CN102154698B - 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 Industrialized processing technique 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 again white stone, 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 the fields such as microelectronics, aerospace, military project are badly in need of always, especially optical grade large-size sapphire material, because it has stable performance, the huge market demand, comprehensive utilization ratio and added value of product high, become in recent years both at home and abroad research and development and industrialization focus.
China began to propose " national Semiconductor Lighting " plan from 2003; and beginning to take shape in recent years the large-scale production ability of LED product; 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 Bridgman 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.Although kyropoulos can prepare weight greater than 31kg, or even greater than the optical grade large size sapphire crystal of 85kg, the method crystal growth yield rate is lower at present, generally only has about 65%, has greatly limited further applying of the 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 the growing large-size sapphire crystallization 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 crucible of single crystal furnace with 31-95 kg purity, installs the seed crystal that diameter is 12-22mm at seed rod, closes mono-crystal furnace cover, 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 ℃, stopped heating, 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 states was stable, 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 states was stable;
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, at the above 4-8 mm of liquid level place baking seed crystal, seed crystal lower end temperature is raise gradually near the bath surface temperature.
3. undergauge: after stablizing 10-25 minute, turn down first the seed rod height 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 is reduced 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 with 2-10 rev/min speed rotary seed crystal rod, regulate simultaneously heater voltage, 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 for the first time seeding, form the seeding first paragraph; After stablizing 5 minutes, with 2-15 rev/min speed rotary seed crystal rod, regulate heater voltage, be warming up to 2052-2055 ℃, carry out the undergauge second time, the seed crystal diameter is reduced to 8-11mm; Upwards lift seed rod with 1-3.5mm/ minute speed, and with 2-10 rev/min speed rotary seed crystal rod, regulate simultaneously heater voltage, with the speed cooling of 0.5-2 ℃/h, carry out the seeding second time; 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 semisphere.
Beneficial effect of the present invention is:
1. can grow size surpasses 95kg greater than Φ 330 * 350 mm, weight large size optical grade sapphire crystal.
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, greatly improved the large size sapphire crystal quality.
3. by while the way that lifts the seed rod temperature adjustment, cooperate suitable seed rod rotation, strictly control the seeding form, the seed crystal diameter is evenly dwindled, avoided owing to the seeding morphological mutation causes additional defects is introduced sapphire crystal.
4. increase substantially kyropoulos growing large-size sapphire crystal and grow into power, 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 larger, and crystal grows into more advantages of higher of power.Thereby the present invention has broad application prospects, and applying of this technology can create obvious Social benefit and economic benefit.
(4) description of drawings
Fig. 1 is 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 crucible of single crystal furnace with 31 kg purity, installs the seed crystal that diameter is 12mm at seed rod, closes mono-crystal furnace cover, 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 ℃, stopped heating, 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 states was stable, 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 states was stable;
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, with 10 rev/mins speed rotary seed crystal rod, regulate heater voltage, be warming up to 2052 ℃, this moment, seed crystal began fusing, and after 5 minutes, the seed crystal diameter is reduced 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 simultaneously heater voltage, 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 for the first time seeding, form the seeding first paragraph; After stablizing 5 minutes, with 10 rev/mins speed rotary seed crystal rod, regulate heater voltage, be warming up to 2052 ℃, carry out the undergauge second time, the seed crystal diameter is reduced to 8mm; Upwards lift seed rod with 1mm/ minute speed, and with 8 rev/mins speed rotary seed crystal rod, regulate simultaneously heater voltage, with the speed cooling of 0.5 ℃/h, carry out seeding second time, formation seeding second segment; 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, seeding first paragraph 2 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 crucible of single crystal furnace with 85 kg purity, installs the seed crystal that diameter is 18mm at seed rod, closes mono-crystal furnace cover, 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 ℃, stopped heating, 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 states was stable, 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 states was stable;
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, being positioned at baking seed crystal in 4 mm places more than the liquid level, seed crystal lower end temperature is raise gradually near the bath surface temperature.
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, with 5 rev/mins speed rotary seed crystal rod, regulate heater voltage, be warming up to 2055 ℃, this moment, seed crystal began fusing, and after 15 minutes, the seed crystal diameter is reduced 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 simultaneously heater voltage, 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 for the first time seeding, form the seeding first paragraph; After stablizing 5 minutes, with 5 rev/mins speed rotary seed crystal rod, regulate heater voltage, be warming up to 2055 ℃, carry out the undergauge second time, the seed crystal diameter is reduced to 10mm; Upwards lift seed rod with 1.5mm/ minute speed, and with 4 rev/mins speed rotary seed crystal rod, regulate simultaneously heater voltage, with the speed cooling of 1 ℃/h, carry out the seeding second time; 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 (1)
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 crucible of single crystal furnace, install seed crystal at seed rod, close mono-crystal furnace cover, start cooling water recirculation system and start vacuum system, then start heating system, the adjusting heater voltage all melts raw material and reaches liquid level Convection states steady state, concrete steps comprise: I, with 31-95 kg high purity aluminium oxide material purity〉99.997% pack in the crucible of single crystal furnace, install the seed crystal that diameter is 12-22mm at seed rod, close mono-crystal furnace cover, start cooling water recirculation system; II, startup vacuum system make furnace pressure reach 10
-3Pa; III, the heating system that starts, the adjusting heater voltage, heat temperature raising, when temperature reaches 2150 ℃, stopped heating, raw material all melts; Be incubated after 3-5 hour, regulate heater voltage, be cooled to 2060 ℃, the liquid level Convection states is stable, keeps cold heart position and crucible geometric centre relative deviation 5-30 mm in the melt; IV, the auxiliary thermoregulating system of startup are regulated temperature field in furnace, and 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 states is stable;
(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, concrete steps comprise: 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;
(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 the heater voltage intensification, after seed crystal begins fusing, the cooling of adjusting heater voltage, seed rod stops the rotation, concrete steps comprise: after stablizing 10-25 minute, turn down first the seed rod height, 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 is reduced 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;
(4) seeding step repeatedly: upwards lift and rotary seed crystal rod, regulate simultaneously the heater voltage cooling, the part melt begins crystallization around seed crystal, finishes for the first time seeding, stable after rotary seed crystal rod again, regulate heater voltage and heat up, finish for the second time undergauge; Upwards lift again and rotary seed crystal rod, regulate simultaneously the heater voltage cooling, carry out the seeding second time, through forming the seeding latter end behind 3-10 the seeding, finish the seeding form, concrete steps comprise: upwards lift seed rod with 1-3mm/ minute speed, and with 2-10 rev/min speed rotary seed crystal rod, regulate simultaneously heater voltage, 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 for the first time seeding, form the seeding first paragraph; After stablizing 5 minutes, with 2-15 rev/min speed rotary seed crystal rod, regulate heater voltage, be warming up to 2052-2055 ℃, carry out the undergauge second time, the seed crystal diameter is reduced to 8-11mm; Upwards lift seed rod with 1-3.5mm/ minute speed, and with 2-10 rev/min speed rotary seed crystal rod, regulate simultaneously heater voltage, with the speed cooling of 0.5-2 ℃/h, carry out the seeding second time; 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 semisphere;
Large-size sapphire single-crystal refers to that size surpasses the large size optical grade sapphire crystal of 95kg greater than Φ 330 * 350 mm, weight.
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| 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 |
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| CN106987902A (en) * | 2017-03-20 | 2017-07-28 | 宁夏佳晶科技有限公司 | A kind of cold core shouldering for synthetic sapphire lifts preparation method |
| CN107059115A (en) * | 2017-04-20 | 2017-08-18 | 山西中聚晶科半导体有限公司 | A kind of kyropoulos prepare the growing method of sapphire crystal |
| 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 |
| CN109834584B (en) * | 2019-03-18 | 2021-01-29 | 内蒙古中环光伏材料有限公司 | Processing method of multistage reducing seed crystal and multistage reducing seed crystal |
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Address after: 150001 room 3, unit 101, building B1, Li Hua District, Daowai District, Heilongjiang, Harbin, China Patentee after: HARBIN AURORA OPTOELECTRONICS TECHNOLOGY CO., LTD. Address before: 150001 room 3, unit 101, building B1, Li Hua District, Daowai District, Heilongjiang, Harbin, China Patentee before: Harbin Aurora Optoelectronics Technology Co., Ltd. |
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Denomination of invention: Method for controlling seeding form in process of preparing large-sized sapphire single crystal by Kyropoulos method Effective date of registration: 20180929 Granted publication date: 20130123 Pledgee: Longjiang bank Limited by Share Ltd Harbin Development Zone sub branch Pledgor: HARBIN AURORA OPTOELECTRONICS TECHNOLOGY CO., LTD. Registration number: 2018990000856 Denomination of invention: Method for controlling seeding form in process of preparing large-sized sapphire single crystal by Kyropoulos method Effective date of registration: 20180929 Granted publication date: 20130123 Pledgee: Longjiang bank Limited by Share Ltd Harbin Development Zone sub branch Pledgor: HARBIN AURORA OPTOELECTRONICS TECHNOLOGY CO., LTD. Registration number: 2018990000856 |
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Date of cancellation: 20200509 Granted publication date: 20130123 Pledgee: Longjiang bank Limited by Share Ltd Harbin Development Zone sub branch Pledgor: HARBIN AURORA OPTOELECTRONICS TECHNOLOGY Co.,Ltd. Registration number: 2018990000856 |