CN105350070A - Method for controlling oxygen content of czochralski-method silicon single crystals by means of frequency conversion magnetic field - Google Patents

Method for controlling oxygen content of czochralski-method silicon single crystals by means of frequency conversion magnetic field Download PDF

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Publication number
CN105350070A
CN105350070A CN201510904739.XA CN201510904739A CN105350070A CN 105350070 A CN105350070 A CN 105350070A CN 201510904739 A CN201510904739 A CN 201510904739A CN 105350070 A CN105350070 A CN 105350070A
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CN
China
Prior art keywords
magnetic field
plc
length value
monocrystalline
single crystal
Prior art date
Legal status (The legal status 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 status listed.)
Pending
Application number
CN201510904739.XA
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Chinese (zh)
Inventor
孙毅
于书瀚
孙昊
郑海峰
朱鹏浩
王林
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Tianjin Huanou Semiconductor Material Technology Co Ltd
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Tianjin Huanou Semiconductor Material Technology Co Ltd
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Priority to CN201510904739.XA priority Critical patent/CN105350070A/en
Publication of CN105350070A publication Critical patent/CN105350070A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20Controlling or regulating
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B30/00Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
    • C30B30/04Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions using magnetic fields

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a method for controlling the oxygen content of czochralski-method silicon single crystals by means of a frequency conversion magnetic field. The method comprises the steps that multiple nodes are set on single crystal length values in the preparation process, and the single crystal length value of each node corresponds to a magnetic field intensity value; a PLC reads pulse signals from a coder in real time, the current single crystal length is calculated according to the single crystal length value corresponding to one pulse signal, and the magnetic field intensity is further calculated and displayed through a touch screen; the magnetic field intensity is adjusted and controlled by taking parameters of all the nodes as a basis. According to the method, control over the magnetic field intensity is achieved by means of the frequency conversion magnetic field device, and not only is magnetic field energy consumption reduced, but also the single crystal oxygen content can be controlled; the set PLC can monitor magnetic field currents in real time and achieve gradually-varied and gradual adjustment on the magnetic field intensity, if an alarm is given, the alarm can be fed back to the PLC in time, and then the magnetic field is closed to achieve self-protection of the magnetic field.

Description

A kind of method utilizing variable frequency magnetic field to control crystal for straight drawing monocrystal oxygen level
Technical field
The present invention relates to the production method of silicon single-crystal, especially relate to a kind of method utilizing variable frequency magnetic field to control crystal for straight drawing monocrystal oxygen level.
Background technology
Crystal for straight drawing monocrystal is magnetic field crystal pulling technique (MCZ), compares non-magnetic field technique (CZ) and there are following relative merits: advantage is: 1) monocrystalline oxygen level can control at lower level (< 8E17atm/cm 3);
2) single crystal orientation homogeneity is more excellent; 3) defect generation probability is indirectly controlled by controlling oxygen level.Its shortcoming is: the increase by 1) causing fixed cost owing to increasing magnetic field; 2) opening magnetic field in crystal pulling process causes energy consumption to increase.Present stage adds in the vertical pulling method product in magnetic field, and when magneticstrength is stabilized in 800 Gauss (magnet power 5KW/h), magnetic field energy consumption on average accounts for 1.5% of blow-on cost.Therefore, how to reduce magnetic field energy consumption, and can better to control again monocrystalline oxygen level be the problem that those skilled in the art research and develop.
Summary of the invention
In view of above-mentioned prior art present situation, the invention provides a kind of method utilizing variable frequency magnetic field to control crystal for straight drawing monocrystal oxygen level.The method utilizes variable frequency magnetic field device to control crystal for straight drawing monocrystal oxygen level, by the code device signal of induction monocrystalline length measuring, changes magneticstrength according to monocrystalline length, thus obtains the monocrystalline oxygen level wanting to obtain.
The technical scheme that the present invention takes is: a kind of method utilizing variable frequency magnetic field to control crystal for straight drawing monocrystal oxygen level, it is characterized in that, monocrystalline length value in preparation process is arranged several nodes by the method, a monocrystalline length value corresponding field strength values respectively of each node; In single crystal preparation process, the PLC of variable frequency magnetic field device reads pulse signal in real time from encoder, this pulse signal is current monocrystalline length value, according to the monocrystalline length value corresponding to a pulse signal, the pulse value of reading is calculated current monocrystalline length, calculate current magneticstrength according to current monocrystalline length-gauge, and shown by touch-screen; PLC obtains the magneticstrength in current single crystal preparation process by magnetic field trigger board in real time simultaneously, and is shown by touch-screen; Then a corresponding field strength values is distinguished for foundation with the monocrystalline length value of each node, regulable control magneticstrength.
Monocrystalline length value in preparation process is arranged seven nodes by the method, and the corresponding field strength values of monocrystalline length value difference of each node is as following table:
Monocrystalline length value Magneticstrength
First node 100mm 1200GS
Section Point 300mm 1000GS
3rd node 500mm 700GS
4th node 700mm 400GS
5th node 900mm 600GS
6th node 1100mm 800GS
Variable frequency magnetic field device of the present invention comprises PLC, encoder and touch-screen; Monocrystalline length measuring connects encoder, and encoder connects PLC, and PLC is connected with magnetic field trigger board, touch-screen respectively, and magnetic field trigger board connects magnetic field electrical control cubicles, and magnetic field electrical control cubicles connects PLC.
The beneficial effect that the present invention produces is: the present invention utilizes variable frequency magnetic field device to achieve control to magneticstrength, adopts the method to not only reduce magnetic field energy consumption, and can control monocrystalline oxygen level again.The setting to PLC is realized by touch-screen; PLC after arranging can monitor in real time to field supply; and gradual change is realized to magneticstrength; mild adjustment; if reporting to the police in use appears in field system; alarm message can also be fed back to PLC in time, realize magnetic field self-protection to close magnetic field.
Accompanying drawing explanation
Fig. 1 is variable frequency magnetic field device catenation principle block diagram of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described:
With reference to Fig. 1, variable frequency magnetic field device of the present invention comprises PLC, encoder and touch-screen; Monocrystalline length measuring connects encoder, and encoder connects PLC, and PLC is connected with magnetic field trigger board, touch-screen respectively, and magnetic field trigger board connects magnetic field electrical control cubicles, and magnetic field electrical control cubicles connects PLC.
The present invention utilizes the technical process of variable frequency magnetic field control crystal for straight drawing monocrystal oxygen level as follows:
(1) choose intrinsic raw material (N or the P type raw material that resistivity is greater than 2000 ohm), and be that 75 ~ 120kw melts by it with material power, the material time is 3 ~ 8 hours.
(2) step (1) is added phosphorus alloy doping agent (concentration is 0.0001 ~ 0.001) by normal doping (100 ~ 2000mg), use conventional furnace pressure 14torr ~ 20torr to carry out baking 30 minutes.
(3), after having toasted, 800 Gauss field intensity are used to carry out crystal pulling, in isometrical process, by the code device signal of induction monocrystalline length measuring, obtain current monocrystalline length, change magneticstrength according to monocrystalline length, thus obtain the monocrystalline oxygen level wanting to obtain.
The present invention is provided with automatic mode, parameter set button on touch screen operation panel, is realized the switch of Magnetic Field Automatic Control by button.In isometrical process, can select to adopt " automatic mode " or " optimum configurations " two kinds of modes to control, if select " automatic mode ", then touch screen interface shows the magneticstrength corresponding to monocrystalline length of each node in seven nodes, namely realizes automatically regulating.If Selection parameter is arranged, then carry out manual regulation, expect that monocrystalline oxygen level is higher, just reduce magneticstrength, expect that monocrystalline oxygen level is lower, just increase magneticstrength.
The present invention can show current monocrystalline length value, magnetic field set value, magnetic field feedback value on touch screen operation panel, draws change curve according to the magneticstrength that monocrystalline production technique is arranged and shows on the touchscreen.
The PLC of variable frequency magnetic field device reads out pulse signal from encoder, this pulse signal is actual is monocrystalline length value, then corresponding how many mm of 1 pulse are calculated, then press when each maintenance and start automatic control, make note Changqing 0, PLC according to the pulse value counting read, concrete monocrystalline length can be calculated, then PLC coding, calculates the control signal of controlling magnetic field intensity.
The encoder model that variable frequency magnetic field device adopts is E6B2-CWZ6C.

Claims (3)

1. utilize variable frequency magnetic field to control a method for crystal for straight drawing monocrystal oxygen level, it is characterized in that, the monocrystalline length value in preparation process is arranged several nodes by the method, a monocrystalline length value corresponding field strength values respectively of each node; In single crystal preparation process, the PLC of variable frequency magnetic field device reads pulse signal in real time from encoder, this pulse signal is current monocrystalline length value, according to the monocrystalline length value corresponding to a pulse signal, the pulse value of reading is calculated current monocrystalline length, calculate current magneticstrength according to current monocrystalline length-gauge, and shown by touch-screen; PLC obtains the magneticstrength in current single crystal preparation process by magnetic field trigger board in real time simultaneously, and is shown by touch-screen; Then a corresponding field strength values is distinguished for foundation with the monocrystalline length value of each node, regulable control magneticstrength.
2. a kind of method utilizing variable frequency magnetic field to control crystal for straight drawing monocrystal oxygen level according to claim 1, it is characterized in that, monocrystalline length value in preparation process is arranged seven nodes by the method, and the corresponding field strength values of monocrystalline length value difference of each node is as following table:
3. a kind of method utilizing variable frequency magnetic field to control crystal for straight drawing monocrystal oxygen level according to claim 1, it is characterized in that, described variable frequency magnetic field device comprises PLC, encoder and touch-screen; Monocrystalline length measuring connects encoder, and encoder connects PLC, and PLC is connected with magnetic field trigger board, touch-screen respectively, and magnetic field trigger board connects magnetic field electrical control cubicles, and magnetic field electrical control cubicles connects PLC.
CN201510904739.XA 2015-12-09 2015-12-09 Method for controlling oxygen content of czochralski-method silicon single crystals by means of frequency conversion magnetic field Pending CN105350070A (en)

Priority Applications (1)

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CN201510904739.XA CN105350070A (en) 2015-12-09 2015-12-09 Method for controlling oxygen content of czochralski-method silicon single crystals by means of frequency conversion magnetic field

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Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0461769A1 (en) * 1990-05-25 1991-12-18 Shin-Etsu Handotai Company Limited Method for pulling up semiconductor single crystal
EP0462741A2 (en) * 1990-06-21 1991-12-27 Shin-Etsu Handotai Company Limited Method for pulling up semiconductor single crystal
CN1508299A (en) * 2002-12-19 2004-06-30 �����ɷ� Silicon monocrystal and its producing method
CN1807703A (en) * 2005-01-20 2006-07-26 上海合晶硅材料有限公司 Low oxygen control method in czochralski silicon monocrystal
CN101133193A (en) * 2004-12-30 2008-02-27 Memc电子材料有限公司 Controlling melt-solid interface shape of a growing silicon crystal using a variable magnetic field
CN101133192A (en) * 2004-12-30 2008-02-27 Memc电子材料有限公司 Electromagnetic pumping of liquid silicon in a crystal growing process
CN101423976A (en) * 2007-11-02 2009-05-06 斯尔瑞恩公司 Semiconductor single crystal growth method having improvement in oxygen concentration characteristics
CN101906658A (en) * 2008-10-08 2010-12-08 天津希力斯新能源技术研发有限公司 Process for straightly pulling silicon single crystal by using permanent magnetic field and accessory equipment
CN102220629A (en) * 2011-07-25 2011-10-19 天津市环欧半导体材料技术有限公司 Method and system for controlling automatic growth of zone-melt crystal by adopting diameter process
CN103710745A (en) * 2013-12-26 2014-04-09 南京晶升能源设备有限公司 Method for automatically controlling growth of 85-120kg sapphire crystals
CN104278321A (en) * 2013-07-12 2015-01-14 环球晶圆日本股份有限公司 Silicon single crystal and method for manufacture thereof

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0461769A1 (en) * 1990-05-25 1991-12-18 Shin-Etsu Handotai Company Limited Method for pulling up semiconductor single crystal
EP0462741A2 (en) * 1990-06-21 1991-12-27 Shin-Etsu Handotai Company Limited Method for pulling up semiconductor single crystal
CN1508299A (en) * 2002-12-19 2004-06-30 �����ɷ� Silicon monocrystal and its producing method
CN101133193A (en) * 2004-12-30 2008-02-27 Memc电子材料有限公司 Controlling melt-solid interface shape of a growing silicon crystal using a variable magnetic field
CN101133192A (en) * 2004-12-30 2008-02-27 Memc电子材料有限公司 Electromagnetic pumping of liquid silicon in a crystal growing process
CN1807703A (en) * 2005-01-20 2006-07-26 上海合晶硅材料有限公司 Low oxygen control method in czochralski silicon monocrystal
CN101423976A (en) * 2007-11-02 2009-05-06 斯尔瑞恩公司 Semiconductor single crystal growth method having improvement in oxygen concentration characteristics
CN101906658A (en) * 2008-10-08 2010-12-08 天津希力斯新能源技术研发有限公司 Process for straightly pulling silicon single crystal by using permanent magnetic field and accessory equipment
CN102220629A (en) * 2011-07-25 2011-10-19 天津市环欧半导体材料技术有限公司 Method and system for controlling automatic growth of zone-melt crystal by adopting diameter process
CN104278321A (en) * 2013-07-12 2015-01-14 环球晶圆日本股份有限公司 Silicon single crystal and method for manufacture thereof
CN103710745A (en) * 2013-12-26 2014-04-09 南京晶升能源设备有限公司 Method for automatically controlling growth of 85-120kg sapphire crystals

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