the cooling system that are arranged at described body of heater; Described vacuum system is communicated with the inner chamber of described body of heater; Described handle system is arranged at the top of described body of heater; Described handle system comprises and lifts power set and lift with described the seed rod that power set is connected; Also comprise a Controlling System, described Controlling System is electrically connected to described power supply, described heating system, described cooling system and described handle system, it is characterized in that, described heating system comprises a well heater, a crucible and a supporting structure, described supporting structure comprises a pillar stiffener, described well heater is arranged at described supporting structure top, and described crucible is arranged in described well heater; Described supporting structure also comprises that two are individually fixed in the pallet of described pillar stiffener top and bottom; Described cooling system comprises an air-cooling apparatus, described pillar stiffener hollow, and described air-cooling apparatus is arranged in described pillar stiffener, and the pallet at described pillar stiffener top forms the through hole corresponding with the hollow bulb of described pillar stiffener.
2. the equipment of growing sapphire monocrystalline as claimed in claim 1, is characterized in that: described well heater is cage shape; Between described well heater and described body of heater, be provided with thermal insulation layer.
3. the equipment of growing sapphire monocrystalline as claimed in claim 1, is characterized in that: described cooling system comprises water cooling loop; In the sidewall of described body of heater or chassis, be provided with described water cooling loop.
4. the equipment of growing sapphire monocrystalline as claimed in claim 3, is characterized in that: in described seed rod, be provided with described water cooling loop.
5. the equipment of growing sapphire monocrystalline as claimed in claim 1, is characterized in that: described vacuum system comprises vacuum device, and described vacuum device is communicated with the cavity of described body of heater by a valve tube; Described vacuum device adopt in mechanical pump, lobe pump, diffusion pump and molecular pump one of or arbitrary combination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320555834.XU CN203530480U (en) | 2013-09-06 | 2013-09-06 | Equipment for growing sapphire single crystals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320555834.XU CN203530480U (en) | 2013-09-06 | 2013-09-06 | Equipment for growing sapphire single crystals |
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| CN203530480U true CN203530480U (en) | 2014-04-09 |
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| CN201320555834.XU Expired - Fee Related CN203530480U (en) | 2013-09-06 | 2013-09-06 | Equipment for growing sapphire single crystals |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103422163A (en) * | 2013-09-06 | 2013-12-04 | 上海森松压力容器有限公司 | Device and method for growing sapphire single crystals |
| CN105803529A (en) * | 2015-01-16 | 2016-07-27 | 丰田自动车株式会社 | Method for producing SiC single crystal |
| CN106835278A (en) * | 2017-01-13 | 2017-06-13 | 许昌天戈硅业科技有限公司 | A kind of crystal growth furnace heater and sapphire crystal growing furnace |
| CN106868594A (en) * | 2017-01-13 | 2017-06-20 | 许昌天戈硅业科技有限公司 | A kind of low energy consumption sapphire crystal growing furnace |
-
2013
- 2013-09-06 CN CN201320555834.XU patent/CN203530480U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103422163A (en) * | 2013-09-06 | 2013-12-04 | 上海森松压力容器有限公司 | Device and method for growing sapphire single crystals |
| CN105803529A (en) * | 2015-01-16 | 2016-07-27 | 丰田自动车株式会社 | Method for producing SiC single crystal |
| CN106835278A (en) * | 2017-01-13 | 2017-06-13 | 许昌天戈硅业科技有限公司 | A kind of crystal growth furnace heater and sapphire crystal growing furnace |
| CN106868594A (en) * | 2017-01-13 | 2017-06-20 | 许昌天戈硅业科技有限公司 | A kind of low energy consumption sapphire crystal growing furnace |
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| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: Workshop 1, building 1, No. 458, Zhongmin Road, Maogang Town, Songjiang District, Shanghai, 201607 Patentee after: Shanghai Senyong Engineering Equipment Co.,Ltd. Address before: 200137 building 3, No. 562, Gaoxiang Ring Road, Pudong New Area, Shanghai Patentee before: SHANGHAI MORIMATSU PRESSURE VESSEL Co.,Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140409 |