CN104860315B - A kind of reduction furnace progress control method - Google Patents
A kind of reduction furnace progress control method Download PDFInfo
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- CN104860315B CN104860315B CN201410066852.0A CN201410066852A CN104860315B CN 104860315 B CN104860315 B CN 104860315B CN 201410066852 A CN201410066852 A CN 201410066852A CN 104860315 B CN104860315 B CN 104860315B
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Abstract
The present invention provides a kind of reduction furnace progress control method, and the method includes：Initial pressure in reduction furnace is set to 0.45 0.6MPa, initial temperature is set to 1,120 1150 DEG C；Control trichlorosilane and hydrogen persistently feed, and form gaseous mixture, and in reduction furnace running, the gaseous mixture are persistently delivered in reduction furnace, so that the gaseous mixture is persistently reacted in reduction furnace；It is delivered in 05 hours of reduction furnace by the gaseous mixture, by the temperature control in reduction furnace at 900 1100 DEG C；When the gaseous mixture is reacted to 30 60 hours in reduction furnace, according to the gentle field distribution of heterogeneity phantom in reduction furnace, apply the electric current of varying strength to each layer silicon rod in reduction furnace at interval of a period of time, to ensure that the balanced gentle field of thermal field is balanced in reduction furnace, and the temperature in reduction furnace is maintained at 900 1100 DEG C, until reduction furnace blowing out.
Description
Technical field
The present invention relates to polycrystalline reduction technical field, and in particular to a kind of production of polysilicon
During reduction furnace progress control method.
Background technology
At present, in polysilicon production process, the maximum reduction furnace of operation is 36 pairs of rods, existing 36 pairs of rods both at home and abroad
In reduction furnace operation control technique, influenceed by gas field in stove, silicon rod temperature is higher at nearly tail gas hole, causes the gentle field of thermal field in stove
Skewness weighs, and the uneven normal operation for directly restricting reduction furnace of the gentle field distribution of thermal field, cause atomization so that in reduction furnace
Environment becomes cloudy, produce fine silica powder, and easily fall stove.Produced silica flour brings very to reducing furnace system equipment and lower procedure
Many adverse effects, serious challenge is proposed to product quality.
With the development of polycrystalline reduction technology, reduction furnace more and more tends to maximization, using 48 pairs of polysilicons of rod also
Former stove is the development trend of polycrystalline reduction technique.48 pairs of rod reduction furnaces increase due to horizontal volume, silicon rod increasing number, reduction
The unbalanced phenomenon of the gentle field distribution of thermal field can be protruded more in stove, more be also easy to produce the abnormal problems such as atomization.
Therefore, a kind of reduction furnaces operation control programs for being applied to the 48 pairs of rod reduction furnaces are needed badly, is asked with solving above-mentioned technology
Topic.
The content of the invention
The present invention is for above shortcomings in the prior art, there is provided a kind of reduction furnace progress control method, is used to solve
The certainly uneven problem of the gentle field distribution of the large-scale reduction furnace thermal field of 48 pairs of rods.
The present invention is in order to solve the above technical problems, adopt the following technical scheme that：
The present invention provides a kind of reduction furnace progress control method, and silicon rod layer distributed in reduction furnace, methods described includes
Following steps：
Initial pressure in reduction furnace is set to 0.45-0.6MPa, initial temperature is set to 1120-1150 DEG C；
Control trichlorosilane and hydrogen persistently feed, and form gaseous mixture, and in reduction furnace running, by the mixing
Gas is persistently delivered in reduction furnace, so that the gaseous mixture is persistently reacted in reduction furnace；
In 0-5 hours that the gaseous mixture is delivered to reduction furnace, by the temperature control in reduction furnace in 900-1100
℃；
When the gaseous mixture is reacted to 30-60 hours in reduction furnace, according to the gentle field of heterogeneity phantom in reduction furnace point
Cloth, the electric current of varying strength is applied at interval of a period of time to each layer silicon rod in reduction furnace, to ensure that thermal field is balanced in reduction furnace
Gentle field is balanced, and the temperature in reduction furnace is maintained at into 900-1100 DEG C, until reduction furnace blowing out.
Preferably, tail gas hole is arranged in the middle of chassis of reducing furnace, and silicon rod is in concentric circles layer distributed with tail gas hole；It is described every
Certain interval of time applies the electric current of varying strength to each layer silicon rod in reduction furnace, specifically includes：
Using split-phase current control, electricity is applied with default current strength amplification to every layer of silicon rod in reduction furnace per hour
Stream, and according to from the close-by examples to those far off, the current strength amplification of each layer silicon rod is gradually incremented by with the distance away from tail gas hole.
Preferably, the current strength amplification of each layer silicon rod is 3-8A/h.
Preferably, tail gas hole is uniformly distributed in the outside of chassis of reducing furnace, and the multipair silicon rod in the middle of chassis of reducing furnace is made
For core is justified, and as ground floor, remaining silicon rod layer distributed, and be distributed in concentric circles with core circle；
The electric current for applying varying strength to each layer silicon rod in reduction furnace at interval of a period of time, specifically includes：
Using split-phase current control, electricity is applied with default current strength amplification to every layer of silicon rod in reduction furnace per hour
Stream, and according to the distance justified with the core from the close-by examples to those far off, the current strength amplification of each layer silicon rod is gradually successively decreased.
Preferably, the current strength amplification of each layer silicon rod is 0-8A/h.
Preferably, when the gaseous mixture initially being delivered into reduction furnace, hydrogen and trichlorosilane rubs in the gaseous mixture
You are than being 2-10：1；
Methods described also includes：
In 0-5 hours that the gaseous mixture is delivered to reduction furnace, by hydrogen in the gaseous mixture and trichlorosilane
Mol ratio is adjusted to 2-5：1, and keep the mol ratio；
5-10 hours before reduction furnace blowing out, the mol ratio of hydrogen and trichlorosilane in the gaseous mixture of reduction furnace will be delivered to
It is adjusted to 3-5：1, until reduction furnace blowing out.
Preferably, when the gaseous mixture initially being delivered into reduction furnace, hydrogen and trichlorosilane rubs in the gaseous mixture
You are than being 6-8：1.
Further, when the gaseous mixture is reacted to 30-60 hours in reduction furnace, methods described also includes：
Reduce water-carrying capacity on the high temperature for entering feed preheater, and open the charging of tail gas heat exchanger and bypass, being used to will be defeated
The temperature control of the trichlorosilane of reduction furnace and the gaseous mixture of hydrogen is delivered at 100 DEG C -160 DEG C.
Preferably, reduce water-carrying capacity on the high temperature for entering feed preheater, and open the charging of tail gas heat exchanger and bypass, use
So that the temperature control of the trichlorosilane of reduction furnace and the gaseous mixture of hydrogen will be delivered at 120 DEG C -150 DEG C.
Preferably, the initial pressure in reduction furnace is set to 0.55MPa, initial temperature is set to 1130-1140 DEG C.
The present invention is layered setting by by silicon rod in reduction furnace, when the gaseous mixture of trichlorosilane and hydrogen is in reduction furnace
When being reacted to 30-60 hours, according to the gentle field distribution of thermal field in stove, each layer silicon rod in reduction furnace is applied at interval of a period of time
The electric current of varying strength reaches the purpose of the gentle field of thermal field in equalizing furnace, reduces atomization and the rate of falling stove, can be by the non-life of reduction furnace
The product time shortens 2-3 hours, and reduction furnace effective rate of utilization improves about 1.2%；The loss of the auxiliary materials such as graphite, silicon core is reduced, lifting is exempted from
Material yield is washed, electrode damage rate is reduced, production cost is reduced；Reduce the number of times of the dismounting reduction furnace that stove causes, reduce work
Intensity and human cost；Reduce polysilicon surface pollution, Improving The Quality of Products；Silicon rod falls, clears up silicon in reducing disassembly process
Powder dodges the emergency risk such as quick-fried, improves production security；Reduce because atomization produces infringement of the silica flour to lower procedure, improve equipment
Energy.
Brief description of the drawings
Fig. 1 is the structural representation of polycrystalline silicon reduction system provided in an embodiment of the present invention.
Specific embodiment
Below in conjunction with the accompanying drawing in the present invention, clear, complete description is carried out to the technical scheme in the present invention, shown
So, described embodiment is a part of embodiment of the invention, rather than whole embodiments.Based on the implementation in the present invention
Example, the every other embodiment that those of ordinary skill in the art are obtained on the premise of creative work is not made all belongs to
In the scope of protection of the invention.
Production of polysilicon is delivered in reduction furnace by nozzle by by the gaseous mixture of trichlorosilane and hydrogen, with reduction
Silicon rod in stove carries out reduction reaction.Multipair silicon rod is distributed with the chassis of reduction furnace, trichlorosilane exists with the gaseous mixture of hydrogen
Under the conditions of certain temperature and pressure, there is reduction reaction with silicon rod, finally give polysilicon.
The embodiment of the present invention provides a kind of reduction furnace progress control method, is used to solve large-scale reduction furnace（48 pairs of reduction furnaces）
Atomization, the problems such as falling stove caused by interior thermal field is uneven, thus improve the production efficiency of reduction furnace and the yield of polysilicon product with
Quality.
Fig. 1 is the knot for implementing a kind of polycrystalline silicon reduction system that embodiment of the present invention reduction furnace progress control method is used
Structure schematic diagram, as shown in figure 1, the polycrystalline silicon reduction system includes reduction furnace 5, feed preheater 2, tail gas heat exchanger 4, chuck
Pipe 7, the first mixing arrangement 1 and the second mixing arrangement 3.In the polycrystalline silicon reduction system, by flash tank（Do not painted in figure
Show）In on 130 DEG C of high temperature water be passed through jacket pipe 7 and carry out thermal energy exchange with the high-temperature tail gas from reduction furnace 5 out, heat energy is handed over
After changing, high-temperature tail gas enter tail gas heat exchanger 4 in, wherein all the way on high temperature water be directly entered return main as high-temperature tempering simultaneously
Flash tank is returned to, the material formed after water mixes into feed preheater 2 with hydrogen and trichlorosilane on another road high temperature enters
Return main is entered back into after row thermal energy exchange as high-temperature tempering and flash tank is returned to.In reduction furnace 5, multipair silicon rod layering
Set.Below in conjunction with Fig. 1, the course of work to polycrystalline silicon reduction system is described in detail.
After the trichlorosilane of hydrogen and liquid mixes through the first mixing arrangement 1, into feed preheater 2, fed with entering
Water carries out thermal energy exchange on the high temperature all the way of preheater 2, and the trichlorosilane gasification of liquid is gas, so as to obtain hydrogen and trichlorine
The gaseous mixture of hydrogen silicon, the gaseous mixture carries out secondary mixing through the second mixing arrangement 3 again.Secondary mixed gaseous mixture can basis
The charging of tail gas heat exchanger bypasses 6 unlatching and is divided into two-way, and gaseous mixture enters tail gas heat exchanger 4 and enters tail gas heat exchange all the way
The high-temperature tail gas of device 4 carry out thermal energy exchange, again via being delivered to reduction furnace 5 again after tail gas heat exchanger 4 after thermal energy exchange；Another road
Gaseous mixture is then fed directly to reduction furnace 5 via the charging bypass 6 of tail gas heat exchanger 4.It is anti-in reduction furnace 5 during initial charge
Should not yet start, tail gas heat exchanger 4 only serves the effect of transmission gaseous mixture, it is produced in reduction furnace with the carrying out of reaction
High-temperature tail gas out enter tail gas heat exchanger 4 through by jacket pipe 7 afterwards from reduction furnace 5.On the one hand, the high temperature in jacket pipe 7 is flowed through
Upper water carries out thermal energy exchange with high-temperature tail gas, so as to reduce the temperature of high-temperature tail gas；On the other hand, a part flows through jacket pipe 7
High temperature on water be transported to feed preheater 2, be used to enter promoting the circulation of qi to the trichlorosilane in material using the heat energy of water on high temperature
Change, so as to the material heating to entering in feed preheater 2.
Below in conjunction with Fig. 1, reduction furnace progress control method of the invention is described in detail.As shown in figure 1, the method
May comprise steps of：
Step 101,0.45-0.6MPa is set to by the initial pressure in reduction furnace, and initial temperature is set to 1120-1150
℃。
Preferably, the initial pressure in reduction furnace is set to 0.55MPa, initial temperature is set to 1130-1140 DEG C.
Step 102, control trichlorosilane and hydrogen persistently feed, and form gaseous mixture, and in reduction furnace running, will
The gaseous mixture is persistently delivered in reduction furnace, so that the gaseous mixture is persistently reacted in reduction furnace.
Specifically, the first hydrogen charging in control hydrogen feed tube road, for example, by hydrogen with the flow elder generation of 15-25kg/h
The first mixing arrangement 1 is delivered to, then is delivered in feed preheater 2, in hydrogen fill process, be gradually opened trichlorosilane and enter
Trichlorosilane inlet valve on expects pipe road, to control the feed rate of trichlorosilane.
Trichlorosilane normality is liquid, and the trichlorosilane of gaseous hydrogen and liquid is delivered to through the first mixing arrangement 1
Feed preheater 2, the two carries out thermal energy exchange in feed preheater 2 with high-temperature tempering so that the trichlorosilane gasification of liquid
It is gas, obtains the gaseous mixture of trichlorosilane and hydrogen.
The gaseous mixture is exported to the second mixing arrangement 3 from feed preheater 2, carries out secondary mixing, is further ensured that trichlorine
Hydrogen silicon is sufficiently mixed with hydrogen.Tail gas heat exchanger 4 is transported to by the mixed gaseous mixture of the second mixing arrangement 3, then by
Exported in tail gas heat exchanger 4 and by nozzle（Do not illustrated in figure）It is delivered in reduction furnace 5.
In order to reach preferable reaction result, when the gaseous mixture initially being delivered into reduction furnace 5, reduction can will be entered
Hydrogen is controlled in 2-10 with the mol ratio of trichlorosilane in the gaseous mixture of stove：1, for example, can be by by the flow of hydrogen
Control to be realized in 0-5500kg/h in 0-250kg/h and by the flow control of trichlorosilane.Preferably, by hydrogen in the gaseous mixture
Gas is controlled in 6-8 with the mol ratio of trichlorosilane：1.
Step 103, in 0-5 hours that the gaseous mixture is delivered to reduction furnace, the temperature control in reduction furnace is existed
900-1150℃。
Specifically, the gaseous mixture is being delivered to 0-5 hours of reduction furnace（I.e. gaseous mixture is reacted in reduction furnace
0-5 hours）It is interior, every 1 hour, it is necessary to apply electric current with certain current strength amplification by the silicon rod in reduction furnace,
So as to be heated to silicon rod, it is ensured that reaction temperature.For example, during initial charge, being applied respectively on each layer silicon rod in reduction furnace
Plus the initial current of 100A, afterwards, according to the current strength amplification of 10A/h for each layer silicon rod applies electric current, starting with electric current
Intensity amplification applies the 1st hour of electric current, and 110A is applied on each layer silicon rod, and the 2nd hour applies on each layer silicon rod
120A, by that analogy.
Preferably, can be that each layer silicon rod applies electric current by split-phase current control.Split-phase current control refers to, by entirely
Portion's silicon rod is divided into multigroup, and the logarithm of every group of silicon rod is identical, and every group of silicon rod is a phase silicon rod, is the electric current that every phase silicon rod applies
Intensity is identical, for example, 48 pairs of silicon rods are divided into 6 phases, per mutually including 8 pairs of silicon rods.The purpose of split-phase current control is, by quantity
More silicon rod be split as it is multigroup, be easy to control.
In reacted in reduction furnace 0-5 hours, by the temperature control in reduction furnace 5 at 900-1150 DEG C, can be with
The initial operating stage abnormal conditions such as stove and the stripping of silicon core are greatly reduced.
Step 104, when the mixed gas are reacted to 30-60 hours in reduction furnace, according to thermal field in reduction furnace point
The gentle field distribution of cloth, the electric current of varying strength is applied at interval of a period of time, to ensure that thermal field is equal in reduction furnace to each layer silicon rod
Weighing apparatus, and the temperature in reduction furnace is maintained at 900-1100 DEG C, until reduction furnace blowing out.
Specifically, when the mixed gas are reacted to 30-60 hours in reduction furnace, according to heterogeneity phantom in reduction furnace
Gentle field distribution, at interval of the electric current for applying varying strength for 1 hour to each layer silicon rod, to ensure that thermal field is balanced in reduction furnace.
Wherein, distribution mode of the tail gas hole on chassis of reducing furnace mainly has 2 kinds, and one kind is tail gas hole position in reduction furnace bottom
The centre of disk, it is a kind of be the outside that tail gas hole is uniformly distributed in chassis of reducing furnace, i.e. chassis circumference at.For both tail gas
Pore size distribution mode, the processing mode that electric current is applied to silicon rod is different, individually below to under both tail gas pore size distribution modes
Electric current applying mode elaborate.
When tail gas hole position is in the middle of chassis of reducing furnace, silicon rod is in concentric circles layer distributed with tail gas hole（That is silicon
Rod is distributed around tail gas hole in concentric circles centered on tail gas hole）.Varying strength is applied to each layer silicon rod per hour
Electric current, specifically include：Using split-phase current control, electricity is applied with default current strength amplification to every layer of silicon rod per hour
Stream, it is preferred that each layer of current strength amplification of silicon rod is 3-8A/h, and according to the distance away from tail gas hole from the close-by examples to those far off, respectively
The current strength amplification of layer silicon rod is gradually incremented by.
By basis with the distance away from tail gas hole from the close-by examples to those far off, the current strength amplification that each layer silicon rod applies gradually is passed
Increase, can effectively reduce silicon rod temperature in the uneven caused stove of the gentle field distribution of thermal field in stove and differ the problems such as with local atomization,
Improve silicon rod quality.
When tail gas hole is uniformly distributed in the outside of chassis of reducing furnace, will be some right in the middle of chassis of reducing furnace
（Such as 3-6 pairs）Silicon rod is justified as core, remaining silicon rod and the core circle in concentric circles layer distributed core justify outward
Enclose.Apply the electric current of varying strength to each layer silicon rod per hour, specifically include：Using split-phase current control, per hour to every layer
Silicon rod applies electric current with default current strength amplification, it is preferred that each layer of current strength amplification of silicon rod is 0-8A/h, and root
According to the distance justified with the core from the close-by examples to those far off, the current strength amplification of each layer silicon rod is gradually successively decreased.
The distance justified with the core by basis from the close-by examples to those far off, is gradually passed the current strength amplification that each layer silicon rod applies
Subtract, can effectively reduce silicon rod temperature in the uneven caused stove of the gentle field distribution of thermal field in stove and differ the problems such as with local atomization,
Improve silicon rod quality.
It should be noted that by the temperature control of reduction furnace 5 at 900-1150 DEG C afterwards, the thermal field according to reduction furnace
Gentle field distribution is distributed, before applying the electric current of varying strength to each layer silicon rod per hour, it is still desirable to according to described in step 103
Mode, every 1 hour, be the silicon rod in reduction furnace applied electric current with identical current strength amplification, and silicon rod is heated,
To ensure reaction temperature.
In polysilicon production process, if hydrogen is too small with the proportioning of trichlorosilane, the growth rate of polysilicon is too fast,
It is unfavorable for the control of surface topography and the suppression of back reaction and the control to being atomized；If the proportioning of hydrogen and trichlorosilane
Greatly, then the speed of growth of polysilicon is limited, yield is influenceed.In order to by the growth rate of polysilicon control rational scope it
Interior, with the carrying out of reaction, polysilicon diameter gradually increases, it is necessary to be adjusted accordingly to the proportioning of hydrogen and trichlorosilane
It is whole.Further, methods described is further comprising the steps of：
By initial ratio（That is mol ratio）It is 2-10：1 hydrogen is delivered to reduction furnace 5 with the gaseous mixture of trichlorosilane,
In 0-5 hours of the mixing solid/liquid/gas reactions, be gradually decrease to for the proportioning of the two by the doses of synchronous adjustment hydrogen and trichlorosilane
2-5：1, and the proportioning is kept in follow-up course of reaction.
5-10 hours before reduction furnace blowing out, will be delivered to hydrogen and trichlorosilane in the gaseous mixture of reduction furnace 5 mole
Than being adjusted to 3-5：1.
In order to further reduce the temperature of tail gas, and the heat energy in tail gas is effectively used, will can be arranged on also
Jacket pipe 7 between former stove 5 and tail gas heat exchanger 4 is connected with feed preheater 2, is used to flow through the high temperature all the way of jacket pipe 7
Upper water is introduced into feed preheater 2, so as to entering the material in feed preheater 2（The mixture of hydrogen and trichlorosilane）Enter
Row heating.
When gaseous mixture is reacted to 30-60 hours in reduction furnace 5, methods described also includes：Reduction enters feeding preheating
The flow of water on the high temperature of device 2, and the charging bypass 6 of tail gas heat exchanger is opened, it is used to be delivered to the trichlorosilane of reduction furnace 5
With the temperature control of the gaseous mixture of hydrogen at 100 DEG C -160 DEG C.It should be noted that during the subsequent reactions of reduction furnace,
The temperature of gaseous mixture is controlled at 100 DEG C -160 DEG C always, until reduction furnace blowing out.
By feeding temperature control at 100 DEG C -160 DEG C, can effectively postpone to be atomized the time started, in control reduction furnace
Atomizating phenomenon has better effects.
Specifically, in the polycrystalline silicon reduction system, feed preheater 2 is connected with water return pipeline, water return pipeline it is another
End connect with return main, into the high temperature of feed preheater 2 on water through water return pipeline entrance return main in, formation high temperature
Backwater.Wherein, the water return pipeline is provided with valve 8.By control valve 8, can control to enter the high temperature of feed preheater 2
The flow of upper water, by reducing the flow for carrying out water on the high temperature of thermal energy exchange with the material entered in feed preheater 2,
That is, will reduce for the flow of water on the high temperature of the trichlorosilane that gasifies, can reduce vaporized trichlorosilane, so as to reduce
The temperature of material, is finally lowered into the temperature of the gaseous mixture of reduction furnace.
After opening the charging bypass 6 of tail gas heat exchanger 4, may be such that a part of material does not enter tail gas heat exchanger 4, not with tail
Gas carries out thermal energy exchange, therefore temperature is low compared with the temperature for entering the material for carrying out thermal energy exchange in tail gas heat exchanger, the part thing
Material is entered back into reduction furnace 5 after mixing with the material that thermal energy exchange is carried out by tail gas heat exchanger 4, so as to reduce be delivered to reduction
The temperature of the material of stove 5.
It should be noted that reducing into the flow of water on the high temperature of feed preheater 2 and entering for unlatching tail gas heat exchanger 4
Material 6 the two operating procedures of bypass can be performed synchronously, it is also possible to individually perform one of them.
Preferably, will can be delivered to the temperature control of the trichlorosilane of reduction furnace 5 and the gaseous mixture of hydrogen 120 DEG C-
150 DEG C, and during reduction furnace subsequent reactions, the temperature of gaseous mixture is controlled at 120 DEG C -150 DEG C, until reduction furnace always
Blowing out.
By above-mentioned steps as can be seen that the present invention provide reduction furnace progress control method by by silicon rod in reduction furnace
Interior layering is set, and according to the gentle field distribution of thermal field in stove, applies the electric current of varying strength to each layer silicon rod per hour to reach
The purpose of the gentle field of thermal field in equalizing furnace, reduces atomization and the rate of falling stove, can be shortened into 2-3 separate unit reduction furnace nonproductive time small
When, reduction furnace effective rate of utilization improves about 1.2%；The loss of the auxiliary materials such as graphite, silicon core is reduced, disposable material yield is lifted, electricity is reduced
Pole spoilage, reduces production cost；Reduce the number of times of the dismounting reduction furnace that stove causes, reduce working strength and human cost；
Reduce polysilicon surface pollution, Improving The Quality of Products；Silicon rod in disassembly process is reduced to fall, clear up silica flour and dodge the accident wind such as quick-fried
Danger, improves production security；Reduce because atomization produces infringement of the silica flour to lower procedure, improve equipment performance.
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, but
It should be appreciated that these descriptions are simply to further illustrate the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
Embodiment 1
Embodiment 1 is situation of the tail gas hole position in the middle of chassis of reducing furnace.48 pairs of silicon rods are divided into 4 layers and are arranged at reduction furnace bottom
On disk, each layer silicon rod is distributed with tail gas hole in concentric circles.
Initial pressure in reduction furnace 5 is set to 0.55MPa, initial temperature is set to 1120-1150 DEG C.At the beginning of hydrogen
Beginning flow is 15-25kg/h, in fill process, is gradually opened trichlorosilane regulating valve, makes trichlorosilane and the same high temperature of hydrogen
Upper water carries out thermal energy exchange in feed preheater 2, obtains the gaseous mixture of trichlorosilane and hydrogen, and the gaseous mixture is again via tail
Gas heat exchanger 4 is delivered in reduction furnace 5, so as to realize feeding reduction furnace 5.
When the gaseous mixture initially being delivered into reduction furnace 5, the mol ratio of hydrogen and the gaseous mixture of trichlorosilane is controlled
In 6-8：1.Preferably, in start production 3 hours, by the temperature control in reduction furnace 5 at 900-1150 DEG C.Initial charge
When, the initial current of 100A is applied on each layer silicon rod.
When the gaseous mixture of trichlorosilane and hydrogen is reacted to 40h in reduction furnace 5, synchronous adjustment hydrogen and trichlorosilane
Usage amount, the mol ratio of the gaseous mixture of hydrogen and trichlorosilane is gradually decreased to 2-5：1, until steady production.
When the mixing solid/liquid/gas reactions of trichlorosilane and hydrogen proceed to 40h, using split-phase current control, according in reduction furnace
Heterogeneity phantom and gas Flow Field Distribution, apply the electric current of varying strength, to ensure thermal field in reduction furnace to each layer silicon rod per hour
Balanced gentle field is balanced.It is as follows to the control process that each layer silicon rod applies different current strength using split-phase electric current：
Because tail gas hole position is in the middle part of chassis of reducing furnace, the temperature for more closing on the silicon rod in tail gas hole is higher, silicon rod week
The temperature of thermal field for enclosing is also higher, therefore, in order to keep in reduction furnace 5 the balanced gentle field of thermal field balanced, according to away from tail gas hole
Distance, the current strength that each layer silicon rod applies gradually is increased according to order from the near to the remote, and with the reaction time
Increase, be that the current strength amplification that each layer silicon rod applies also gradually is incremented by.In order to keep the temperature in reduction furnace 5 constant, often
Hour is increased the current strength that every layer of silicon rod applies with default current strength amplification.
Specifically, the 1st layer of the first current strength amplification of silicon rod is 3A/h；2nd layer of the second current strength amplification of silicon rod
It is 4A/h；3rd layer of the 3rd current strength amplification of silicon rod is 6A/h；4th layer of the 4th current strength amplification of silicon rod is 8A/h.
During 0-39 hours that gaseous mixture is reacted in reduction furnace 5, uniformly applied on each layer silicon rod per hour
Plus the electric current amplification of (X) A/h, X is variable, can be that response situation is set according to the time of reduction reaction.
If gaseous mixture is reacted to 40 hours in reduction furnace 5, the current strength applied on each layer silicon rod is Y, works as mixing
When gas is reacted to 41 hours in the reduction furnace 5, according to above-mentioned setting, the electric current of (Y+3) A/h is applied to the 1st layer of silicon rod, to the
2 layers of silicon rod apply the electric current of (Y+4) A/h, and the electric current of (Y+6) A/h is applied to the 3rd layer of silicon rod, and (Y+8) is applied to the 4th layer of silicon rod
The electric current of A/h；By that analogy, until reduction furnace blowing out.
When the gaseous mixture of trichlorosilane and hydrogen is reacted to 40h in reduction furnace 5, feed preheater is synchronously lowered into
The high-temperature tempering flow of 130 DEG C of 2, and open tail gas heat exchanger charging bypass 6, be used to by temperature of charge control 100 DEG C-
Between 160 DEG C.
The 5-10h before reduction furnace blowing out, by reduction furnace feeding gaseous mixture mol ratio（H2:SiHCl3）It is adjusted to 3-5：1, adjust
Kept during whole temperature-resistant in reduction furnace 5（900-1100℃）, until reduction furnace blowing out.
Embodiment 2
Embodiment 2 is the outside that tail gas hole is uniformly distributed in chassis of reducing furnace（At the circumference on chassis）Situation.48 pairs of silicon
Rod is arranged on chassis of reducing furnace, and the 3-6 in the middle of chassis of reducing furnace is justified to silicon rod as core（As the 1st layer silicon rod）, its
Remaining silicon rod is divided into 3 layers（Layer 2-4 silicon rod）, each layer silicon rod is with core circle in concentric circles distribution.
Reduction furnace operation control process is same as Example 1 in embodiment 2, will not be repeated here, embodiment 2 and embodiment
1 difference is that the control process for applying different current strength to each layer silicon rod using split-phase electric current is different, in embodiment 2, adopts
It is as follows to the control process that each layer silicon rod applies different current strength with split-phase electric current：
The outside of chassis of reducing furnace is uniformly distributed in due to tail gas hole（At the circumference on chassis）, more close on the silicon rod in tail gas hole
Temperature it is higher, the temperature of thermal field around it is higher, therefore, in order to keep in reduction furnace 5 the balanced gentle field of thermal field balanced, according to
The distance justified with the core, is gradually reduced according to the current strength from the close-by examples to those far off to the applying of each layer silicon rod, and to each layer
The current strength amplification that silicon rod applies gradually is successively decreased.In order to keep the temperature in reduction furnace 5 constant, every layer of silicon rod is applied per hour
Plus current strength increased with default current strength amplification.
Specifically, the 1st layer of the first current strength amplification of silicon rod is 7A/h；2nd layer of the second current strength amplification of silicon rod
It is 5A/h；3rd layer of the 3rd current strength amplification of silicon rod is 4A/h；4th layer of the 4th current strength amplification of silicon rod is 3A/h.
During 0-39 hours that mixed gas are reacted in reduction furnace 5, uniformly apply on each layer silicon rod per hour
(X) the electric current amplification of A/h, X is variable, can be that response situation is set according to the time of reduction reaction.
If mixed gas are reacted to 40 hours in reduction furnace 5, the electric current applied on each layer silicon rod is Y, works as gaseous mixture
When body is reacted to 41 hours in reduction furnace 5, according to above-mentioned setting, the electric current of (Y+7) A/h is applied to the 1st layer of silicon rod, to the 2nd
Layer silicon rod applies the electric current of (Y+5) A/h, and the electric current of (Y+4) A/h is applied to the 3rd layer of silicon rod, and (Y+3) A/ is applied to the 4th layer of silicon rod
The electric current of h；By that analogy, until reduction furnace blowing out.
Every production target in embodiment 1,2 and existing reduction furnace operation control technique is as shown in table 1.
Table 1
It can be seen from Table 1 that, embodiment 1,2 in terms of the reduction furnace number of falling stove, the rate of falling rod and cauliflower material occupation rate significantly
Decline, especially the rate of falling rod is greatly reduced, so that disposable material yield is lifted, production cost declines, the labour intensity of employee
Reduce, product apparent mass lifting, while also greatly improving job safety coefficient.Additionally, embodiment 1,2 is in polysilicon yield
On be substantially improved, so as to reduce production cost.The atomization time started is delayed, so as to shorten atomization duration, improve product quality.
Compared with prior art, this method is by controlling pressure, temperature and the trichlorosilane of reduction furnace and the stream of hydrogen
Amount and proportioning, feeding temperature is controlled by adjusting existing equipment, and reacting polysilicon hydrogen reduction can be rapidly performed by well,
Reduce because situations such as heterogeneity phantom inequality and exhaust temperature excessively high caused stove, silicon meat are abnormal and are atomized.By adjusting work
Skill parameter and system control parameters, solve the problems, such as thermal field in reduction furnace, gas field distribution and the too high problem of exhaust temperature, it is ensured that
Heat energy is rationally utilized, the proportioning of Optimization of Hydrogen and trichlorosilane, reducing energy consumption, reduction furnace is grown under existence conditions
Phase effective high-efficiency operation.
It is understood that the embodiment of above principle being intended to be merely illustrative of the present and the exemplary implementation for using
Mode, but the invention is not limited in this.For those skilled in the art, essence of the invention is not being departed from
In the case of god and essence, various changes and modifications can be made therein, and these variations and modifications are also considered as protection scope of the present invention.
Claims (9)
1. a kind of reduction furnace progress control method, it is characterised in that silicon rod layer distributed in reduction furnace, methods described include with
Lower step：
Initial pressure in reduction furnace is set to 0.45-0.6MPa, initial temperature is set to 1120-1150 DEG C；
Control trichlorosilane and hydrogen persistently feed, and form gaseous mixture, and in reduction furnace running, the gaseous mixture is held
It is continuous to be delivered in reduction furnace, so that the gaseous mixture is persistently reacted in reduction furnace；
In 0-5 hours that the gaseous mixture is delivered to reduction furnace, by the temperature control in reduction furnace at 900-1100 DEG C；
When the gaseous mixture is reacted to 30-60 hours in reduction furnace, according to the gentle field distribution of heterogeneity phantom in reduction furnace, often
Certain interval of time applies the electric current of varying strength to each layer silicon rod in reduction furnace, to ensure the balanced gentle field of thermal field in reduction furnace
Equilibrium, and the temperature in reduction furnace is maintained at 900-1100 DEG C, until reduction furnace blowing out；
When the gaseous mixture initially being delivered into reduction furnace, hydrogen and the mol ratio of trichlorosilane are 2-10 in the gaseous mixture：
1；
The gaseous mixture being delivered to 0-5 hours of reduction furnace in, by hydrogen in the gaseous mixture and trichlorosilane mole
Than being adjusted to 2-5：1, and keep the mol ratio；
5-10 hours before reduction furnace blowing out, hydrogen is adjusted with the mol ratio of trichlorosilane in being delivered to the gaseous mixture of reduction furnace
It is 3-5：1, until reduction furnace blowing out.
2. the method for claim 1, it is characterised in that tail gas hole is arranged in the middle of chassis of reducing furnace, silicon rod and tail gas
Hole is in concentric circles layer distributed；
The electric current for applying varying strength to each layer silicon rod in reduction furnace at interval of a period of time, specifically includes：
Using split-phase current control, electric current is applied with default current strength amplification to every layer of silicon rod in reduction furnace per hour, and
According to from the close-by examples to those far off, the current strength amplification of each layer silicon rod is gradually incremented by with the distance away from tail gas hole.
3. method as claimed in claim 2, it is characterised in that the current strength amplification of each layer silicon rod is 3-8A/h.
4. the method for claim 1, it is characterised in that tail gas hole is uniformly distributed in the outside of chassis of reducing furnace, will be also
Multipair silicon rod in the middle of former furnace hearth plate is justified as core, and used as ground floor, remaining silicon rod layer distributed, and with the core
Circle is distributed in concentric circles；
The electric current for applying varying strength to each layer silicon rod in reduction furnace at interval of a period of time, specifically includes：
Using split-phase current control, electric current is applied with default current strength amplification to every layer of silicon rod in reduction furnace per hour, and
According to the distance justified with the core from the close-by examples to those far off, the current strength amplification of each layer silicon rod is gradually successively decreased.
5. method as claimed in claim 4, it is characterised in that the current strength amplification of each layer silicon rod is 0-8A/h.
6. the method for claim 1, it is characterised in that initial when the gaseous mixture is delivered into reduction furnace, it is described mixed
The mol ratio for closing hydrogen and trichlorosilane in gas is 6-8：1.
7. the method as described in claim any one of 1-6, it is characterised in that when the gaseous mixture is reacted in reduction furnace
At 30-60 hours, methods described also includes：
Reduce water-carrying capacity on the high temperature for entering feed preheater, and open the charging of tail gas heat exchanger and bypass, be used to be delivered to
The temperature control of the trichlorosilane of reduction furnace and the gaseous mixture of hydrogen is at 100 DEG C -160 DEG C.
8. method as claimed in claim 7, it is characterised in that reduce water-carrying capacity on the high temperature for entering feed preheater, and open
The charging bypass of tail gas heat exchanger is opened, the trichlorosilane for being used to be delivered to reduction furnace exists with the temperature control of the gaseous mixture of hydrogen
120℃-150℃。
9. the method as described in claim any one of 1-6, it is characterised in that be set to the initial pressure in reduction furnace
0.55MPa, initial temperature is set to 1130-1140 DEG C.
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| CN109319787B (en) * | 2018-11-02 | 2021-12-21 | 中国南玻集团股份有限公司 | Reduction device and process for efficiently producing polycrystalline silicon |
| CN115092932B (en) * | 2022-07-04 | 2023-08-22 | 衡阳凯新特种材料科技有限公司 | Reduction furnace for producing polycrystalline silicon and feeding control method |
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| CN201473328U (en) * | 2009-08-10 | 2010-05-19 | 上海森和投资有限公司 | Tail gas outlet structure of polysilicon hydrogen reducing furnace |
| CN101759185A (en) * | 2009-12-31 | 2010-06-30 | 江苏中能硅业科技发展有限公司 | Method for manufacturing polysilicon silicon rod |
| CN101870471A (en) * | 2010-07-08 | 2010-10-27 | 江苏中能硅业科技发展有限公司 | High-efficiency large polycrystalline silicon reducing furnace |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN201473328U (en) * | 2009-08-10 | 2010-05-19 | 上海森和投资有限公司 | Tail gas outlet structure of polysilicon hydrogen reducing furnace |
| CN101759185A (en) * | 2009-12-31 | 2010-06-30 | 江苏中能硅业科技发展有限公司 | Method for manufacturing polysilicon silicon rod |
| CN101870471A (en) * | 2010-07-08 | 2010-10-27 | 江苏中能硅业科技发展有限公司 | High-efficiency large polycrystalline silicon reducing furnace |
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