CN107720756A - A kind of polycrystalline silicon reducing furnace - Google Patents
A kind of polycrystalline silicon reducing furnace Download PDFInfo
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- CN107720756A CN107720756A CN201711067662.0A CN201711067662A CN107720756A CN 107720756 A CN107720756 A CN 107720756A CN 201711067662 A CN201711067662 A CN 201711067662A CN 107720756 A CN107720756 A CN 107720756A
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- fluid layer
- chassis
- cold air
- hydrogen
- reduction furnace
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of polycrystalline silicon reducing furnace, includes body of heater, chassis and electrode, and the inside of reduction furnace is divided into three thermal current layer, crystal silicon vitellarium and cold air fluid layer regions, and cold air fluid layer is located at the bottom of reduction furnace, and it connects with chassis；Hydrogen nozzle is provided with chassis, spraying hydrogen gas stream towards reduction furnace by hydrogen nozzle forms cold air fluid layer；Hot gas fluid layer is located at the top of reduction furnace, and hot gas fluid layer bottom is 100 500mm with the distance at the top of silicon rod.The present invention has advantages below：First, polysilicon rod highly less than hot gas fluid layer at the top of reduction furnace, avoids silicon rod from causing the fusing of silicon rod crossbeam, growth cauliflower material exposed to top hot gas fluid layer；Second, polycrystalline silicon growth area gas phase and polycrystalline silicon rod temperature are held in suitable material reaction, the temperature of deposition, the whole rod of polysilicon can with output with high-quality；3rd, cold air fluid layer can make reduction furnace bottom remain at low-temperature condition, prevent material from being deposited on magnet ring, graphite base and electrode.
Description
Technical field
The present invention relates to technical field of polysilicon production, and in particular to a kind of polycrystalline silicon reducing furnace.
Background technology
Improved Siemens are the mainstream technologys for producing polysilicon in the world, and its nucleus equipment is reduction furnace, reduction furnace
Operation principle is that the mixing gas reaction of trichlorosilane and hydrogen is generated into polysilicon by energization high temperature silicon core and is deposited on silicon
On core, final product is deposited on the polysilicon on silicon core, and product is finally produced in the form of polycrystalline silicon rod from reduction furnace.
The reaction mass of polycrystalline silicon reducing furnace enters from chassis, and reaction end gas also goes out from chassis, although this, which enters outlet mode, has
Help the mixing of material and extend the residence time of material, but also cause temperature at the top and bottom of reduction furnace too high, and reduce
Furnace roof portion and the too high normal operation that can influence reduction furnace of bottom temp.The too high one side of head temperature can make silicon core fuse,
Cause to open stove failure；On the other hand top material sedimentation rate can be made too fast, causes the formation of puffed rice material.And bottom temp mistake
It is high that insulation magnet ring surface on the one hand can be made to tie silicon, and then increase the risk of reduction furnace ground connection stop jumping, and cause the loss of material,
Because silicon and insulation magnet ring have different modulus of elasticity, the damage so magnet ring of surface knot silicon easily bursts apart；Another aspect bottom
The too high increase that organic insulation can be made to be carbonized, and then cause contamination of products and maintenance cost of portion's temperature.In addition, reduction furnace
A part of material can decompose in gaseous environment in running produces indefinite form silicon, and indefinite form silicon (i.e. silica flour) can be enriched in bottom
Panel surface, the black matrix coefficient on chassis can be increased by being enriched in the indefinite form silicon of chassis surface, and then cause the loss of furnace heat, this
The indefinite form silicon of outer enrichment can reunite at high temperature, and then can also increase the risk of reduction furnace ground connection stop jumping.
In summary, there is structure design defect in existing polycrystalline silicon reducing furnace, and drawbacks described above not only influences polysilicon product
Quality, the stable operation of reduction furnace is also drastically influence, therefore how to optimize polycrystalline-silicon reducing furnace structure, before can solving
The problem of existing is stated as being currently needed for being badly in need of the problem solved.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of stable operation of achievable polycrystalline silicon reducing furnace, high-quality are more
The output of crystalline silicon rod and the polycrystalline silicon reducing furnace for reducing production of polysilicon cost.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：A kind of polycrystalline silicon reducing furnace, includes stove
Body, chassis and electrode, body of heater are installed on chassis, and electrode is located in body of heater and is installed on chassis, and air inlet is provided with chassis
Mouth and gas outlet, silicon rod are grown on electrode, it is characterised in that：By to body of heater height parameter and temperature in furnace parameter
Control, is divided into three thermal current layer, crystal silicon vitellarium and cold air fluid layer regions by the inside of the reduction furnace, wherein,
Cold air fluid layer is located at the bottom of reduction furnace, and it connects with chassis；Cold air fluid layer is by the hydrogen that is sprayed upward from chassis
Air-flow is formed, and some hydrogen nozzles are provided with chassis, and hydrogen nozzle is to being connected to hydrogen gas supply mechanism, by hydrogen nozzle towards also
Former stove injection hydrogen gas stream is by the temperature control of cold air fluid layer between 200-600 DEG C；The hydrogen sprayed by hydrogen nozzle will
The silica flour for being enriched in chassis surface is maintained at fluidized state, and the silica flour in fluidized state is served as hot anti-with its bigger surface area
Carrier is penetrated, reflection supplement is carried out to the heat of furnace interior and reduces the loss of reduction furnace heat；In addition, in cold gas fluid layer
Low temperature hydrogen bottom silica flour is in fluidized state, silica flour is not enriched on chassis, chassis can remain relatively low
Coefficient of blackness；
Hot gas fluid layer is located at the top of reduction furnace, and hot gas fluid layer at the top of reduction furnace with the distance at the top of silicon rod by will set
For 1000-1500mm, and it is 100-500mm to form hot gas fluid layer bottom with the distance at the top of silicon rod, and this distance can form silicon rod
Structure away from hot gas fluid layer；
Between hot gas fluid layer and cold air fluid layer, silicon rod is grown in the crystal silicon vitellarium for crystal silicon vitellarium, crystal silicon life
The gas phase temperature control in long area is 800-900 DEG C；Silicon rod temperature is maintained at 1000-1200 DEG C, and optimal is 1000 DEG C.
Further, the height that the cold air fluid layer extends up from chassis upper table is 50-200mm, in cold air fluid layer
200-600 DEG C of low temperature hydrogen accounts at least the 90% of whole cold air fluid layer.
Further, the hydrogen nozzle is uniformly arranged on inside chassis, and the interior table on the top of hydrogen nozzle and chassis
Face is mutually flush；A diameter of 2-5mm of hydrogen nozzle.
Further, the nozzle of the hydrogen nozzle is provided with screen cloth, and the sieve diameter of the screen cloth is 0.05-
0.1mm, the screen cloth are made of high chromium-nickel austenitic stainless steel.
Further, the inner surface on the chassis is coated with heat-reflective coating, and the heat-reflective coating is silver coating, will
Heat reflexes to crystal silicon vitellarium.
Preferably, the top of the body of heater is dome structure, and body of heater top and the distance at the top of silicon rod are 1200-
1300mm, the gas phase temperature control of crystal silicon vitellarium is 850 DEG C；The height of the cold air fluid layer is 100mm, and its temperature is maintained at
300-500℃。
The present invention is directed to existing polycrystalline-silicon reducing furnace structure defect, creatively by setting different parameters to reduce
Furnace interior is divided into three working regions, is hot gas fluid layer, the crystal silicon vitellarium at middle part and the cold airflow of bottom at top respectively
Layer, can so reach following effect：First, polysilicon rod highly less than hot gas fluid layer at the top of reduction furnace, so avoids
Silicon rod causes the fusing of silicon rod crossbeam exposed to top hot gas fluid layer, grows the problem of cauliflower material；Second, middle part polycrystalline silicon growth
Area's gas phase and polycrystalline silicon rod temperature are held in suitable material reaction, the temperature of deposition, can ensure that polycrystalline silicon rod is integrally uniform
Growth, and then output has the whole rod of the polysilicon of high-quality；3rd, bottom cold air fluid layer can remain reduction furnace bottom
In low-temperature condition, the low temperature hydrogen environment of bottom can prevent material from being deposited on magnet ring, graphite base and electrode, can reduce
The loss of material, the service life of the parts such as magnet ring is improved, save the disposal costs of the parts such as magnet ring, while reduction is greatly reduced
Stove is grounded stop jumping rate, ensures the stable operation of reduction furnace.
During existing polycrystalline silicon reducing furnace operation, chassis can be covered by silica flour, add chassis coefficient of blackness so that big calorimetric
Amount is lost by chassis, and the hydrogen that the present invention is sprayed using bottom cold air flow nozzle can make silica flour be maintained at fluidized state, is located
There is high surface area in the silica flour of fluidized state, heat reflection carrier can be served as, and then reduce reduction furnace thermal loss.
Chassis silica flour is in fluidized state all the time in the technology of the present invention, therefore chassis can remain low blackness system
Number, and the chassis with silver coating can further reduce chassis coefficient of blackness, and then chassis heat reflection efficiency is substantially improved, drop
Low reduction furnace thermal loss, realize the energy-saving run of reduction furnace.
Brief description of the drawings
Fig. 1 is schematic structural view of the invention.
In figure, 1 is body of heater, and 2 be chassis, and 3 be electrode, and 4 be silicon rod, and 5 be gas outlet, and 6 be hydrogen nozzle, and 7 be material gas
Stream, 8 be hot gas fluid layer, and 9 be crystal silicon vitellarium, and 10 be cold air fluid layer, and 11 be silica flour, and 12 be hydrogen gas stream.
Embodiment
In the present embodiment, reference picture 1, the polycrystalline silicon reducing furnace includes body of heater 1, chassis 2 and electrode 3, and body of heater 1 is pacified
Loaded on chassis 2, electrode 3 is located in body of heater 1 and is installed on chassis 2, and air inlet and gas outlet 5, silicon rod are provided with chassis 2
Raw 4 are longer than on electrode 3；By the control to the height parameter of body of heater 1 and the inside temperature parameter of body of heater 1, by the inside of the reduction furnace
It is divided into 10 3 hot gas fluid layer 8, crystal silicon vitellarium 9 and cold air fluid layer regions, wherein,
Cold air fluid layer 10 is located at the bottom of reduction furnace, and it connects with chassis 2；Cold air fluid layer 10 by spraying upward from chassis 2
Hydrogen gas stream 12 formed, some hydrogen nozzles 6 are provided with chassis 2, hydrogen nozzle 6 passes through to being connected to hydrogen gas supply mechanism
Hydrogen nozzle 6 towards reduction furnace spray hydrogen gas stream 12 by the temperature control of cold air fluid layer 10 between 200-600 DEG C；Pass through hydrogen
Nozzle 6 spray hydrogen the silica flour 11 for being enriched in the surface of chassis 2 is maintained at fluidized state, the silica flour 11 in fluidized state with
Its bigger surface area serves as heat reflection carrier, and reflection supplement is carried out to the heat inside body of heater 1 and reduces reduction furnace heat
Loss；In addition, the low temperature hydrogen in cold gas fluid layer 10 makes bottom silica flour 11 be in fluidized state, silica flour 11 is set not to be enriched with
On chassis 2, chassis 2 can remain relatively low coefficient of blackness；
Hot gas fluid layer 8 is located at the top of reduction furnace, and hot gas fluid layer 8 is by by the distance at the top of reduction furnace with the top of silicon rod 4
1000-1500mm is arranged to, is 100-500mm so as to form the distance of the bottom of hot gas fluid layer 8 and the top of silicon rod 4, this distance can
Form structure of the silicon rod away from hot gas fluid layer 8；Material pneumatic 7 is latter through to thermal current from the air inlet on chassis 2 into body of heater 1
Layer 8, finally reduction furnace is discharged from the gas outlet 5 on chassis 2 after being reacted in crystal silicon vitellarium 9.
Between hot gas fluid layer 8 and cold air fluid layer 10, silicon rod 4 is grown in the crystal silicon vitellarium 9 for crystal silicon vitellarium 9,
The gas phase temperature control of crystal silicon vitellarium 9 is 800-900 DEG C；The temperature of silicon rod 4 is maintained at 1000-1200 DEG C, and optimal is 1000
℃。
The height that the cold air fluid layer 10 extends up from the upper table of chassis 2 is 50-200mm, 200- in cold air fluid layer 10
600 DEG C of low temperature hydrogen accounts at least the 90% of whole cold air fluid layer 10.
The hydrogen nozzle 6 is uniformly arranged on inside chassis 2, and the inner surface at the top of hydrogen nozzle 6 and chassis 2 is mutual
Flush；A diameter of 2-5mm of hydrogen nozzle 6.
The nozzle of the hydrogen nozzle 6 is provided with screen cloth (not shown), and the sieve diameter of the screen cloth is 0.05-
0.1mm, the screen cloth are made of high chromium-nickel austenitic stainless steel.
The inner surface on the chassis 2 is coated with heat-reflective coating, and the heat-reflective coating is silver coating, and heat is reflected
To crystal silicon vitellarium 9.
The top of the body of heater 1 is dome structure, and the distance at the top of body of heater 1 and the top of silicon rod 4 is 1200-1300mm, brilliant
The gas phase temperature control in silicon growth area 9 is 850 DEG C；The height of the cold air fluid layer 10 is 100mm, and its Optimal Temperature is 300-
500℃。
The present invention is described in detail above, described above, only the preferred embodiments of the invention, when can not
Limit the scope of the present invention, i.e., it is all to make equivalent changes and modifications according to the application scope, it all should still belong to covering scope of the present invention
It is interior.
Claims (6)
1. a kind of polycrystalline silicon reducing furnace, including body of heater, chassis and electrode, body of heater is installed on chassis, and electrode is located in body of heater
And be installed on chassis, air inlet and gas outlet are provided with chassis, silicon rod is grown on electrode, it is characterised in that：By right
The control of body of heater height parameter and temperature in furnace parameter, the inside of the reduction furnace is divided into thermal current layer, crystal silicon vitellarium
And three regions of cold air fluid layer, wherein,
Cold air fluid layer is located at the bottom of reduction furnace, and it connects with chassis；Cold air fluid layer is by the hydrogen gas stream that is sprayed upward from chassis
Formed, some hydrogen nozzles are provided with chassis, hydrogen nozzle is to being connected to hydrogen gas supply mechanism, by hydrogen nozzle towards reduction furnace
Injection hydrogen gas stream is by the temperature control of cold air fluid layer between 200-600 DEG C；The hydrogen sprayed by hydrogen nozzle will be enriched with
Fluidized state is maintained in the silica flour of chassis surface, the silica flour in fluidized state serves as heat reflection with its bigger surface area and carried
Body, reflection supplement is carried out to the heat of furnace interior and reduces the loss of reduction furnace heat；
Hot gas fluid layer is located at the top of reduction furnace, and hot gas fluid layer at the top of reduction furnace with the distance at the top of silicon rod by will be arranged to
1000-1500mm, and it is 100-500mm to form hot gas fluid layer bottom with the distance at the top of silicon rod, forms silicon rod away from thermal current
The structure of layer；
Crystal silicon vitellarium is between hot gas fluid layer and cold air fluid layer, and silicon rod is grown in the crystal silicon vitellarium, crystal silicon vitellarium
Gas phase temperature control be 800-900 DEG C.
2. polycrystalline silicon reducing furnace according to claim 1, it is characterised in that：The cold air fluid layer is face-up from chassis upper table
The height of extension is 50-200mm, and 200-600 DEG C of low temperature hydrogen accounts at least the 90% of whole cold air fluid layer in cold air fluid layer.
3. polycrystalline silicon reducing furnace according to claim 1, it is characterised in that：The hydrogen nozzle is uniformly arranged in chassis
Portion, and the top of hydrogen nozzle and the inner surface on chassis are mutually flush；A diameter of 2-5mm of hydrogen nozzle.
4. polycrystalline silicon reducing furnace according to claim 3, it is characterised in that：The nozzle of the hydrogen nozzle is provided with sieve
Net, the sieve diameter of the screen cloth is 0.05-0.1mm, and the screen cloth is made of high chromium-nickel austenitic stainless steel.
5. polycrystalline silicon reducing furnace according to claim 1, it is characterised in that：The inner surface on the chassis is coated with heat reflection
Coating, the heat-reflective coating are silver coating.
6. polycrystalline silicon reducing furnace according to claim 1, it is characterised in that：The top of the body of heater is dome structure, stove
Distance at the top of body and at the top of silicon rod is 1200-1300mm, and the gas phase temperature control of crystal silicon vitellarium is 850 DEG C；The cold air
The height of fluid layer is 100mm, and its temperature is maintained at 300-500 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711067662.0A CN107720756A (en) | 2017-11-03 | 2017-11-03 | A kind of polycrystalline silicon reducing furnace |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711067662.0A CN107720756A (en) | 2017-11-03 | 2017-11-03 | A kind of polycrystalline silicon reducing furnace |
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| Publication Number | Publication Date |
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| CN107720756A true CN107720756A (en) | 2018-02-23 |
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| CN201711067662.0A Pending CN107720756A (en) | 2017-11-03 | 2017-11-03 | A kind of polycrystalline silicon reducing furnace |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108545745A (en) * | 2018-05-14 | 2018-09-18 | 上海森松新能源设备有限公司 | A kind of 72 pairs of stick polycrystalline silicon reducing furnaces |
| CN112938985A (en) * | 2021-03-01 | 2021-06-11 | 江苏鑫华半导体材料科技有限公司 | Polycrystalline silicon reduction furnace and polycrystalline silicon chemical vapor deposition method |
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| US5904981A (en) * | 1998-05-27 | 1999-05-18 | Tokuyama Corporation | Polycrystal silicon rod having an improved morphyology |
| CN102001660A (en) * | 2010-11-24 | 2011-04-06 | 天津大学 | Polysilicon reducing furnace with multiple gas outlets on chassis |
| CN102557038A (en) * | 2011-12-31 | 2012-07-11 | 江苏中能硅业科技发展有限公司 | Preparation method of polycrystalline silicon |
| CN102659109A (en) * | 2012-04-27 | 2012-09-12 | 四川新光硅业科技有限责任公司 | Polycrystalline silicon reduction furnace |
| CN204434296U (en) * | 2015-02-28 | 2015-07-01 | 内蒙古鄂尔多斯电力冶金股份有限公司氯碱化工分公司 | A kind of polycrystalline silicon reducing furnace |
| CN106115711A (en) * | 2016-06-23 | 2016-11-16 | 南京德邦金属装备工程股份有限公司 | A kind of polycrystalline silicon reducing furnace |
-
2017
- 2017-11-03 CN CN201711067662.0A patent/CN107720756A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5904981A (en) * | 1998-05-27 | 1999-05-18 | Tokuyama Corporation | Polycrystal silicon rod having an improved morphyology |
| CN102001660A (en) * | 2010-11-24 | 2011-04-06 | 天津大学 | Polysilicon reducing furnace with multiple gas outlets on chassis |
| CN102557038A (en) * | 2011-12-31 | 2012-07-11 | 江苏中能硅业科技发展有限公司 | Preparation method of polycrystalline silicon |
| CN102659109A (en) * | 2012-04-27 | 2012-09-12 | 四川新光硅业科技有限责任公司 | Polycrystalline silicon reduction furnace |
| CN204434296U (en) * | 2015-02-28 | 2015-07-01 | 内蒙古鄂尔多斯电力冶金股份有限公司氯碱化工分公司 | A kind of polycrystalline silicon reducing furnace |
| CN106115711A (en) * | 2016-06-23 | 2016-11-16 | 南京德邦金属装备工程股份有限公司 | A kind of polycrystalline silicon reducing furnace |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108545745A (en) * | 2018-05-14 | 2018-09-18 | 上海森松新能源设备有限公司 | A kind of 72 pairs of stick polycrystalline silicon reducing furnaces |
| CN112938985A (en) * | 2021-03-01 | 2021-06-11 | 江苏鑫华半导体材料科技有限公司 | Polycrystalline silicon reduction furnace and polycrystalline silicon chemical vapor deposition method |
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Application publication date: 20180223 |
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