CN106276913B - The method that polysilicon is manufactured after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas - Google Patents
The method that polysilicon is manufactured after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas Download PDFInfo
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- C01B33/00—Silicon; Compounds thereof
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- 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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Abstract
The method that polysilicon is manufactured after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas, it is related to the method for improved Siemens production polysilicon.The present invention solves existing improved Siemens production of polysilicon condition by thermodynamic (al) limitation, the problem of high energy consumption, conversion efficiency are low, production cost is high be present.Method：More polycrystalline reduction furnace apparatus are cascaded, the outlet of each polycrystalline reduction furnace apparatus connects the entrance of next polycrystalline reduction furnace apparatus using pipeline, is sequentially connected, is passed through unstrpped gas, and reduction reaction occurs in silicon wicking surface, forms polycrystalline silicon rod.Or more polycrystalline reduction furnace apparatus are cascaded, the outlet of each polycrystalline reduction furnace apparatus connects the entrance of next polycrystalline reduction furnace apparatus using pipeline, it is sequentially connected, connect the entrance of each polycrystalline reduction furnace apparatus respectively using feed supplement pipeline, obtain series devices, unstrpped gas is passed through, reduction reaction occurs in silicon wicking surface, forms polycrystalline silicon rod.
Description
Technical field
The present invention relates to the method for production polysilicon.
Background technology
Polysilicon is a kind of form of elemental crystal silicon, and it has excellent characteristic of semiconductor, in photovoltaic industry and micro- electricity
Sub-industry is widely applied, such as semiconductor devices, integrated circuit and solar battery sheet, be all by silicon materials prepare and
Into.At present, domestic and international more than 80% production of polysilicon enterprise, polysilicon is carried out using the improved Siemens of comparative maturity
Production.Its production principle is that trichlorosilane and hydrogen are passed into the polycrystalline silicon reducing furnace reaction chamber of bell-jar, at 1100 DEG C
CVD reduction chemical reactions occur for the silicon wicking surface of left and right, react the silicon wafer particle deposition of generation in silicon wicking surface so that silicon core is straight
The constantly thicker formation polycrystalline silicon rod in footpath, the polysilicon that thus method is prepared, its purity can reach 99.9999%, or even can
Up to 99.999999999%.Although improved Siemens produce, the advantages of polysilicon, is a lot, and can produce the more of high-purity
Crystal silicon product, but because improved Siemens working condition is by thermodynamic (al) limitation, high energy consumption, efficiency for a long time all be present
Low, many deficiencies such as cost is high, conversion ratio of TCS is low, it is badly in need of carrying out scrap build, production technology for problem above excellent
Change, be the emphasis of current polysilicon industry research and development.
In order to improve polysilicon yield, improve conversion ratio of TCS, reduction energy consumption, reduction production cost, most enterprises
By rationally designing the modes such as chassis of reducing furnace layout, electrode structure, jet size, optimization polysilicon production process formula come real
Now improve reduction furnace yield, reduce the purpose of energy consumption.Although this method has necessarily to improved Siemens production of polysilicon
Gain effect, but gain range is limited, and can not effectively improve conversion ratio of TCS, reduces energy consumption.Therefore, for existing
The present situation of improved Siemens production technology, it is necessary to which polysilicon yield can be greatly improved, reduce energy consumption and life by developing one kind
The process of cost is produced, increases Business Economic Benefit and the market competitiveness.
The content of the invention
The present invention is to solve existing improved Siemens production of polysilicon condition by thermodynamic (al) limitation, for a long time all
Many deficiencies such as high energy consumption, conversion efficiency be low be present, in order to solve the problems, such as the production cost of polysilicon, and provide improvement
The method that polysilicon is manufactured after the Siemens process polycrystalline silicon reduction recovered cycling and reutilization of furnace exhaust gas.
The method of polysilicon is manufactured after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas is
Carry out according to the following steps：More improved Siemens polycrystalline reduction furnace apparatus are cascaded, except last improvement
Outside Siemens process polycrystalline silicon reduction furnace apparatus, using gas piping by each improved Siemens polycrystalline reduction furnace apparatus
Offgas outlet is connected to the air inlet of next improved Siemens polycrystalline reduction furnace apparatus, is sequentially connected, and at every
Flowmeter and flow control valve are installed on gas piping, obtain series devices；Unstrpped gas is passed through to the First of series devices
The air inlet of improved Siemens polycrystalline reduction furnace apparatus, in improved Siemens process polycrystalline silicon reduction furnace equipment chassis
The nozzle arrangements of even distribution, the reduction intracavitary portion of improved Siemens polycrystalline reduction furnace apparatus is injected into, in the silicon of high temperature
Chemical vapor deposition reduction reaction occurs for wicking surface, and the silicon wafer particulate of reduction reaction generation will fully adsorb deposition on silicon core,
Gradually form polycrystalline silicon rod；More described improved Siemens polycrystalline silicon reducing furnace number of devices are N, and 10 >=N >=2, N is just
Integer；
And each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, exchanged heat using gas-gas
Device makes the gas and the improved Siemens polycrystalline reduction furnace apparatus tail into improved Siemens polycrystalline reduction furnace apparatus
The tail gas of gas outlet is exchanged heat, and control enters gas into the improved Siemens polycrystalline reduction furnace apparatus air inlet
Temperature is 140 DEG C~160 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improvement Siemens
Temperature control of the tail gas of method polycrystalline silicon reducing furnace equipment offgas outlet after gas-to-gas heat exchanger exchanges heat is 80 DEG C~110 DEG C；
Or each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, exchanged heat using gas-gas
Device makes the gas and the improved Siemens polycrystalline reduction furnace apparatus tail into improved Siemens polycrystalline reduction furnace apparatus
The tail gas of gas outlet is exchanged heat, and control enters gas into the improved Siemens polycrystalline reduction furnace apparatus air inlet
Temperature is 200 DEG C~300 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improvement Siemens
Temperature control of the tail gas of method polycrystalline silicon reducing furnace equipment offgas outlet after gas-to-gas heat exchanger exchanges heat is 100 DEG C~200
℃；
Or in addition to last improved Siemens polycrystalline reduction furnace apparatus, each improved Siemens polysilicon is also
One gas-to-gas heat exchanger of former furnace apparatus series connection, makes to enter improved Siemens polycrystalline reduction furnace apparatus using gas-to-gas heat exchanger
The tail gas of gas and the improved Siemens polycrystalline reduction furnace apparatus offgas outlet exchanged heat, control enters improvement west
The gas temperature that enters of Men Zifa polycrystalline silicon reducing furnace equipment air inlets is 200 DEG C~300 DEG C；Except two improvement west gate reciprocal
Outside sub- method polycrystalline silicon reducing furnace equipment, the tail gas of each improved Siemens polycrystalline reduction furnace apparatus offgas outlet passes through
Temperature control after gas-to-gas heat exchanger heat exchange is 100 DEG C~200 DEG C, second from the bottom improved Siemens polycrystalline silicon reducing furnace
Temperature control of the tail gas of equipment offgas outlet after gas-to-gas heat exchanger exchanges heat is 200 DEG C~300 DEG C；
Series devices are more from First improved Siemens polycrystalline reduction furnace apparatus to a last improved Siemens
Silicon core quantity built in crystal silicon reduction furnace apparatus is successively decreased；When more improved Siemens polycrystalline silicon reducing furnace number of devices are N, and 10
During >=N ＞ 2, described silicon core quantity is ni, then ni-1-ni≤ni-2-ni-1, wherein niIt is i-th improved Siemens polysilicon
Reduce the quantity of silicon core built in furnace apparatus；It is described as more improved Siemens polycrystalline silicon reducing furnace number of devices N=2
Silicon core quantity is n1And n2, n1＞ n2≥1/3n1, wherein n1It is silicon built in First improved Siemens polycrystalline reduction furnace apparatus
The quantity of core, n2It is the quantity of silicon core built in second improved Siemens polycrystalline reduction furnace apparatus；
The described raw material gas flow being passed through in improved Siemens polycrystalline reduction furnace apparatus is Q, thenWherein QiIt is that i-th improved Siemens polycrystalline reduction furnace apparatus is independent mould
The gas flow needed during formula, N are the quantity for the improved Siemens polycrystalline reduction furnace apparatus being connected in series.
The method of polysilicon is manufactured after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas is
Carry out according to the following steps：More improved Siemens polycrystalline reduction furnace apparatus are cascaded, except last improvement
Outside Siemens process polycrystalline silicon reduction furnace apparatus, using gas piping by each improved Siemens polycrystalline reduction furnace apparatus
Offgas outlet is connected with the air inlet of next improved Siemens polycrystalline reduction furnace apparatus, is sequentially connected, and every
Flowmeter and flow control valve are installed on individual gas piping, and in addition to First improved Siemens polycrystalline reduction furnace apparatus,
It is connected using air inlet of multiple feed supplement gas pipings successively with each improved Siemens polycrystalline reduction furnace apparatus,
Flowmeter and flow control valve are installed on each feed supplement gas piping, obtain series devices；Unstrpped gas is passed through into series connection to set
The air inlet of standby First improved Siemens polycrystalline reduction furnace apparatus, and changed by feed supplement gas piping to each
Good Siemens process polycrystalline silicon reduction furnace apparatus supplement unstrpped gas, in improved Siemens process polycrystalline silicon chassis of reducing furnace equipment
The nozzle arrangements of even distribution, the reduction intracavitary portion of improved Siemens polycrystalline reduction furnace apparatus is injected into, in the silicon of high temperature
Chemical vapor deposition reduction reaction occurs for wicking surface, and the silicon wafer particulate of reduction reaction generation will fully adsorb deposition on silicon core,
Gradually form polycrystalline silicon rod；More described improved Siemens polycrystalline silicon reducing furnace number of devices are N, and 10 >=N >=2, N is just
Integer；
And each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, exchanged heat using gas-gas
Device makes the gas and the improved Siemens polycrystalline reduction furnace apparatus tail into improved Siemens polycrystalline reduction furnace apparatus
The tail gas of gas outlet is exchanged heat, and control enters gas into the improved Siemens polycrystalline reduction furnace apparatus air inlet
Temperature is 140 DEG C~160 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improvement Siemens
Temperature control of the tail gas of method polycrystalline silicon reducing furnace equipment offgas outlet after gas-to-gas heat exchanger exchanges heat is 80 DEG C~110 DEG C；
Or each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, exchanged heat using gas-gas
Device makes the gas and the improved Siemens polycrystalline reduction furnace apparatus tail into improved Siemens polycrystalline reduction furnace apparatus
The tail gas of gas outlet is exchanged heat, and control enters gas into the improved Siemens polycrystalline reduction furnace apparatus air inlet
Temperature is 200 DEG C~300 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improvement Siemens
Temperature control of the tail gas of method polycrystalline silicon reducing furnace equipment offgas outlet after gas-to-gas heat exchanger exchanges heat is 100 DEG C~200
℃；
Series devices are more from First improved Siemens polycrystalline reduction furnace apparatus to a last improved Siemens
Silicon core quantity built in crystal silicon reduction furnace apparatus is successively decreased；When more improved Siemens polycrystalline silicon reducing furnace number of devices are N, and 10
During >=N ＞ 2, described silicon core quantity is ni, then ni-1-ni≤ni-2-ni-1, wherein niIt is i-th improved Siemens polysilicon
Reduce the quantity of silicon core built in furnace apparatus；It is described when more improved Siemens polycrystalline silicon reducing furnace number of devices are N=2
Silicon core quantity be n1And n2, n1＞ n2≥1/3n1, wherein n1It is built in First improved Siemens polycrystalline reduction furnace apparatus
The quantity of silicon core, n2It is the quantity of silicon core built in second improved Siemens polycrystalline reduction furnace apparatus；
The described raw material gas flow for being passed through improved Siemens polycrystalline reduction furnace apparatus is Q, thenWherein QiIt is that i-th improved Siemens polycrystalline reduction furnace apparatus is independent mould
The gas flow needed during formula, N are the quantity for the improved Siemens polycrystalline reduction furnace apparatus being connected in series；
Described supplement unstrpped gas is Qb, Qi≥Qbi>=0, wherein QiIt is i-th improved Siemens polycrystalline silicon reducing furnace
The gas flow that equipment needs when being independent pattern, QbiIt is i-th improved Siemens polycrystalline reduction furnace apparatus supplement raw material
Gas flow.
Advantages of the present invention：Process proposed by the present invention and traditional separate unit improved Siemens polycrystalline silicon reducing furnace
The ability of individually producing is compared, and gain effect is notable.By flowing of the unstrpped gas in more polycrystalline silicon reducing furnaces, add into
Expect flowing velocity, flow strength and residence time of each reactant inside reduction furnace in gas, the one of TCS can be significantly improved
Secondary conversion ratio.Meanwhile the charge flow rate of increase makes reduction furnace internal gas flow field more uniform and stable, avoids independent reduction furnace
The gas flow fluctuation occurred during production reduces the situation of deposition efficiency, is more uniformly distributed polysilicon deposition, is fine and close, effectively improving
Polysilicon yield.By the direct utilization to reduction furnace higher temperature tail gas, the energy consumption in production process is significantly reduced, is saved
The about cost of tail gas separation purification process.In addition, more improved Siemens polycrystalline silicon reducing furnace series connection and identical quantity
Separate unit improved Siemens polycrystalline silicon reducing furnace, which individually produces, to be compared, and can be saved the substantial amounts of production time, improves enterprise
Prouctiveness, be more beneficial for efficient industrial production.
Brief description of the drawings
Fig. 1 is the structural representation of series devices in embodiment one；
Fig. 2 is the structural representation of series devices in embodiment three；
Fig. 3 is the structural representation of series devices in example IV.
Embodiment
Embodiment one：Present embodiment is that the recovered circulation of improved Siemens polysilicon reducing furnace tail gas is sharp again
Carried out according to the following steps with the method for rear manufacturing polysilicon：By more improved Siemens polycrystalline reduction furnace apparatus
It is cascaded, in addition to last improved Siemens polycrystalline reduction furnace apparatus, is improved each using gas piping
The offgas outlet of Siemens process polycrystalline silicon reduction furnace apparatus is connected to next improved Siemens polycrystalline reduction furnace apparatus
Air inlet, it is sequentially connected, and flowmeter and flow control valve is installed on every gas piping, obtains series devices；By original
Material gas is passed through the air inlet of the First improved Siemens polycrystalline reduction furnace apparatus of series devices, improved Siemens
Equally distributed nozzle arrangements in method polycrystalline silicon reducing furnace equipment chassis, it is injected into improved Siemens polycrystalline silicon reducing furnace and sets
Standby reduction intracavitary portion, chemical vapor deposition reduction reaction occurs in the silicon wicking surface of high temperature, the silicon wafer of reduction reaction generation is micro-
Grain will fully adsorb deposition on silicon core, gradually form polycrystalline silicon rod；More described improved Siemens polycrystalline silicon reducing furnaces
Number of devices is N, and 10 >=N >=2, N are positive integer；
And each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, exchanged heat using gas-gas
Device makes the gas and the improved Siemens polycrystalline reduction furnace apparatus tail into improved Siemens polycrystalline reduction furnace apparatus
The tail gas of gas outlet is exchanged heat, and control enters gas into the improved Siemens polycrystalline reduction furnace apparatus air inlet
Temperature is 140 DEG C~160 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improvement Siemens
Temperature control of the tail gas of method polycrystalline silicon reducing furnace equipment offgas outlet after gas-to-gas heat exchanger exchanges heat is 80 DEG C~110 DEG C；
Or each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, exchanged heat using gas-gas
Device makes the gas and the improved Siemens polycrystalline reduction furnace apparatus tail into improved Siemens polycrystalline reduction furnace apparatus
The tail gas of gas outlet is exchanged heat, and control enters gas into the improved Siemens polycrystalline reduction furnace apparatus air inlet
Temperature is 200 DEG C~300 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improvement Siemens
Temperature control of the tail gas of method polycrystalline silicon reducing furnace equipment offgas outlet after gas-to-gas heat exchanger exchanges heat is 100 DEG C~200
℃；
Or in addition to last improved Siemens polycrystalline reduction furnace apparatus, each improved Siemens polysilicon is also
One gas-to-gas heat exchanger of former furnace apparatus series connection, makes to enter improved Siemens polycrystalline reduction furnace apparatus using gas-to-gas heat exchanger
The tail gas of gas and the improved Siemens polycrystalline reduction furnace apparatus offgas outlet exchanged heat, control enters improvement west
The gas temperature that enters of Men Zifa polycrystalline silicon reducing furnace equipment air inlets is 200 DEG C~300 DEG C；Except two improvement west gate reciprocal
Outside sub- method polycrystalline silicon reducing furnace equipment, the tail gas of each improved Siemens polycrystalline reduction furnace apparatus offgas outlet passes through
Temperature control after gas-to-gas heat exchanger heat exchange is 100 DEG C~200 DEG C, second from the bottom improved Siemens polycrystalline silicon reducing furnace
Temperature control of the tail gas of equipment offgas outlet after gas-to-gas heat exchanger exchanges heat is 200 DEG C~300 DEG C；
Series devices are more from First improved Siemens polycrystalline reduction furnace apparatus to a last improved Siemens
Silicon core quantity built in crystal silicon reduction furnace apparatus is successively decreased；When more improved Siemens polycrystalline silicon reducing furnace number of devices are N, and 10
During >=N ＞ 2, described silicon core quantity is ni, then ni-1-ni≤ni-2-ni-1, wherein niIt is i-th improved Siemens polysilicon
Reduce the quantity of silicon core built in furnace apparatus；It is described as more improved Siemens polycrystalline silicon reducing furnace number of devices N=2
Silicon core quantity is n1And n2, n1＞ n2≥1/3n1, wherein n1It is silicon built in First improved Siemens polycrystalline reduction furnace apparatus
The quantity of core, n2It is the quantity of silicon core built in second improved Siemens polycrystalline reduction furnace apparatus；
The described raw material gas flow being passed through in improved Siemens polycrystalline reduction furnace apparatus is Q, thenWherein QiIt is that i-th improved Siemens polycrystalline reduction furnace apparatus is independent mould
The gas flow needed during formula, N are the quantity for the improved Siemens polycrystalline reduction furnace apparatus being connected in series.
The advantages of present embodiment：The process that present embodiment proposes and traditional separate unit improvement west gate
Sub- method polycrystalline silicon reducing furnace individually produces ability and compared, and gain effect is notable.By unstrpped gas in more polycrystalline silicon reducing furnaces
In flowing, add flowing velocity, flow strength and residence time of each reactant inside reduction furnace in feed gas, can
To significantly improve TCS conversion ratio.Meanwhile the charge flow rate of increase makes reduction furnace internal gas flow field more uniformly steady
Fixed, avoiding the gas flow fluctuation occurred during independent reduction furnace production reduces the situation of deposition efficiency, makes polysilicon deposition more
To be uniform, fine and close, polysilicon yield is effectively increased.By the direct utilization to reduction furnace higher temperature tail gas, it is greatly reduced
Energy consumption in production process, has saved the cost of tail gas separation purification process.In addition, more improved Siemens polysilicons are also
Former stove series connection can save a large amount of compared with the separate unit improved Siemens polycrystalline silicon reducing furnace of identical quantity individually produces
Production time, improve the prouctiveness of enterprise, be more beneficial for efficient industrial production.
Embodiment two：The difference of present embodiment and embodiment one is：More described improvement
Silicon core used in Siemens process polycrystalline silicon reduction furnace apparatus is circle silicon core or square silicon core.It is other identical with embodiment one.
Embodiment three：The difference of present embodiment and one of embodiment one or two is：Described
Unstrpped gas is the mixed gas of trichlorosilane, dichlorosilane and hydrogen, and wherein the mol ratio of hydrogen and trichlorosilane is (2
~4):1, and the mass percent of dichlorosilane is 4%~6% in the gross mass of trichlorosilane and dichlorosilane.It is other
It is identical with embodiment one or two.
Embodiment four：The difference of present embodiment and one of embodiment one to three is：Described
The gas piping external sheath connected between improved Siemens polycrystalline reduction furnace apparatus has insulation material.Other and specific reality
It is identical to apply mode one to three.
Embodiment five：The difference of present embodiment and one of embodiment one to four is：Described
More improved Siemens polycrystalline silicon reducing furnace number of devices are N, N=2.It is other identical with embodiment one to four.
Embodiment six：Present embodiment is that the recovered circulation of improved Siemens polysilicon reducing furnace tail gas is sharp again
Carried out according to the following steps with the method for rear manufacturing polysilicon：By more improved Siemens polycrystalline reduction furnace apparatus
It is cascaded, in addition to last improved Siemens polycrystalline reduction furnace apparatus, is improved each using gas piping
The air inlet of the offgas outlet and next improved Siemens polycrystalline reduction furnace apparatus of Siemens process polycrystalline silicon reduction furnace apparatus
Entrance is connected, and is sequentially connected, and flowmeter and flow control valve are installed on each gas piping, and except First improvement west
Outside Men Zifa polycrystalline silicon reducing furnace equipment, using multiple feed supplement gas pipings successively with each improved Siemens polysilicon also
The air inlet of former furnace apparatus is connected, and flowmeter and flow control valve are installed on each feed supplement gas piping, is connected
Equipment；Unstrpped gas is passed through to the air inlet of the First improved Siemens polycrystalline reduction furnace apparatus of series devices, and
Unstrpped gas, improved Siemens are supplemented to each improved Siemens polycrystalline reduction furnace apparatus by feed supplement gas piping
Equally distributed nozzle arrangements spray, is injected into improved Siemens polycrystalline silicon reducing furnace in method polycrystalline silicon reduction furnace base plate equipment
The reduction intracavitary portion of equipment, chemical vapor deposition reduction reaction, the silicon wafer of reduction reaction generation occurs in the silicon wicking surface of high temperature
Particulate will fully adsorb deposition on silicon core, gradually form polycrystalline silicon rod；More described improved Siemens polycrystalline reductions
Furnace apparatus quantity is N, and 10 >=N >=2, N are positive integer；
And each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, exchanged heat using gas-gas
Device makes the gas and the improved Siemens polycrystalline reduction furnace apparatus tail into improved Siemens polycrystalline reduction furnace apparatus
The tail gas of gas outlet is exchanged heat, and control enters gas into the improved Siemens polycrystalline reduction furnace apparatus air inlet
Temperature is 140 DEG C~160 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improvement Siemens
Temperature control of the tail gas of method polycrystalline silicon reducing furnace equipment offgas outlet after gas-to-gas heat exchanger exchanges heat is 80 DEG C~110 DEG C；
Or each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, exchanged heat using gas-gas
Device makes the gas and the improved Siemens polycrystalline reduction furnace apparatus tail into improved Siemens polycrystalline reduction furnace apparatus
The tail gas of gas outlet is exchanged heat, and control enters gas into the improved Siemens polycrystalline reduction furnace apparatus air inlet
Temperature is 200 DEG C~300 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improvement Siemens
Temperature control of the tail gas of method polycrystalline silicon reducing furnace equipment offgas outlet after gas-to-gas heat exchanger exchanges heat is 100 DEG C~200
℃；
Series devices are more from First improved Siemens polycrystalline reduction furnace apparatus to a last improved Siemens
Silicon core quantity built in crystal silicon reduction furnace apparatus is successively decreased；When more improved Siemens polycrystalline silicon reducing furnace number of devices are N, and 10
During >=N ＞ 2, described silicon core quantity is ni, then ni-1-ni≤ni-2-ni-1, wherein niIt is i-th improved Siemens polysilicon
Reduce the quantity of silicon core built in furnace apparatus；It is described when more improved Siemens polycrystalline silicon reducing furnace number of devices are N=2
Silicon core quantity be n1And n2, n1＞ n2≥1/3n1, wherein n1It is built in First improved Siemens polycrystalline reduction furnace apparatus
The quantity of silicon core, n2It is the quantity of silicon core built in second improved Siemens polycrystalline reduction furnace apparatus；
The described raw material gas flow for being passed through improved Siemens polycrystalline reduction furnace apparatus is Q, thenWherein QiIt is that i-th improved Siemens polycrystalline reduction furnace apparatus is independent mould
The gas flow needed during formula, N are the quantity for the improved Siemens polycrystalline reduction furnace apparatus being connected in series；
Described supplement unstrpped gas is Qb, Qi≥Qbi>=0, wherein QiIt is i-th improved Siemens polycrystalline silicon reducing furnace
The gas flow that equipment needs when being independent pattern, QbiIt is i-th improved Siemens polycrystalline reduction furnace apparatus supplement raw material
Gas flow.
The advantages of present embodiment：The process that present embodiment proposes and traditional separate unit improvement west gate
Sub- method polycrystalline silicon reducing furnace individually produces ability and compared, and gain effect is notable.By unstrpped gas in more polycrystalline silicon reducing furnaces
In flowing, add flowing velocity, flow strength and residence time of each reactant inside reduction furnace in feed gas, can
To significantly improve TCS conversion ratio.Meanwhile the charge flow rate of increase makes reduction furnace internal gas flow field more uniformly steady
Fixed, avoiding the gas flow fluctuation occurred during independent reduction furnace production reduces the situation of deposition efficiency, makes polysilicon deposition more
To be uniform, fine and close, polysilicon yield is effectively increased.By the direct utilization to reduction furnace higher temperature tail gas, it is greatly reduced
Energy consumption in production process, has saved the cost of tail gas separation purification process.In addition, more improved Siemens polysilicons are also
Former stove series connection can save a large amount of compared with the separate unit improved Siemens polycrystalline silicon reducing furnace of identical quantity individually produces
Production time, improve the prouctiveness of enterprise, be more beneficial for efficient industrial production.
Embodiment seven：The difference of present embodiment and embodiment six is：More described improvement
Silicon core used in Siemens process polycrystalline silicon reduction furnace apparatus is circle silicon core or square silicon core.It is other identical with embodiment six.
Embodiment eight：The difference of present embodiment and one of embodiment six or seven is：Described
Unstrpped gas is the mixed gas of trichlorosilane, dichlorosilane and hydrogen, and wherein the mol ratio of hydrogen and trichlorosilane is (2
~4):1, and the mass percent of dichlorosilane is 4%~6% in the gross mass of trichlorosilane and dichlorosilane.It is other
It is identical with embodiment six or seven.
Embodiment nine：The difference of present embodiment and one of embodiment six to eight is：Described
The gas piping external sheath connected between improved Siemens polycrystalline reduction furnace apparatus has insulation material.Other and specific reality
It is identical to apply mode six to eight.
Embodiment ten：The difference of present embodiment and one of embodiment six to nine is：Described
Supplement unstrpped gas is the mol ratio of the mixed gas, wherein hydrogen and trichlorosilane of trichlorosilane, dichlorosilane and hydrogen
For (2~4):1, and the mass percent of dichlorosilane is 4%~6% in the gross mass of trichlorosilane and dichlorosilane.
It is other identical with embodiment six to nine.
Using the effect of the following examples checking present invention：
Embodiment one：
The present embodiment, the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas are illustrated with reference to Fig. 1
The method for manufacturing polysilicon afterwards, step are as follows：
More improved Siemens polycrystalline reduction furnace apparatus are cascaded, except last improved Siemens is more
Outside crystal silicon reduction furnace apparatus, the offgas outlet of each improved Siemens polycrystalline reduction furnace apparatus is connected using gas piping
The air inlet of next improved Siemens polycrystalline reduction furnace apparatus is connected to, is sequentially connected, and on every gas piping
Flowmeter and flow control valve are installed, obtain series devices；
And each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, exchanged heat using gas-gas
Device makes the gas and the improved Siemens polycrystalline reduction furnace apparatus tail into improved Siemens polycrystalline reduction furnace apparatus
The tail gas of gas outlet is exchanged heat, and control enters gas into the improved Siemens polycrystalline reduction furnace apparatus air inlet
Temperature is 145 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improved Siemens polysilicon
It is 100 DEG C to reduce temperature control of the tail gas of furnace apparatus offgas outlet after gas-to-gas heat exchanger exchanges heat；
Described series devices include 1, second improvement west gate of First improved Siemens polycrystalline reduction furnace apparatus
Sub- method polycrystalline silicon reducing furnace equipment 2, the first gas-to-gas heat exchanger 9, the second gas-to-gas heat exchanger 10, exhaust gas recovery system 12, first
Gas piping 13, second gas pipeline 14, third gas pipeline 15, the 4th gas piping 16, the 5th gas piping 17, the 6th gas
The gas piping 19 of body pipeline 18 and the 7th；
First gas pipeline 13 is connected with the feed(raw material)inlet of the first gas-to-gas heat exchanger 9, the original of the first gas-to-gas heat exchanger 9
Material outlet and the first gas entrance 1-1 of First improved Siemens polycrystalline reduction furnace apparatus 1 pass through second gas pipeline
14 are connected, and the first gas outlet 1-2 of First improved Siemens polycrystalline reduction furnace apparatus 1 and the first gas-gas exchange heat
The gas inlet of device 9 is connected by third gas pipeline 15, and offgas outlet and the second gas-gas of the first gas-to-gas heat exchanger 9 are changed
The feed(raw material)inlet of hot device 10 is connected by the 4th gas piping 16, the material outlet of the second gas-to-gas heat exchanger 10 and second
The second gas entrance 2-1 of improved Siemens polycrystalline reduction furnace apparatus 2 is connected by the 5th gas piping 17, second
Second gas the outlet 2-2 and the second gas-to-gas heat exchanger 10 of improved Siemens polycrystalline reduction furnace apparatus 2 gas inlet lead to
Cross the 6th gas piping 18 to be connected, offgas outlet and the exhaust gas recovery system 12 of the second gas-to-gas heat exchanger 10 pass through the 7th gas
Body pipeline 19 is connected；First gas pipeline 13, second gas pipeline 14, third gas pipeline 15, the 4th gas piping 16,
Flowmeter and flow control valve are respectively equipped with five gas pipings 17, the 6th gas piping 18 and the 7th gas piping 19；
Unstrpped gas is passed through to the air inlet of the First improved Siemens polycrystalline reduction furnace apparatus of series devices,
Equally distributed nozzle arrangements in improved Siemens process polycrystalline silicon reduction furnace equipment chassis, it is more to be injected into improved Siemens
Crystal silicon reduces the reduction intracavitary portion of furnace apparatus, and chemical vapor deposition reduction reaction, reduction reaction occurs in the silicon wicking surface of high temperature
The silicon wafer particulate of generation will fully adsorb deposition on silicon core, gradually form polycrystalline silicon rod；More described improved Siemens
Polycrystalline silicon reducing furnace number of devices is N, N=2；
Series devices are more from First improved Siemens polycrystalline reduction furnace apparatus to a last improved Siemens
Silicon core quantity built in crystal silicon reduction furnace apparatus is successively decreased；The number of silicon core in First improved Siemens polycrystalline reduction furnace apparatus 1
Measure as 36 pairs, the quantity of silicon core is 24 pairs in second improved Siemens polycrystalline reduction furnace apparatus 2；
The described raw material gas flow being passed through in improved Siemens polycrystalline reduction furnace apparatus is Q, then Q=1.3 (Q1
+Q2), wherein Q1It is the gas flow needed when First improved Siemens polycrystalline reduction furnace apparatus 1 is independent pattern, Q2
It is the gas flow needed when second improved Siemens polycrystalline reduction furnace apparatus 2 is independent pattern；
Described first gas pipeline 13, second gas pipeline 14, third gas pipeline 15, the 4th gas piping 16,
Five gas pipings 17, the 6th gas piping 18 and the external sheath of the 7th gas piping 19 have insulation material；
Silicon core used in more described improved Siemens polycrystalline reduction furnace apparatus is circle silicon core；
Described unstrpped gas is the mixed gas of trichlorosilane, dichlorosilane and hydrogen, wherein hydrogen and trichlorine hydrogen
The mol ratio of silicon is (2~4):1, and the mass percent of dichlorosilane is in the gross mass of trichlorosilane and dichlorosilane
4%.
Enhancing effect：Compared with separate unit improved Siemens polycrystalline silicon reducing furnace equipment works independently, realize that yield is lifted
25%~35%, a conversion ratio improves 15%~20%, and energy consumption reduces by 5%~10%.
Embodiment two：The difference of embodiment and embodiment one is：Each improved Siemens polycrystalline silicon reducing furnace
Equipment one gas-to-gas heat exchanger of series connection, makes the gas into improved Siemens polycrystalline reduction furnace apparatus using gas-to-gas heat exchanger
The tail gas of body and the improved Siemens polycrystalline reduction furnace apparatus offgas outlet is exchanged heat, and control enters the improvement Siemens
The gas temperature that enters of method polycrystalline silicon reducing furnace equipment air inlet is 300 DEG C；Except last improved Siemens polysilicon
Reduce outside furnace apparatus, the tail gas of each improved Siemens polycrystalline reduction furnace apparatus offgas outlet passes through gas-to-gas heat exchanger
Temperature control after heat exchange is 150 DEG C.It is other identical with embodiment one.
Enhancing effect：Compared with separate unit improved Siemens polycrystalline silicon reducing furnace equipment works independently, realize that yield is lifted
25%~35%, a conversion ratio improves 15%~20%, and energy consumption reduces by 10%~15%.
Embodiment three：The present embodiment is illustrated with reference to Fig. 2, the difference of embodiment and embodiment one is：Except last
Outside one improved Siemens polycrystalline reduction furnace apparatus, each improved Siemens polycrystalline reduction furnace apparatus is connected one
Gas-to-gas heat exchanger, make the gas into improved Siemens polycrystalline reduction furnace apparatus and improvement west using gas-to-gas heat exchanger
The tail gas of Men Zifa polycrystalline silicon reducing furnace equipment offgas outlets is exchanged heat, and control enters the improved Siemens polycrystalline reduction
The gas temperature that enters of furnace apparatus air inlet is 300 DEG C；In addition to two improved Siemens polycrystalline reduction furnace apparatus reciprocal,
Temperature control of the tail gas of each improved Siemens polycrystalline reduction furnace apparatus offgas outlet after gas-to-gas heat exchanger exchanges heat
150 DEG C are made as, the tail gas of second from the bottom improved Siemens polycrystalline reduction furnace apparatus offgas outlet passes through gas-to-gas heat exchanger
Temperature control after heat exchange is 300 DEG C；
Described series devices include 1, second improvement west gate of First improved Siemens polycrystalline reduction furnace apparatus
Sub- method polycrystalline silicon reducing furnace equipment 2, the first gas-to-gas heat exchanger 9, exhaust gas recovery system 12, first gas pipeline 13, second gas
Pipeline 14, third gas pipeline 15, the 4th gas piping 25 and the 5th gas piping 26；
First gas pipeline 13 is connected with the feed(raw material)inlet of the first gas-to-gas heat exchanger 9, the original of the first gas-to-gas heat exchanger 9
Material outlet and the first gas entrance 1-1 of First improved Siemens polycrystalline reduction furnace apparatus 1 pass through second gas pipeline
14 are connected, and the first gas outlet 1-2 of First improved Siemens polycrystalline reduction furnace apparatus 1 and the first gas-gas exchange heat
The gas inlet of device 9 is connected by third gas pipeline 15, the offgas outlet of the first gas-to-gas heat exchanger 9 and second improvement
The second gas entrance 2-1 of Siemens process polycrystalline silicon reduction furnace apparatus 2 is connected by the 4th gas piping 25, second improvement
The second gas outlet 2-2 of Siemens process polycrystalline silicon reduction furnace apparatus 2 passes through the 5th gas piping 26 with exhaust gas recovery system 12
It is connected；First gas pipeline 13, second gas pipeline 14, third gas pipeline 15, the 4th gas piping 25 and the 5th gas
Flowmeter and flow control valve are installed respectively on pipeline 26.It is other identical with embodiment one.
Enhancing effect：Compared with separate unit improved Siemens polycrystalline silicon reducing furnace equipment works independently, realize that yield is lifted
25%~35%, a conversion ratio improves 15-20%, and energy consumption reduces by 10%~15%, and can save a gas-gas heat exchange
Device.
Example IV：
The present embodiment, the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas are illustrated with reference to Fig. 3
The method for manufacturing polysilicon afterwards, step are as follows：
More improved Siemens polycrystalline reduction furnace apparatus are cascaded, except last improved Siemens is more
Crystal silicon reduction furnace apparatus outside, using gas piping by the offgas outlet of each improved Siemens polycrystalline reduction furnace apparatus with
The air inlet of next improved Siemens polycrystalline reduction furnace apparatus is connected, and is sequentially connected, and in each gas piping
Upper installation flowmeter and flow control valve, and in addition to First improved Siemens polycrystalline reduction furnace apparatus, utilize multiple benefits
Expect that air inlet of the gas piping successively with each improved Siemens polycrystalline reduction furnace apparatus is connected, in each feed supplement
Flowmeter and flow control valve are installed on gas piping, obtain series devices；
Each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, utilizes gas-to-gas heat exchanger
Make the gas and the improved Siemens polycrystalline reduction furnace apparatus tail gas into improved Siemens polycrystalline reduction furnace apparatus
The tail gas of outlet is exchanged heat, and control enters gas temperature into the improved Siemens polycrystalline reduction furnace apparatus air inlet
Spend for 150 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improved Siemens polysilicon is also
Temperature control of the tail gas of former furnace apparatus offgas outlet after gas-to-gas heat exchanger exchanges heat is 100 DEG C；
Described series devices include 1, second improvement west gate of First improved Siemens polycrystalline reduction furnace apparatus
Sub- 2, the 3rd improved Siemens polycrystalline reduction furnace apparatus 3 of method polycrystalline silicon reducing furnace equipment, the first gas-to-gas heat exchanger 9,
Two gas-to-gas heat exchangers 10, the 3rd gas-to-gas heat exchanger 11, exhaust gas recovery system 12, first gas pipeline 13, second gas pipeline
14th, third gas pipeline 15, the 4th gas piping 16, the 5th gas piping 17, the 6th gas piping 18, the 7th gas piping
19th, the 8th gas piping 20, the 9th gas piping 21, the tenth gas piping 22, the first feed supplement gas piping 23 and the second feed supplement
Gas piping 24；
First gas pipeline 13 is connected with the feed(raw material)inlet of the first gas-to-gas heat exchanger 9, the original of the first gas-to-gas heat exchanger 9
Material outlet and the first gas entrance 1-1 of First improved Siemens polycrystalline reduction furnace apparatus 1 pass through second gas pipeline
14 are connected, and the first gas outlet 1-2 of First improved Siemens polycrystalline reduction furnace apparatus 1 and the first gas-gas exchange heat
The gas inlet of device 9 is connected by third gas pipeline 15, and offgas outlet and the second gas-gas of the first gas-to-gas heat exchanger 9 are changed
The feed(raw material)inlet of hot device 10 is connected by the 4th gas piping 16, the material outlet of the second gas-to-gas heat exchanger 10 and second
The second gas entrance 2-1 of improved Siemens polycrystalline reduction furnace apparatus 2 is connected by the 5th gas piping 17, second
Second gas the outlet 2-2 and the second gas-to-gas heat exchanger 10 of improved Siemens polycrystalline reduction furnace apparatus 2 gas inlet lead to
Cross the 6th gas piping 18 to be connected, the raw material of the offgas outlet and the 3rd gas-to-gas heat exchanger 11 of the second gas-to-gas heat exchanger 10 enters
Mouth is connected by the 7th gas piping 19, and the material outlet of the 3rd gas-to-gas heat exchanger 11 and the 3rd improved Siemens are more
The third gas entrance 3-1 of crystal silicon reduction furnace apparatus 1 is connected by the 8th gas piping 20, and the 3rd improved Siemens are more
The third gas outlet 3-2 of crystal silicon reduction furnace apparatus 1 and the gas inlet of the 3rd gas-to-gas heat exchanger 11 pass through the 9th gas piping
21 are connected, and the offgas outlet of the 3rd gas-to-gas heat exchanger 11 is connected with exhaust gas recovery system 12 by the tenth gas piping 22；
And the 4th gas piping 16 be provided with the first feed supplement gas piping 23, the 7th gas piping 19 is provided with the second feed supplement
Gas piping 24；
First gas pipeline 13, second gas pipeline 14, third gas pipeline 15, the 4th gas piping 16, the 5th gas
Pipeline 17, the 6th gas piping 18, the 7th gas piping 19, the 8th gas piping 20, the 9th gas piping 21, the tenth flue
Flowmeter and flow control valve are respectively equipped with road 22, the first feed supplement gas piping 23 and the second feed supplement gas piping 24；
Unstrpped gas is passed through to the air inlet of the First improved Siemens polycrystalline reduction furnace apparatus of series devices,
And unstrpped gas, improved west gate are supplemented to each improved Siemens polycrystalline reduction furnace apparatus by feed supplement gas piping
Equally distributed nozzle arrangements in sub- method polycrystalline silicon reduction furnace base plate equipment, are injected into improved Siemens polycrystalline silicon reducing furnace
The reduction intracavitary portion of equipment, chemical vapor deposition reduction reaction, the silicon wafer of reduction reaction generation occurs in the silicon wicking surface of high temperature
Particulate will fully adsorb deposition on silicon core, gradually form polycrystalline silicon rod；More described improved Siemens polycrystalline reductions
Furnace apparatus quantity is N, N=3；
Series devices are more from First improved Siemens polycrystalline reduction furnace apparatus to a last improved Siemens
Silicon core quantity is successively decreased in crystal silicon reduction furnace apparatus；The quantity of silicon core in First improved Siemens polycrystalline reduction furnace apparatus 1
For 36 pairs, the quantity of silicon core is 24 pairs in second improved Siemens polycrystalline reduction furnace apparatus 2, the 3rd improvement Siemens
The quantity of silicon core is 12 pairs in method polycrystalline silicon reducing furnace equipment 3；
The described raw material gas flow for being passed through improved Siemens polycrystalline reduction furnace apparatus is Q, then Q=1.3 (Q1+Q2
+Q3), wherein Q1It is the gas flow needed when First improved Siemens polycrystalline reduction furnace apparatus 1 is independent pattern, Q2
It is the gas flow needed when second improved Siemens polycrystalline reduction furnace apparatus 2 is independent pattern, Q3It is the 3rd to change
The gas flow that good Siemens process polycrystalline silicon reduction furnace apparatus 3 needs when being independent pattern；
Described supplement unstrpped gas is Qb, Qb2=1/5Q2, Qb3=1/4Q3, wherein Q1It is First improved Siemens
The gas flow that polycrystalline reduction furnace apparatus 1 needs when being independent pattern, Qb2It is second improved Siemens polycrystalline reduction
Furnace apparatus 2 supplements raw material gas flow, Qb3It is that the 3rd improved Siemens polycrystalline reduction furnace apparatus 3 supplements raw material gas flow
Amount；
Described first gas pipeline 13, second gas pipeline 14, third gas pipeline 15, the 4th gas piping 16,
Five gas pipings 17, the 6th gas piping 18, the 7th gas piping 19, the 8th gas piping 20, the 9th gas piping the 21, the tenth
Gas piping 22, the first feed supplement gas piping 23 and the external sheath of the second feed supplement gas piping 24 have insulation material；
Silicon core used in more described improved Siemens polycrystalline reduction furnace apparatus is circle silicon core；
Described unstrpped gas is the mixed gas of trichlorosilane, dichlorosilane and hydrogen, wherein hydrogen and trichlorine hydrogen
The mol ratio of silicon is (2~4):1, and the mass percent of dichlorosilane is in the gross mass of trichlorosilane and dichlorosilane
4%.
Described supplement unstrpped gas is the mixed gas of trichlorosilane, dichlorosilane and hydrogen, wherein hydrogen and three
The mol ratio of chlorine hydrogen silicon is (2~4):1, and in the gross mass of trichlorosilane and dichlorosilane dichlorosilane quality percentage
Number is 4%.
Enhancing effect：Compared with separate unit improved Siemens polycrystalline silicon reducing furnace equipment works independently, yield lifting 30%
~40%, a conversion ratio improves more than 15%~20%, and energy consumption reduces by 7%~10%.
Embodiment five：The difference of embodiment and example IV is：Each improved Siemens polycrystalline silicon reducing furnace
Equipment one gas-to-gas heat exchanger of series connection, makes the gas into improved Siemens polycrystalline reduction furnace apparatus using gas-to-gas heat exchanger
The tail gas of body and the improved Siemens polycrystalline reduction furnace apparatus offgas outlet is exchanged heat, and control enters the improvement Siemens
The gas temperature that enters of method polycrystalline silicon reducing furnace equipment air inlet is 300 DEG C；Except last improved Siemens polysilicon
Reduce outside furnace apparatus, the tail gas of each improved Siemens polycrystalline reduction furnace apparatus offgas outlet passes through gas-to-gas heat exchanger
Temperature control after heat exchange is 150 DEG C.It is other identical with example IV.
Enhancing effect：Compared with separate unit improved Siemens polycrystalline silicon reducing furnace equipment works independently, realize that yield is lifted
30%~40%, a conversion ratio improves 15%~20%, and energy consumption reduces by 12%~15%.
Claims (10)
1. manufacturing the method for polysilicon after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas, it is special
Sign is：After the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas manufacture polysilicon method be by
What following steps were carried out：More improved Siemens polycrystalline reduction furnace apparatus are cascaded, except last improvement west
Outside Men Zifa polycrystalline silicon reducing furnace equipment, using gas piping by the tail of each improved Siemens polycrystalline reduction furnace apparatus
Gas exports the air inlet for being connected to next improved Siemens polycrystalline reduction furnace apparatus, is sequentially connected, and in every gas
Flowmeter and flow control valve are installed on body pipeline, obtain series devices；The First that unstrpped gas is passed through to series devices changes
The air inlet of good Siemens process polycrystalline silicon reduction furnace apparatus, in improved Siemens process polycrystalline silicon reduction furnace equipment chassis uniformly
The nozzle arrangements of distribution, the reduction intracavitary portion of improved Siemens polycrystalline reduction furnace apparatus is injected into, in the silicon core of high temperature
Chemical vapor deposition reduction reaction occurs for surface, and the silicon wafer particulate of reduction reaction generation will fully adsorb deposition on silicon core, by
Step forms polycrystalline silicon rod；More described improved Siemens polycrystalline silicon reducing furnace number of devices are N, and 10 >=N >=2, N are just whole
Number；
And each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, made using gas-to-gas heat exchanger
Gas into improved Siemens polycrystalline reduction furnace apparatus goes out with the improved Siemens polycrystalline reduction furnace apparatus tail gas
The tail gas of mouth is exchanged heat, and control enters gas temperature into the improved Siemens polycrystalline reduction furnace apparatus air inlet
For 140 DEG C~160 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improved Siemens are more
Temperature control of the tail gas of crystal silicon reduction furnace apparatus offgas outlet after gas-to-gas heat exchanger exchanges heat is 80 DEG C~110 DEG C；
Or each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, made using gas-to-gas heat exchanger
Gas into improved Siemens polycrystalline reduction furnace apparatus goes out with the improved Siemens polycrystalline reduction furnace apparatus tail gas
The tail gas of mouth is exchanged heat, and control enters gas temperature into the improved Siemens polycrystalline reduction furnace apparatus air inlet
For 200 DEG C~300 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improved Siemens are more
Temperature control of the tail gas of crystal silicon reduction furnace apparatus offgas outlet after gas-to-gas heat exchanger exchanges heat is 100 DEG C~200 DEG C；
Or in addition to last improved Siemens polycrystalline reduction furnace apparatus, each improved Siemens polycrystalline silicon reducing furnace
Equipment one gas-to-gas heat exchanger of series connection, makes the gas into improved Siemens polycrystalline reduction furnace apparatus using gas-to-gas heat exchanger
The tail gas of body and the improved Siemens polycrystalline reduction furnace apparatus offgas outlet is exchanged heat, and control enters the improvement Siemens
The gas temperature that enters of method polycrystalline silicon reducing furnace equipment air inlet is 200 DEG C~300 DEG C；Except two improved Siemens reciprocal
Outside polycrystalline reduction furnace apparatus, the tail gas of each improved Siemens polycrystalline reduction furnace apparatus offgas outlet passes through gas-gas
Temperature control after heat exchanger heat exchange is 100 DEG C~200 DEG C, second from the bottom improved Siemens polycrystalline reduction furnace apparatus tail
Temperature control of the tail gas of gas outlet after gas-to-gas heat exchanger exchanges heat is 200 DEG C~300 DEG C；
Series devices are from First improved Siemens polycrystalline reduction furnace apparatus to a last improved Siemens polysilicon
Silicon core quantity built in reduction furnace apparatus is successively decreased；When more improved Siemens polycrystalline silicon reducing furnace number of devices are N, and 10 >=N
During ＞ 2, described silicon core quantity is ni, then ni-1-ni≤ni-2-ni-1, wherein niIt is i-th improved Siemens polycrystalline reduction
The quantity of silicon core built in furnace apparatus；As more improved Siemens polycrystalline silicon reducing furnace number of devices N=2, described silicon core
Quantity is n1And n2, n1＞ n2≥1/3n1, wherein n1It is silicon core built in First improved Siemens polycrystalline reduction furnace apparatus
Quantity, n2It is the quantity of silicon core built in second improved Siemens polycrystalline reduction furnace apparatus；
The described raw material gas flow being passed through in improved Siemens polycrystalline reduction furnace apparatus is Q, thenWherein QiIt is that i-th improved Siemens polycrystalline reduction furnace apparatus is independent mould
The gas flow needed during formula, N are the quantity for the improved Siemens polycrystalline reduction furnace apparatus being connected in series.
2. system is produced after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas according to claim 1
The method for making polysilicon, it is characterised in that：Silicon core used in more described improved Siemens polycrystalline reduction furnace apparatus is circle
Silicon core or square silicon core.
3. system is produced after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas according to claim 1
The method for making polysilicon, it is characterised in that：Described unstrpped gas is the gaseous mixture of trichlorosilane, dichlorosilane and hydrogen
The mol ratio of body, wherein hydrogen and trichlorosilane is (2~4):1, and dichloro in the gross mass of trichlorosilane and dichlorosilane
The mass percent of dihydro silicon is 4%~6%.
4. system is produced after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas according to claim 1
The method for making polysilicon, it is characterised in that：The flue connected between described improved Siemens polycrystalline reduction furnace apparatus
Road external sheath has insulation material.
5. system is produced after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas according to claim 1
The method for making polysilicon, it is characterised in that：More described improved Siemens polycrystalline silicon reducing furnace number of devices are N, N=2.
6. manufacturing the method for polysilicon after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas, it is special
Sign is：After the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas manufacture polysilicon method be by
What following steps were carried out：More improved Siemens polycrystalline reduction furnace apparatus are cascaded, except last improvement west
Outside Men Zifa polycrystalline silicon reducing furnace equipment, using gas piping by the tail of each improved Siemens polycrystalline reduction furnace apparatus
Gas outlet is connected with the air inlet of next improved Siemens polycrystalline reduction furnace apparatus, is sequentially connected, and each
Flowmeter and flow control valve are installed on gas piping, and in addition to First improved Siemens polycrystalline reduction furnace apparatus, profit
It is connected with air inlet of multiple feed supplement gas pipings successively with each improved Siemens polycrystalline reduction furnace apparatus,
Flowmeter and flow control valve are installed on each feed supplement gas piping, obtain series devices；Unstrpped gas is passed through series devices
First improved Siemens polycrystalline reduction furnace apparatus air inlet, and by feed supplement gas piping to each improve
Siemens process polycrystalline silicon reduction furnace apparatus supplement unstrpped gas, in improved Siemens process polycrystalline silicon chassis of reducing furnace equipment uniformly
The nozzle arrangements of distribution, the reduction intracavitary portion of improved Siemens polycrystalline reduction furnace apparatus is injected into, in the silicon core of high temperature
Chemical vapor deposition reduction reaction occurs for surface, and the silicon wafer particulate of reduction reaction generation will fully adsorb deposition on silicon core, by
Step forms polycrystalline silicon rod；More described improved Siemens polycrystalline silicon reducing furnace number of devices are N, and 10 >=N >=2, N are just whole
Number；
And each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, made using gas-to-gas heat exchanger
Gas into improved Siemens polycrystalline reduction furnace apparatus goes out with the improved Siemens polycrystalline reduction furnace apparatus tail gas
The tail gas of mouth is exchanged heat, and control enters gas temperature into the improved Siemens polycrystalline reduction furnace apparatus air inlet
For 140 DEG C~160 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improved Siemens are more
Temperature control of the tail gas of crystal silicon reduction furnace apparatus offgas outlet after gas-to-gas heat exchanger exchanges heat is 80 DEG C~110 DEG C；
Or each improved Siemens polycrystalline reduction furnace apparatus one gas-to-gas heat exchanger of series connection, made using gas-to-gas heat exchanger
Gas into improved Siemens polycrystalline reduction furnace apparatus goes out with the improved Siemens polycrystalline reduction furnace apparatus tail gas
The tail gas of mouth is exchanged heat, and control enters gas temperature into the improved Siemens polycrystalline reduction furnace apparatus air inlet
For 200 DEG C~300 DEG C；In addition to last improved Siemens polycrystalline reduction furnace apparatus, each improved Siemens are more
Temperature control of the tail gas of crystal silicon reduction furnace apparatus offgas outlet after gas-to-gas heat exchanger exchanges heat is 100 DEG C~200 DEG C；
Series devices are from First improved Siemens polycrystalline reduction furnace apparatus to a last improved Siemens polysilicon
Silicon core quantity built in reduction furnace apparatus is successively decreased；When more improved Siemens polycrystalline silicon reducing furnace number of devices are N, and 10 >=N
During ＞ 2, described silicon core quantity is ni, then ni-1-ni≤ni-2-ni-1, wherein niIt is i-th improved Siemens polycrystalline reduction
The quantity of silicon core built in furnace apparatus；When more improved Siemens polycrystalline silicon reducing furnace number of devices are N=2, described silicon
Core quantity is n1And n2, n1＞ n2≥1/3n1, wherein n1It is silicon core built in First improved Siemens polycrystalline reduction furnace apparatus
Quantity, n2It is the quantity of silicon core built in second improved Siemens polycrystalline reduction furnace apparatus；
The described raw material gas flow for being passed through improved Siemens polycrystalline reduction furnace apparatus is Q, thenWherein QiIt is that i-th improved Siemens polycrystalline reduction furnace apparatus is independent mould
The gas flow needed during formula, N are the quantity for the improved Siemens polycrystalline reduction furnace apparatus being connected in series；
Described supplement unstrpped gas is Qb, Qi≥Qbi>=0, wherein QiIt is i-th improved Siemens polycrystalline reduction furnace apparatus
For the gas flow needed during independent pattern, QbiIt is i-th improved Siemens polycrystalline reduction furnace apparatus supplement unstrpped gas
Flow.
7. system is produced after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas according to claim 6
The method for making polysilicon, it is characterised in that：Silicon core used in more described improved Siemens polycrystalline reduction furnace apparatus is circle
Silicon core or square silicon core.
8. system is produced after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas according to claim 6
The method for making polysilicon, it is characterised in that：Described unstrpped gas is the gaseous mixture of trichlorosilane, dichlorosilane and hydrogen
The mol ratio of body, wherein hydrogen and trichlorosilane is (2~4):1, and dichloro in the gross mass of trichlorosilane and dichlorosilane
The mass percent of dihydro silicon is 4%~6%.
9. system is produced after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas according to claim 6
The method for making polysilicon, it is characterised in that：The flue connected between described improved Siemens polycrystalline reduction furnace apparatus
Road external sheath has insulation material.
10. produced after the recovered cycling and reutilization of improved Siemens polysilicon reducing furnace tail gas according to claim 6
The method for manufacturing polysilicon, it is characterised in that：Described supplement unstrpped gas is the mixed of trichlorosilane, dichlorosilane and hydrogen
Gas is closed, the wherein mol ratio of hydrogen and trichlorosilane is (2~4):1, and in the gross mass of trichlorosilane and dichlorosilane
The mass percent of dichlorosilane is 4%~6%.
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| CN102167327A (en) * | 2011-04-08 | 2011-08-31 | 天津大学 | Reaction system for producing polycrystalline silicon by using multiple polycrystalline silicon reduction furnaces and operating method of reaction system |
| CN103159217A (en) * | 2013-03-07 | 2013-06-19 | 江西景德半导体新材料有限公司 | Polysilicon reducing furnace tail gas silicon powder collection device and application method |
| CN103382019A (en) * | 2013-06-25 | 2013-11-06 | 内蒙古同远企业管理咨询有限责任公司 | Recycling purification process for reducing tail gas and recycling system hydrogen gas by improved Siemens method |
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| CN102167327A (en) * | 2011-04-08 | 2011-08-31 | 天津大学 | Reaction system for producing polycrystalline silicon by using multiple polycrystalline silicon reduction furnaces and operating method of reaction system |
| CN103159217A (en) * | 2013-03-07 | 2013-06-19 | 江西景德半导体新材料有限公司 | Polysilicon reducing furnace tail gas silicon powder collection device and application method |
| CN103382019A (en) * | 2013-06-25 | 2013-11-06 | 内蒙古同远企业管理咨询有限责任公司 | Recycling purification process for reducing tail gas and recycling system hydrogen gas by improved Siemens method |
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