WO2016082361A1 - 蓝宝石单晶生长plc闭环控制方法 - Google Patents

蓝宝石单晶生长plc闭环控制方法 Download PDF

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Publication number
WO2016082361A1
WO2016082361A1 PCT/CN2015/073475 CN2015073475W WO2016082361A1 WO 2016082361 A1 WO2016082361 A1 WO 2016082361A1 CN 2015073475 W CN2015073475 W CN 2015073475W WO 2016082361 A1 WO2016082361 A1 WO 2016082361A1
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Prior art keywords
crystal
growth
temperature
weight
power
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PCT/CN2015/073475
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English (en)
French (fr)
Chinese (zh)
Inventor
裴广庆
王佳麒
罗亮远
黄小卫
柳祝平
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元亮科技有限公司
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Priority to JP2016568099A priority Critical patent/JP6325691B2/ja
Publication of WO2016082361A1 publication Critical patent/WO2016082361A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/20—Aluminium oxides

Definitions

  • the invention relates to a sapphire single crystal growth control method, in particular to a sapphire single crystal growth PLC closed-loop control method, belonging to the technical field of crystal growth.
  • Sapphire single crystal has excellent comprehensive properties such as good transparency, high mechanical strength, excellent chemical stability and good thermal conductivity. First of all, it has ultra-high hardness and very low friction coefficient, which is second only to diamond in nature; it has high optical transmission in ultra-wideband (300nm ⁇ 5000nm); sapphire single crystal also has excellent resistance to acid and alkali corrosion. Generally, acid and alkali can not be eroded under normal temperature and even in molten state, so the commercial application of sapphire single crystal as a high-end optoelectronic material has emerged.
  • the object of the present invention is to overcome the deficiencies in the prior art and provide a closed-loop control method for sapphire single crystal growth PLC, which can realize real-time integrated control of large-size, high-quality sapphire single crystal automatic growth, high control precision and good stability. .
  • a closed-loop control method for sapphire single crystal growth PLC is characterized in that: a load cell, a temperature sensor, a water flow sensor, a water pressure transmitter, and a human-machine operating system are installed on the sapphire growth furnace.
  • the crystal growth curve parameters and PID parameters are imported into the operating system.
  • the operating system compares the actual weight of the crystal according to the automatically read load cell, compares the crystal growth curve, adjusts the output power and the temperature and water flow of each node, so that the crystal follows the established process.
  • Automatic growth specifically includes the following steps:
  • the seed crystal is contacted with the liquid surface to maintain the temperature inside the furnace, and the control power varies from ⁇ 1 to 5 kW, the rising speed of the control crystal rod is 500-1000r/h, and the rotation speed is 200-500r/h. Pull the seed crystal to a length of 30-40mm thin neck;
  • shoulder and equal diameter growth During the process of shoulder and equal diameter growth, the operating system automatically adjusts the power lifting and lowering, and automatically adjusts the crystal rod, furnace water temperature and pulling speed according to different growth stages to meet the crystal. The temperature gradient required for growth;
  • the specific process of adjusting the power rise and fall of the operating system is: sampling every other sampling period t (t is 5 to 30 seconds), and obtaining a variation value m1 of the theoretical growth weight and a change value of the actual weight of the crystal in a sampling period t.
  • the PID operation is performed on m1 and m2. Since the comparison base is too small, the stability of the PID operation is deteriorated, causing the fluctuation of the power fluctuation amplitude to be large; and when the base is too large, the control delay is too large, so the constant M is introduced.
  • the setting range of M is 1000 ⁇ 3000, PID operation is performed on m1+M and m2+M, and then the output power u is adjusted;
  • the calculation formula of the output power u is obtained: when m1>m2, the operating system controls the output power to decrease; when m1 ⁇ m2, the operating system controls the output transmission rate to rise;
  • the sampling period t is 20 to 30 s
  • the M value is 1000 to 2000
  • the K P is 20% to 30%
  • the T I is 40 s to 80 s
  • the T D is 10 s to 20 s
  • the power lifting rate is less than 1 kW/h.
  • the crystal temperature of the crystal rod is controlled at 35-40 °C
  • the water temperature of the furnace is controlled at 30-35 °C
  • the pulling speed is controlled at 1 ⁇ 1.5 mm/h;
  • the sampling period t is 10-20s, the M value is 1500 ⁇ 2500, the K P is 30% ⁇ 40%, the T I is 80s ⁇ 120s, the T D is 20s ⁇ 30s, and the power lifting rate is less than 0.8kW/ h;
  • the crystal water temperature is controlled at 40 ⁇ 45 ° C, the furnace water temperature is controlled at 35 ⁇ 40 ° C, the pulling speed is controlled at 0.8 ⁇ 1.2 mm / h;
  • the sampling period t is 5 to 10 s
  • the M value is 2000 to 3000
  • the K P is 40% to 50%
  • the T I is 120 s to 160 s
  • the T D is 30 s to 40 s
  • the power lifting rate is less than 0.5 kW/ h
  • the crystal water temperature is controlled at 45 ⁇ 50 ° C
  • the furnace water temperature is controlled at 40 ⁇ 45 ° C
  • the pulling speed is controlled at 0.4 ⁇ 0.8 mm / h;
  • the shouldering stage means that the crystal weight is 0 to 15% of the weight of the feed.
  • the equal-diameter period means that the crystal weight is 15 to 50% of the weight of the feed.
  • the later stage of the equal diameter means that the crystal weight is 50 to 95% of the weight of the feed.
  • the water pressure is maintained at 0.12 to 0.18 MPa throughout the growth process.
  • the operating system adjusts the power once every sampling time.
  • the invention introduces an optimized PLC closed-loop control system on a sapphire growth furnace, and automatically compares the actual weight of the crystal obtained by the load cell, and compares the crystal growth curve parameters introduced in the system.
  • the system can realize the rapid response of PLC closed-loop control system and improve the control of crystal growth by setting appropriate PID control parameters (proportion coefficient, integration time, differential time, sampling period, amplification).
  • PID control parameters proportion coefficient, integration time, differential time, sampling period, amplification.
  • the system also uses the installed temperature sensor, water flow sensor and water pressure transmitter to automatically adjust the parameters such as water temperature, water pressure and speed, and the system realizes crystal growth.
  • Embodiment 1 A closed-loop control method for sapphire single crystal growth PLC, mounting a load cell (weight accuracy of one hundred thousandth), a temperature sensor (temperature control accuracy of 0.1 ° C), a water flow sensor, and a sapphire growth furnace, Water pressure transmitter and human-machine operating system, crystal growth curve parameters and PID parameters are imported into the operating system.
  • the operating system calculates the actual weight of the crystal according to the automatically read load cell, compares the crystal growth curve, adjusts the output power and each The node temperature and water flow rate enable the crystal to grow automatically according to the established process; specifically, the following steps are included:
  • the seed crystal is contacted with the liquid surface to maintain the temperature inside the furnace, and the power change is controlled at ⁇ 1 ⁇ 5kW.
  • the rising speed of the control rod is 500r/h, and the rotation speed is 200r/h, so that the seed crystal is pulled.
  • shoulder and equal diameter growth During the process of shoulder and equal diameter growth, the operating system automatically adjusts the power lifting and lowering, and automatically adjusts the crystal rod, furnace water temperature and pulling speed according to different growth stages to meet the crystal. The temperature gradient required for growth;
  • the specific process of adjusting the power rise and fall of the operating system is: sampling every other sampling period t (t is 5 to 30 seconds), and obtaining a variation value m1 of the theoretical growth weight and a change value of the actual weight of the crystal in a sampling period t.
  • the PID operation is performed on m1 and m2. Since the comparison base is too small, the stability of the PID operation is deteriorated, causing the fluctuation of the power fluctuation amplitude to be large; and when the base is too large, the control delay is too large, so the constant M is introduced.
  • the setting range of M is 1000 ⁇ 3000, PID operation is performed on m1+M and m2+M, and then the output power u is adjusted;
  • the shoulder stage (crystal weight is 0-15% of the weight of the feed), the sampling period t is 20s, the M value is 1000, the K P is 20%, the T I is 40s, the T D is 10s, and the power lifting rate is less than 1kW/ h; the crystal water temperature is controlled at 35 ° C, the furnace water temperature is controlled at 30 ° C, and the pulling speed is controlled at 1 mm / h;
  • the sampling period t is 10s
  • the M value is 1500
  • the K P is 30%
  • the T I is 80s
  • the T D is 20s
  • the power lifting rate is less than 0.8kW. /h
  • the crystal water temperature is controlled at 40 ° C
  • the furnace water temperature is controlled at 35 ° C
  • the pulling speed is controlled at 0.8 mm / h;
  • Crystal weight is 50 ⁇ 95% of feed weight
  • sampling period t is 5s
  • M value is 2000
  • K P is 40%
  • T I is 120s
  • T D is 30s
  • power lifting rate is less than 0.5kW /h
  • the crystal water temperature is controlled at 45 ° C
  • the furnace water temperature is controlled at 40 ° C
  • the pulling speed is controlled at 0.4 mm / h;
  • the system automatically controls the water pressure to be maintained at 0.12 MPa throughout the growth process.
  • Embodiment 2 A closed-loop control method for sapphire single crystal growth PLC, mounting a load cell (weight accuracy of one hundred thousandth), a temperature sensor (temperature control accuracy of 0.1 ° C), a water flow sensor, and a sapphire growth furnace.
  • Water pressure transmitter and human-machine operating system, crystal growth curve parameters and PID parameters are imported into the operating system.
  • the operating system calculates the actual weight of the crystal according to the automatically read load cell, compares the crystal growth curve, adjusts the output power and each The node temperature and water flow rate enable the crystal to grow automatically according to the established process; specifically, the following steps are included:
  • the bottom seed crystal contacts the liquid surface, maintains the furnace temperature, and controls the power change in ⁇ 1 ⁇ 5kW, controls the crystal rod rising speed at 1000r/h, and rotates at 500r/h, so that the seed crystal pulls a neck with a length of 40 mm;
  • shoulder and equal diameter growth During the process of shoulder and equal diameter growth, the operating system automatically adjusts the power lifting and lowering, and automatically adjusts the crystal rod, furnace water temperature and pulling speed according to different growth stages to meet the crystal. The temperature gradient required for growth;
  • the specific process of adjusting the power rise and fall of the operating system is: sampling every other sampling period t (t is 5 to 30 seconds), and obtaining a variation value m1 of the theoretical growth weight and a change value of the actual weight of the crystal in a sampling period t.
  • PID operation is performed on m1 and m2. Since the comparison base is too small, the stability of the PID operation is deteriorated, causing the power fluctuation range to fluctuate greatly; and when the base is too large, the control delay is too large, so the constant M is introduced.
  • the setting range of M is 1000 ⁇ 3000, PID operation is performed on m1+M and m2+M, and then the output power u is adjusted;
  • the operating system controls the output power to decrease, and the larger the difference, the faster the power reduction rate; when m1 ⁇ m2, the operating system controls the output transmission rate to rise, and The larger the difference, the faster the rate of power rise;
  • the shoulder stage (crystal weight is 0-15% of the weight of the feed), the sampling period t is 30s, the M value is 2000, the K P is 30%, the T I is 80s, the T D is 20s, and the power lifting rate is less than 1kW/ h; the crystal water temperature is controlled at 40 ° C, the furnace water temperature is controlled at 35 ° C, and the pulling speed is controlled at 1.5 mm / h;
  • the sampling period t is 20s
  • the M value is 2500
  • the K P is 40%
  • the T I is 120s
  • the T D is 30s
  • the power lifting rate is less than 0.8kW. /h
  • the crystal water temperature is controlled at 45 ° C
  • the furnace water temperature is controlled at 40 ° C
  • the pulling speed is controlled at 1.2 mm / h;
  • crystal weight is 50 ⁇ 95% of the weight of the feed
  • sampling period t is 10s
  • M value is 3000
  • K P is 50%
  • T I is 160s
  • T D is 40s
  • power lifting rate is less than 0.5kW /h
  • the crystal water temperature is controlled at 50 ° C
  • the furnace water temperature is controlled at 45 ° C
  • the pulling speed is controlled at 0.8 mm / h;
  • the system automatically controls the water pressure to be maintained at 0.18 MPa throughout the growth process.
  • Embodiment 3 A closed-loop control method for sapphire single crystal growth PLC, installing a load cell (weight accuracy of one hundred thousandth), a temperature sensor (temperature control accuracy of 0.1 ° C), a water flow sensor, and a sapphire growth furnace, Water pressure transmitter and human-machine operating system, crystal growth curve parameters and PID parameters are imported into the operating system.
  • the operating system calculates the actual weight of the crystal according to the automatically read load cell, compares the crystal growth curve, adjusts the output power and each The node temperature and water flow rate enable the crystal to grow automatically according to the established process; specifically, the following steps are included:
  • the seed crystal is contacted with the liquid surface to maintain the temperature in the furnace, and the power variation is controlled at ⁇ 1 ⁇ 5kW.
  • the rising speed of the control rod is 600r/h, and the rotation speed is 400r/h, so that the seed crystal is pulled. a neck with a length of 35 mm;
  • shoulder and equal diameter growth During the process of shoulder and equal diameter growth, the operating system automatically adjusts the power lifting and lowering, and automatically adjusts the crystal rod, furnace water temperature and pulling speed according to different growth stages to meet the crystal. The temperature gradient required for growth;
  • the specific process of adjusting the power rise and fall of the operating system is: sampling every other sampling period t (t is 5 to 30 seconds), and obtaining a variation value m1 of the theoretical growth weight and a change value of the actual weight of the crystal in a sampling period t.
  • the PID operation is performed on m1 and m2. Since the comparison base is too small, the stability of the PID operation is deteriorated, causing the fluctuation of the power fluctuation amplitude to be large; and when the base is too large, the control delay is too large, so the constant M is introduced.
  • the setting range of M is 1000 ⁇ 3000, PID operation is performed on m1+M and m2+M, and then the output power u is adjusted;
  • the operating system controls the output power to decrease, and the larger the difference, the faster the power reduction rate; when m1 ⁇ m2, the operating system controls the output transmission rate to rise, and The larger the difference, the faster the rate of power rise;
  • the shoulder stage (crystal weight is 0-15% of the weight of the feed), the sampling period t is 25s, the M value is 1500, the K P is 25%, the T I is 60s, the T D is 15s, and the power lifting rate is less than 1kW/ h; the crystal water temperature is controlled at 36 ° C, the furnace water temperature is controlled at 32 ° C, and the pulling speed is controlled at 1.2 mm / h;
  • the sampling period t is 16s
  • the M value is 2000
  • the K P is 30% to 40%
  • the T I is 100s
  • the T D is 25s
  • the rate of power rise and fall Less than 0.8kW/h
  • the crystal water temperature is controlled at 42 °C
  • the furnace water temperature is controlled at 36 °C
  • the pulling speed is controlled at 1 mm/h;
  • crystal weight is 50 ⁇ 95% of the weight of the feed
  • sampling period t is 6s
  • M value is 2500
  • K P is 45%
  • T I is 150s
  • T D is 35s
  • power lifting rate is less than 0.5kW /h
  • the crystal water temperature is controlled at 46 ° C
  • the furnace water temperature is controlled at 42 ° C
  • the pulling speed is controlled at 0.6 mm / h;
  • the system automatically controls the water pressure to be maintained at 0.16 MPa throughout the growth process.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
PCT/CN2015/073475 2014-11-26 2015-03-02 蓝宝石单晶生长plc闭环控制方法 WO2016082361A1 (zh)

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CN115198351A (zh) * 2022-08-19 2022-10-18 中国电子科技集团公司第二十六研究所 一种自动生长低温敏感人工晶体材料加热功率控制方法
CN117668740A (zh) * 2024-02-02 2024-03-08 浙江晶盛机电股份有限公司 蓝宝石的长速异常检测方法、装置、电子装置和存储介质

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CN106283178A (zh) * 2016-08-30 2017-01-04 中国科学院合肥物质科学研究院 一种大尺寸提拉法单晶生长设计和控制方法
CN106435731B (zh) * 2016-08-31 2019-03-26 南京晶升能源设备有限公司 蓝宝石炉自动引晶控制系统和单晶炉引晶控制方法
CN109722715A (zh) * 2017-10-27 2019-05-07 江苏维福特科技发展股份有限公司 晶体生长加热系统
CN108221045A (zh) * 2018-01-24 2018-06-29 新疆工程学院 一种晶体生长炉温度控制系统
CN108441941B (zh) * 2018-02-13 2021-01-15 中山大学 熔体本征对流波动的原位探测方法、控制方法及控制系统
CN108624952A (zh) * 2018-04-25 2018-10-09 上海翌波光电科技股份有限公司 一种晶体生长控制装置及控制方法
CN112458533A (zh) * 2020-10-30 2021-03-09 山东新升光电科技有限责任公司 一种蓝宝石单晶生长系统及方法
CN112725883B (zh) * 2020-12-24 2022-03-22 宁夏盾源聚芯半导体科技股份有限公司 控制单晶硅尾部长度的方法及单晶炉收尾方法

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CN115198351A (zh) * 2022-08-19 2022-10-18 中国电子科技集团公司第二十六研究所 一种自动生长低温敏感人工晶体材料加热功率控制方法
CN115198351B (zh) * 2022-08-19 2023-11-24 中国电子科技集团公司第二十六研究所 一种自动生长低温敏感人工晶体材料加热功率控制方法
CN117668740A (zh) * 2024-02-02 2024-03-08 浙江晶盛机电股份有限公司 蓝宝石的长速异常检测方法、装置、电子装置和存储介质

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