CN102758251A - Method for controlling sapphire seeding form of Kyropoulos method - Google Patents
Method for controlling sapphire seeding form of Kyropoulos method Download PDFInfo
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- CN102758251A CN102758251A CN2012102793583A CN201210279358A CN102758251A CN 102758251 A CN102758251 A CN 102758251A CN 2012102793583 A CN2012102793583 A CN 2012102793583A CN 201210279358 A CN201210279358 A CN 201210279358A CN 102758251 A CN102758251 A CN 102758251A
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Abstract
The invention discloses a method for controlling a sapphire seeding form of a Kyropoulos method. The method comprises that an aluminum oxide raw material is placed in a mono-crystal furnace crucible, seed crystal is installed on a seed crystal rod, a vacuum system and a heating system are started, the voltage of the heating system is adjusted, so that the aluminum oxide raw material is melted completely, a convectional stable state of a melt surface is achieved, and the deviation distance of a cold core of a liquid level and a geometric centre of the crucible is less than 20mm; the seed crystal position is adjusted slowly, then the seed crystal is close to the melt liquid surface gradually, simultaneously, the working voltage of the heating system is adjusted, and the melting of the seed crystal is avoided; preheating is performed for 30 minutes at a position of 2-5mm from the lower end portion of the seed crystal to the melt liquid surface; and the seed crystal is rotated through a traditional Czochralski process, the working voltage of the heating system is adjusted, the diameter of the end portion of crystallization is controlled to be less than 50mm and shouldering is started to be performed after the cold core is coated by the end portion of the crystallization. By the aid of the method, the form of the end portion of the crystallization can be well controlled, the operation is simple, and the success ratio and the yield of the seed crystal are improved.
Description
Technical field
The present invention relates to a kind of sapphire growth technology, especially a kind of kyropoulos sapphire seeding configuration control method belongs to the technical field that sapphire prepares.
Background technology
Sapphire crystal (being commonly called as corundum), from vacuum, ultraviolet, visible, near infrared until infraredly all have a high optical transmittance, also have high mechanical strength, extremely low uptake factor.The high temperature refractoriness of sapphire crystal; Good chemicalstability; It is good laser host material; Be the window material of various optical elements and infrared military installation, satellite spatial technology, high intensity laser beam, be to use the most general blue-light semiconductor diode (LED) and the substrate material of diode LD, almost spread all over all substrate applications fields.At present, sapphire growth method mainly contains crystal pulling method (Cz), guided mode method (EFG), kyropoulos (Ky), heat-exchanging method (HEM) etc.Wherein, the kyropoulos growing system has the optimum temperature gradation that is fit to sapphire crystal growth.In the process of growth or when finishing, crystal does not contact with crucible, has significantly reduced its stress, can obtain high-quality macrocrystal, is the main stream approach of present sapphire crystal growth.Under the perfect condition; The cold heart of melt overlaps with the crucible geometric centre, but in real work, the distribution of heating member can not reach the perfect condition of design; The heterogeneity that the distance of thermoscreen and crucible and thermoscreen are inner causes the cold heart of melt not overlap with the geometric centre of crucible.Therefore in the whole technological process of kyropoulos growing sapphire, seeding is a most important step.In this process, make the crystallization end cover the cold heart and the place's shouldering of the self cooling heart.All in the world kyropoulos sapphire single-crystal stoves seeding automated operation of all being unrealized at present, whole seeding process depends on seeding slip-stick artist's experience and operant level, and does not have the standard and the working specification of unified quantization.
Summary of the invention
The objective of the invention is to overcome the deficiency that exists in the prior art, a kind of kyropoulos sapphire seeding configuration control method is provided, it is easy to operate, improves seeding success ratio and yield rate.
According to technical scheme provided by the invention, a kind of kyropoulos sapphire seeding configuration control method, said sapphire seeding configuration control method comprises the steps:
A, alumina raw material is packed in the single crystal growing furnace crucible; Seed crystal is installed on seed rod; Start vacuum system and heating system; Regulate the voltage of heating system,, and make the cold heart of liquid level and crucible geometric centre depart from less than 20mm so that alumina raw material all melts and reaches bath surface convectional stability state;
B, slowly regulate the seed crystal position, make seed crystal move closer to melt liquid level, regulate the WV of heating system simultaneously, to avoid the seed crystal fusion;
C, at bottom and above-mentioned melt liquid level 2 ~ 5mm place's preheating 30min ~ 60min of seed crystal;
D, utilize traditional czochralski process, the rotation seed crystal is regulated the WV of heating system, and the diameter of crystallization control end is less than 50mm, and begins shouldering after making the crystallization end cover the cold heart.
In the said steps d, the speed of seed crystal rotation is 2 ~ 3rpm, and the spreading rate of seed crystal contact melt liquid level starting stage crystallization end is less than 0.3mm/min, and regulates according to said spreading rate and to lift height,, with the diameter of crystallization control end less than 50mm.
When the spreading rate of said crystallization end was 0.2mm ~ 0.3mm/min, every 5min lifted seed crystal once, and lift highly is 1.5 ~ 2mm at every turn.
When the spreading rate of said crystallization end was 0 ~ 0.2mm/min, per 5 ~ 10min lifted seed crystal once, and lift highly is 1 ~ 1.5mm at every turn.
Advantage of the present invention: in the seeding process, cooperate the seed crystal rotation, avoided " long monolateral " phenomenon that the crystallization end occurs under the non-rotating state, and be beneficial to the operator observes the crystallization end in the seeding process form; Utilize traditional crystal pulling method, and will lift height and pitch time of lifting for twice and the spreading rate of crystallization end and be based upon on the quantized basis, preferably the form of crystallization control end; Lift fit adjustment voltage in the process, size that can the crystallization control end, and make the crystallization end cover the cold heart and begin shouldering, easy to operate, improve seeding success ratio and yield rate.
Embodiment
Below in conjunction with specific embodiment the present invention is described further.
In order to improve the seeding success ratio, and sapphire seeding morphology Control is formed a kind of unified quantitative criteria, sapphire seeding configuration control method of the present invention comprises the steps:
A, alumina raw material is packed in the single crystal growing furnace crucible; Seed crystal is installed on seed rod; Start vacuum system and heating system; Regulate the voltage of heating system,, and make the cold heart of liquid level and crucible geometric centre depart from less than 20mm so that alumina raw material all melts and reaches bath surface convectional stability state;
Usually, changing the material stage, at first adopt higher speed up voltage; Be generally 1000mV/h, near the raw material fusing point, stop, adopting less rate adaptation voltage; Raw material is heated fully, evenly, can avoids crucible is damaged simultaneously.
During practical implementation, generally about 11V, corresponding sapphire fusing point is 2050 ℃ to change material voltage.When voltage is raised to 10.6 V, stop the two-forty up voltage, use the regulations speed of 50 ~ 200mV/h instead.Abundant in order to change material, voltage will be elevated on the fusing point, just more than 11 volts.
B, slowly regulate the seed crystal position, make seed crystal move closer to melt liquid level, regulate the WV of heating system simultaneously, to avoid the seed crystal fusion;
Because for raw material is fully melted, the temperature of melt is higher than fusing point, also just is higher than the seeding temperature.In the process of decline seed crystal, utilize LOAD CELLS relatively sensitiveer, descend if find seed crystal weight; Stop the seed crystal that descends immediately, reduce voltage 30-50mV simultaneously, 20min is with the continued seed crystal that descends; Seek suitable seeding temperature with the weight of utilizing seed crystal, guarantee carrying out smoothly of seeding.
C, at bottom and above-mentioned melt liquid level 2 ~ 5mm place's preheating 30min ~ 60min of seed crystal; Through preheating, eliminate stress;
Owing to do not have TP in the sapphire single-crystal stove, all temperature regulation all occur with the VR of correspondence.The voltage of preheating is exactly seed crystal 2 ~ 5mm place above liquid level, and seed crystal weight is stable, and pairing voltage when promptly fusion not taking place is within being about of the voltage material voltage ± 0.5v of preheating.The voltage that also has only this moment is in the scope that spreading rate just can be described in the text behind seed crystal contact liquid level.
D, utilize traditional czochralski process, the rotation seed crystal is regulated the WV of heating system, and the diameter of crystallization control end is less than 50mm, and begins shouldering after making the crystallization end cover the cold heart.
Wherein, the speed of seed crystal rotation is 2 ~ 3rpm, and the spreading rate of seed crystal contact melt liquid level starting stage crystallization end is less than 0.3mm/min, and regulates according to said spreading rate and to lift height,, with the diameter of crystallization control end less than 50mm.When the spreading rate of said crystallization end was 0.2mm ~ 0.3mm/min, every 5min lifted seed crystal once, and lift highly is 1.5 ~ 2mm at every turn.When the spreading rate of said crystallization end was 0 ~ 0.2mm/min, per 5 ~ 10min lifted seed crystal once, and lift highly is 1 ~ 1.5mm at every turn.
During the prior art seeding, the non-rotation seeding of the employing that has, the employing that has rotation seeding, the discontinuous rotation seeding of the employing that has, what we adopted is the mode of rotating seeding continuously, the rotation of seed crystal is set at 2 ~ 3rpm.The rotation seeding is beneficial to operator's observation continuously.Of the present inventionly be to utilize seed crystal weight to seek suitable seeding voltage; Because the sapphire single-crystal stove does not generally have TP at present; Lean on operator's experience to confirm seeding voltage, unreliable, confirm the time of lifting, lift these technologies highly according to spreading rate; Through above-mentioned these processing parameters being set up the standard of a unified quantization, to improve the seeding success ratio.
The present invention cooperates the seed crystal rotation in the seeding process, avoided " long monolateral " phenomenon that the crystallization end occurs under the non-rotating state, and be beneficial to the operator observes the crystallization end in the seeding process form; Utilize traditional crystal pulling method, and will lift height and pitch time of lifting for twice and the spreading rate of crystallization end and be based upon on the quantized basis, preferably the form of crystallization control end; Lift fit adjustment voltage in the process, size that can the crystallization control end, and make the crystallization end cover the cold heart and begin shouldering.
Claims (4)
1. a kyropoulos sapphire seeding configuration control method is characterized in that, said sapphire seeding configuration control method comprises the steps:
(a), alumina raw material is packed in the single crystal growing furnace crucible; Seed crystal is installed on seed rod; Start vacuum system and heating system; Regulate the voltage of heating system,, and make the cold heart of liquid level and crucible geometric centre depart from less than 20mm so that alumina raw material all melts and reaches bath surface convectional stability state;
(b), slowly regulate the seed crystal position, make seed crystal move closer to melt liquid level, regulate the WV of heating system simultaneously, to avoid the seed crystal fusion;
(c), at bottom and above-mentioned melt liquid level 2 ~ 5mm place's preheating 30min ~ 60min of seed crystal;
(d), utilize traditional czochralski process, the rotation seed crystal is regulated the WV of heating system, the diameter of crystallization control end is less than 50mm, and begins shouldering after making the crystallization end cover the cold heart.
2. kyropoulos sapphire seeding configuration control method according to claim 1; It is characterized in that: in the said step (d); The speed of seed crystal rotation is 2 ~ 3rpm, and the spreading rate of seed crystal contact melt liquid level starting stage crystallization end is less than 0.3mm/min, and regulates according to said spreading rate and to lift height;, with the diameter of crystallization control end less than 50mm.
3. kyropoulos sapphire seeding configuration control method according to claim 2 is characterized in that: when the spreading rate of said crystallization end was 0.2mm ~ 0.3mm/min, every 5min lifted seed crystal once, and lift highly is 1.5 ~ 2mm at every turn.
4. kyropoulos sapphire seeding configuration control method according to claim 2, it is characterized in that: when the spreading rate of said crystallization end was 0 ~ 0.2mm/min, per 5 ~ 10min lifted seed crystal once, and lift highly is 1 ~ 1.5mm at every turn.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103451729A (en) * | 2013-09-17 | 2013-12-18 | 无锡鼎晶光电科技有限公司 | Growth method of square sapphire |
| CN103806091A (en) * | 2014-02-26 | 2014-05-21 | 闽能光电集团有限公司 | Automatic control method for sapphire crystals in edge-defined film-fed growth |
| CN104109904A (en) * | 2014-05-27 | 2014-10-22 | 上海佳宇信息技术有限公司 | Seeding method of sapphire crystal growth kyropoulos method |
| CN104264216A (en) * | 2014-10-12 | 2015-01-07 | 刘瑜 | High-reliability automatic seeding process for sapphire crystal growth through kyropoulos method |
| CN104562198A (en) * | 2014-12-12 | 2015-04-29 | 宁波循泽电子科技有限公司 | Method for improving growth of kyropoulos method sapphire single crystal |
| CN104674345A (en) * | 2014-12-26 | 2015-06-03 | 浙江东海蓝玉光电科技有限公司 | Seeding control method for large-size sapphire crystals growing through Kyropulos method |
| CN104674340A (en) * | 2014-12-26 | 2015-06-03 | 浙江东海蓝玉光电科技有限公司 | Rotary necking and seeding control method used in large-size sapphire crystal growth through kyropoulos method |
| CN104911708A (en) * | 2015-06-15 | 2015-09-16 | 哈尔滨奥瑞德光电技术股份有限公司 | Growth method for preparing square sapphire crystal by Kyropoulos process |
| CN106149048A (en) * | 2015-07-02 | 2016-11-23 | 宁夏佳晶科技有限公司 | A kind of KY method sapphire coarse vacuum growing method |
| CN116575114A (en) * | 2023-07-14 | 2023-08-11 | 内蒙古晶环电子材料有限公司 | Seeding method |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103451729A (en) * | 2013-09-17 | 2013-12-18 | 无锡鼎晶光电科技有限公司 | Growth method of square sapphire |
| CN103806091A (en) * | 2014-02-26 | 2014-05-21 | 闽能光电集团有限公司 | Automatic control method for sapphire crystals in edge-defined film-fed growth |
| CN104109904A (en) * | 2014-05-27 | 2014-10-22 | 上海佳宇信息技术有限公司 | Seeding method of sapphire crystal growth kyropoulos method |
| CN104264216A (en) * | 2014-10-12 | 2015-01-07 | 刘瑜 | High-reliability automatic seeding process for sapphire crystal growth through kyropoulos method |
| CN104562198B (en) * | 2014-12-12 | 2017-04-12 | 宁波循泽电子科技有限公司 | Method for improving growth of kyropoulos method sapphire single crystal |
| CN104562198A (en) * | 2014-12-12 | 2015-04-29 | 宁波循泽电子科技有限公司 | Method for improving growth of kyropoulos method sapphire single crystal |
| CN104674345A (en) * | 2014-12-26 | 2015-06-03 | 浙江东海蓝玉光电科技有限公司 | Seeding control method for large-size sapphire crystals growing through Kyropulos method |
| CN104674340A (en) * | 2014-12-26 | 2015-06-03 | 浙江东海蓝玉光电科技有限公司 | Rotary necking and seeding control method used in large-size sapphire crystal growth through kyropoulos method |
| CN104911708A (en) * | 2015-06-15 | 2015-09-16 | 哈尔滨奥瑞德光电技术股份有限公司 | Growth method for preparing square sapphire crystal by Kyropoulos process |
| 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 |
| CN106149048A (en) * | 2015-07-02 | 2016-11-23 | 宁夏佳晶科技有限公司 | A kind of KY method sapphire coarse vacuum growing method |
| CN116575114A (en) * | 2023-07-14 | 2023-08-11 | 内蒙古晶环电子材料有限公司 | Seeding method |
| CN116575114B (en) * | 2023-07-14 | 2023-11-28 | 内蒙古晶环电子材料有限公司 | Seeding method |
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