WO2003052175A1 - Equipement de production en 'chute d'eau' pour la croissance de cristaux - Google Patents

Equipement de production en 'chute d'eau' pour la croissance de cristaux Download PDF

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Publication number
WO2003052175A1
WO2003052175A1 PCT/IB2001/002641 IB0102641W WO03052175A1 WO 2003052175 A1 WO2003052175 A1 WO 2003052175A1 IB 0102641 W IB0102641 W IB 0102641W WO 03052175 A1 WO03052175 A1 WO 03052175A1
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WO
WIPO (PCT)
Prior art keywords
control
vacuum
weight sensor
unit
growth
Prior art date
Application number
PCT/IB2001/002641
Other languages
English (en)
Inventor
Mark Fielker
Igor Kuznetsov
Original Assignee
Mark Fielker
Igor Kuznetsov
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mark Fielker, Igor Kuznetsov filed Critical Mark Fielker
Priority to PCT/IB2001/002641 priority Critical patent/WO2003052175A1/fr
Publication of WO2003052175A1 publication Critical patent/WO2003052175A1/fr

Links

Classifications

    • 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
    • C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos 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
    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20—Controlling or regulating
    • 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
    • C30B15/20—Controlling or regulating
    • C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
    • C30B15/28—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal using weight changes of the crystal or the melt, e.g. flotation methods
    • 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

  • Production equipment can be utilized for oxide single crystal growth, particularly of single crystals of sapphire, by the Czochralski and Kyropoulus methods in the vacuum environment and equipped with a system of control of the growing single crystal through a string weight sensor (international priority obtained by virtue of PCT/IB01/02281 ).
  • the invention in question has vast application in the semiconductor, electronics and instrument-making industries.
  • Production equipment "Waterfall” can also be used for research purposes that are geared to creation and development of new technologies of oxide single crystal growth.
  • the prototype of the production equipment for single crystal growth “Waterfall” was a production unit "Omega 3" designed and built by a Lugansk production company "Zavod Donets” in 1986 to serve as the base model for subsequent developments.
  • a resistive heating unit “Omega 3” was designed for bulk single crystal growth of leucosapphire by the Czochralski and Kyropoulus methods in the vacuum with the maximum output diameter of Similar equipment to the production equipment "Waterfall” is "Astra” of a Lugansk company “Zavod Donets” and a production unit "Oxypuller” of Cyberstar.
  • Resistive heating production equipment Waterfall
  • a high precision string weight sensor has been designed for automated crystal growth processes of bulk leucosapphire in the vacuum environment and by the Czochralski and Kyropoulus methods.
  • the maximum diameter of single crystals that can be grown on the given equipment is 150 mm.
  • the system of control equipped with a string weight sensor allows for the growth of single crystals with preset geometric parameters and weight by means of high precision control of these parameters in the process of growth.
  • This equipment allows for the growth of a range of other oxide single crystals in the vacuum environment, than single crystals of sapphire.
  • This production equipment consists of the following parts and sections: a Load Bearing Frame (1 ), a Vacuum Chamber (2) with water-cooled walls, a Heat Unit (3) with a resistive heater, a Rack of Drives (4), a Standard and Accelerated Displacement Drive (5), a Manual Control Unit (6), a Manual Lifting Drive for the Top Lid (7), Current Leads (8), Viewing Windows (9), Horizontal Displacement Unit for X and Y (10), Rod Rotation Drives (11 ), a Sylphon Unit (12), a Hollow water-cooled Rod (13), a String Weight Sensor (14) with an Electronic Section (15), a Power Cabinet (16), a Control Rack (17), an Industrial Workstation (18), a Control Unit (19), a Control Unit for the Vacuum Set (21 ).
  • the principle units of the equipment are mounted on the Load Bearing Frame
  • the Vacuum Chamber (2) with the Heat Unit (3) is the workspace for conducting of technological processes of bulk leucosapphire single crystal growth.
  • the Rack of Drives (4) that is mounted up on the top slab of the Load Bearing Frame comprises displacement drives and rod rotation drives (5 and 11 ), respectively, the Manual Control Unit (6), the Manual Lifting Drive for the Top Lid (7).
  • the Manual Control Unit (6) is used for performing tasks for adjusting of the rod rotation at the preparatory stage of the process of growth.
  • Manual Lifting Drive for the Top Lid (7) is used for the purposes of loading and unloading of the Vacuum Chamber (2).
  • Vacuum Chamber (2) serve the purpose of fixation of the heater and securing of power supply from the Power Cabinet.
  • Viewing Windows placed on the lid of the Vacuum Chamber (2) are used for observation purposes of the alignment of the geometric axes of the seed crystal and the crucible with a charge inside, as well as before the beginning of the technological process of growth, as well as for the purposes of visual control of the process of insertion of the seed crystal and overgrowth of the crystal.
  • Alignment of the axis of the seed crystal with the axis of the crucible or the melt is conducted by means of the precision angle of the horizontal displacement of the rod along the axes of X and Y (10).
  • the Sylphon unit (12) contains a vacuum rod seal that serves the purpose of a compensator when horizontal displacements occur.
  • the Hollow water-cooled Rod (13) serves the purpose of a moving feed- through in the Vacuum Chamber (2) and consists of a pull and a seed crystal that are mounted up to the weight sensor.
  • the String Weight Sensor (14) with the Electronic Section (15) mounted on the top of the Hollow Rod (13) provides for the automated control of the geometric sizes and weight of the growing crystal by means of periodic weighing and calculation of the weight increment at a time unit.
  • the Power Cabinet (16) has been designed for voltage transformation of the three-phase power grid into the voltage required to power a resistive heating crucible and other sections of the equipment.
  • the Control Rack (17) that is located on the left-hand side of the Load Bearing Unit (1 ) and contains the Industrial PC-based Workstation (18), the Control Unit (19) and the Control Unit for the Vacuum Set (20).
  • the system of control controls the equipment in accordance with the initially set parameters, and performs further control of the process flow by means of the sensors. If necessary, the system of control makes a decision concerning changes of the preset parameters.
  • the Control Unit (19) installed into the Control Rack (17) is the executive section of the system of control of the equipment.
  • the Control Unit for the Vacuum Set (20) that is installed into the Control Rack (17) controls the Vacuum Set (21 ) in the automated and manual modes.
  • the Vacuum Set (21 ) serves the purpose of creation of high vacuum in the Vacuum Chamber (2).
  • the system of control is equipped with a feedback function that detects the weight increment of the growing crystal.
  • a signal generated by the string weight sensor is transmitted to the PC-based system of control and is processed there by the control software. With the change of weight increment for a time unit, the system of control changes the rate of crystal growth and the power going into the resistive heating crucible.
  • This production equipment consists of the following parts and sections: a
  • This equipment has been designed to be utilized indoors at the air temperature of 20-25 °C (68-77 °F) and the relative humidity rate of 50 ⁇ 10%.
  • the premises should be equipped with combined extract and input ventilation.
  • Power to this equipment is supplied from a four-wire power grid of three phase AC current (with a neutral wire) with the voltage of 380 V and the frequency of 50 Hz.
  • the quality of the water supplied to the equipment in use be close to that of potable water with the solid residual not exceeding 1gr per liter, and the bacteria level not exceeding 100 pcs. per m 3 and the pressure of 250 ⁇ 50 KPa. Average water consumption is 3 M 3 per hr.
  • the incoming water temperature should not exceed 30°C with the maintenance accuracy
  • This equipment should be connected to the following:
  • ⁇ exhaust branch pipe of the mechanical roughing-down pump is supposed to be hooked to the system of centralized cleansing of exhaust fumes from the roughing-down pumps.

Landscapes

  • 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)

Abstract

La présente invention concerne un équipement de production en « chute d'eau » pour la croissance d'un monocristal de corindon incolore par les méthodes Czochralski et Kyropoulos et sous vide avec chauffage ohmique, un capteur de poids à fil étant en outre utilisé. Selon la présente invention, un seul capteur de poids à fil est utilisé sur cet équipement en vue de l'automatisation du procédé technologique de croissance monocristalline de corindon incolore afin de permettre la croissance selon les paramètres existants. Le capteur de poids est monté sur l'extrémité supérieure de la tige creuse mobile. Un germe monocristallin est attaché au fil actif du capteur de poids par la tige de commande. Les modifications du cristal en croissance sont détectées par le capteur de poids en tant que signal électrique qui est immédiatement transmis au système de commande basé sur un PC. L'utilisation d'un capteur de poids sur cet équipement rend possible l'automatisation de la croissance de monocristaux présentant une taille et un poids prédéterminés désirés, du fait que les paramètres du cristal au cours de sa croissance peuvent être commandés avec une grande précision.
PCT/IB2001/002641 2001-12-19 2001-12-19 Equipement de production en 'chute d'eau' pour la croissance de cristaux WO2003052175A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/IB2001/002641 WO2003052175A1 (fr) 2001-12-19 2001-12-19 Equipement de production en 'chute d'eau' pour la croissance de cristaux

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/IB2001/002641 WO2003052175A1 (fr) 2001-12-19 2001-12-19 Equipement de production en 'chute d'eau' pour la croissance de cristaux

Publications (1)

Publication Number Publication Date
WO2003052175A1 true WO2003052175A1 (fr) 2003-06-26

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/IB2001/002641 WO2003052175A1 (fr) 2001-12-19 2001-12-19 Equipement de production en 'chute d'eau' pour la croissance de cristaux

Country Status (1)

Country Link
WO (1) WO2003052175A1 (fr)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102534757A (zh) * 2012-01-06 2012-07-04 南京师范大学 基于工业总线的晶体生长智能控制系统
CN102691103A (zh) * 2012-06-14 2012-09-26 中国科学院半导体研究所 一种采用双重控制技术生长蓝宝石晶体的方法
CN104328498A (zh) * 2014-11-26 2015-02-04 元亮科技有限公司 蓝宝石单晶生长自动化综合控制工艺
RU2560395C1 (ru) * 2014-02-14 2015-08-20 Федеральное государственное унитарное предприятие Экспериментальный завод научного приборостроения со Специальным конструкторским бюро Российской академии наук Способ автоматического управления с обратной связью процессом выращивания монокристаллов методом киропулоса
CN104894643A (zh) * 2015-05-20 2015-09-09 内蒙古晶环电子材料有限公司 一种新型蓝宝石上轴结构
CN105177704A (zh) * 2015-10-23 2015-12-23 苏州晶特晶体科技有限公司 一种稳定性高的长晶炉用晶体称重装置
CN109338468A (zh) * 2018-11-21 2019-02-15 南京晶升能源设备有限公司 一种晶体称重装置
CN110344108A (zh) * 2019-08-21 2019-10-18 眉山博雅新材料有限公司 上提拉真空炉
RU216127U1 (ru) * 2022-06-15 2023-01-17 Общество с ограниченной ответственностью "КрОМ" Устройство для выращивания монокристаллов

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1434527A (en) * 1972-09-08 1976-05-05 Secr Defence Growth of crystalline material
SU406402A1 (ru) * 1970-11-12 1985-06-07 Подольский химико-металлургический завод Устройство дл выт гивани слитков из расплава
US4600564A (en) * 1983-09-06 1986-07-15 Crismatec Machine for pulling monocrystals

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU406402A1 (ru) * 1970-11-12 1985-06-07 Подольский химико-металлургический завод Устройство дл выт гивани слитков из расплава
GB1434527A (en) * 1972-09-08 1976-05-05 Secr Defence Growth of crystalline material
US4600564A (en) * 1983-09-06 1986-07-15 Crismatec Machine for pulling monocrystals

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102534757A (zh) * 2012-01-06 2012-07-04 南京师范大学 基于工业总线的晶体生长智能控制系统
CN102691103A (zh) * 2012-06-14 2012-09-26 中国科学院半导体研究所 一种采用双重控制技术生长蓝宝石晶体的方法
RU2560395C1 (ru) * 2014-02-14 2015-08-20 Федеральное государственное унитарное предприятие Экспериментальный завод научного приборостроения со Специальным конструкторским бюро Российской академии наук Способ автоматического управления с обратной связью процессом выращивания монокристаллов методом киропулоса
CN104328498A (zh) * 2014-11-26 2015-02-04 元亮科技有限公司 蓝宝石单晶生长自动化综合控制工艺
CN104894643A (zh) * 2015-05-20 2015-09-09 内蒙古晶环电子材料有限公司 一种新型蓝宝石上轴结构
CN105177704A (zh) * 2015-10-23 2015-12-23 苏州晶特晶体科技有限公司 一种稳定性高的长晶炉用晶体称重装置
CN109338468A (zh) * 2018-11-21 2019-02-15 南京晶升能源设备有限公司 一种晶体称重装置
CN110344108A (zh) * 2019-08-21 2019-10-18 眉山博雅新材料有限公司 上提拉真空炉
RU216127U1 (ru) * 2022-06-15 2023-01-17 Общество с ограниченной ответственностью "КрОМ" Устройство для выращивания монокристаллов

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