CN102154698A - Method for controlling seeding form in process of preparing large-sized sapphire single crystal by Kyropoulos method - Google Patents
Method for controlling seeding form in process of preparing large-sized sapphire single crystal by Kyropoulos method Download PDFInfo
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Abstract
The invention provides a method for controlling seeding form in process of preparing a large-sized sapphire single crystal by a Kyropoulos method. By using the method, four technical processes of preparation work, roasting a seed crystal, diameter shrinkage and multiple-seeding are finished in the process of growing the large-sized sapphire single crystal. Based on a Kyropoulos seeding method, the method is greatly improved and has the advantages that a grown crystal has higher quality and larger size, the success rate of the crystal growing is higher and the like.
Description
(1) technical field
A kind of sapphire suitability for industrialized production technology that relates to of the present invention is specifically related to seeding method in a kind of growing sapphire monocrystalline process.
(2) background technology
Sapphire claims white stone again, be that hardness is only second to adamantine crystalline material in the world, owing to have good physics, machinery, chemistry and infrared light transmission performance, it is the material that fields such as microelectronics, aerospace, military project are badly in need of always, especially optical grade large-size sapphire material, because it has characteristics such as stable performance, the huge market demand, comprehensive utilization ratio and added value of product height, become in recent years research and development and industrialization focus both at home and abroad.
China began to propose " national semiconductor lighting engineering " plan from 2003; and beginning to take shape the large-scale production ability of LED product in recent years; but be positioned at the substrate material of the upstream of LED industrial chain; especially large-size sapphire material; because technical threshold is high, is the bottleneck that this industry further develops always.
The technology of preparing of sapphire single-crystal comprises crystal pulling method, flame melt method, falling crucible method, temperature gradient method, guided mode method, heat-exchanging method, horizontal orientation freezing method, kyropoulos, cold core shouldering micropulling method etc., and wherein kyropoulos is a kind of method of the most suitable large-scale industrial production of generally acknowledging in the world at present.Though kyropoulos can prepare weight greater than 31kg, or even greater than the optical grade large size sapphire crystal of 85kg, this method crystal growth yield rate is lower at present, generally has only about 65%, has greatly limited further applying of this method.
(3) summary of the invention
The object of the present invention is to provide a kind of have can increase substantially the large-size sapphire single-crystal yield rate, the growing crystal optical quality more kyropoulos of advantages of higher prepares the control method of seeding form in the large-size sapphire single-crystal process.
The object of the present invention is achieved like this: in growing large-size sapphire crystal process, finish preparation work, baking seed crystal, undergauge, seeding four part technological processs repeatedly, specific embodiment is as follows:
1. preparation work: (1) is that 99.996% high purity aluminium oxide raw material is packed in the single crystal growing furnace crucible with 31-95 kg purity, installs the seed crystal that diameter is 12-22mm on seed rod, closes the monocrystalline bell, starts cooling water recirculation system; (2) start vacuum system, make furnace pressure reach 10
-3Pa.(3) start heating system, regulate heater voltage, heat temperature raising when temperature reaches 2150 ℃, stops heating, and this moment, raw material all melted; Be incubated after 3-5 hour, regulate heater voltage, be cooled to 2060 ℃, observe the melt liquid level state, this moment, the liquid level convection current was in stable condition, cold heart position and crucible geometric centre relative deviation 5-30 mm in the melt; (4) start auxiliary thermoregulating system, regulate temperature field in furnace, the interior cold heart position of melt is overlapped with crucible geometric centre position; Regulate heater voltage, be cooled to 2050 ℃, observe the melt liquid level state, this moment, the liquid level convection current was in stable condition;
2. baking seed crystal: turn down the seed rod height with 2-10mm/ minute speed, make the seed crystal lower end move closer to liquid level,, seed crystal lower end temperature is raise gradually near the bath surface temperature at the above 4-8 mm of liquid level place baking seed crystal.
3. undergauge: after stablizing 10-25 minute, turn down the seed rod height earlier and make seed crystal insert the following 3-6mm of melt liquid level, seed crystal is neither grown up at this moment, does not also melt; After stablizing 5 minutes, speed rotary seed crystal rod with 2-15 rev/min, regulate heater voltage, be warming up to 2052-2055 ℃, this moment, seed crystal began fusing, after 5-15 minute, the seed crystal diameter contracts to 10-12mm, regulates heater voltage, is cooled to 2045-2048 ℃, the seed rod that stops the rotation, this moment, seed crystal no longer melted; Keep being warming up to 2050 ℃ after 0.5-2 minute.
4. many seedings: upwards lift seed rod with 1-3mm/ minute speed, and, regulate heater voltage simultaneously with 2-10 rev/min speed rotary seed crystal rod, with the speed cooling of 0.5-2 ℃/h, the part melt begins crystallization around seed crystal, and beginning is seeding for the first time; After 5-15 minute, after the seeding section highly reaches 5-20mm, stop to lift and rotating, finish seeding for the first time, form first section of seeding; After stablizing 5 minutes,, regulate heater voltage, be warming up to 2052-2055 ℃, carry out the undergauge second time, the seed crystal diameter is contracted to 8-11mm with 2-15 rev/min speed rotary seed crystal rod; Upwards lift seed rod with 1-3.5mm/ minute speed, and, regulate heater voltage simultaneously,, carry out the seeding second time with the speed cooling of 0.5-2 ℃/h with 2-10 rev/min speed rotary seed crystal rod; Make the seed crystal diameter progressively be contracted to 4-8mm through behind 3-10 seeding, finish the seeding technological process, form the seeding latter end, seeding latter end bottom form is a semisphere.
Beneficial effect of the present invention is:
1. can grow size and surpass the large size optical grade sapphire crystal of 95kg greater than Φ 330 * 350 mm, weight.
2. by repeatedly undergauge and repeatedly seeding, progressively dwindle the seed crystal diameter, avoided cloud and mist, bubble, fault, the twin crystal defective of seed crystal inside are introduced sapphire crystal, improved the large size sapphire crystal quality greatly.
3. by while lifting the thermoregulated way of seed rod, cooperate suitable seed rod rotation, strict control seeding form is evenly dwindled the seed crystal diameter, has avoided owing to the seeding morphological mutation causes additional defects is introduced sapphire crystal.
4. increase substantially kyropoulos growing large-size sapphire crystal growth success ratio, can reach more than 80%.
In sum, kyropoulos preparation of the present invention has been carried out significant improvement greater than the control method of seeding form in the large-size sapphire single-crystal process of 31kg on original kyropoulos seeding method basis, it is higher to have the growing crystal quality, and size is bigger, and crystal growth such as has higher success rate at advantage.Thereby the present invention has broad application prospects, and applying of this technology can create obvious social and economic benefit.
(4) description of drawings
Fig. 1 is a seeding form synoptic diagram of the present invention.
(5) embodiment
The present invention is further illustrated below in conjunction with the drawings and specific embodiments:
Embodiment one: the present embodiment specific embodiment is as follows:
1. preparation work: (1) is that 99.996% high purity aluminium oxide raw material is packed in the single crystal growing furnace crucible with 31 kg purity, installs the seed crystal that diameter is 12mm on seed rod, closes the monocrystalline bell, starts cooling water recirculation system; (2) start vacuum system, make furnace pressure reach 10
-3Pa.(3) start heating system, regulate heater voltage, heat temperature raising when temperature reaches 2150 ℃, stops heating, and this moment, raw material all melted; Be incubated after 3 hours, regulate heater voltage, be cooled to 2060 ℃, observe the melt liquid level state, this moment, the liquid level convection current was in stable condition, and cold heart position and crucible geometric centre relative deviation are less than 15mm in the melt; (4) start auxiliary thermoregulating system, regulate temperature field in furnace, the interior cold heart position of melt is overlapped with crucible geometric centre position; Regulate heater voltage, be cooled to 2050 ℃, observe the melt liquid level state, this moment, the liquid level convection current was in stable condition;
2. baking seed crystal: turn down the seed rod height with 5mm/ minute speed, make the seed crystal lower end move closer to liquid level, baking seed crystal in 8 mm places raises gradually near the bath surface temperature seed crystal lower end temperature more than liquid level.
3. undergauge: after stablizing 10 minutes, will turn down the seed rod height and make seed crystal insert the following 3mm of melt liquid level, seed crystal is neither grown up at this moment, does not also melt; After stablizing 5 minutes,, regulate heater voltage, be warming up to 2052 ℃ with 10 rev/mins speed rotary seed crystal rod, this moment, seed crystal began fusing, and after 5 minutes, the seed crystal diameter contracts to 10mm, regulated heater voltage, be cooled to 2048 ℃, the seed rod that stops the rotation, this moment, seed crystal no longer melted; Keep being warming up to 2050 ℃ after 0.5 minute.
4. many seedings: upwards lift seed rod with 1mm/ minute speed, and with 8 rev/mins speed rotary seed crystal rod, regulate heater voltage simultaneously, with the speed cooling of 0.5 ℃/h, the part melt begins crystallization around seed crystal, and beginning is seeding for the first time; After 6 minutes, after the seeding section highly reaches 6mm, stop to lift and rotating, finish seeding for the first time, form first section of seeding; After stablizing 5 minutes,, regulate heater voltage, be warming up to 2052 ℃, carry out the undergauge second time, the seed crystal diameter is contracted to 8mm with 10 rev/mins speed rotary seed crystal rod; Upwards lift seed rod with 1mm/ minute speed, and, regulate heater voltage simultaneously, with the speed cooling of 0.5 ℃/h, carry out seeding second time, second section of formation seeding with 8 rev/mins speed rotary seed crystal rod; Through making the seed crystal diameter progressively be contracted to 4mm behind 5 seedings, finish the seeding technological process, form the seeding latter end.In conjunction with Fig. 1, first section 2 of seeding is in seed crystal 1 lower end among the figure, and seeding latter end 3 is at least significant end.
Embodiment two: the present embodiment specific embodiment is as follows:
1. preparation work: (1) is that 99.996% high purity aluminium oxide raw material is packed in the single crystal growing furnace crucible with 85 kg purity, installs the seed crystal that diameter is 18mm on seed rod, closes the monocrystalline bell, starts cooling water recirculation system; (2) start vacuum system, make furnace pressure reach 10
-3Pa.(3) start heating system, regulate heater voltage, heat temperature raising when temperature reaches 2150 ℃, stops heating, and this moment, raw material all melted; Be incubated after 5 hours, regulate heater voltage, be cooled to 2060 ℃, observe the melt liquid level state, this moment, the liquid level convection current was in stable condition, cold heart position and crucible geometric centre relative deviation 30 mm in the melt; (4) start auxiliary thermoregulating system, regulate temperature field in furnace, the interior cold heart position of melt is overlapped with crucible geometric centre position; Regulate heater voltage, be cooled to 2050 ℃, observe the melt liquid level state, this moment, the liquid level convection current was in stable condition;
2. baking seed crystal: turn down the seed rod height with 2mm/ minute speed, make the seed crystal lower end move closer to liquid level,, seed crystal lower end temperature is raise gradually near the bath surface temperature being positioned at baking seed crystal in 4 mm places more than the liquid level.
3. undergauge: after stablizing 25 minutes, will turn down the seed rod height and make seed crystal insert the following 6mm of melt liquid level, seed crystal is neither grown up at this moment, does not also melt; After stablizing 5 minutes,, regulate heater voltage, be warming up to 2055 ℃ with 5 rev/mins speed rotary seed crystal rod, this moment, seed crystal began fusing, and after 15 minutes, the seed crystal diameter contracts to 12mm, regulated heater voltage, be cooled to 2045 ℃, the seed rod that stops the rotation, this moment, seed crystal no longer melted; Keep being warming up to 2050 ℃ after 1 minute.
4. many seedings: upwards lift seed rod with 1.5mm/ minute speed, and with 4 rev/mins speed rotary seed crystal rod, regulate heater voltage simultaneously, with the speed cooling of 1 ℃/h, the part melt begins crystallization around seed crystal, and beginning is seeding for the first time; After 15 minutes, after the seeding section highly reaches 12mm, stop to lift and rotating, finish seeding for the first time, form first section of seeding; After stablizing 5 minutes,, regulate heater voltage, be warming up to 2055 ℃, carry out the undergauge second time, the seed crystal diameter is contracted to 10mm with 5 rev/mins speed rotary seed crystal rod; Upwards lift seed rod with 1.5mm/ minute speed, and, regulate heater voltage simultaneously,, carry out the seeding second time with the speed cooling of 1 ℃/h with 4 rev/mins speed rotary seed crystal rod; Through making the seed crystal diameter progressively be contracted to 6mm behind 8 seedings, finish the seeding technological process, form the seeding latter end.
Claims (5)
1. a kyropoulos prepares the control method of seeding form in the large-size sapphire single-crystal process, it is characterized in that described control method technological process concrete steps are: (1) preparation work step: the high purity aluminium oxide raw material is packed in the single crystal growing furnace crucible, on seed rod, install seed crystal, close the monocrystalline bell, start cooling water recirculation system and start vacuum system, start heating system then, the adjusting heater voltage all melts raw material and reaches the in stable condition state of liquid level convection current; (2) baking seed crystal step: turn down the seed rod height, make the seed crystal lower end move closer to liquid level baking seed crystal, and seed crystal lower end temperature is raise gradually near the bath surface temperature; (3) undergauge step: turn down the seed rod height make seed crystal insert melt liquid level following stable after, rotary seed crystal rod is also regulated heater voltage and is heated up, and after seed crystal begins fusing, regulates the heater voltage cooling, seed rod stops the rotation; (4) seeding step repeatedly: upwards lift and rotary seed crystal rod, regulate the heater voltage cooling simultaneously, the part melt begins crystallization around seed crystal, finishes seeding for the first time, stable after rotary seed crystal rod again, regulate heater voltage and heat up, finish undergauge for the second time; Upwards lift again and rotary seed crystal rod, regulate the heater voltage cooling simultaneously, carry out the seeding second time,, finish the seeding form through forming the seeding latter end behind 3-10 the seeding.
2. kyropoulos according to claim 1 prepares the control method of seeding form in the large-size sapphire single-crystal process, it is characterized in that described preparation work step comprises: (1) is with 31-95 kg high purity aluminium oxide material purity〉99.997% pack in the single crystal growing furnace crucible, on seed rod, install the seed crystal that diameter is 12-22mm, close the monocrystalline bell, start cooling water recirculation system; (2) start vacuum system, make furnace pressure reach 10
-3Pa; (3) start heating system, regulate heater voltage, heat temperature raising when temperature reaches 2150 ℃, stops heating, and raw material all melts; Be incubated after 3-5 hour, regulate heater voltage, be cooled to 2060 ℃, the liquid level convection current is in stable condition, keeps cold heart position and crucible geometric centre relative deviation 5-30 mm in the melt; (4) start auxiliary thermoregulating system, regulate temperature field in furnace, the interior cold heart position of melt is overlapped with crucible geometric centre position; Regulate heater voltage, be cooled to 2050 ℃, the liquid level convection current is in stable condition.
3. kyropoulos according to claim 2 prepares the control method of seeding form in the large-size sapphire single-crystal process, it is characterized in that described baking seed crystal step comprises: turn down the seed rod height with 2-10mm/ minute speed, make the seed crystal lower end move closer to liquid level, at the above 4-8 mm of liquid level place baking seed crystal.
4. kyropoulos according to claim 3 prepares the control method of seeding form in the large-size sapphire single-crystal process, it is characterized in that described undergauge step comprises: after stablizing 10-25 minute, turn down the seed rod height earlier, make seed crystal insert the following 3-6mm of melt liquid level, after stablizing 5 minutes, with 2-15 rev/min speed rotary seed crystal rod, regulate heater voltage, be warming up to 2052-2055 ℃, this moment, seed crystal began fusing, after 5-15 minute, the seed crystal diameter contracts to 10-12mm, regulates heater voltage, be cooled to 2045-2048 ℃, the seed rod that stops the rotation, this moment, seed crystal no longer melted, and kept being warming up to 2050 ℃ after 0.5-2 minute.
5. kyropoulos according to claim 4 prepares the control method of seeding form in the large-size sapphire single-crystal process, it is characterized in that described repeatedly seeding step comprises: upwards lift seed rod with 1-3mm/ minute speed, and with 2-10 rev/min speed rotary seed crystal rod, regulate heater voltage simultaneously, speed cooling with 0.5-2 ℃/h, the part melt begins crystallization around seed crystal, and beginning is seeding for the first time; After 5-15 minute, after the seeding section highly reaches 5-20mm, stop to lift and rotating, finish seeding for the first time, form first section of seeding; After stablizing 5 minutes,, regulate heater voltage, be warming up to 2052-2055 ℃, carry out the undergauge second time, the seed crystal diameter is contracted to 8-11mm with 2-15 rev/min speed rotary seed crystal rod; Upwards lift seed rod with 1-3.5mm/ minute speed, and, regulate heater voltage simultaneously,, carry out the seeding second time with the speed cooling of 0.5-2 ℃/h with 2-10 rev/min speed rotary seed crystal rod; Make the seed crystal diameter progressively be contracted to 4-8mm through behind 3-10 seeding, finish the seeding technological process, form the seeding latter end, seeding latter end bottom form is a semisphere.
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| CN102560623A (en) * | 2012-02-09 | 2012-07-11 | 常州亿晶光电科技有限公司 | Preparation method of large-size sapphire single crystal |
| CN102691103A (en) * | 2012-06-14 | 2012-09-26 | 中国科学院半导体研究所 | Method for growing sapphire crystals by double control technology |
| CN102758251A (en) * | 2012-08-08 | 2012-10-31 | 无锡鼎晶光电科技有限公司 | Method for controlling sapphire seeding form of Kyropoulos method |
| CN102797033A (en) * | 2012-08-15 | 2012-11-28 | 四川欣蓝光电科技有限公司 | Seeding process controlling method for growing large-size sapphire crystal with soaked-growth method |
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| CN102560623A (en) * | 2012-02-09 | 2012-07-11 | 常州亿晶光电科技有限公司 | Preparation method of large-size sapphire single crystal |
| CN102560623B (en) * | 2012-02-09 | 2015-06-24 | 常州亿晶光电科技有限公司 | Preparation method of large-size sapphire single crystal |
| CN102691103B (en) * | 2012-06-14 | 2015-04-15 | 中国科学院半导体研究所 | Method for growing sapphire crystals by double control technology |
| CN102691103A (en) * | 2012-06-14 | 2012-09-26 | 中国科学院半导体研究所 | Method for growing sapphire crystals by double control technology |
| CN102758251A (en) * | 2012-08-08 | 2012-10-31 | 无锡鼎晶光电科技有限公司 | Method for controlling sapphire seeding form of Kyropoulos method |
| CN102758251B (en) * | 2012-08-08 | 2016-01-20 | 无锡鼎晶光电科技有限公司 | Kyropoulos sapphire seeding configuration control method |
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| CN103074671A (en) * | 2012-11-05 | 2013-05-01 | 浙江东海蓝玉光电科技有限公司 | Soaking method for reducing large size sapphire crystal bubble |
| CN103074671B (en) * | 2012-11-05 | 2015-10-28 | 浙江东海蓝玉光电科技有限公司 | A kind of kyropoulos reducing large size sapphire crystal bubble |
| CN103194791A (en) * | 2013-04-24 | 2013-07-10 | 哈尔滨工业大学 | Horizontal directional region melt-crystallization preparation method of large-dimension plate-like sapphire mono-crystal |
| CN103194791B (en) * | 2013-04-24 | 2016-05-04 | 哈尔滨工业大学 | The horizontal orientation district clinkering crystal preparation method of the tabular sapphire monocrystal of large scale |
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| CN104911708B (en) * | 2015-06-15 | 2017-10-27 | 哈尔滨奥瑞德光电技术有限公司 | Kyropoulos prepare the growing method of square sapphire crystal |
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| CN105839177B (en) * | 2016-04-08 | 2018-06-19 | 齐齐哈尔市泰兴机械加工有限责任公司 | A kind of lifting preparation method stage by stage of large size single crystal body |
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| CN109487334A (en) * | 2018-11-22 | 2019-03-19 | 太原理工大学 | A kind of kyropoulos sapphire based on random distribution melts brilliant inoculation state control method |
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