CN101775649A - Intermediate-frequency furnace combined type square heater for polycrystalline silicon ingot casting or purification - Google Patents

Intermediate-frequency furnace combined type square heater for polycrystalline silicon ingot casting or purification Download PDF

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Publication number
CN101775649A
CN101775649A CN201010117292A CN201010117292A CN101775649A CN 101775649 A CN101775649 A CN 101775649A CN 201010117292 A CN201010117292 A CN 201010117292A CN 201010117292 A CN201010117292 A CN 201010117292A CN 101775649 A CN101775649 A CN 101775649A
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China
Prior art keywords
graphite
heater
square
polycrystalline silicon
carbon fiber
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CN201010117292A
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Chinese (zh)
Inventor
林安中
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BEIJING ZHONGLIAN SOLAR TECHNOLOGY Co Ltd
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BEIJING ZHONGLIAN SOLAR TECHNOLOGY Co Ltd
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Priority to CN201010117292A priority Critical patent/CN101775649A/en
Publication of CN101775649A publication Critical patent/CN101775649A/en
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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
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002Crucibles or containers for supporting the melt
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Resistance Heating (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention relates to a low-cost combined type square heater for polycrystalline silicon ingot casting or purification, which belongs to the technical field of manufacture of polycrystalline silicon ingots or purifying furnaces. The heater receives the induction heating of a square copper coil by using a square heat insulation layer. The conventional heater processed by the integral graphite is replaced, the cost of the heater is greatly reduced due to the composition of the graphite sheets, and the design method prevents the destruction caused by poor contact of the combined heater. The square combined heater is characterized in that the graphite sheets are combined into an upper square graphite coil and a lower square graphite coil; the edge connecting part of the graphite sheets is processed into a sawtooth shape and fixed by carbon fiber screws after combination; graphite slurry is coated on all connecting surfaces and the connecting surfaces of the carbon fiber screws; the graphite coils are sintered into a whole by high-temperature sintering; the upper graphite coil and the lower graphite coil are stacked together to use, and then the square combined heater is formed.

Description

Polycrystalline silicon ingot casting or purification intermediate frequency furnace combined type square heater
Technical field:
The present invention relates to the structure of the graphite heater of a kind of polycrystalline silicon ingot or purifying furnace or purification furnace, belong to the structure Design and the manufacturing technology field of the well heater of polycrystalline silicon ingot or purifying furnace or purification furnace.
Technical background
The employing intermediate frequency furnace carries out polycrystalline silicon ingot casting and purification is one of the crystal growth in solar cell silicon materials field and means of purification.The characteristics of intermediate frequency furnace are that used graphite heater is the graphite of whole shape, do not need joint-cutting to improve into strips and regulate its resistivity, thereby than the long service life that adopts the electrical resistance method graphite heater and be easy to processing.The general heating in medium frequency formula polycrystalline silicon ingot or purifying furnace that uses is the heater coil of employing garden shape and the well heater of garden shape, the square crucible used with polycrystal silicon ingot do not form heat transfer space closely, and graphite heater is that the graphite by an integral body machines, want car to go to the centre of heating member in the processing, cause very big waste very high because of the cost of well heater, special in ingot casting during for hundreds of KG weight, can cause big graphite block to be difficult for obtaining or cost too high.Purification furnace is that intermediate frequency ingot furnace commonly used carries out, and when adopting vacuum to purify, it is bad that phenomenons such as regular meeting's generation jumping material make that well heater is easy to, and further improved the cost of well heater.In polycrystalline silicon ingot casting and material smelting process thereof, often need the development square ingot, to obtain best material use efficiency.This moment, used crucible was a quadrate, when considering the energy-conservation of whole heating system, as changing square from the garden shape of routine heating in medium frequency coil (being generally copper coil).Because silicon materials are semi-conductors, heating in medium frequency is not directly to sense on the silicon materials, but senses on the graphite body of its earthenware an ancient official title portion, and the thermal energy conduction that is produced by graphite body is in crucible, because of normal this graphite body of title is a graphite heater.At this moment will be with the induction heater in the coil, also make square, better with the coupling of square crucible like this, can save energy.This square heater, ideal state are the well heaters that adopts the big machining graphite squarely tubular of monoblock, to guarantee the generation of circular induced current, to reach the purpose of heating.When particularly silicon materials being purified, because material impure and used high vacuum, high-temperature to purify, be big, adopt knockdown well heater can reduce the cost of well heater significantly the loss of well heater.Conventional well heater is to go to its inside to process with the graphite car of monoblock, and the material cost of manufacturing is very high.
High electric current on the well heater is to form annular flow, it is smooth and easy that used well heater will guarantee that the electric current mobile reliably reaches, just might cause partial high contact resistance if any the junction, can cause sparking to wait and destroy well heater, or cause local excess temperature can the security of polycrystalline ingot casting crucible be exerted an influence, reliable method could use knockdown graphite heater so have very, and the present invention has just provided this kind method.
Summary of the invention:
The present invention provides the well heater of heating in medium frequency formula polycrystalline silicon ingot or purifying furnace cheaply or purification furnace.
This combination heater is made up of 8 graphite flakes, per 4 graphite flakes are formed a quadrate graphite circle, spination is processed in the junction, edge of graphite flake, after four combinations, fix with the carbon fiber screw between per two, handing-over between the graphite circle is that step-like that platform mutually combines is processed at the place up and down, after finishing processing, use black lead wash to be applied on the interface of all interfaces of graphite circle and carbon fiber screw, through being warmed up to 1200 ℃ slowly, make the graphite circle sinter integral body into, the graphite circle is built and is lumped together use up and down, has just formed square combination heater, graphite circle junction is nature handing-over up and down, does not go up black lead wash, can change separately in order to one of them bad time.When intermediate frequency furnace has the design of the heating of going up, add a graphite flake on the top of this combination heater, just form combination heater with last hot-plate.Graphite flake uses highdensity electrode graphite or three high graphite are processed, to guarantee its work-ing life.
The present invention is from reducing the cost of well heater, the structure design of combined type square heater being provided.Because the weight of the silicon ingot of practicability has all reached 270--450Kg at present, the length of side of well heater can reach about 900mm.Combination heater is made up of four graphite flakes, can reduce cost significantly, and is easier to obtain material source.The structure iron of combination heater is seen Fig. 1.The contact resistance that reduces the graphite flake junction makes and forms good circular induced current is core purpose of the present invention, design increases the contact area and the reliability of graphite flake, and be coated in the contact surface place with graphite slurry, through high temperature sintering to form better contact.
Adopting the carbon fiber screw among the present invention is in order to strengthen making up the structural strength of crucible, to use black lead wash to apply in the junction of screw and screw and graphite cake, increase electrically contacting property and sound construction degree behind oversintering.Therefore the contact surface of carbon fiber screw does not directly contact with furnace atmosphere in addition, and life-time service can be prevented the chance of oxidation, has prevented because of the junction loose contact and causes the damage of well heater because of the spark phenomenon that exists big electric current to cause.
Heat graphite circle also forming of one up and down, be divided into then as considering cost and local convertibility that to heat the graphite circle up and down more reasonable by four plates.
The present invention tests in practical application, confirms that combination heater can normally provide good heating and have good electrical contact , Full foot ingot casting and the requirement of the medium-term and long-term stability of purifying.
Description of drawings:
Fig. 1 is the integral layout of the present invention in stove
Fig. 2 is the structure iron of graphite heating sheet
Fig. 3 is the structure iron of graphite heating circle up and down
Embodiment:
The present invention adopts electrode graphite to make the low square heater of knockdown cost, the structure of graphite cake comprises Shangyang tooth plate [9] and side-view [13] thereof, goes up cloudy tooth plate [10] and side-view [14] thereof, adopt its each two to be combined into graphite circle [17], each two of cloudy tooth plates [12] are combined into down graphite circle [18] to adopt Xiayang tooth plate [11] to reach down.The rib-loop hole [15] (perpendicular to the plate face) of wearing transmitting plate is arranged on the positive tooth on the positive tooth plate, and the rib-loop hole [16] (being parallel to the plate face) that the cloudy teeth groove place on cloudy tooth plate has has used carbon fiber spiral shell nail Even to connect this two kinds of plates.The graphite circle is combined into well heater [1] [2] up and down, just contains top firing graphite cake [3] when last heating collar is arranged.Thermal insulation layer [4] is close in the outside of combination heater, and the outside of thermal insulation layer is the square ruhmkorff coil [5] [6] that copper pipe constitutes.Crucible [8] is placed in the well heater at stove [7] center and carries out the melting polycrystalline silicon material, and the crucible that slowly descends is then cast silicon ingot in the mode of directional freeze.The present invention tests in the ingot furnace of 160-200KG polycrystal silicon ingot and purification furnace, draws the good ingot casting and the result of purification.This scheme is formally produced the ingot furnace that can be used on the above silicon ingot of casting 450KG when using, and the thickness of graphite cake and highly constant mainly is to increase the outside dimension of well heater and increase reinforcing carbon fiber screw number just can.

Claims (6)

1. the graphite combination heater used of the polycrystalline silicon ingot or purifying furnace of a heating in medium frequency or purification furnace, in the branch following two layers, its structure is a quadrate, form with the combination of graphite cake forms, its form is to adopt the carbon fiber screw to fix, and the junction between graphite cake applies black lead wash and formed an integral body afterwards through oversintering.
2. well heater according to claim 1 can be that branch is two-layer up and down, also can be one deck, and ingot furnace such as design have last heating collar, can form heating member adding a cover a graphite cake on the graphite circle.
Described in the claim 1 in down two layered heatings adopt two of processing Chengyang, two ends odontolith China ink plates and two of cloudy tooth graphite cakes to closely combine.
4. the use carbon fiber screw described in the claim 3, but be not limited only to the carbon fiber screw, also comprise and use the graphite screw.
5. be highdensity electrode graphite or three high graphite according to the used graphite cake of claim 1.
6. well heater according to claim 1 can comprise upper heater, also can not comprise upper heater, and upper heater is made up of a square graphite cake.
CN201010117292A 2010-03-04 2010-03-04 Intermediate-frequency furnace combined type square heater for polycrystalline silicon ingot casting or purification Pending CN101775649A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103614772A (en) * 2013-12-13 2014-03-05 光为绿色新能源股份有限公司 Polysilicon ingot heating method and polysilicon ingot furnace utilizing same
CN103642977A (en) * 2013-12-03 2014-03-19 夏致俊 Flat-shaped medium-frequency furnace body
CN103696002A (en) * 2013-12-16 2014-04-02 英利集团有限公司 Electromagnetic and resistance mixed heating thermal field structure of ingot furnace and using method of electromagnetic and resistance mixed heating thermal field structure
CN108221048A (en) * 2018-04-10 2018-06-29 江苏高照新能源发展有限公司 A kind of layering snakelike polycrystalline silicon ingot casting graphite side heater
CN110803705A (en) * 2018-08-06 2020-02-18 贵州中水材料科技有限公司 Recovery method of silicon powder and silicon ingot prepared by same
CN112616303A (en) * 2020-11-20 2021-04-06 东北大学 Structure for shielding magnetic field in HRS (high resolution scanner) legal directional solidification process

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1158861A (en) * 1965-07-16 1969-07-23 United Aircraft Corp Improvements in and relating to a Mold Heater
US20060219162A1 (en) * 2005-04-01 2006-10-05 G.T. Equipment Technologies, Inc. Solidification of crystalline silicon from reusable crucible molds
CN101092740A (en) * 2007-07-17 2007-12-26 佳科太阳能硅(厦门)有限公司 Method for purifying polysilicon, and solidification device
JP2008201619A (en) * 2007-02-20 2008-09-04 Shin Etsu Handotai Co Ltd Graphite crucible and apparatus for manufacturing silicon single crystal with it
CN101265607A (en) * 2007-11-12 2008-09-17 中国电子科技集团公司第四十八研究所 Graphite heater for polycrystalline silicon casting ingot process
CN201183846Y (en) * 2008-01-28 2009-01-21 常州天合光能有限公司 Thermal field structure of polycrystalline silicon casting furnace
CN201473322U (en) * 2009-08-13 2010-05-19 杨清泉 Special-purpose square graphite crucible for casting solar energy polysilicon

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1158861A (en) * 1965-07-16 1969-07-23 United Aircraft Corp Improvements in and relating to a Mold Heater
US20060219162A1 (en) * 2005-04-01 2006-10-05 G.T. Equipment Technologies, Inc. Solidification of crystalline silicon from reusable crucible molds
JP2008201619A (en) * 2007-02-20 2008-09-04 Shin Etsu Handotai Co Ltd Graphite crucible and apparatus for manufacturing silicon single crystal with it
CN101092740A (en) * 2007-07-17 2007-12-26 佳科太阳能硅(厦门)有限公司 Method for purifying polysilicon, and solidification device
CN101265607A (en) * 2007-11-12 2008-09-17 中国电子科技集团公司第四十八研究所 Graphite heater for polycrystalline silicon casting ingot process
CN201183846Y (en) * 2008-01-28 2009-01-21 常州天合光能有限公司 Thermal field structure of polycrystalline silicon casting furnace
CN201473322U (en) * 2009-08-13 2010-05-19 杨清泉 Special-purpose square graphite crucible for casting solar energy polysilicon

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103642977A (en) * 2013-12-03 2014-03-19 夏致俊 Flat-shaped medium-frequency furnace body
CN103614772A (en) * 2013-12-13 2014-03-05 光为绿色新能源股份有限公司 Polysilicon ingot heating method and polysilicon ingot furnace utilizing same
CN103696002A (en) * 2013-12-16 2014-04-02 英利集团有限公司 Electromagnetic and resistance mixed heating thermal field structure of ingot furnace and using method of electromagnetic and resistance mixed heating thermal field structure
CN103696002B (en) * 2013-12-16 2016-06-15 英利集团有限公司 The ingot furnace thermal field structure of electromagnetism and resistance Hybrid Heating and using method
CN108221048A (en) * 2018-04-10 2018-06-29 江苏高照新能源发展有限公司 A kind of layering snakelike polycrystalline silicon ingot casting graphite side heater
CN110803705A (en) * 2018-08-06 2020-02-18 贵州中水材料科技有限公司 Recovery method of silicon powder and silicon ingot prepared by same
CN112616303A (en) * 2020-11-20 2021-04-06 东北大学 Structure for shielding magnetic field in HRS (high resolution scanner) legal directional solidification process
CN112616303B (en) * 2020-11-20 2022-02-11 东北大学 Structure for shielding magnetic field in HRS (high resolution scanner) legal directional solidification process

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Application publication date: 20100714