CN109292777A - Polycrystalline silicon reducing furnace opens the silicon core breakdown method of furnace, opens the method and device of furnace method, production polysilicon - Google Patents
Polycrystalline silicon reducing furnace opens the silicon core breakdown method of furnace, opens the method and device of furnace method, production polysilicon Download PDFInfo
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- CN109292777A CN109292777A CN201710606238.2A CN201710606238A CN109292777A CN 109292777 A CN109292777 A CN 109292777A CN 201710606238 A CN201710606238 A CN 201710606238A CN 109292777 A CN109292777 A CN 109292777A
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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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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
- F27D2007/063—Special atmospheres, e.g. high pressure atmospheres
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Abstract
The invention discloses a kind of polycrystalline silicon reducing furnaces to open the silicon core breakdown method of furnace, opens the method and device of furnace method, production polysilicon, silicon core breakdown method is the following steps are included: be passed through non-oxidizing gas displacement into the polycrystalline silicon reducing furnace of furnace to be opened, it is passed through 380~400 DEG C of hydrogen again to be replaced, the silicon core in polycrystalline silicon reducing furnace is preheated by hydrogen；It squeezes into voltage and carries out the breakdown of silicon core.When squeezing into voltage and being punctured, the hydrogen in polycrystalline silicon reducing furnace is still 380~400 DEG C at this time, and can maintain silicon core is conductor, not will lead to silicon core electric current, voltage fluctuation, realizes the breakdown of silicon core.Silicon core breakdown method can puncture the silicon core of the resistivity of 200~300 Ω cm, promote conversion ratio of reduction, since the resistivity of breakdown silicon core greatly improves, reducing the prior art is the phosphorus impurities for reducing silicon core resistivity and ensureing the breakdown of silicon core and mixing, so improving polysilicon product quality, and avoid introducing silicon nitride inclusions.
Description
Technical field
The invention belongs to technical field of polysilicon production, and in particular to a kind of polycrystalline silicon reducing furnace opens the silicon core breakdown side of furnace
Method, the method and device for opening furnace method, producing polysilicon.
Background technique
Polysilicon is key raw material used in integrated circuit and photovoltaic power generation, is former material necessary to national new energy development
Material.In the epoch of the worsening shortages of fossil energy instantly, the emergence of new energy has become inexorable trend.
In the polysilicon production process in China, 90% production of polysilicon enterprise is raw using improved Siemens polysilicon
Production. art, the technique using in non-oxidizing gas environment, silicon core to resistivity lower than 100 Ω cm with 5500~
After 6000V voltage breakdown, non-oxidizing gas is displaced with hydrogen, by elevated currents, silicon core temperature is promoted, three will be refined
Chlorine hydrogen silicon and hydrogen, which enter according to the ratio in polycrystalline silicon reducing furnace, carries out reduction reaction production polysilicon.
The characteristics of improved Siemens polysilicon production process is that technique is more mature, has the knowhow of decades,
Major part enterprise of China uses this method.But there is also several big apparent defects for this method:
One, voltage breakdown is carried out to silicon core using in non-oxidizing gas environment, to silicon in non-oxidizing gas environment
When core punctures, silicon nitride inclusions can be generated because silicon wicking surface reacts, be operated in the nitrogen environment of low-pressure, it is easy to introduce silicon
Powder impurity etc., the quality problems for easily leading to the removing of silicon core occur or residual moisture cause the silicon core of silicon rod remove, the indigo plant quality such as film
Problem leads to polysilicon defect ware.And the breakdown operating time is longer, and 5500V~6000V voltage is utilized more than to silicon core and is carried out
When breakdown operation, there is 5% probability that electric insulating part is caused to damage, and causes to open furnace failure.
Two, in current China's production of polysilicon enterprise, energy consumption is generally higher, reaches 1 ton of polysilicon consumption 8~10 of every production
Ten thousand degree of electricity, and polycrystalline silicon reducing furnace power consumption then reaches 5~5.5 ten thousand degree of electricity/ton silicon.
Three, the reduction reaction process of current China's production of polysilicon, one time conversion ratio is generally lower, average 10.0%~
Between 10.5%.
Four, in the reaction end gas thermal energy removal process of polycrystalline silicon reducing furnace, due to using technique earlier, every polycrystalline
Si reduction furnace corresponds to a set of heat reclaim unit, and a large amount of high-pressure water heatings using for cooling down the furnace tube of polycrystalline silicon reducing furnace,
The heat that polycrystalline silicon reducing furnace is taken out of is taken away by high-pressure water heating, causes heat utilization rate not high, in heat exchanger leakage water inlet,
It will lead to halt production and product quality glide rapidly, and system is huge, equipment is huge more, overhaul, is difficult in maintenance.The above reason is led
Cost increase in polysilicon production process is caused, the system failure is frequent, and enterprise competitiveness is caused to decline.
Five, in current improved Siemens polysilicon production process, using silicon core resistivity control 100 Ω cm with
Under, it can be excessive due to resistivity if more than 100 Ω cm, can not puncture to silicon core leads to open furnace failure, and silicon core resistivity
It improves, reduces the prior art to reduce silicon core resistivity and ensureing that silicon core punctures, and the phosphorus impurities mixed, then product polycrystalline is siliceous
Amount is obviously improved effect.
Summary of the invention
The technical problem to be solved by the present invention is to aiming at the above shortcomings existing in the prior art, provide a kind of polysilicon
Reducing furnace start-up furnace silicon core breakdown method, open furnace method, produce polysilicon method and device, the present invention in silicon core breakdown side
Method is replaced by being passed through 380~400 DEG C of hydrogen, then is squeezed into voltage and carried out the breakdown of silicon core, can puncture 200~300
The silicon core of the resistivity of Ω cm promotes conversion ratio of reduction.
It solves technical solution used by present invention problem and is to provide a kind of silicon core that polycrystalline silicon reducing furnace opens furnace to hit
Wear method, comprising the following steps:
It is passed through non-oxidizing gas displacement into the polycrystalline silicon reducing furnace of furnace to be opened, then is passed through 380~400 DEG C of hydrogen
It is replaced, the silicon core in polycrystalline silicon reducing furnace is preheated by hydrogen；
It squeezes into voltage and carries out the breakdown of silicon core.When treating the polycrystalline reduction progress non-oxidizing gas displacement for opening furnace, not
Heating, can't generate silicon nitride, silicon nitride inclusions would not be also introduced in polysilicon production process.
Preferably, the non-oxidizing gas is one or more of nitrogen, argon gas, helium.It is first passed through non-oxide
Gas is replaced, then is passed through hydrogen displacement, can prevent from exploding.
Preferably, the voltage is 2000~6000V.
Preferably, the voltage is 2000~3000V.For compared with the existing technology, silicon core is used in the present invention
The voltage of breakdown substantially reduces, to improve the service life of polycrystalline silicon reducing furnace electrical component, reduces polycrystalline reduction
The electrical component spoilage of furnace.
Use 5500~6000V voltage breakdown silicon core of the traditional forms of enterprises in compared with the existing technology is more in the present invention
When crystal silicon reduction furnace silicon core voltage breakdown, breakdown applied voltage is 2000~3000V, due to the decline of breakdown voltage, is made electrical
Insulating element and 40%~50% or more electrical component damage probability decline.And breakdown is more efficient, by the breakdown of the traditional forms of enterprises
It is 1.0~1.2 hours time-consuming, it drops to 30~40 minutes, and realize and puncture in silicon core hydrogen environment, reduces the removing of silicon core, indigo plant
The generation of film can be promoted to 200~300 Ω cm, to polysilicon product matter by the silicon core resistivity used by 100 Ω cm of <
It measures more excellent.
Preferably, it is replaced by hydrogen, the pressure in the polycrystalline silicon reducing furnace of the furnace to be opened is 20~100KPa.
Preferably, the specific method of the hydrogen that 380~400 DEG C are passed through into the polycrystalline silicon reducing furnace of furnace to be opened
Are as follows:
Hydrogen is heated using the high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace；Reuse neighbour
The reaction end gas of nearly polycrystalline silicon reducing furnace heats hydrogen, hydrogen is heated to 380~400 DEG C, to the polycrystalline of furnace to be opened
Hydrogen is passed through in Si reduction furnace.
The present invention also provides a kind of polycrystalline silicon reducing furnaces to open furnace method, comprising the following steps:
By above-mentioned method, the silicon core treated in the polycrystalline silicon reducing furnace for opening furnace carries out the breakdown of silicon core；
Hydrogen sky is burnt；
It is passed through hydrogen, trichlorosilane into the polycrystalline silicon reducing furnace of furnace to be opened, chemical vapour deposition reaction is carried out, in silicon core
Surface deposition production polysilicon, completes polycrystalline silicon reducing furnace and opens furnace.
It is preferably, described to be passed through trichlorosilane into the polycrystalline silicon reducing furnace of furnace to be opened method particularly includes:
Trichlorosilane is heated using the high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace；Make again
Trichlorosilane is heated with the reaction end gas of neighbouring polycrystalline silicon reducing furnace, is passed through three into the polycrystalline silicon reducing furnace of furnace to be opened
Chlorine hydrogen silicon.
Preferably, trichlorosilane is heated to 380~400 DEG C using the reaction end gas of neighbouring polycrystalline silicon reducing furnace.
The present invention also provides a kind of methods for producing polysilicon, comprising the following steps:
Furnace method is opened by above-mentioned polycrystalline silicon reducing furnace to carry out opening furnace；
It is passed through hydrogen, trichlorosilane into polycrystalline silicon reducing furnace, carries out chemical vapour deposition reaction, is deposited in silicon wicking surface
Produce polysilicon.
It is preferably, described to be passed through into polycrystalline silicon reducing furnace hydrogen, trichlorosilane method particularly includes:
Hydrogen is passed through into neighbouring polycrystalline silicon reducing furnace and/or the high pressure for being used to cool down its furnace tube of itself polycrystalline silicon reducing furnace
Hot water carries out primary preheating, again by the intermediate heating of reaction end gas progress of neighbouring polycrystalline silicon reducing furnace；
It is used to cool down its furnace tube for what trichlorosilane passed through neighbouring polycrystalline silicon reducing furnace and/or itself polycrystalline silicon reducing furnace
High-pressure water heating carries out primary preheating, again by the intermediate heating of reaction end gas progress of neighbouring polycrystalline silicon reducing furnace；
The trichlorosilane of the hydrogen of middle rank heating and middle rank heating is mixed to get gaseous mixture, then also by itself polysilicon
The reaction end gas of former furnace carries out charging heating, and the gaseous mixture after charging heating is passed into polycrystalline silicon reducing furnace.
Preferably, hydrogen is 140~150 DEG C by the temperature after primary preheating, then passes through the temperature after middle rank heating
It is 380~400 DEG C；
Trichlorosilane is 140~150 DEG C by the temperature after primary preheating, then passing through the temperature after middle rank heating is 380
~400 DEG C；
Gaseous mixture is 420~450 DEG C by the temperature after charging heating.
Preferably, the temperature of the high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace is 155~160
DEG C, pressure is 0.7~0.8MPa；The temperature of the reaction end gas of neighbouring polycrystalline silicon reducing furnace is 500~550 DEG C；Itself polycrystalline
The temperature of the reaction end gas of Si reduction furnace is 500~550 DEG C.
Preferably, using hydrogen as the carrier gas of trichlorosilane, by neighbouring polycrystalline silicon reducing furnace for cooling down its furnace
The high-pressure water heating of cylinder carries out primary preheating, again by the intermediate heating of reaction end gas progress of neighbouring polycrystalline silicon reducing furnace, then with
The trichlorosilane of middle rank heating is mixed to get gaseous mixture.
The present invention also provides the devices that polysilicon is produced used in a kind of method of above-mentioned production polysilicon, comprising:
Trichlorosilane preliminary heater, for being passed through the use of neighbouring polycrystalline silicon reducing furnace and/or itself polycrystalline silicon reducing furnace
In the high-pressure water heating of its cooling furnace tube, primary preheating is carried out to the trichlorosilane for being passed through trichlorosilane preliminary heater；
Trichlorosilane middle rank heater is connect with the trichlorosilane preliminary heater, the trichlorosilane middle rank heating
Device is used to be passed through the reaction end gas of neighbouring polycrystalline silicon reducing furnace, preheats to the primary of passing through for being passed through trichlorosilane middle rank heater
Trichlorosilane carry out intermediate heating；
Hydrogen preliminary heater, for be passed through neighbouring polycrystalline silicon reducing furnace and/or itself polycrystalline silicon reducing furnace for cold
But the high-pressure water heating of its furnace tube carries out primary preheating to the hydrogen for being passed through hydrogen preliminary heater；
Hydrogen middle rank heater is connect with the hydrogen preliminary heater, and the hydrogen middle rank heater is for being passed through neighbour
The reaction end gas of close polycrystalline silicon reducing furnace carries out middle rank to the hydrogen for passing through primary preheating for being passed through hydrogen middle rank heater and adds
Heat；
Mixer is connect with the trichlorosilane middle rank heater, the hydrogen middle rank heater, the mixer respectively
Hydrogen mixing for that will pass through the trichlorosilane of middle rank heating and by middle rank heating, obtains gaseous mixture；
Feed heater is connect with the mixer, and the feed heater is for being passed through itself polycrystalline silicon reducing furnace
Reaction end gas carries out charging heating to the gaseous mixture for being passed through feed heater；
Polycrystalline silicon reducing furnace is connect with the feed heater, and the polycrystalline silicon reducing furnace is used for the polycrystalline to furnace to be opened
It is passed through 380~400 DEG C of hydrogen in Si reduction furnace to be replaced, pre-add is carried out to the silicon core in polycrystalline silicon reducing furnace by hydrogen
Heat squeezes into voltage and carries out the breakdown of silicon core；The polycrystalline silicon reducing furnace is also used to open furnace, production polysilicon.
125~130 DEG C of the high-pressure water heating of the 0.7~0.8MPa come from flash zone conveying, into polycrystalline silicon reducing furnace
Furnace tube exchanges heat with polycrystalline silicon reducing furnace, and the temperature of the high-pressure water heating after heat exchange is 155~160 DEG C, from polycrystalline silicon reducing furnace
Out 155~160 DEG C, after the high-pressure water heating mixing of 0.7~0.8MPa, into hydrogen preheater, trichlorosilane preheater,
After exchanging heat, the temperature of high-pressure water heating is down to 125~130 DEG C, is delivered to flash zone, is recycled.
Silicon core is punctured in the prior art, by (adding centainly phosphorous to the silicon core material of production silicon core to silicon core p-doped
Coating, to reduce the resistivity of silicon core) technique, to reduce silicon core resistivity, silicon core resistivity less than 100 Ω cm,
To ensure silicon core breakdown rate.There is experimental data to show the silicon core of non-p-doped, if initial phosphorous content is 150~200ppt, resistance
Rate is 300~400 Ω cm, and the silicon core phosphorus content after p-doped can reach 1000~2000ppt, and resistance is decreased to less than 100 Ω
cm.Because silicon core phosphorus content rises, polycrystalline silicon rod product phosphorus content can be impacted, phosphorus content averagely promotes 50~100ppt,
Resistivity declines 100~150 Ω cm.
Silicon core breakdown method in the present invention can puncture the silicon core of the resistivity of 200~300 Ω cm, then only need a small amount of
P-doped does not need p-doped, therefore, can reduce polycrystalline silicon rod product 50~100ppt of phosphorus content, resistivity promotes 100~150
Ω cm, product silicon rod entirety grade will have 20% probability to promote a grade, i.e., promoted 20% by solar energy select quality
To electron level, there is 20% probability that will be promoted to solar energy select quality by solar energy primes, have 20% probability will be by the sun
Energy seconds is promoted to solar energy primes, therefore quality is promoted by a relatively large margin.
The silicon core in polycrystalline silicon reducing furnace is preheated by 380~400 DEG C of hydrogen in the present invention, may make silicon
Core becomes conductor, and when squeezing into voltage and being punctured, the hydrogen in polycrystalline silicon reducing furnace is still 380~400 DEG C at this time, can be tieed up
Holding silicon core is that therefore conductor not will lead to silicon core electric current, voltage fluctuation, therefore can realize that silicon core punctures.Silicon core in the present invention
Breakdown method can puncture the silicon core of the resistivity of 200~300 Ω cm, promote conversion ratio of reduction, compared with the existing technology
For, since the resistivity of breakdown silicon core greatly improves, reduce the prior art to reduce silicon core resistivity and ensureing the breakdown of silicon core
And the phosphorus impurities mixed, so greatly improving polysilicon product quality, and avoid in the polysilicon produced in the prior art
Introduce silicon nitride inclusions.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the silicon core puncture device that polycrystalline silicon reducing furnace in the embodiment of the present invention 2 opens furnace；
Fig. 2 is the structural schematic diagram of the device of the production polysilicon in the embodiment of the present invention 7.
In figure: 1- refining trichlorosilane holding vessel；2- trichlorosilane preliminary heater；3- trichlorosilane middle rank heater；
4- hydrogen preliminary heater；5- hydrogen middle rank heater；6- mixer；7- feed heater；8- polycrystalline silicon reducing furnace；9- silicon
Core.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, with reference to the accompanying drawing and specific embodiment party
Present invention is further described in detail for formula.
Embodiment 1
The silicon core for opening furnace the present embodiment provides a kind of polycrystalline silicon reducing furnace punctures method, comprising the following steps:
(1) it is passed through non-oxidizing gas displacement into the polycrystalline silicon reducing furnace of furnace to be opened, then is passed through 380~400 DEG C of hydrogen
Gas is replaced, and is preheated by hydrogen to the silicon core in polycrystalline silicon reducing furnace；
(2) it squeezes into voltage and carries out the breakdown of silicon core.
The silicon core in polycrystalline silicon reducing furnace is preheated by 380~400 DEG C of hydrogen in the present embodiment, may make
Silicon core becomes conductor, and when squeezing into voltage and being punctured, the hydrogen in polycrystalline silicon reducing furnace is still 380~400 DEG C at this time, can
Maintenance silicon core is that therefore conductor not will lead to silicon core electric current, voltage fluctuation, therefore can realize that silicon core punctures.In the present embodiment
Silicon core breakdown method can puncture the silicon core of the resistivity of 200~300 Ω cm, conversion ratio of reduction be promoted, relative to existing
For technology, since the resistivity of breakdown silicon core greatly improves, reduces the prior art to reduce silicon core resistivity and ensure silicon core
The phosphorus impurities of breakdown and incorporation, so greatly improving polysilicon product quality, and avoid the polycrystalline produced in the prior art
Silicon nitride inclusions are introduced in silicon.
Embodiment 2
As shown in Figure 1, the present embodiment provides 9 puncture devices of silicon core that a kind of polycrystalline silicon reducing furnace 8 opens furnace, comprising:
Hydrogen preliminary heater 4, for being passed through the high-pressure water heating for being used to cool down its furnace tube of neighbouring polycrystalline silicon reducing furnace 8,
Primary preheating is carried out to the hydrogen for being passed through hydrogen preliminary heater 4；
Hydrogen middle rank heater 5, connect with hydrogen preliminary heater 4, and hydrogen middle rank heater 5 is used to be passed through neighbouring more
The reaction end gas of crystal silicon reduction furnace 8 carries out intermediate heating to the hydrogen by primary preheating for being passed through hydrogen middle rank heater 5；
Polycrystalline silicon reducing furnace 8 is connect with hydrogen middle rank heater 5, and polycrystalline silicon reducing furnace 8 carries out silicon for squeezing into voltage
Core 9 punctures.
The present embodiment provides a kind of 9 breakdown methods of silicon core that furnace is opened using above-mentioned apparatus progress polycrystalline silicon reducing furnace 8, including
Following steps:
(1) hot high pressure for being used to cool down its furnace tube of neighbouring polycrystalline silicon reducing furnace 8 is passed through into hydrogen preliminary heater 4
Water heats the hydrogen for being passed through hydrogen preliminary heater 4.
(2) reaction end gas of neighbouring polycrystalline silicon reducing furnace 8 is passed through into hydrogen middle rank heater 5 again, to being passed through in hydrogen
The hydrogen by primary preheating of grade heater 5 is heated, and hydrogen is heated to 380 DEG C.
(3) it is passed through non-oxidizing gas nitrogen displacement oxygen content into the polycrystalline silicon reducing furnace 8 of furnace to be opened and is less than 500ppm
Afterwards, then be passed through 380 DEG C of hydrogen carry out displacement non-oxidizing gas content displacement be less than 2000ppm, by hydrogen replace so as to
Opening the pressure in the polycrystalline silicon reducing furnace 8 of furnace is 60KPa, carries out pre-add to the silicon core 9 in polycrystalline silicon reducing furnace 8 by hydrogen
Heat.Specifically, the non-oxidizing gas in the present embodiment is nitrogen.
(4) voltage for squeezing into 4500V carries out silicon core 9 and punctures.
The silicon core 9 in polycrystalline silicon reducing furnace 8 is preheated by 380 DEG C of hydrogen in the present embodiment, may make silicon
Core 9 becomes conductor, and in the voltage for squeezing into 4500V, and the hydrogen in polycrystalline silicon reducing furnace 8 is still 380 DEG C at this time, can maintain silicon
Core 9 is that therefore conductor not will lead to 9 electric current of silicon core, voltage fluctuation, therefore can realize that silicon core 9 punctures.Silicon in the present embodiment
The silicon core 9 that 9 breakdown method of core can puncture the resistivity of 200 Ω cm by squeezing into the voltage of 4500V promotes primary turn of reduction
Rate, compared with the existing technology for, due to breakdown silicon core 9 resistivity greatly improve, reduce the prior art for reduce silicon
Core resistivity ensures that silicon core punctures, and the phosphorus impurities mixed, so greatly improving polysilicon product quality, and avoids existing
Silicon nitride inclusions are introduced in the polysilicon produced in technology.
Embodiment 3
The present embodiment provides a kind of devices using in above-described embodiment 2 to carry out the silicon core breakdown that polycrystalline silicon reducing furnace opens furnace
Method, comprising the following steps:
(1) high-pressure water heating for being used to cool down its furnace tube of neighbouring polycrystalline silicon reducing furnace is passed through into hydrogen preliminary heater,
The hydrogen for being passed through hydrogen preliminary heater is heated.
(2) reaction end gas of neighbouring polycrystalline silicon reducing furnace is passed through into hydrogen middle rank heater again, it is intermediate to hydrogen is passed through
The hydrogen by primary preheating of heater is heated, and hydrogen is heated to 400 DEG C.
(3) it is passed through non-oxidizing gas argon gas displacement oxygen content into the polycrystalline silicon reducing furnace of furnace to be opened and is less than 500ppm
Afterwards, then be passed through 400 DEG C of hydrogen carry out displacement non-oxidizing gas argon content displacement be less than 2000ppm, by hydrogen displacement make
Obtaining the pressure in the polycrystalline silicon reducing furnace of furnace to be opened is 20KPa, carries out pre-add to the silicon core in polycrystalline silicon reducing furnace by hydrogen
Heat.
(4) voltage for squeezing into 3000V carries out the breakdown of silicon core.
The silicon core 9 in polycrystalline silicon reducing furnace 8 is preheated by 400 DEG C of hydrogen in the present embodiment, may make silicon
Core 9 becomes conductor, and in the voltage for squeezing into 3000V, and the hydrogen in polycrystalline silicon reducing furnace 8 is still 400 DEG C at this time, can maintain silicon
Core 9 is that therefore conductor not will lead to 9 electric current of silicon core, voltage fluctuation, therefore can realize that silicon core 9 punctures.Silicon in the present embodiment
The silicon core 9 that 9 breakdown method of core can puncture the resistivity of 250 Ω cm by squeezing into the voltage of 3000V promotes primary turn of reduction
Rate, compared with the existing technology for, due to breakdown silicon core 9 resistivity greatly improve, reduce the prior art for reduce silicon
Core resistivity ensures that silicon core punctures, and the phosphorus impurities mixed, so greatly improving polysilicon product quality, and avoids existing
Silicon nitride inclusions are introduced in the polysilicon produced in technology.
Embodiment 4
The present embodiment provides a kind of devices using in above-described embodiment 2 to carry out the silicon core breakdown that polycrystalline silicon reducing furnace opens furnace
Method, comprising the following steps:
(1) high-pressure water heating for being used to cool down its furnace tube of neighbouring polycrystalline silicon reducing furnace is passed through into hydrogen preliminary heater,
The hydrogen for being passed through hydrogen preliminary heater is heated.
(2) reaction end gas of neighbouring polycrystalline silicon reducing furnace is passed through into hydrogen middle rank heater again, it is intermediate to hydrogen is passed through
The hydrogen by primary preheating of heater is heated, and hydrogen is heated to 390 DEG C.
(3) non-oxidizing gas helium replacement oxygen content is passed through into the polycrystalline silicon reducing furnace of furnace to be opened less than 500ppm
Afterwards, then be passed through 390 DEG C of hydrogen carry out displacement non-oxidizing gas helium content displacement be less than 2000ppm, by hydrogen displacement make
Obtaining the pressure in the polycrystalline silicon reducing furnace of furnace to be opened is 100KPa, carries out pre-add to the silicon core in polycrystalline silicon reducing furnace by hydrogen
Heat.
(4) voltage for squeezing into 6000V carries out the breakdown of silicon core.
Polycrystalline silicon reducing furnace in the present embodiment opens the silicon core breakdown method of furnace, can puncture the resistivity of 290 Ω cm
Silicon core.
Embodiment 5
The present embodiment provides a kind of devices using in above-described embodiment 2 to carry out the silicon core breakdown that polycrystalline silicon reducing furnace opens furnace
Method, the difference with embodiment 4 are as follows: breakdown voltage 2500V can puncture the silicon core of the resistivity of 270 Ω cm.
Embodiment 6
The present embodiment provides a kind of polycrystalline silicon reducing furnaces to open furnace method, comprising the following steps:
By Examples 1 to 5 either method, the silicon core treated in the polycrystalline silicon reducing furnace for opening furnace carries out the breakdown of silicon core；
Hydrogen sky is burnt；
It is passed through hydrogen, trichlorosilane into the polycrystalline silicon reducing furnace of furnace to be opened, chemical vapour deposition reaction is carried out, in silicon core
Surface deposition production polysilicon, completes polycrystalline silicon reducing furnace and opens furnace.
Preferably, trichlorosilane is passed through into the polycrystalline silicon reducing furnace of furnace to be opened method particularly includes:
Trichlorosilane is heated using the high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace；Make again
Trichlorosilane is heated with the reaction end gas of neighbouring polycrystalline silicon reducing furnace, is passed through three into the polycrystalline silicon reducing furnace of furnace to be opened
Chlorine hydrogen silicon.
Preferably, trichlorosilane is heated using the reaction end gas of neighbouring polycrystalline silicon reducing furnace, the trichlorine hydrogen after heating
The temperature of silicon is identical as the temperature for the hydrogen for entering polycrystalline silicon reducing furnace.
Embodiment 7
As shown in Fig. 2, the present embodiment provides a kind of devices for producing polysilicon, comprising:
Refining trichlorosilane holding vessel 1, for storing refining trichlorosilane；
Trichlorosilane preliminary heater 2 is connect with refining trichlorosilane holding vessel 1, and trichlorosilane preliminary heater 2 is used for
The high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace and/or itself polycrystalline silicon reducing furnace 8 is passed through to trichlorine hydrogen
Silicon carries out primary preheating；
Trichlorosilane middle rank heater 3, connect with trichlorosilane preliminary heater 2, and trichlorosilane middle rank heater 3 is used for
The reaction end gas for being passed through neighbouring polycrystalline silicon reducing furnace carries out intermediate heating to the trichlorosilane by primary preheating；
Hydrogen preliminary heater 4, for being passed through being used for for neighbouring polycrystalline silicon reducing furnace and/or itself polycrystalline silicon reducing furnace 8
The high-pressure water heating of its cooling furnace tube carries out primary preheating to hydrogen；
Hydrogen middle rank heater 5, connect with hydrogen preliminary heater 4, and hydrogen middle rank heater 5 is used to be passed through neighbouring more
The reaction end gas of crystal silicon reduction furnace carries out intermediate heating to the hydrogen by primary preheating；
Mixer 6 is connect with trichlorosilane middle rank heater 3, hydrogen middle rank heater 5 respectively, and mixer 6 is used for will
Trichlorosilane by middle rank heating and the hydrogen mixing by middle rank heating, obtain gaseous mixture；
Feed heater 7 is connect with mixer 6, and feed heater 7 is used to be passed through the reaction of itself polycrystalline silicon reducing furnace 8
Tail gas carries out charging heating to gaseous mixture；
Polycrystalline silicon reducing furnace 8 is connect with feed heater 7, and polycrystalline silicon reducing furnace 8 is used for the polycrystalline reduction to furnace to be opened
It is passed through 390 DEG C of hydrogen in furnace 8 to be replaced, the silicon core 9 in polycrystalline silicon reducing furnace 8 is preheated by hydrogen, is squeezed into
The voltage of 2000V carries out silicon core 9 and punctures；Polycrystalline silicon reducing furnace 8 is also used to open furnace, production polysilicon.
The present embodiment also provides a kind of method for producing polysilicon using the device of above-mentioned production polysilicon, including following
Step:
Furnace method is opened by the polycrystalline silicon reducing furnace 8 in embodiment 5 to carry out opening furnace；
The electric current for passing through silicon core 9 by being promoted, is promoted to 1100 DEG C for 9 temperature of silicon core, passes through above-mentioned production polysilicon
Device is passed through hydrogen, trichlorosilane into polycrystalline silicon reducing furnace 8, carries out chemical vapour deposition reaction, deposits and gives birth on 9 surface of silicon core
Produce polysilicon.
125~130 DEG C of the high-pressure water heating of the 0.7~0.8MPa come from flash zone conveying, into polycrystalline silicon reducing furnace 8
Furnace tube exchanges heat with polycrystalline silicon reducing furnace 8, and the temperature of the high-pressure water heating after heat exchange is 155~160 DEG C, also from 9 polysilicons
It is pre- into hydrogen preheater, trichlorosilane after former furnace 8 come out 155~160 DEG C, the mixing of the high-pressure water heating of 0.7~0.8MPa
Hot device, after exchanging heat, the temperature of high-pressure water heating is down to 125~130 DEG C, is delivered to flash zone, is recycled.
Preferably, hydrogen, trichlorosilane are passed through into polycrystalline silicon reducing furnace 8 method particularly includes:
Hydrogen is passed through into neighbouring polycrystalline silicon reducing furnace and/or itself polycrystalline silicon reducing furnace 8 by hydrogen preliminary heater 4
High-pressure water heating for cooling down its furnace tube carries out primary preheating, specifically, hydrogen is passed through hydrogen preliminary heater 4 in the present embodiment
Tube side, the high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace is passed through the shell side of hydrogen preliminary heater 4,
It is certainly not limited to this.The temperature of the high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace is 155~160 DEG C,
Pressure is 0.7~0.8MPa, and hydrogen is 140~150 DEG C by the temperature after primary preheating.Pass through hydrogen middle rank heater 5 again
Hydrogen is subjected to intermediate heating by the reaction end gas of neighbouring polycrystalline silicon reducing furnace, specifically, hydrogen is passed through in the present embodiment
The tube side of hydrogen middle rank heater 5, the reaction end gas of neighbouring polycrystalline silicon reducing furnace are passed through the shell side of hydrogen middle rank heater 5,
It is certainly not limited to this.The temperature of the reaction end gas of neighbouring polycrystalline silicon reducing furnace is 500~550 DEG C, and hydrogen is added by middle rank
Temperature after heat is 380~400 DEG C.The temperature of the high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace is lower to be
155~160 DEG C, primary preheating is carried out to hydrogen, as the first order energy；The reaction end gas of neighbouring polycrystalline silicon reducing furnace
More a height of 500~550 DEG C of temperature, intermediate heating is carried out to hydrogen, as the second level energy；It can make neighbouring polycrystalline
The heat of the reaction end gas of the high-pressure water heating and neighbouring polycrystalline silicon reducing furnace for cooling down its furnace tube of Si reduction furnace obtains
It utilizes, to substantially increase the utilization rate of energy.
Refining trichlorosilane in refining trichlorosilane holding vessel 1 is passed into trichlorosilane preliminary heater 2, passes through three
Chlorine hydrogen silicon preliminary heater 2 by trichlorosilane pass through neighbouring polycrystalline silicon reducing furnace and/or itself polycrystalline silicon reducing furnace 8 be used for it is cold
But the high-pressure water heating of its furnace tube carries out primary preheating, specifically, trichlorosilane is passed through the preheating of trichlorosilane primary in the present embodiment
The high-pressure water heating for cooling down its furnace tube of the tube side of device 2, neighbouring polycrystalline silicon reducing furnace is passed through trichlorosilane preliminary heater 2
Shell side is certainly not limited to this.The temperature of the high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace is 155~
160 DEG C, pressure is 0.7~0.8MPa, and trichlorosilane is 140~150 DEG C by the temperature after primary preheating.Pass through trichlorine again
The reaction end gas of neighbouring polycrystalline silicon reducing furnace is carried out intermediate heating by hydrogen silicon middle rank heater 3, specifically, three in the present embodiment
Chlorine hydrogen silicon is passed through the tube side of trichlorosilane middle rank heater 3, and the reaction end gas of neighbouring polycrystalline silicon reducing furnace is passed through trichlorosilane
The shell side of intermediate heater 3, is certainly not limited to this.The temperature of the reaction end gas of neighbouring polycrystalline silicon reducing furnace is 500~550
DEG C, trichlorosilane is 380~400 DEG C by the temperature after middle rank heating.Neighbouring polycrystalline silicon reducing furnace is used to cool down its furnace tube
High-pressure water heating temperature it is lower be 155~160 DEG C, primary preheating is carried out to trichlorosilane, as the first order energy；It is adjacent
More a height of 500~550 DEG C of the temperature of the reaction end gas of close polycrystalline silicon reducing furnace, intermediate heating is carried out to trichlorosilane, is made
For the second level energy；It can make the high-pressure water heating and neighbouring polycrystalline for being used to cool down its furnace tube of neighbouring polycrystalline silicon reducing furnace
The heat of the reaction end gas of Si reduction furnace is utilized, to substantially increase the utilization rate of energy.
The trichlorosilane of the hydrogen of middle rank heating and middle rank heating is each led into and is mixed to get gaseous mixture in gaseous mixture,
Gaseous mixture is passed into feed heater 7 again, charging heating is carried out by the reaction end gas of itself polycrystalline silicon reducing furnace 8, specifically
, gaseous mixture is passed into the tube side of feed heater 7 in the present embodiment, the reaction end gas of itself polycrystalline silicon reducing furnace 8 be passed through into
The shell side for expecting heater 7, is certainly not limited to this.The temperature of the reaction end gas of itself polycrystalline silicon reducing furnace 8 is 500~550 DEG C,
Gaseous mixture is 420~450 DEG C by the temperature after charging heating, and the gaseous mixture after charging heating is passed into polycrystalline silicon reducing furnace
In 8.
Meanwhile the method for the production polysilicon in the present embodiment will produce generate after polycrystalline reduction reaction it is a large amount of remaining
Heat, 80% heat is used to heat will be into hydrogen, the trichlorosilane of polycrystalline silicon reducing furnace 8, and only 20% heat is to hot high pressure
Water transport, therefore heat utilization rate is very high, can control the feeding temperature of gaseous mixture to 420~450 DEG C, therefore polysilicon is also
9 electric current of silicon core can be greatly reduced in former furnace 8, also can control the reaction temperature under equal conditions.Because gaseous mixture feeding temperature reaches 420
~450 DEG C, 200 DEG C compared with the traditional forms of enterprises are higher by about 250 DEG C, therefore thermal field more evenly, more fill by reaction in polycrystalline silicon reducing furnace 8
Point, the heating time of cold material, hydrogen is reduced, the reaction time is extended, therefore the production polysilicon in polycrystalline silicon reducing furnace 8
One time conversion ratio is promoted, polysilicon yield Synchronous lifting.Simultaneously as after feeding temperature is promoted, it is warm with reacting for silicon core 9
Degree difference reduce, caused by can reducing due to temperature difference fall stick.
And in the production of conventional multi-crystalline silicon enterprise, a large amount of waste heats generated after the reduction reaction of polysilicon are produced, only 30% time
Heating feeding temperature is closed at, 70% thermal energy is used to exchange heat with high-pressure water heating, therefore the energy of current domestic production of polysilicon enterprise
Consumption is high, and reduction power consumption can be greatly reduced in the device of the production polysilicon in the present embodiment, and reduction power consumption is more at home
In crystal silicon manufacturing enterprise, accounts for total power consumption ratio and reach 65%, therefore is comparable using the device of the production polysilicon in the present embodiment
Conventional apparatus power consumption decline 30%~36%.
The high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace refers at least two neighbours in the present embodiment
Nearly polycrystalline silicon reducing furnace for cooling down the high-pressure water heating of its furnace tube, the reaction end gas of neighbouring polycrystalline silicon reducing furnace refer to
The reaction end gas of few two neighbouring polycrystalline silicon reducing furnaces.Specifically, the polycrystalline silicon reducing furnace 8 in the present embodiment is 1# polycrystalline
Si reduction furnace 8, neighbouring polycrystalline silicon reducing furnace are 2#~9# polycrystalline silicon reducing furnace 8 (totally 8), altogether 9 polycrystalline silicon reducing furnaces, 9
Platform polycrystalline silicon reducing furnace shares trichlorosilane preliminary heater 2, trichlorosilane middle rank heater 3 heats trichlorosilane, shares
Hydrogen preliminary heater 4, hydrogen middle rank heater 5 heat hydrogen, then will be after the heating of trichlorosilane middle rank heater 3
Trichlorosilane distributes to the respective mixer 6 of 1#~9# polycrystalline silicon reducing furnace, and will be after the heating of hydrogen middle rank heater 5
Hydrogen distribute to the respective mixer 6 of 1#~9# polycrystalline silicon reducing furnace, hydrogen and trichlorosilane are in 1#~9# polycrystalline reduction
It mixes, is entered back into the respective feed heater 7 of 1#~9# polycrystalline silicon reducing furnace in the respective mixer 6 of furnace.That is, this implementation
Every polycrystalline silicon reducing furnace is respectively correspondingly arranged a mixer 6 for mixing in example, and a feed heater 7 is for feeding
Heating.
The device of production polysilicon in the present embodiment is using centralized heat exchange mode, by the tail of more polycrystalline silicon reducing furnaces
After gas collects, concentrate the production in being different from the prior art into hydrogen middle rank heater 5, trichlorosilane middle rank heater 3 more
The corresponding 1 set of heating device of every polycrystalline silicon reducing furnace of the device of crystal silicon, no common heating device, to greatly reduce
It is heated using trichlorosilane preliminary heater 2, trichlorosilane middle rank heater 3, trichlorosilane middle rank heater 3, hydrogen middle rank
The quantity of device 5, thus reduce equipment investment, and the device heat loss of the production polysilicon in the present embodiment is smaller, heat utilization
Rate is higher, it is easier to manage.The device of production polysilicon in the present embodiment
Preferably, using hydrogen as the carrier gas of trichlorosilane, by neighbouring polycrystalline silicon reducing furnace for cooling down its furnace
The high-pressure water heating of cylinder carries out primary preheating, again by the intermediate heating of reaction end gas progress of neighbouring polycrystalline silicon reducing furnace, then with
The trichlorosilane of middle rank heating is mixed to get gaseous mixture.Specifically, in the present embodiment, the hydrogen come from exhaust gas processing device, one
Part enters refining trichlorosilane holding vessel 1, by refining trichlorosilane holding vessel 1 boost in pressure to 1.2~1.3MPa, thus
Power source is formed, carrier gas hydrogen makes refining trichlorosilane constantly be delivered to subsequent trichlorosilane preliminary heater 2.
The device of production polysilicon in through this embodiment has the following beneficial effects: come the method for producing polysilicon
1) through this embodiment in production polysilicon device, can will enter polycrystalline silicon reducing furnace 8 hydrogen, trichlorine hydrogen
Silicon temperature is promoted to 420~450 DEG C by 160~180 DEG C, a conversion ratio of polycrystalline silicon reducing furnace 8 can be promoted, by existing skill
10.0~10.5% of the traditional forms of enterprises in art are promoted to 11.5~12.0%, and under equal conditions, it is siliceous can to increase production polycrystalline every year
Amount 18~20%.
2) through this embodiment in production polysilicon device, the electric consumption of polycrystalline silicon reducing furnace 8 can be greatly decreased, by
Average 53~55 degree of electricity/kilogram silicon of the traditional forms of enterprises in the prior art, drop to 35~38 degree of electricity/kilogram silicon hereinafter, electricity consumption
Consumption decline 30~36%.
3) compared with the existing technology in the traditional forms of enterprises use 5500~6000V voltage breakdown silicon core 9, in the present embodiment
Polycrystalline silicon reducing furnace 8 in silicon core 9 by voltage breakdown when, breakdown applied voltage 2000V made due to the decline of breakdown voltage
Insulating element and 40%~50% or more electrical component damage probability decline.And breakdown is more efficient, by the breakdown of the traditional forms of enterprises
It is 1.0~1.2 hours time-consuming, it drops to 30~40 minutes, and realize and puncture in 9 hydrogen environment of silicon core, the removing of reduction silicon core 9,
The generation of blue film.300 Ω cm can be promoted to, the prior art is reduced by 9 resistivity of silicon core used by 100 Ω cm of <
Ensure that silicon core punctures to reduce silicon core resistivity, and the phosphorus impurities mixed, it is more excellent to polysilicon quality.
4) the device intake air temperature by production polysilicon in this present embodiment is about 200~300 DEG C high compared with Traditional Method, therefore
Silicon rod temperature difference in intake air temperature and normal production is 200~300 DEG C small, the silicon rod ratio of falling stick as caused by temperature difference
Reduce 30~40%.
5) decline 30 compared with the device electric consumption of traditional mode of production polysilicon by the device of production polysilicon in this present embodiment
~36% or more, therefore demand current is smaller, can by the polycrystalline silicon reducing furnace 8 of traditional same type, current transmission by 2200~
2500A, drops to 1500A hereinafter, cable, the bronze medal that power transmission uses may be selected smaller number, expense of reducing investment outlay, therefore
Barrier rate is lower, needs transformer capacity smaller.
6) centralized management is used by the device of production polysilicon in this present embodiment, is different from every of the traditional forms of enterprises
Reduction furnace is equipped with 1 set of heat-exchanger rig, and the device of this production polysilicon greatly reduces the quantity of equipment, and when heat exchange, most of
Heat exchanger does not need hot water participation, and having does not influence to continue to produce when slight damage, and the device compared to traditional mode of production polysilicon is very big
Optimization, the device of every set production polysilicon can reduce inspection, operation, more than 4 people of maintenance personnel.New polysilicon enterprise is building
When, 20,000,000 yuan/ten thousand tons silicon can be at least saved, equipment investment is reduced.
Silicon core breakdown method in the present embodiment can puncture the silicon core of the resistivity of 300 Ω cm, then do not need p-doped, because
This, can reduce polycrystalline silicon rod product phosphorus content 100ppt, and product silicon rod entirety grade promotes a grade, i.e., by solar energy spy
Grade product are promoted to electron level, therefore quality is promoted by a relatively large margin.
In the present embodiment, it will not need to carry out p-doped process to silicon core, therefore polycrystalline silicon rod product phosphorus can be reduced
Content 100ppt, resistivity promotes 150 Ω cm, therefore production polysilicon product quality is more excellent, is that polysilicon enterprise is extensive
Production electronic grade product creates good condition.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, however the present invention is not limited thereto.For those skilled in the art, essence of the invention is not being departed from
In the case where mind and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.
Claims (14)
1. a kind of silicon core breakdown method that polycrystalline silicon reducing furnace opens furnace, which comprises the following steps:
It is passed through non-oxidizing gas displacement into the polycrystalline silicon reducing furnace of furnace to be opened, then is passed through 380~400 DEG C of hydrogen and is set
It changes, the silicon core in polycrystalline silicon reducing furnace is preheated by hydrogen；
It squeezes into voltage and carries out the breakdown of silicon core.
2. the silicon core breakdown method that polycrystalline silicon reducing furnace according to claim 1 opens furnace, which is characterized in that the voltage is
2000~6000V.
3. the silicon core breakdown method that polycrystalline silicon reducing furnace according to claim 2 opens furnace, which is characterized in that the voltage is
2000~3000V.
4. the silicon core breakdown method that polycrystalline silicon reducing furnace according to claim 1 opens furnace, which is characterized in that set by hydrogen
It changes, the pressure in the polycrystalline silicon reducing furnace of the furnace to be opened is 20~100KPa.
5. the silicon core breakdown method that polycrystalline silicon reducing furnace according to claim 1 opens furnace, which is characterized in that described to wait open
380~400 DEG C of hydrogen is passed through in the polycrystalline silicon reducing furnace of furnace method particularly includes:
Hydrogen is heated using the high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace；It reuses neighbouring more
The reaction end gas of crystal silicon reduction furnace heats hydrogen, and hydrogen is heated to 380~400 DEG C, to furnace to be opened polysilicon also
Hydrogen is passed through in former furnace.
6. a kind of polycrystalline silicon reducing furnace opens furnace method, which comprises the following steps:
By method described in Claims 1 to 5 any one, the silicon core treated in the polycrystalline silicon reducing furnace for opening furnace carries out silicon core
Breakdown；
Hydrogen sky is burnt；
It is passed through hydrogen, trichlorosilane into the polycrystalline silicon reducing furnace of furnace to be opened, chemical vapour deposition reaction is carried out, in silicon wicking surface
Deposition production polysilicon, completes polycrystalline silicon reducing furnace and opens furnace.
7. polycrystalline silicon reducing furnace according to claim 6 opens furnace method, which is characterized in that the polysilicon to furnace to be opened
Trichlorosilane is passed through in reduction furnace method particularly includes:
Trichlorosilane is heated using the high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace；Reuse neighbour
The reaction end gas of nearly polycrystalline silicon reducing furnace heats trichlorosilane, and trichlorine hydrogen is passed through into the polycrystalline silicon reducing furnace of furnace to be opened
Silicon.
8. polycrystalline silicon reducing furnace according to claim 7 opens furnace method, which is characterized in that use neighbouring polycrystalline silicon reducing furnace
Reaction end gas trichlorosilane is heated to 380~400 DEG C.
9. a kind of method for producing polysilicon, which comprises the following steps:
Furnace method is opened by polycrystalline silicon reducing furnace described in claim 6~8 any one to carry out opening furnace；
It is passed through hydrogen, trichlorosilane into polycrystalline silicon reducing furnace, carries out chemical vapour deposition reaction, deposits and produces in silicon wicking surface
Polysilicon.
10. producing the method for polysilicon according to claim 9, which is characterized in that described to be passed through into polycrystalline silicon reducing furnace
Hydrogen, trichlorosilane method particularly includes:
Hydrogen is passed through into neighbouring polycrystalline silicon reducing furnace and/or the high-pressure water heating for being used to cool down its furnace tube of itself polycrystalline silicon reducing furnace
Carry out primary preheating, again by the intermediate heating of reaction end gas progress of neighbouring polycrystalline silicon reducing furnace；
Trichlorosilane is passed through into neighbouring polycrystalline silicon reducing furnace and/or the high pressure for being used to cool down its furnace tube of itself polycrystalline silicon reducing furnace
Hot water carries out primary preheating, again by the intermediate heating of reaction end gas progress of neighbouring polycrystalline silicon reducing furnace；
The trichlorosilane of the hydrogen of middle rank heating and middle rank heating is mixed to get gaseous mixture, then passes through itself polycrystalline silicon reducing furnace
Reaction end gas carry out charging heating, by charging heating after gaseous mixture be passed into polycrystalline silicon reducing furnace.
11. producing the method for polysilicon according to claim 10, which is characterized in that
Hydrogen is 140~150 DEG C by the temperature after primary preheating, then passing through the temperature after middle rank heating is 380~400 DEG C；
Trichlorosilane is 140~150 DEG C by the temperature after primary preheating, then passing through the temperature after middle rank heating is 380~400
℃；
Gaseous mixture is 420~450 DEG C by the temperature after charging heating.
12. producing the method for polysilicon according to claim 10, which is characterized in that being used for for neighbouring polycrystalline silicon reducing furnace is cold
But the temperature of the high-pressure water heating of its furnace tube is 155~160 DEG C, and pressure is 0.7~0.8MPa；Neighbouring polycrystalline silicon reducing furnace it is anti-
The temperature for answering tail gas is 500~550 DEG C；The temperature of the reaction end gas of itself polycrystalline silicon reducing furnace is 500~550 DEG C.
13. producing the method for polysilicon according to claim 10, which is characterized in that using hydrogen as the load of trichlorosilane
Gas carries out primary preheating by the high-pressure water heating for cooling down its furnace tube of neighbouring polycrystalline silicon reducing furnace, again by neighbouring more
The reaction end gas of crystal silicon reduction furnace carries out intermediate heating, then is mixed to get gaseous mixture with the trichlorosilane of middle rank heating.
14. the device that polysilicon is produced used in the method for polysilicon is produced described in a kind of claim 9~13 any one,
It is characterised by comprising:
Trichlorosilane preliminary heater, for be passed through neighbouring polycrystalline silicon reducing furnace and/or itself polycrystalline silicon reducing furnace for cold
But the high-pressure water heating of its furnace tube carries out primary preheating to the trichlorosilane for being passed through trichlorosilane preliminary heater；
Trichlorosilane middle rank heater is connect with the trichlorosilane preliminary heater, and the trichlorosilane middle rank heater is used
In the reaction end gas for being passed through neighbouring polycrystalline silicon reducing furnace, to three by primary preheating for being passed through trichlorosilane middle rank heater
Chlorine hydrogen silicon carries out intermediate heating；
Hydrogen preliminary heater, for be passed through neighbouring polycrystalline silicon reducing furnace and/or itself polycrystalline silicon reducing furnace for cooling down it
The high-pressure water heating of furnace tube carries out primary preheating to the hydrogen for being passed through hydrogen preliminary heater；
Hydrogen middle rank heater is connect with the hydrogen preliminary heater, and the hydrogen middle rank heater is neighbouring for being passed through
The reaction end gas of polycrystalline silicon reducing furnace carries out intermediate heating to the hydrogen by primary preheating for being passed through hydrogen middle rank heater；
Mixer is connect with the trichlorosilane middle rank heater, the hydrogen middle rank heater respectively, and the mixer is used for
Trichlorosilane by middle rank heating and the hydrogen by middle rank heating are mixed, gaseous mixture is obtained；
Feed heater is connect with the mixer, and the feed heater is used to be passed through the reaction of itself polycrystalline silicon reducing furnace
Tail gas carries out charging heating to the gaseous mixture for being passed through feed heater；
Polycrystalline silicon reducing furnace is connect with the feed heater, the polycrystalline silicon reducing furnace be used for furnace to be opened polysilicon also
It is passed through 380~400 DEG C of hydrogen in former furnace to be replaced, the silicon core in polycrystalline silicon reducing furnace is preheated by hydrogen,
It squeezes into voltage and carries out the breakdown of silicon core；The polycrystalline silicon reducing furnace is also used to open furnace, production polysilicon.
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| CN110451511A (en) * | 2019-08-26 | 2019-11-15 | 洛阳中硅高科技有限公司 | Polycrystalline silicon reducing furnace and its open furnace method |
| 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 |
| CN113264528A (en) * | 2021-04-15 | 2021-08-17 | 江苏鑫华半导体材料科技有限公司 | Method for producing electronic grade polycrystalline silicon |
| CN113955758A (en) * | 2021-11-25 | 2022-01-21 | 新疆大全新能源股份有限公司 | Control method for preventing silicon core from peeling in polycrystalline silicon production |
| CN114014322A (en) * | 2021-11-30 | 2022-02-08 | 江苏鑫华半导体材料科技有限公司 | Method for improving purity of polycrystalline silicon |
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