CN103614765A - Method of heating graphite to grow sapphire crystal - Google Patents
Method of heating graphite to grow sapphire crystal Download PDFInfo
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- CN103614765A CN103614765A CN201310533979.4A CN201310533979A CN103614765A CN 103614765 A CN103614765 A CN 103614765A CN 201310533979 A CN201310533979 A CN 201310533979A CN 103614765 A CN103614765 A CN 103614765A
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Abstract
The invention discloses a method of heating graphite to grow sapphire crystal. The method uses a sapphire crystal growth device and is characterized in that: a graphite barrel and a carbon felt material are taken as a heat insulation layer, argon gas or helium gas is taken as a protective gas, graphite is taken as a heater, then raw materials in a tungsten crucible or in a tungsten and molybdenum alloy crucible are melt through an irradiation heating method, then the molten raw materials are subjected to processes of seeding, necking, shouldering, equal-diameter growing, and separating the crystal from the crucible so as to complete the crystal growth. The method can achieve precise control of growth of large-size sapphire crystal, and has the characteristics of low cost and high quality crystal.
Description
Technical field
The present invention relates to the growth method of sapphire crystal, specifically a kind of method of graphite heating growing sapphire crystal.
Background technology
Sapphire crystal has stable chemical property, good mechanical property, good heat conductivity and electric insulating quality, have unique mechanics, optical property, and resistance to chemical attack, high temperature resistant, heat conduction good, hardness is high, can under mal-condition, work, be a kind of desirable optics starting material.Sapphire crystal have near ultraviolet to the infrared very wide scope that sees through, be widely used in the GaN substrate material of high-brightness LED, the substrate material of large-scale integrated circuit, special optical components and parts, high energy are surveyed and the window material of high power laser light.In recent years due to the increasing rapidly of the market requirements such as LED illumination, LED TV, its technology of preparing is widely studied, and the main stream approach that at present prepared by large size sapphire crystal is kyropoulos, heat-exchanging method and falling crucible method.
Wherein crucible method contacts with crucible because of the crystal growing, and because crucible is different from the thermal expansivity of crystal, in temperature-fall period, crucible can produce stress and increase the probability of crystal cleavage the crystal growing, and yield rate is difficult to improve.Heat-exchanging method technique is relatively ripe, generally can prepare sapphire crystal more than 300 mm diameter, but equipment cost is very high.Kyropoulos because of its can the relatively large sapphire crystal of growth size, suitable equipment cost and being adopted in a large number gradually.But traditional kyropoulos heating and heat-insulation system adopt tungsten and molybdenum material to make, tungsten and molybdenum material is at high temperature yielding, after repeatedly using, can cause thermal field skewness in stove, increases the difficulty of crystal growth technique, greatly reduce the yield of crystal production, thereby greatly increase the growth cost of crystal.Patent 200510010116.4 relates to a kind of " cold core shouldering micropulling proparation method of large-size sapphire single-crystal ", the method is by the mode of resistive heating, adopt the insulation of tungsten radiation shield, under vacuum condition through heating raw, seeding, shouldering, isometrically lift, cooling and annealing process procedure, but in this method technological process, thermograde is very little, technological process is controlled very difficult, needs very high peopleware, and level of automation is difficult to improve.
Summary of the invention
A kind of method that the object of this invention is to provide graphite heating growing sapphire crystal, it is too small that the method has been optimized in traditional kyropoulos sapphire crystal growth process temperature gradient of solid-liquid interface, and cause the crystal restive problem of growing; Overcome the shortcomings such as traditional kyropoulos crystal growing furnace temperature field is yielding, power consumption is high simultaneously, can realize the precision of sapphire crystal growth to control, there is low cost, the high-quality feature of crystal.
Technical solution of the present invention is as follows:
A kind of method of graphite heating growing sapphire crystal; comprise a sapphire crystal growth device; its feature is: adopt graphite bucket and carbon felt material as thermal insulation layer; argon gas or helium are as shielding gas, and graphite is as well heater, by the mode of radiation heating; make after the raw material fusing in tungsten or miramint crucible; pass through seeding, necking down, shouldering, isodiametric growth and crystal and crucible detach procedure again, complete crystal growth, the method comprises the following steps:
1. adopt purity be 99.99% and above aluminum oxide as growth raw material;
2., after shove charge finishes, be evacuated to vacuum tightness higher than 6 * 10
-2pa then slowly passes into argon or helium gas flow atmosphere in burner hearth, and in process of growth, furnace pressure is controlled within the scope of 10～100torr,
3. by more than crucible heating to 2050 ℃, reduce seed rod, make the bottom surface of seed crystal apart from the position of the liquid level 1～3cm of aluminum oxide, if turning white, seed crystal bottom becomes mellow and full, need to have shaken seed rod, lower the temperature 2～5 ℃, after standing 1～2 hour, again shake down seed rod, the bottom surface that makes seed crystal is apart from the position of the liquid level 1～3cm of aluminum oxide and observe, when seed crystal bottom is unchanged, shake seed rod under can continuing, after being contacted with melt, seed crystal mentions again, when described seed crystal chap, temperature is raise 2～5 ℃, after standing 1～2 hour, continue to attempt, until seed crystal is constant, complete seeding process,
4. by seed crystal in melt after standing 30 minutes, with the pulling rate of 0.2mm/h, upwards lift seed rod, keep temperature-resistant, when lifting length, reach after 3～8mm, complete necking down process;
5. take speed as 0.25 ℃/h reduces system temperature, make liquid level temperature lower than 0.5～2 ℃ of melting temperature, pulling rate remains on 0.2mm/h, realizes the shouldering growth of gem crystal, when the increasing amount of crystal quality per hour reaches 300g, completes shouldering process;
6. enter the isodiametric growth stage, the increasing amount of the quality per hour of assurance crystal is between 300～500g, and pulling rate remains on 0.2mm/h simultaneously;
7. when the total mass of crystal that shows growth is when adding raw materials quality to equate, observe again 30 minutes, if display quality no longer changes, increase pulling rate to 2mm/h, crystal and crucible are departed from, then take speed as 4 ℃/h reduction system temperature, until furnace temperature is 1900 ℃, take speed as 8 ℃/h reduction system temperature is until furnace temperature is 1700 ℃ again, finally take speed as 25 ℃/h reduction system temperature is to room temperature.
Technique effect of the present invention:
Described in the method, install and adopt graphite as heating element, optimized " birdcage " resistance volatility and short problem of life-span in traditional kyropoulos growing sapphire crystal process, thereby make crystal growth be easy to control, be beneficial to the automatization control that realizes crystal growth; Graphite bucket and carbon felt material be as thermal insulation layer, and heat-insulation system makes simply, not yielding, and high insulating effect, life cycle is long, cost is low, and this is reduced holistic cost, is beneficial to the industrialized development of sapphire crystal growth.
The inventive method can realize the precision of large size sapphire crystal growth and control, and has low cost, the high-quality feature of crystal.
Accompanying drawing explanation
Fig. 1 is graphite heating growing sapphire crystal device schematic diagram of the present invention, in figure: 1-seed rod, 2-upper heat protection screen, 3-carbon-to-carbon lagging material, 4-graphite heater, 5-crucible cover, 6-graphite bucket, 7-crucible, 8-seed crystal, 9-crystal, 10-melt, 11-crucible pallet, 12-crucible pressure pin, 13-bottom lagging material.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described, but should not limit the scope of the invention with this.
Adopt method growing sapphire crystal embodiment 1 of the present invention:
Press shown in Fig. 1, on the device of graphite heating growing sapphire crystal of the present invention, install crystal growing furnace, alumina raw material is packed in tungsten crucible, be evacuated to vacuum tightness higher than 6 * 10
-2during Pa, pass into argon gas and make furnace chamber pressure remain on 10torr left and right, start to heat up raw material is melted, by more than crucible heating to 2050 ℃, reduce seed rod, make seed crystal apart from the position of liquid level 1cm, if turn white in seed crystal bottom, become mellow and full, need to have shaken seed rod, lower the temperature 2 ℃.After standing 1 hour, again shake down seed rod and observe, until seed crystal bottom is unchanged, shake seed rod under can continuing, mention after seed crystal and melt are connect, if band material raises temperature 2 ℃, after standing 1 hour, continue trial, until be not with material, complete seeding process; After realizing seeding, make seed crystal in melt after standing 30 minutes, with the pulling rate of 0.2mm/h, upwards lift seed rod, keep temperature-resistant, when lifting length, reach after 3mm, complete necking down process; Take slope as 0.25 ℃/h reduces system temperature, make liquid level temperature lower than 0.5 ℃ of melting temperature, pulling rate remains on 0.2mm/h, thereby realizes the shouldering growth of gem crystal, when the increasing amount of crystal quality per hour reaches 300g, completes shouldering process; Grow into the isometrical stage, the increasing amount of the quality per hour of assurance crystal is between 300g, and pulling rate remains on 0.2mm/h simultaneously; When the quality of crystal that shows growth is when adding raw materials quality to equate, observe again 30 minutes, if display quality no longer changes, increase pulling rate to 2mm/h, crystal and crucible are departed from, then take slope as 4 ℃/h reduction system temperature is until furnace temperature is 1900 ℃, then take slope as 8 ℃/h reduction system temperature is until furnace temperature is 1700 ℃, finally take slope as 25 ℃/h reduction system temperature is to room temperature.
Adopt method growing sapphire crystal embodiment 2 of the present invention:
By shown in Fig. 1, install crystal growing furnace, alumina raw material is packed in tungsten crucible, be evacuated to vacuum tightness higher than 6 * 10
-2during Pa, pass into helium and make furnace chamber pressure remain on 100torr left and right, start to heat up raw material is melted, by more than crucible heating to 2050 ℃, reduce seed rod, make seed crystal apart from the position of liquid level 3cm, if turn white in seed crystal bottom, become mellow and full, need to have shaken seed rod, lower the temperature 5 ℃.After standing 2 hours, again shake down seed rod and observe, until seed crystal bottom is unchanged, shake seed rod under can continuing, mention after seed crystal and melt are connect, if band material raises temperature 5 ℃, after standing 2 hours, continue trial, until be not with material, complete seeding process; After realizing seeding, make seed crystal in melt after standing 30 minutes, with the pulling rate of 0.2mm/h, upwards lift seed rod, keep temperature-resistant, when lifting length, reach after 8mm, complete necking down process; Reduce slowly heating power, make liquid level temperature lower than 2 ℃ of melting temperatures, pulling rate remains on 0.2mm/h, thereby realizes the shouldering growth of gem crystal, when the increasing amount of crystal quality per hour reaches 300g, completes shouldering process; Grow into the isometrical stage, the increasing amount of the quality per hour of assurance crystal is between 500g, and pulling rate remains on 0.2mm/h simultaneously; When the quality of crystal that shows growth is when adding raw materials quality to equate, observe again 30 minutes, if display quality no longer changes, increase pulling rate to 2mm/h, crystal and crucible are departed from, then take slope as 4 ℃/h reduction system temperature is until furnace temperature is 1900 ℃, then take slope as 8 ℃/h reduction system temperature is until furnace temperature is 1700 ℃, finally take slope as 25 ℃/h reduction system temperature is to room temperature.
Adopt method growing sapphire crystal embodiment 3 of the present invention:
By shown in Fig. 1, install crystal growing furnace, alumina raw material is packed in tungsten crucible, be evacuated to vacuum tightness higher than 6 * 10
-2during Pa, pass into argon gas and make furnace chamber pressure remain on 100torr left and right, start to heat up raw material is melted, by more than crucible heating to 2050 ℃, reduce seed rod, make seed crystal apart from the position of liquid level 2cm, if turn white in seed crystal bottom, become mellow and full, need to have shaken seed rod, lower the temperature 3 ℃.After standing 2 hours, again shake down seed rod and observe, until seed crystal bottom is unchanged, shake seed rod under can continuing, mention after seed crystal and melt are connect, if band material, raises temperature 2～5 ℃, after standing 2 hours, continue to attempt, until be not with material, complete seeding process; After realizing seeding, make seed crystal in melt after standing 30 minutes, with the pulling rate of 0.2mm/h, upwards lift seed rod, keep temperature-resistant, when lifting length, reach after 5mm, complete necking down process; Reduce slowly heating power, make liquid level temperature lower than 1 ℃ of melting temperature, pulling rate remains on 0.2mm/h, thereby realizes the shouldering growth of gem crystal, when the increasing amount of crystal quality per hour reaches 300g, completes shouldering process; Grow into the isometrical stage, the increasing amount of the quality per hour of assurance crystal is between 400g, and pulling rate remains on 0.2mm/h simultaneously; When the quality of crystal that shows growth is when adding raw materials quality to equate, observe again 30 minutes, if display quality no longer changes, increase pulling rate to 2mm/h, crystal and crucible are departed from, then take slope as 4 ℃/h reduction system temperature is until furnace temperature is 1900 ℃, then take slope as 8 ℃/h reduction system temperature is until furnace temperature is 1700 ℃, finally take slope as 25 ℃/h reduction system temperature is to room temperature.
Adopt method growing sapphire crystal embodiment 4 of the present invention:
By shown in Fig. 1, install crystal growing furnace, alumina raw material is packed in tungsten crucible, be evacuated to vacuum tightness higher than 6 * 10
-2during Pa, pass into helium and make furnace chamber pressure remain on 50torr left and right, start to heat up raw material is melted, by more than crucible heating to 2050 ℃, reduce seed rod, make seed crystal apart from the position of liquid level 1cm, if turn white in seed crystal bottom, become mellow and full, need to have shaken seed rod, lower the temperature 2 ℃.After standing 1 hour, again shake down seed rod and observe, until seed crystal bottom is unchanged, shake seed rod under can continuing, mention after seed crystal and melt are connect, if band material raises temperature 2 ℃, after standing 2 hours, continue trial, until be not with material, complete seeding process; After realizing seeding, make seed crystal in melt after standing 30 minutes, with the pulling rate of 0.2mm/h, upwards lift seed rod, keep temperature-resistant, when lifting length, reach after 8mm, complete necking down process; Reduce slowly heating power, make liquid level temperature lower than 2 ℃ of melting temperatures, pulling rate remains on 0.2mm/h, thereby realizes the shouldering growth of gem crystal, when the increasing amount of crystal quality per hour reaches 300g, completes shouldering process; Grow into the isometrical stage, the increasing amount of the quality per hour of assurance crystal is between 400g, and pulling rate remains on 0.2mm/h simultaneously; When the quality of crystal that shows growth is when adding raw materials quality to equate, observe again 30 minutes, if display quality no longer changes, increase pulling rate to 2mm/h, crystal and crucible are departed from, then take slope as 4 ℃/h reduction system temperature is until furnace temperature is 1900 ℃, then take slope as 8 ℃/h reduction system temperature is until furnace temperature is 1700 ℃, finally take slope as 25 ℃/h reduction system temperature is to room temperature.
Claims (1)
1. the method for a graphite heating growing sapphire crystal; comprise a sapphire crystal growth device; it is characterized in that: adopt graphite bucket and carbon felt material as thermal insulation layer; argon gas or helium are as shielding gas, and graphite is as well heater, by the mode of radiation heating; make after the raw material fusing in tungsten or miramint crucible; pass through seeding, necking down, shouldering, isodiametric growth and crystal and crucible detach procedure again, complete crystal growth, the method comprises the following steps:
1. adopt purity be 99.99% and above aluminum oxide as growth raw material;
2., after shove charge finishes, be evacuated to vacuum tightness higher than 6 * 10
-2pa then slowly passes into argon or helium gas flow atmosphere in burner hearth, and in process of growth, furnace pressure is controlled within the scope of 10～100torr,
3. by more than crucible heating to 2050 ℃, reduce seed rod, make the bottom surface of seed crystal apart from the position of the liquid level 1～3cm of aluminum oxide, if turning white, seed crystal bottom becomes mellow and full, need to have shaken seed rod, lower the temperature 2～5 ℃, after standing 1～2 hour, again shake down seed rod, the bottom surface that makes seed crystal is apart from the position of the liquid level 1～3cm of aluminum oxide and observe, when seed crystal bottom is unchanged, shake seed rod under can continuing, after being contacted with melt, seed crystal mentions again, when described seed crystal chap, temperature is raise 2～5 ℃, after standing 1～2 hour, continue to attempt, until seed crystal is constant, complete seeding process,
4. by seed crystal in melt after standing 30 minutes, with the pulling rate of 0.2mm/h, upwards lift seed rod, keep temperature-resistant, when lifting length, reach after 3～8mm, complete necking down process;
5. take speed as 0.25 ℃/h reduces system temperature, make liquid level temperature lower than 0.5～2 ℃ of melting temperature, pulling rate remains on 0.2mm/h, realizes the shouldering growth of gem crystal, when the increasing amount of crystal quality per hour reaches 300g, completes shouldering process;
6. enter the isodiametric growth stage, the increasing amount of the quality per hour of assurance crystal is between 300～500g, and pulling rate remains on 0.2mm/h simultaneously;
7. when the total mass of crystal that shows growth is when adding raw materials quality to equate, observe again 30 minutes, if display quality no longer changes, increase pulling rate to 2mm/h, crystal and crucible are departed from, then take speed as 4 ℃/h reduction system temperature, until furnace temperature is 1900 ℃, take speed as 8 ℃/h reduction system temperature is until furnace temperature is 1700 ℃ again, finally take speed as 25 ℃/h reduction system temperature is to room temperature.
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Cited By (7)
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| CN105297131A (en) * | 2014-07-17 | 2016-02-03 | 胜高股份有限公司 | Single crystal manufacturing method and device |
| JP2016204166A (en) * | 2015-04-15 | 2016-12-08 | 住友金属鉱山株式会社 | Crystal growth apparatus |
| CN106702490A (en) * | 2016-08-30 | 2017-05-24 | 天通银厦新材料有限公司 | Growth equipment of sapphire crystal |
| CN106987903A (en) * | 2017-03-27 | 2017-07-28 | 宁夏佳晶科技有限公司 | A kind of improved large scale synthetic sapphire production technology |
| CN107268081A (en) * | 2017-06-06 | 2017-10-20 | 界首市七曜新能源有限公司 | A kind of Sapphire Substrate preparation technology |
| CN116411338A (en) * | 2023-06-12 | 2023-07-11 | 内蒙古晶环电子材料有限公司 | Material boiling process for producing sapphire single crystal |
| CN117512778A (en) * | 2024-01-02 | 2024-02-06 | 内蒙古晶环电子材料有限公司 | Abnormality monitoring method for heat insulation structure |
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| CN105297131A (en) * | 2014-07-17 | 2016-02-03 | 胜高股份有限公司 | Single crystal manufacturing method and device |
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| CN107268081A (en) * | 2017-06-06 | 2017-10-20 | 界首市七曜新能源有限公司 | A kind of Sapphire Substrate preparation technology |
| CN116411338A (en) * | 2023-06-12 | 2023-07-11 | 内蒙古晶环电子材料有限公司 | Material boiling process for producing sapphire single crystal |
| CN117512778A (en) * | 2024-01-02 | 2024-02-06 | 内蒙古晶环电子材料有限公司 | Abnormality monitoring method for heat insulation structure |
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Application publication date: 20140305 |