CN110451511A - Polycrystalline silicon reducing furnace and its open furnace method - Google Patents
Polycrystalline silicon reducing furnace and its open furnace method Download PDFInfo
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- CN110451511A CN110451511A CN201910790996.3A CN201910790996A CN110451511A CN 110451511 A CN110451511 A CN 110451511A CN 201910790996 A CN201910790996 A CN 201910790996A CN 110451511 A CN110451511 A CN 110451511A
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 94
- 230000009467 reduction Effects 0.000 claims abstract description 84
- 239000000463 material Substances 0.000 claims abstract description 57
- 230000008676 import Effects 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 205
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 238000001514 detection method Methods 0.000 claims description 14
- 230000015556 catabolic process Effects 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 2
- 229920005591 polysilicon Polymers 0.000 description 16
- 239000000047 product Substances 0.000 description 14
- 239000010453 quartz Substances 0.000 description 12
- 229910052710 silicon Inorganic materials 0.000 description 12
- 239000010703 silicon Substances 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 11
- 239000000356 contaminant Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 241001465382 Physalis alkekengi Species 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 206010014357 Electric shock Diseases 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- 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
- C01B33/037—Purification
-
- 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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
- C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
-
- 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
- C30B29/02—Elements
- C30B29/06—Silicon
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of polycrystalline silicon reducing furnace and its furnace method is opened, polycrystalline silicon reducing furnace includes: chassis, and chassis is equipped with air inlet pipe and an air outlet pipe；High value silicon core, is located on chassis；Furnace tube is restored, suitable for being located on chassis, restores in furnace tube and defines cavity；Gas heater is formed with gas feed and gas vent on gas heater；Material system heat exchanger is formed with material system import and material system outlet on material system heat exchanger；Gas pipeline, gas pipeline are configured to and one of being connected in gas vent and material system outlet；Wherein, the gas after gas heater heats is suitable for entering in cavity via gas pipeline and air inlet pipe to heat high value silicon core.Polycrystalline silicon reducing furnace according to the present invention heats gas by gas heater, is preheated the high value silicon core in reduction furnace by hot gas, and whole system belongs to closed system, while gas purity can guarantee, easy to operate, securely and reliably.
Description
Technical field
The present invention relates to polysilicon manufacture technology fields, more particularly, to a kind of polycrystalline silicon reducing furnace and polycrystalline silicon reducing furnace
Open furnace method.
Background technique
In the related technology, the manufacturing enterprise for preparing high pure electronic level polysilicon is substantially all using traditional built-in quartz
The heating method of lamp is heated to silicon core, however, such mode is relatively complicated, is needed repeatedly to replace reduction furnace gas, torn open
Other impurities are possible to during dress to fall into reduction furnace, reduction furnace still needs to livewire work there are security risk in operating process,
Also it is unfavorable for the raising of electronic-grade polycrystalline silicon purity.
Summary of the invention
The present invention is directed at least solve one of the technical problems existing in the prior art.For this purpose, one object of the present invention
It is to propose that a kind of polycrystalline silicon reducing furnace, the polycrystalline silicon reducing furnace are easy to operate and safe and reliable.
It is another object of the present invention to propose a kind of polycrystalline silicon reducing furnace to open furnace method, and described to open furnace method advantageous
Furnace is opened in realization high value silicon core.
Polycrystalline silicon reducing furnace according to an embodiment of the present invention, comprising: chassis, the chassis are equipped with air inlet pipe and outlet
Pipe；High value silicon core, the high value silicon core are located on the chassis；Furnace tube is restored, the reduction furnace tube is suitable for being provide with
On the chassis, cavity is defined in the reduction furnace tube；Gas heater is formed with gas on the gas heater
Import and gas vent；Material system heat exchanger is formed with material system import and material system on the material system heat exchanger
System outlet；Gas pipeline, the gas pipeline be configured to the gas vent and the material system outlet in wherein
One connection；Wherein, the gas after gas heater heating be suitable for via the gas pipeline and the air inlet pipe into
Enter in the cavity to heat the high value silicon core.
Polycrystalline silicon reducing furnace according to an embodiment of the present invention heats gas by gas heater, by hot
Gas preheats the high value silicon core in reduction furnace, and whole system belongs to closed system, while gas purity can guarantee, operation
Simplicity, securely and reliably, so as to solve the problems, such as that high value silicon core is difficult to open furnace in the related technology, improves electronic-grade polycrystalline silicon
Purity stability reduces the introducing of system contaminants, produces high pure electronic grade polysilicon product.
In addition, polycrystalline silicon reducing furnace according to the above embodiment of the present invention also has following additional technical characteristic:
According to some embodiments of the present invention, the gas is high purity inert gas.
Further, the high purity inert gas is nitrogen.
In some embodiments of the invention, the gas is high-purity hydrogen.
According to some embodiments of the present invention, the gas outlet is equipped with first switch valve, the material system outlet
Place is equipped with second switch valve, the first switch valve and one of closing and another opening in the second switch valve.
In some embodiments of the invention, the gas pipeline is equipped with temperature detection part to detect through the air inlet pipe
Into the temperature of the gas in the cavity.
According to some embodiments of the present invention, the gas pipeline is equipped with pressure detecting part to detect through the air inlet pipe
Into the pressure of the gas in the cavity.
According to some embodiments of the present invention, the resistivity of the high value silicon core is not less than 1000 Ω cm.
The polycrystalline silicon reducing furnace of embodiment opens furnace method according to a second aspect of the present invention, comprising: pacifies high value silicon core
It is filled on the chassis of the polycrystalline silicon reducing furnace, and is provide with reduction furnace cylinder on the chassis；Into the reduction furnace with
One predetermined amount of flow is passed through the gas of the first predetermined time to replace the air in the reduction furnace；Gas heater is opened, by institute
Gas is stated to be heated to predetermined temperature and the gas after heating is passed through the second predetermined time in the reduction furnace with second flow；It closes
The gas heater is closed, stops the air inlet into the reduction furnace, and the pressure in the reduction furnace is maintained into predetermined pressure；
High value silicon core after heated gas treatment is subjected to breakdown processing.
Further, first predetermined time is 0.25h-0.5h；And/or second predetermined time is 1.5h-2.0h；
And/or the predetermined temperature is 250 DEG C -300 DEG C；And/or the first flow is 150Nm3；And/or the second flow is
150Nm3；And/or the predetermined pressure is 0.05mpa.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Above-mentioned and/or additional aspect of the invention and advantage will become from the description of the embodiment in conjunction with the following figures
Obviously and it is readily appreciated that, in which:
Fig. 1 is a schematic diagram of polycrystalline silicon reducing furnace according to an embodiment of the present invention, wherein the arrow in figure is directed toward generation
The flow direction of table gas.
Appended drawing reference:
Polycrystalline silicon reducing furnace 100,
Chassis 1, air inlet pipe 11, escape pipe 12,
High value silicon core 2,
Reduction furnace tube 3, cavity 30,
Gas heater 4, gas feed 41, gas vent 42, first switch valve 421,
Material system heat exchanger 5, material system import 51, material system outlet 52,
Gas pipeline 6, temperature detection part 61, pressure detecting part 62.
Specific embodiment
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, and for explaining only the invention, and is not considered as limiting the invention.
In the related technology, polycrystalline silicon material is reached after the purification of a series of physical-chemical reaction using industrial silicon as raw material
The electronic material of certain purity is a particularly important intermediate products in silicon product industrial chain, is that manufacture is silicon polished, too
The primary raw material of positive energy battery and HIGH-PURITY SILICON product, is information industry and the most basic raw material of New Energy Industry.
Electronic-grade silicon (EG): it is general to require containing Si > 99.9999% or more, it is ultra-pure reach 99.9999999%~
99.999999999% (9~11 9).Its electric conductivity is between the Europe centimetre 10-4-1010.Electronic grade high-purity polysilicon is with 9N or more
It is advisable.
Manufacturing enterprise's substantially all adding using traditional built-in quartz lamp of high pure electronic level polysilicon is prepared at present
Hot mode is heated to silicon core, and the flange hole of diameter about φ 300mm is opened up at the top of reduction furnace, places quartz lamp when needing to start
It is heated in reduction furnace to silicon core, resistivity reduces rapidly after High Resistivity Si core is heated, and is then controlled by high and low voltage electrical equipment
System starts silicon core, further takes out quartz lamp from top after silicon core is breakdown, reduction furnace cannot break while retracting quartz lamp
Electricity will also keep silicon core to be powered and run, and avoid silicon core temperature after power-off from reducing, be difficult to the problem of starting again.
However, above-mentioned silicon core heating method, mainly give silicon core to heat using quartzy lamps and lanterns, there are the shortcomings that it is as follows:
First, this heating method needs the opening holes at the top of reduction furnace, it will cause difficulty of processing and investment cost at the top of equipment, deposit
In equipment top welding seam leakage problem.Second, the heating method uses built-in quartz lamp, needs to dismount the quartzy lamps and lanterns in top, deposit
Reduction furnace internal risks are fallen into ambient atmos or other objects, need again to take reduction furnace dismounting once there is this problem
Out, extremely complex inconvenience is operated.Third, in reduction furnace needing that positive pressure is kept to prevent extraneous gas when disassembly quartz lamp heating device
Body enters in furnace, again with blind plate by top sealing hole after after top, quartz lamp is fully drawn out, needs after closure to close
Cover is hunted leak, and there are sealing surface secondary leakages to handle risk.Fourth, when disassembly quartz lamp heating device, silicon in reduction furnace
Stick is still powered operation, gets an electric shock risk if silicon rod encounters furnace tube moment by wall there are operating personnel.Fifth, quartz lamp is consumptive material, it is past
Multiple high/low temperature switching, inner heat body service life is shorter, higher cost.
Below with reference to the accompanying drawings polycrystalline silicon reducing furnace 100 according to an embodiment of the present invention is described.The polycrystalline silicon reducing furnace 100
It can solve high value silicon core and be difficult to the problem of opening furnace, improve electronic-grade polycrystalline silicon purity stability, reduce drawing for system contaminants
Enter, produces high pure electronic grade polysilicon product.
Referring to Fig.1, polycrystalline silicon reducing furnace 100 according to an embodiment of the present invention, comprising: chassis 1, high value silicon core 2, reduction
Furnace tube 3, gas heater 4, material system heat exchanger 5 and gas pipeline 6.
Specifically, air inlet pipe 11 and escape pipe 12 can be equipped on chassis 1；Gas (such as high-purity gas) can be via
Air inlet pipe 11 enters in reduction furnace, is further discharged via escape pipe 12.
High value silicon core 2 can be located on chassis 1.High value silicon core 2 may include it is multiple, multiple high value silicon cores 2 can
To be spaced apart setting on chassis 1.In the description of the present invention, the meaning of " plurality " is two or more.
Reduction furnace tube 3 is suitable for being located on chassis 1, restores in furnace tube 3 and defines cavity 30.When by high value silicon core
2 when being mounted on chassis 1, and reduction furnace cylinder 3 can be provide on chassis 1, consequently facilitating further on chassis 1 and reduction furnace tube
Closed system is formed between body 3.
It could be formed with gas feed 41 and gas vent 42 on gas heater 4.The heating temperature of gas heater 4 can
To be adaptively adjusted as needed.Wherein, when opening gas heater 4, gas can enter gas via gas feed 41
Heater 4, the gas after the heating of gas heater 4 can be discharged via gas vent 42, in this way can be defeated into reduction furnace
Gas after sending heating, so as to realize the preheating to high value silicon core 2 by hot gas.
It could be formed with material system import 51 and material system outlet 52 on material system heat exchanger 5.Material gas can
To enter material system heat exchanger 5 via material system import 51, then 52 are exported via material system and is further delivered to reduction
In furnace.
Gas pipeline 6 is configured to and one of being connected in gas vent 42 and material system outlet 52.Gas goes out
Mouthfuls 42 are suitable for be connected to by gas pipeline 6, air inlet pipe 11 with cavity 30, material system outlet 52 suitable for pass through gas pipeline 6, into
Tracheae 11 is connected to cavity 30.
For example, gas pipeline 6 may only be connected in gas vent 42 and material system outlet 52 wherein in synchronization
One, when gas pipeline 6 is connected to gas vent 42, gas pipeline 6 is not connected to material system outlet 52；Work as gas pipeline
6 with material system outlet 52 be connected to when, gas pipeline 6 is not connected to gas vent 42.
Polycrystalline silicon reducing furnace 100 according to an embodiment of the present invention can use and (wherein, N number of 9 represent the pure of gas to 9N
Degree.99.9%=3N, 99.99%=4N, 9 more multilist show that the purity of gas is higher) the mode that is heated of high-purity gas it is real
Now to the preheating of high value silicon core 2.
Wherein, the gas (such as high-purity gas) after the heating of gas heater 4 is suitable for via gas pipeline 6 and air inlet pipe
11 enter in cavity 30 to heat high value silicon core 2.It as a result, can be by the high value silicon core 2 in reduction furnace by hot gas
Preheating, whole system belongs to closed system, while gas purity can guarantee, easy to operate, securely and reliably, so as to solve
High value silicon core is difficult to the problem of opening furnace in the related technology, improves electronic-grade polycrystalline silicon purity stability, reduces system contaminants
It introduces, produces high pure electronic grade polysilicon product.
Polycrystalline silicon reducing furnace 100 according to an embodiment of the present invention is adequately utilized high-purity hot nitrogen and passes through flue
Road 6 is sent directly into reduction furnace, can avoid being directly protruding into reduction furnace using quartz lamp, halogen lamp and carbon-point in the related technology
Interior, the polycrystalline silicon reducing furnace 100 of the application, without carrying out dismounting and repeatedly displacement to hole at the top of reduction furnace, mode of operation is more
Add that simple, temperature is adjustable.
Polycrystalline silicon reducing furnace 100 according to an embodiment of the present invention, heats gas by gas heater 4, passes through
Hot gas preheats the high value silicon core 2 in reduction furnace, and whole system belongs to closed system, while gas purity can be protected
Card, it is easy to operate, securely and reliably, so as to solve the problems, such as that high value silicon core is difficult to open furnace in the related technology, improves electronics
Level polysilicon purity stability reduces the introducing of system contaminants, produces high pure electronic grade polysilicon product.
According to some embodiments of the present invention, the gas can be high purity inert gas.Further, high-purity indifferent gas
Body can be for such as nitrogen.As a result, by the way that the gas to be used to the high-purity gas of 9N, can not have to place again in reduction furnace
Any heat medium greatly reduces external impurity and introduces risk, ensure that the stability of product quality.
Certainly, the invention is not limited thereto, and in some optional embodiments of the invention, the gas may be for example
High-purity hydrogen etc..
Referring to Fig.1, according to some embodiments of the present invention, first switch valve 421, material can be equipped at gas vent 42
Second switch valve 521, one of pass in first switch valve 421 and second switch valve 521 can be equipped at system outlet 52
It closes and another is opened.For example, second switch valve 521 is closed when first switch valve 421 is opened；When second switch valve 521 is beaten
When opening, first switch valve 421 is closed.
Specifically, when first switch valve 421 is opened, and second switch valve 521 is closed, the gas can go out via gas
Mouth 42, gas passage 5, air inlet pipe 11 enter in reduction furnace.When second switch valve 521 is opened, and first switch valve 421 is closed,
The gas can export 52, gas passage 5 via material system, air inlet pipe 11 enters in reduction furnace.
In conjunction with Fig. 1, temperature detection part 61 can be equipped in some embodiments of the invention, on gas pipeline 6 to detect
Enter the temperature of the gas in (such as in reduction furnace) cavity 30 through air inlet pipe 11.Temperature detection part 61 can be such as thermometer
Deng by the way that temperature detection part 61 is arranged on gas pipeline 6, convenient for intuitively observing the temperature of air inlet by temperature detection part 61
Degree.
Certainly, in other embodiments of the invention, temperature detection part 61 or other types etc., the present invention couple
This is not especially limited.
According to some embodiments of the present invention, gas pipeline 6 be equipped with pressure detecting part 62 with detect through air inlet pipe 11 into
Enter in cavity 30 pressure of the gas of (such as in reduction furnace).Pressure detecting part 62 can be such as pressure gauge, by gas
Pressure detecting part 62 is set on body pipeline 6, convenient for intuitively observing the pressure of air inlet by pressure detecting part 62.
Certainly, in other embodiments of the invention, pressure detecting part 62 or other types etc., the present invention couple
This is not especially limited.
In some embodiments of the invention, corresponding temperature detection part can also be equipped at escape pipe 12 to detect
The temperature of outlet can also be equipped with corresponding pressure detecting part at escape pipe 12 to detect the pressure of outlet.
According to some embodiments of the present invention, the resistivity of high value silicon core 2 is not less than 1000 Ω cm.For example, at this
In some specific embodiments of invention, the resistivity of high value silicon core 2 can be more than or equal to 1000 Ω cm.In the present invention
Some optional embodiments in, the resistivity of high value silicon core 2 can be the silicon plug etc. not less than 1000 Ω cm.
The specific embodiment of polycrystalline silicon reducing furnace 100 according to the present invention is described with reference to the accompanying drawing.
Referring to Fig.1, polycrystalline silicon reducing furnace 100 according to an embodiment of the present invention, comprising: chassis 1, high value silicon core 2, reduction
Furnace tube 3, gas heater 4, material system heat exchanger 5 and gas pipeline 6.
Specifically, air inlet pipe 11 and escape pipe 12 can be equipped on chassis 1；Gas (such as high-purity gas) can be via
Air inlet pipe 11 enters in reduction furnace, is further discharged via escape pipe 12.
High value silicon core 2 can be located on chassis 1.High value silicon core 2 may include it is multiple, multiple high value silicon cores 2 can
To be spaced apart setting on chassis 1.In the description of the present invention, the meaning of " plurality " is two or more.
Reduction furnace tube 3 is suitable for being located on chassis 1, restores in furnace tube 3 and defines cavity 30.When by high value silicon core
2 when being mounted on chassis 1, and reduction furnace cylinder 3 can be provide on chassis 1, consequently facilitating further on chassis 1 and reduction furnace tube
Closed system is formed between body 3.
It could be formed with gas feed 41 and gas vent 42 on gas heater 4.The heating temperature of gas heater 4 can
To be adaptively adjusted as needed.Wherein, when opening gas heater 4, gas can enter gas via gas feed 41
Heater 4, the gas after the heating of gas heater 4 can be discharged via gas vent 42, in this way can be defeated into reduction furnace
Gas after sending heating, so as to realize the preheating to high value silicon core 2 by hot gas.
It could be formed with material system import 51 and material system outlet 52 on material system heat exchanger 5.Material gas can
To enter material system heat exchanger 5 via material system import 51, then 52 are exported via material system and is further delivered to reduction
In furnace.
Gas pipeline 6 is configured to and one of being connected in gas vent 42 and material system outlet 52.Gas goes out
Mouthfuls 42 are suitable for be connected to by gas pipeline 6, air inlet pipe 11 with cavity 30, material system outlet 52 suitable for pass through gas pipeline 6, into
Tracheae 11 is connected to cavity 30.
For example, gas pipeline 6 may only be connected in gas vent 42 and material system outlet 52 wherein in synchronization
One, when gas pipeline 6 is connected to gas vent 42, gas pipeline 6 is not connected to material system outlet 52；Work as gas pipeline
6 with material system outlet 52 be connected to when, gas pipeline 6 is not connected to gas vent 42.
Polycrystalline silicon reducing furnace 100 according to an embodiment of the present invention can use and (wherein, N number of 9 represent the pure of gas to 9N
Degree.99.9%=3N, 99.99%=4N, 9 more multilist show that the purity of gas is higher) the mode that is heated of high-purity gas it is real
Now to the preheating of high value silicon core 2.
Wherein, the gas (such as high-purity gas) after the heating of gas heater 4 is suitable for via gas pipeline 6 and air inlet pipe
11 enter in cavity 30 to heat high value silicon core 2.It as a result, can be by the high value silicon core 2 in reduction furnace by hot gas
Preheating, whole system belongs to closed system, while gas purity can guarantee, easy to operate, securely and reliably, so as to solve
High value silicon core is difficult to the problem of opening furnace in the related technology, improves electronic-grade polycrystalline silicon purity stability, reduces system contaminants
It introduces, produces high pure electronic grade polysilicon product.
Polycrystalline silicon reducing furnace 100 according to an embodiment of the present invention is adequately utilized high-purity hot nitrogen and passes through flue
Road 6 is sent directly into reduction furnace, can avoid being directly protruding into reduction furnace using quartz lamp, halogen lamp and carbon-point in the related technology
Interior, the polycrystalline silicon reducing furnace 100 of the application, without carrying out dismounting and repeatedly displacement to hole at the top of reduction furnace, mode of operation is more
Add that simple, temperature is adjustable.
Polycrystalline silicon reducing furnace 100 according to an embodiment of the present invention, heats gas by gas heater 4, passes through
Hot gas preheats the high value silicon core 2 in reduction furnace, and whole system belongs to closed system, while gas purity can be protected
Card, it is easy to operate, securely and reliably, so as to solve the problems, such as that high value silicon core is difficult to open furnace in the related technology, improves electronics
Level polysilicon purity stability reduces the introducing of system contaminants, produces high pure electronic grade polysilicon product.
According to some embodiments of the present invention, the gas can be high purity inert gas.Further, high-purity indifferent gas
Body can be for such as nitrogen.As a result, by the way that the gas to be used to the high-purity gas of 9N, can not have to place again in reduction furnace
Any heat medium greatly reduces external impurity and introduces risk, ensure that the stability of product quality.
Referring to Fig.1, according to some embodiments of the present invention, first switch valve 421, material can be equipped at gas vent 42
Second switch valve 521, one of pass in first switch valve 421 and second switch valve 521 can be equipped at system outlet 52
It closes and another is opened.For example, second switch valve 521 is closed when first switch valve 421 is opened；When second switch valve 521 is beaten
When opening, first switch valve 421 is closed.
Specifically, when first switch valve 421 is opened, and second switch valve 521 is closed, the gas can go out via gas
Mouth 42, gas passage 5, air inlet pipe 11 enter in reduction furnace.When second switch valve 521 is opened, and first switch valve 421 is closed,
The gas can export 52, gas passage 5 via material system, air inlet pipe 11 enters in reduction furnace.
In conjunction with Fig. 1, temperature detection part 61 can be equipped in some embodiments of the invention, on gas pipeline 6 to detect
Enter the temperature of the gas in (such as in reduction furnace) cavity 30 through air inlet pipe 11.Temperature detection part 61 can be such as thermometer
Deng by the way that temperature detection part 61 is arranged on gas pipeline 6, convenient for intuitively observing the temperature of air inlet by temperature detection part 61
Degree.
According to some embodiments of the present invention, gas pipeline 6 be equipped with pressure detecting part 62 with detect through air inlet pipe 11 into
Enter in cavity 30 pressure of the gas of (such as in reduction furnace).Pressure detecting part 62 can be such as pressure gauge, by gas
Pressure detecting part 62 is set on body pipeline 6, convenient for intuitively observing the pressure of air inlet by pressure detecting part 62.
In some embodiments of the invention, corresponding temperature detection part can also be equipped at escape pipe 12 to detect
The temperature of outlet can also be equipped with corresponding pressure detecting part at escape pipe 12 to detect the pressure of outlet.
According to some embodiments of the present invention, the resistivity of high value silicon core 2 is not less than 1000 Ω cm.For example, at this
In some specific embodiments of invention, the resistivity of high value silicon core 2 can be more than or equal to 1000 Ω cm.In the present invention
Some optional embodiments in, the resistivity of high value silicon core 2 can be the silicon plug etc. not less than 1000 Ω cm.
Due to the Semiconductor Physics characteristic of polysilicon, the more high then resistivity of temperature is lower, and high temperature nitrogen is to high value silicon core 2
Resistivity reduces rapidly after heating, can solve the problems, such as that High Resistivity Si core cannot puncture.Polysilicon according to an embodiment of the present invention is also
Former furnace 100 enters gas heater 4 using 9N nitrogen, heated gas is passed through reduction furnace by the way that gas heater 4 is arranged
It is interior to be preheated to high value silicon core 2, since the resistivity of being heated of high value silicon core 2 will reduce rapidly, then opened again by power supply system
Dynamic high value silicon core 2 solves the problems, such as that the high High-Voltage Electrical Appliances of resistivity are difficult to puncture silicon core with this.
Polycrystalline silicon reducing furnace 100 according to an embodiment of the present invention, by 9N (wherein, N number of 9 purity for representing gas.
99.9%=3N, 99.99%=4N, 9 more multilist show that the purity of gas is higher) high-purity gas heated, pass through hot gas
Body is preheated to the high value silicon core 2 in reduction furnace, and whole system belongs to closed system, while gas purity can guarantee, operation
Simplicity, securely and reliably, so as to solve the problems, such as that high value silicon core is difficult to open furnace in the related technology, improves electronic-grade polycrystalline silicon
Purity stability reduces the introducing of system contaminants, produces high pure electronic grade polysilicon product.
Polycrystalline silicon reducing furnace according to an embodiment of the present invention has the advantage that first, the present invention can solve reduction furnace roof
Portion punches problem, reduces the processing and manufacturing cost of assembly of reduction furnace, while providing device security.Second, the invention can ensure that
High Resistivity Si core punctures success rate, it is ensured that system stable operation, reduction furnace silicon core are completely in closed system, not by extraneous secondary dirt
Dye, significantly offer stable product quality.Third, heated to silicon core so that each position of silicon core is uniformly heated by gas,
Silicon core is avoided temperature gradient occur, it is possible to provide production efficiency, and meanwhile it is easy to operate, investment cost is lower, easy to maintain.
The polycrystalline silicon reducing furnace of embodiment opens furnace method according to a second aspect of the present invention, comprising: pacifies high value silicon core
It is filled on the chassis of the polycrystalline silicon reducing furnace, and is provide with reduction furnace cylinder on the chassis；Into the reduction furnace with
One predetermined amount of flow is passed through the gas of the first predetermined time to replace the air in the reduction furnace；Gas heater is opened, by institute
Gas is stated to be heated to predetermined temperature and the gas after heating is passed through the second predetermined time in the reduction furnace with second flow；It closes
The gas heater is closed, stops the air inlet into the reduction furnace, and the pressure in the reduction furnace is maintained into predetermined pressure；
High value silicon core after heated gas treatment is subjected to breakdown processing.
The polycrystalline silicon reducing furnace of embodiment opens furnace method according to a second aspect of the present invention, is easy to implement high value silicon core
Open furnace.
Polycrystalline silicon reducing furnace according to an embodiment of the present invention opens furnace method, enters gas heater by being passed through 9N nitrogen
In heated, then high-temperature gas is preheated with high value silicon core, to reduce high value silicon core start-up resistor rate.Equally
Nitrogen heating can also be passed through reduction furnace in reduction furnace end of run blowing out by the gas heater, and the later period is avoided to be passed through cold conditions
Gas causes rapid cooling to hot silicon rod surface, and silicon rod is caused to burst situation.
Polycrystalline silicon reducing furnace according to an embodiment of the present invention opens furnace method, can solve resistivity height, and High-Voltage Electrical Appliances are difficult
The problem of to puncture and the subsequent lower situation of blowing out gas temperature and silicon rod occurs bursting situation when causing.
Further, first predetermined time is 0.25-0.5h；For example, first predetermined time can for 0.25h,
0.35h, 0.45h or 0.5h etc..And/or second predetermined time is 1.5h-2.0h；For example, second predetermined time can
Think 1.5h, 1.75h or 2.0h etc..
And/or the predetermined temperature is 250 DEG C -300 DEG C；For example, the predetermined temperature can be such as 250 DEG C, 265
DEG C, 275 DEG C, 290 DEG C or 300 DEG C etc., in this way by setting 250 DEG C -300 DEG C for the predetermined temperature of heat gas, be conducive to
It the heating time for shortening high value silicon core, improves efficiency.
And/or the first flow is 150Nm3 and/or the second flow is 150Nm3.Wherein, Nm3 refers to and takes the photograph 0
The gas volume of 1 normal atmosphere of family name's degree pressure；N represents standard conditions (Normal Condition), the i.e. condition of air are as follows:
One standard atmospheric pressure, temperature are 0 DEG C, relative humidity 0%.M3 refers to gas volume under actual working state.
And/or the predetermined pressure is 0.05mpa.In this way convenient for further using High-Voltage Electrical Appliances to the progress of high value silicon core
Breakdown is transferred to normal operating after completing starting work.
The polycrystalline silicon reducing furnace of embodiment opens furnace method according to a second aspect of the present invention, further includes that treated in breakdown
On silicon core the step of deposit polycrystalline silicon.Wherein, the step of deposit polycrystalline silicon may include: that object is passed through into polycrystalline silicon reducing furnace
Material, and the electric current of polycrystalline silicon reducing furnace is controlled so that material reaction forms polysilicon.The type of material can be according to existing skill
Art is set, such as material may include trichlorosilane and hydrogen.
A specific embodiment for opening furnace method for polycrystalline silicon reducing furnace according to the present invention is described below.
Specifically, high value silicon core after the installation is completed, buckles reduction furnace tube in reduction furnace, it is passed through into reduction furnace high-purity
Nitrogen is replaced, and drives reduction furnace air, time swap 0.5h away；It is after being replaced, gas heater is (such as high-purity
Nitrogen heater) it opens and is heated to nitrogen, it is then passed through in reduction furnace again, controls the flow about 150Nm3 of nitrogen, nitrogen goes out
200 DEG C of temperature of mouth is heated by hot nitrogen and high value silicon core, due to the heat conductivity of high value silicon core itself, after being heated
Resistivity reduces rapidly, and is convenient for high-voltage breakdown, and time swap about 2h closes gas heater, stops air inlet, restores furnace pressure
It is maintained 0.05mpa, then silicon core is punctured using High-Voltage Electrical Appliances, is transferred to normal operating after completing starting work.
The high-purity gas for the 9N that the present invention uses completely, reduction furnace is interior not to be had to place any heat medium again, is substantially reduced
External impurity introduces risk, ensure that the stability of product quality.
The present invention is on the actual application in actual production, and operational process is reliable and stable, it is ensured that is opened furnace success rate, is contracted
Short to open furnace time and reduction furnace time swap, operation is simple and reliable, it is ensured that electronic-grade polycrystalline silicon stable product quality.
Polycrystalline silicon reducing furnace according to an embodiment of the present invention and its other for opening furnace method are constituted and are operated for ability
All be for the those of ordinary skill of domain it is known, be not detailed herein.
In the description of the present invention, it is to be understood that, term " center ", "upper", "lower", "vertical", "horizontal",
The orientation or positional relationship of the instructions such as "top", "bottom", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, and is only
For the convenience of describing the present invention and simplifying the description, rather than the device or element of indication or suggestion meaning must have specific side
Position is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " illustrative examples ",
The description of " example ", " specific example " or " some examples " etc. means specific features described in conjunction with this embodiment or example, knot
Structure, material or feature are included at least one embodiment or example of the invention.In the present specification, to above-mentioned term
Schematic representation may not refer to the same embodiment or example.Moreover, specific features, structure, material or the spy of description
Point can be combined in any suitable manner in any one or more of the embodiments or examples.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that: not
A variety of change, modification, replacement and modification can be carried out to these embodiments in the case where being detached from the principle of the present invention and objective, this
The range of invention is defined by the claims and their equivalents.
Claims (10)
1. a kind of polycrystalline silicon reducing furnace characterized by comprising
Chassis, the chassis are equipped with air inlet pipe and an air outlet pipe；
High value silicon core, the high value silicon core are located on the chassis；
Furnace tube is restored, the reduction furnace tube is suitable for being located on the chassis, defines cavity in the reduction furnace tube；
Gas heater is formed with gas feed and gas vent on the gas heater；
Material system heat exchanger is formed with material system import and material system outlet on the material system heat exchanger；
Gas pipeline, the gas pipeline are configured to and one of them in the gas vent and material system outlet
Connection；
Wherein, described in the gas after gas heater heating is suitable for entering via the gas pipeline and the air inlet pipe
To heat the high value silicon core in cavity.
2. polycrystalline silicon reducing furnace according to claim 1, which is characterized in that the gas is high purity inert gas.
3. polycrystalline silicon reducing furnace according to claim 2, which is characterized in that the high purity inert gas is nitrogen.
4. polycrystalline silicon reducing furnace according to claim 1, which is characterized in that the gas is high-purity hydrogen.
5. polycrystalline silicon reducing furnace according to claim 1, which is characterized in that the gas outlet is equipped with first switch
Valve, the material system exit are equipped with second switch valve, and wherein one in the first switch valve and the second switch valve
A closing and another opening.
6. polycrystalline silicon reducing furnace according to claim 1, which is characterized in that the gas pipeline is equipped with temperature detection part
To detect the temperature for entering the gas in the cavity through the air inlet pipe.
7. polycrystalline silicon reducing furnace according to claim 1, which is characterized in that the gas pipeline is equipped with pressure detecting part
To detect the pressure for entering the gas in the cavity through the air inlet pipe.
8. polycrystalline silicon reducing furnace described in any one of -7 according to claim 1, which is characterized in that the electricity of the high value silicon core
Resistance rate is not less than 1000 Ω cm.
9. a kind of polycrystalline silicon reducing furnace according to claim 1 to 8 opens furnace method, which is characterized in that, packet
It includes:
High value silicon core is installed to the chassis of the polycrystalline silicon reducing furnace, and is provide with reduction furnace cylinder on the chassis；
The gas of the first predetermined time is passed through with the first predetermined amount of flow into the reduction furnace to replace the sky in the reduction furnace
Gas；
Gas heater is opened, the gas is heated to predetermined temperature and is passed through with second flow the gas after heating described
Second predetermined time in reduction furnace；
The gas heater is closed, the air inlet into the reduction furnace is stopped, and the pressure in the reduction furnace is maintained pre-
Constant-pressure；
High value silicon core after heated gas treatment is subjected to breakdown processing.
10. polycrystalline silicon reducing furnace according to claim 9 opens furnace method, which is characterized in that
First predetermined time is 0.25h-0.5h；And/or
Second predetermined time is 1.5h-2.0h；And/or
The predetermined temperature is 250 DEG C -300 DEG C；And/or
The first flow is 150Nm3；And/or
The second flow is 150Nm3；And/or
The predetermined pressure is 0.05mpa.
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| CN201910790996.3A CN110451511A (en) | 2019-08-26 | 2019-08-26 | Polycrystalline silicon reducing furnace and its open furnace method |
| PCT/CN2020/109236 WO2021036826A1 (en) | 2019-08-26 | 2020-08-14 | Polycrystalline silicon reduction furnace and furnace start method thereof |
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| CN201910790996.3A CN110451511A (en) | 2019-08-26 | 2019-08-26 | Polycrystalline silicon reducing furnace and its open furnace method |
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| WO2021036826A1 (en) * | 2019-08-26 | 2021-03-04 | 中国恩菲工程技术有限公司 | Polycrystalline silicon reduction furnace and furnace start method thereof |
| CN112645334A (en) * | 2020-12-21 | 2021-04-13 | 亚洲硅业(青海)股份有限公司 | Furnace start prediction method and system for polycrystalline silicon reduction furnace, storage medium and terminal |
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