CN104860315A - Reduction furnace operation control method - Google Patents
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- CN104860315A CN104860315A CN201410066852.0A CN201410066852A CN104860315A CN 104860315 A CN104860315 A CN 104860315A CN 201410066852 A CN201410066852 A CN 201410066852A CN 104860315 A CN104860315 A CN 104860315A
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Abstract
The invention provides a reduction furnace operation control method. The method comprises setting initial pressure in a range of 0.45-0.6MPa in a reduction furnace, setting an initial temperature in a range of 1120-1150 DEG C, continuously feeding trichlorosilane and hydrogen to form mixed gas, continuously conveying the mixed gas into the reduction furnace in reduction furnace operation, carrying out a continuous reaction process on the mixed gas in the reduction furnace, controlling a reduction furnace temperature in a range of 900-1100 DEG C in 0-5h after conveying of the mixed gas into the reduction furnace, when the mixed gas undergoes a reaction in the reduction furnace for 30-60h, according to distribution of a hot field and a gas field in the reduction furnace, applying different intensity of currents for all layers of silicon rods in the reduction furnace at time intervals so that equalization of the hot field and the gas field in the reduction furnace are kept, and keeping a reduction furnace temperature in a range of 900-1100 DEG C until the reduction furnace is stopped.
Description
Technical field
The present invention relates to polycrystalline reduction technical field, be specifically related to a kind of production of polysilicon
Reduction furnace progress control method in process.
Background technology
At present, in polysilicon production process, the maximum reduction furnace run both at home and abroad is 36 to rod, and existing 36 run in Controlling Technology to excellent reduction furnace, affect by gas field in stove, nearly tail gas hole place silicon rod temperature is higher, causes the gentle field distribution of thermal field in stove unbalanced, and the uneven normal operation directly restricting reduction furnace of the gentle field distribution of thermal field, cause atomization, make reduction furnace environment become muddy, produce fine silica powder, and easily fall stove.The silica flour produced brings a lot of disadvantageous effect to reducing furnace system equipment and lower procedure, proposes serious challenge to quality product.
Along with the development of polycrystalline reduction technology, reduction furnace is more and more tending towards maximizing, and application 48 is the development trend of polycrystalline reduction technique to the polycrystalline silicon reducing furnace of rod.The 48 pairs of excellent reduction furnaces increase due to horizontal volume, and silicon rod increasing number, in reduction furnace, the unbalanced phenomenon of the gentle field distribution of thermal field can be more outstanding, more easily produces abnormal problem such as atomization grade.
Therefore, need badly and be a kind ofly applicable to 48 control program is run, to solve the problems of the technologies described above to the reduction furnace of excellent reduction furnace.
Summary of the invention
The present invention is directed to above shortcomings in prior art, a kind of reduction furnace progress control method is provided, in order to solve 48 problems to the gentle field distribution inequality of large-scale reduction furnace thermal field of rod.
The present invention, for solving the problems of the technologies described above, adopts following technical scheme:
The invention provides a kind of reduction furnace progress control method, silicon rod is layer distributed in reduction furnace, said method comprising the steps of:
Original pressure in reduction furnace is set to 0.45-0.6MPa, and initial temperature is set to 1120-1150 DEG C;
Control trichlorosilane and hydrogen continue charging, form gas mixture, and in reduction furnace operational process, are continued to be delivered in reduction furnace by described gas mixture, continue to react to make described gas mixture in reduction furnace;
Described gas mixture is delivered in 0-5 hour of reduction furnace, the temperature in reduction furnace is controlled at 900-1100 DEG C;
When described gas mixture, in reduction furnace, be reacted to 30-60 constantly little, according to the gentle field distribution of heterogeneity phantom in reduction furnace, at interval of the electric current of for some time to layer silicon rod applying varying strength each in reduction furnace, to ensure that in reduction furnace, the balanced gentle field of thermal field is balanced, and the temperature in reduction furnace is remained on 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 and tail gas hole are concentric(al) circles layer distributed; Described at interval of the electric current of for some time to layer silicon rod applying varying strength each in reduction furnace, specifically comprise:
Adopt phase-splitting current control, per hour with the strength of current amplification preset, electric current applied to every layer of silicon rod in reduction furnace, and according to the distance apart from tail gas hole from the close-by examples to those far off, the strength of current amplification of each layer silicon rod increases progressively gradually.
Preferably, the strength of current amplification of described each layer silicon rod is 3-8A/h.
Preferably, tail gas hole is uniformly distributed in the outside of chassis of reducing furnace, using the multipair silicon rod in the middle of chassis of reducing furnace as core circle, and as the first layer, and remaining silicon rod layer distributed, and distribute in concentric(al) circles with described core circle;
Described at interval of the electric current of for some time to layer silicon rod applying varying strength each in reduction furnace, specifically comprise:
Adopt phase-splitting current control, per hour with the strength of current amplification preset, electric current is applied to every layer of silicon rod in reduction furnace, and according to the distance with described core circle from the close-by examples to those far off, the strength of current amplification of each layer silicon rod is successively decreased gradually.
Preferably, the strength of current amplification of described each layer silicon rod is 0-8A/h.
Preferably, when initially described gas mixture being delivered to reduction furnace, in described gas mixture, the mol ratio of hydrogen and trichlorosilane is 2-10:1;
Described method also comprises:
Described gas mixture is delivered in 0-5 hour of reduction furnace, the mol ratio of hydrogen and trichlorosilane in described gas mixture is adjusted to 2-5:1, and keeps this mol ratio;
5-10 hour before reduction furnace blowing out, is adjusted to 3-5:1, until reduction furnace blowing out by the mol ratio of hydrogen and trichlorosilane in the gas mixture being delivered to reduction furnace.
Preferably, when initially described gas mixture being delivered to reduction furnace, in described gas mixture, the mol ratio of hydrogen and trichlorosilane is 6-8:1.
Further, when described gas mixture, in reduction furnace, be reacted to 30-60 constantly little, and described method also comprises:
Discharge on the high temperature reducing to enter feed preheater, and open the charging bypass of tail gas heat exchanger, the temperature in order to the gas mixture by the trichlorosilane and hydrogen that are delivered to reduction furnace controls at 100 DEG C-160 DEG C.
Preferably, discharge on the high temperature reducing to enter feed preheater, and open the charging bypass of tail gas heat exchanger, the temperature in order to the gas mixture by the trichlorosilane and hydrogen that are delivered to reduction furnace controls at 120 DEG C-150 DEG C.
Preferably, the original pressure in reduction furnace is set to 0.55MPa, and initial temperature is set to 1130-1140 DEG C.
The present invention is by arranging silicon rod layering in reduction furnace, when the gas mixture of trichlorosilane and hydrogen, in reduction furnace, be reacted to 30-60 constantly little, according to the gentle field distribution of thermal field in stove, at interval of the electric current of for some time to layer silicon rod applying varying strength each in reduction furnace, reach the object of the gentle field of thermal field in equalizing furnace, reduce atomization and the rate of falling stove, reduction furnace can be shortened 2-3 hour unproductive time, reduction furnace effective rate of utilization raising about 1.2%; Reduce the loss of the auxiliary material such as graphite, silicon core, promote disposable material productive rate, reduce electrode damage rate, reduce production cost; Reduce the number of times of the dismounting reduction furnace that stove causes, reduce working strength and human cost; Reduce polysilicon surface to pollute, Improving The Quality of Products; Reduce silicon rod in disassembly process to fall, clear up silica flour and dodge the emergency risks such as quick-fried, raising production security; Reduce because atomization produces silica flour to the infringement of lower procedure, improve equipment performance.
Accompanying drawing explanation
The structural representation of the polycrystalline silicon reduction system that Fig. 1 provides for the embodiment of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the present invention, carry out clear, complete description to the technical scheme in the present invention, obviously, described embodiment is a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not making creative work, all belongs to the scope of protection of the invention.
Production of polysilicon is by being delivered in reduction furnace by the gas mixture of trichlorosilane and hydrogen by nozzle, carries out reduction reaction with the silicon rod in reduction furnace.The chassis of reduction furnace is distributed with multipair silicon rod, and the gas mixture of trichlorosilane and hydrogen, under certain temperature and pressure condition, with silicon rod generation reduction reaction, finally obtains polysilicon.
The embodiment of the present invention provides a kind of reduction furnace progress control method, in order to solve the problems such as uneven atomization, the stove caused of the interior thermal field of large-scale reduction furnace (48 pairs of reduction furnaces), thus improves the production efficiency of reduction furnace and the seed output and quality of polysilicon product.
The structural representation of a kind of polycrystalline silicon reduction system that Fig. 1 uses for enforcement embodiment of the present invention reduction furnace progress control method, as shown in Figure 1, described polycrystalline silicon reduction system comprises reduction furnace 5, feed preheater 2, tail gas heat exchanger 4, jacket pipe 7, first mixing device 1 and the second mixing device 3.In described polycrystalline silicon reduction system, water on the high temperature of 130 DEG C in flash drum (not illustrating in figure) is passed into jacket pipe 7 and carry out thermal energy exchange with high-temperature tail gas out from reduction furnace 5, after thermal energy exchange, high-temperature tail gas enters in tail gas heat exchanger 4, wherein on a road high temperature, water directly enters return main and becomes high-temperature tempering and turn back to flash drum, and on another road high temperature, water enters and enters return main again after the material formed after feed preheater 2 mixes with hydrogen and trichlorosilane carries out thermal energy exchange and become high-temperature tempering and turn back to flash drum.In reduction furnace 5, multipair silicon rod layering is arranged.Below in conjunction with Fig. 1, the working process of polycrystalline silicon reduction system is described in detail.
Hydrogen and liquid trichlorosilane are after the first mixing device 1 mixes, enter feed preheater 2, thermal energy exchange is carried out with water on the road high temperature entering feed preheater 2, liquid trichlorosilane gasification is gas, thus obtaining the gas mixture of hydrogen and trichlorosilane, this gas mixture carries out secondary mixing through the second mixing device 3 again.The mixed gas mixture of secondary can be divided into two-way according to the unlatching of the charging bypass 6 of tail gas heat exchanger, one road gas mixture enters tail gas heat exchanger 4 and carries out thermal energy exchange with the high-temperature tail gas entering tail gas heat exchanger 4, is delivered to reduction furnace 5 more again after thermal energy exchange via after tail gas heat exchanger 4; Another road gas mixture is then directly delivered to reduction furnace 5 via the charging bypass 6 of tail gas heat exchanger 4.During initial charge, the reaction in reduction furnace 5 not yet starts, and tail gas heat exchanger 4 only plays the effect of transmission gas mixture, along with the carrying out of reaction, the high-temperature tail gas produced in reduction furnace from reduction furnace 5 out after through entering tail gas heat exchanger 4 by jacket pipe 7.On the one hand, flow through water and high-temperature tail gas on the high temperature in jacket pipe 7 and carry out thermal energy exchange, thus reduce the temperature of high-temperature tail gas; On the other hand, a part flow through jacket pipe 7 high temperature on water be transported to feed preheater 2, in order to utilize the heat energy of water on high temperature to gasify to the trichlorosilane in material, thus to the heating material entered in feed preheater 2.
Below in conjunction with Fig. 1, reduction furnace progress control method of the present invention is described in detail.As shown in Figure 1, the method can comprise the following steps:
Step 101, the original pressure in reduction furnace is set to 0.45-0.6MPa, and initial temperature is set to 1120-1150 DEG C.
Preferably, the original pressure in reduction furnace is set to 0.55MPa, and initial temperature is set to 1130-1140 DEG C.
Step 102, controls trichlorosilane and hydrogen continues charging, forms gas mixture, and in reduction furnace operational process, is continued to be delivered in reduction furnace by described gas mixture, continue to react to make described gas mixture in reduction furnace.
Concrete, first control the hydrogen feed in hydrogen feed pipeline, such as, hydrogen is first delivered to the first mixing device 1 with the flow of 15-25kg/h, be delivered in feed preheater 2 again, in hydrogen feed process, open the trichlorosilane feed valve on trichlorosilane feeding pipe gradually, to control the feed rate of trichlorosilane.
Trichlorosilane normality is liquid, the hydrogen of gaseous state and liquid trichlorosilane are delivered to feed preheater 2 through the first mixing device 1, the two carries out thermal energy exchange with high-temperature tempering in feed preheater 2, makes liquid trichlorosilane gasification be gas, obtains the gas mixture of trichlorosilane and hydrogen.
This gas mixture exports the second mixing device 3 to from feed preheater 2, carries out secondary mixing, and further guarantee trichlorosilane fully mixes with hydrogen.Be transported to tail gas heat exchanger 4 through the mixed gas mixture of the second mixing device 3, then be delivered in reduction furnace 5 by exporting in tail gas heat exchanger 4 and passing through nozzle (not illustrating in figure).
In order to reach desirable reaction result, when initially described gas mixture being delivered to reduction furnace 5, can the mol ratio of hydrogen and trichlorosilane in the described gas mixture entering reduction furnace be controlled at 2-10:1, such as, can by the flow control of hydrogen be realized at 0-250kg/h and by the flow control of trichlorosilane at 0-5500kg/h.Preferably, the mol ratio of hydrogen and trichlorosilane in described gas mixture is controlled at 6-8:1.
Step 103, being delivered in 0-5 hour of reduction furnace by described gas mixture, controls the temperature in reduction furnace at 900-1150 DEG C.
Concrete, within 0-5 hour (i.e. gas mixture carry out reacting in reduction furnace 0-5 hour) described gas mixture being delivered to reduction furnace, every 1 hour, need by applying electric current to the silicon rod in reduction furnace with certain strength of current amplification, thus silicon rod is heated, ensure temperature of reaction.Such as, during initial charge, each layer silicon rod in reduction furnace applies respectively the initial current of 100A, afterwards, being that each layer silicon rod applies electric current according to the strength of current amplification of 10A/h, starting to apply 1st hour of electric current with strength of current amplification, each layer silicon rod applying 110A, within 2nd hour, on each layer silicon rod, apply 120A, by that analogy.
Preferably, phase-splitting current control can be passed through, for each layer silicon rod applies electric current.Phase-splitting current control refers to, whole silicon rod is divided into many groups, and the logarithm often organizing silicon rod is identical, and often organize silicon rod and be a phase silicon rod, the strength of current applied for every phase silicon rod is identical, such as, 48 pairs of silicon rods is divided into 6 phases, often comprises 8 pairs of silicon rods mutually.The object of phase-splitting current control is, a fairly large number of silicon rod is split as many groups, is convenient to control.
In 0-5 hour that carries out reacting in reduction furnace, the temperature in reduction furnace 5 is controlled at 900-1150 DEG C, significantly can reduce initial operating stage and fall the abnormal conditions such as stove and the stripping of silicon core.
Step 104, when described mixed gas, in reduction furnace, be reacted to 30-60 constantly little, according to the gentle field distribution of heterogeneity phantom in reduction furnace, at interval of the electric current of for some time to each layer silicon rod applying varying strength, to ensure that in reduction furnace, thermal field is balanced, and the temperature in reduction furnace is remained on 900-1100 DEG C, until reduction furnace blowing out.
Concrete, when described mixed gas, in reduction furnace, be reacted to 30-60 constantly little, according to the gentle field distribution of heterogeneity phantom in reduction furnace, at interval of 1 hour, each layer silicon rod applied to the electric current of varying strength, to ensure that in reduction furnace, thermal field is balanced.
Wherein, the distribution mode of tail gas hole on chassis of reducing furnace mainly contains 2 kinds, a kind of centre being tail gas hole and being positioned at chassis of reducing furnace, a kind of outside being tail gas hole and being uniformly distributed in chassis of reducing furnace, i.e. the circumference place on chassis.For these two kinds of tail gas pore distribution modes, processing mode silicon rod being applied to electric current is different, elaborates respectively below to applying mode for the electric current under these two kinds of tail gas pore distribution modes.
Be positioned at the situation in the middle of chassis of reducing furnace for tail gas hole, silicon rod and tail gas hole are concentric(al) circles layer distributed (namely silicon rod is centered by tail gas hole, distributes in concentric circles around tail gas hole).The electric current each layer silicon rod being applied to varying strength per hour, specifically comprise: adopt phase-splitting current control, per hour to every layer of silicon rod with preset strength of current amplification apply electric current, preferably, the strength of current amplification of every one deck silicon rod is 3-8A/h, and according to the distance with distance tail gas hole from the close-by examples to those far off, the strength of current amplification of each layer silicon rod increases progressively gradually.
By according to the distance apart from tail gas hole from the close-by examples to those far off, the strength of current amplification that each layer silicon rod applies is increased progressively gradually, effectively can reduce silicon rod temperature in stove that the gentle field distribution inequality in warm field in stove causes and differ and the problem such as local atomization, raising silicon rod quality.
Tail gas hole is uniformly distributed in the situation in the outside of chassis of reducing furnace, using some in the middle of chassis of reducing furnace to (such as 3-6 to) silicon rod as core circle, remaining silicon rod with described core circle in concentric(al) circles layer distributed in the periphery that core is round.The electric current each layer silicon rod being applied to varying strength per hour, specifically comprise: adopt phase-splitting current control, per hour to every layer of silicon rod with preset strength of current amplification apply electric current, preferably, the strength of current amplification of every one deck silicon rod is 0-8A/h, and according to the distance with described core circle from the close-by examples to those far off, the strength of current amplification of each layer silicon rod is successively decreased gradually.
By according to and described core circle distance from the close-by examples to those far off, the strength of current amplification that each layer silicon rod applies is successively decreased gradually, effectively can reduce silicon rod temperature in stove that the gentle field distribution inequality in warm field in stove causes and differ and the problem such as local atomization, raising silicon rod quality.
It should be noted that, the temperature of reduction furnace 5 is being controlled after 900-1150 DEG C, arrive according to the gentle field distribution of heterogeneity phantom in reduction furnace, before electric current to each layer silicon rod applying varying strength per hour, still need according to the mode described in step 103, every 1 hour, for the silicon rod in reduction furnace applies electric current with identical strength of current amplification, silicon rod is heated, to ensure temperature of reaction.
In polysilicon production process, if the proportioning of hydrogen and trichlorosilane is too small, then the growth velocity of polysilicon is too fast, is unfavorable for the control of surface topography and the suppression of reversed reaction and the control to atomization; If the proportioning of hydrogen and trichlorosilane is excessive, then limits the speed of growth of polysilicon, affect output.In order to control within rational scope by the growth velocity of polysilicon, along with the carrying out of reaction, polysilicon diameter increases gradually, needs to adjust accordingly the proportioning of hydrogen and trichlorosilane.Further, described method is further comprising the steps of:
The hydrogen being 2-10:1 by initial ratio (i.e. mol ratio) and the gas mixture of trichlorosilane are delivered to reduction furnace 5, in 0-5 hour that reacts at described gas mixture, the doses of synchronization control hydrogen and trichlorosilane, the proportioning of the two is decreased to 2-5:1 gradually, and keeps this proportioning in follow-up reaction process.
5-10 hour before reduction furnace blowing out, is adjusted to 3-5:1 by the mol ratio of hydrogen and trichlorosilane in the gas mixture being delivered to reduction furnace 5.
In order to reduce the temperature of tail gas further, and the heat energy in tail gas is effectively used, the jacket pipe 7 be arranged between reduction furnace 5 with tail gas heat exchanger 4 can be connected with feed preheater 2, in order to will flow through jacket pipe 7 a road high temperature on water introduce in feed preheater 2, to heat the material entered in feed preheater 2 (mixture of hydrogen and trichlorosilane).
When gas mixture, in reduction furnace 5, be reacted to 30-60 constantly little, described method also comprises: the flow of water on the high temperature reducing to enter feed preheater 2, and open the charging bypass 6 of tail gas heat exchanger, the temperature in order to the gas mixture by the trichlorosilane and hydrogen that are delivered to reduction furnace 5 controls at 100 DEG C-160 DEG C.It should be noted that, in the subsequent reactions process of reduction furnace, the temperature of gas mixture is controlled at 100 DEG C-160 DEG C always, until reduction furnace blowing out.
Feeding temperature is controlled at 100 DEG C-160 DEG C, can effectively postpone to be atomized the time opening, for the atomization phenomenon of control reduction furnace, there is better effects.
Concrete, in described polycrystalline silicon reduction system, feed preheater 2 is communicated with water return pipeline, and the other end of water return pipeline is communicated with return main, and on the high temperature entering feed preheater 2, water enters through water return pipeline in return main, formation high-temperature tempering.Wherein, described water return pipeline is provided with valve 8.By regulated valve 8, the flow of water on the high temperature that can control to enter feed preheater 2, by reducing the flow of water on the high temperature for carrying out thermal energy exchange with the material entered in feed preheater 2, namely, the flow of water on the high temperature of the trichlorosilane that gasifies is reduced, vaporized trichlorosilane can be made to reduce, thus reduce the temperature of material, final reduction enters the temperature of the gas mixture of reduction furnace.
After opening the charging bypass 6 of tail gas heat exchanger 4, a part of material can be made not enter tail gas heat exchanger 4, thermal energy exchange is not carried out with tail gas, therefore comparatively to enter the temperature of the material carrying out thermal energy exchange in tail gas heat exchanger low for temperature, this partial material with enter again in reduction furnace 5 after tail gas heat exchanger 4 carries out the mixing of materials of thermal energy exchange, thus reduce and be delivered to the temperature of the material of reduction furnace 5.
It should be noted that, on the high temperature reducing to enter feed preheater 2, the flow of water and these two operation stepss of charging bypass 6 of opening tail gas heat exchanger 4 can synchronously perform, and also can perform one of them separately.
Preferably, the temperature of the gas mixture of the trichlorosilane and hydrogen that are delivered to reduction furnace 5 can be controlled at 120 DEG C-150 DEG C, and in reduction furnace subsequent reactions process, the temperature of gas mixture be controlled at 120 DEG C-150 DEG C always, until reduction furnace blowing out.
Can be found out by above-mentioned steps, reduction furnace progress control method provided by the invention is by arranging silicon rod layering in reduction furnace, and according to the gentle field distribution of thermal field in stove, the electric current each layer silicon rod being applied to varying strength per hour, reach the object of the gentle field of thermal field in equalizing furnace, reduce atomization and the rate of falling stove, separate unit reduction furnace can be shortened 2-3 hour unproductive time, reduction furnace effective rate of utilization raising about 1.2%; Reduce the loss of the auxiliary material such as graphite, silicon core, promote disposable material productive rate, reduce electrode damage rate, reduce production cost; Reduce the number of times of the dismounting reduction furnace that stove causes, reduce working strength and human cost; Reduce polysilicon surface to pollute, Improving The Quality of Products; Reduce silicon rod in disassembly process to fall, clear up silica flour and dodge the emergency risks such as quick-fried, raising production security; Reduce because atomization produces silica flour to the infringement of lower procedure, improve equipment performance.
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
Embodiment 1
Embodiment 1 is positioned at the situation in the middle of chassis of reducing furnace for tail gas hole.48 pairs of silicon rods are divided into 4 layers to be arranged on chassis of reducing furnace, and each layer silicon rod and tail gas hole are that concentric(al) circles distributes.
Original pressure in reduction furnace 5 is set to 0.55MPa, and initial temperature is set to 1120-1150 DEG C.The initial flow of hydrogen is 15-25kg/h, when fill process, open trichlorosilane variable valve gradually, trichlorosilane and hydrogen is made in feed preheater 2, to carry out thermal energy exchange with water on high temperature, obtain the gas mixture of trichlorosilane and hydrogen, described gas mixture is delivered in reduction furnace 5 via tail gas heat exchanger 4 again, thus realizes reduction furnace 5 charging.
Initial when described gas mixture is delivered to reduction furnace 5, the mol ratio of the gas mixture of hydrogen and trichlorosilane is controlled at 6-8:1.Preferably, in 3 hours that start to produce, the temperature in reduction furnace 5 is controlled at 900-1150 DEG C.During initial charge, each layer silicon rod all applies the initial current of 100A.
When the gas mixture of trichlorosilane and hydrogen is reacted to 40h in reduction furnace 5, the usage quantity of synchronization control hydrogen and trichlorosilane, makes the mol ratio of the gas mixture of hydrogen and trichlorosilane be reduced to 2-5:1 gradually, until stably manufactured.
When the gas mixture reaction of trichlorosilane and hydrogen proceeds to 40h, adopt phase-splitting current control, according to heterogeneity phantom in reduction furnace and gas Flow Field Distribution, the electric current each layer silicon rod being applied to varying strength per hour, to ensure that in reduction furnace, the balanced gentle field of thermal field is balanced.The control process adopting point phase current to apply different strength of current to each layer silicon rod is as follows:
Because tail gas hole is positioned at the middle part of chassis of reducing furnace, the temperature of more closing on the silicon rod in tail gas hole is higher, temperature of thermal field around this silicon rod is also higher, therefore, in order to keep the balanced gentle field of thermal field in reduction furnace 5 balanced, according to the distance with distance tail gas hole, according to order from the near to the remote, the strength of current that each layer silicon rod applies is increased gradually, and along with the increase in reaction times, the strength of current amplification applied for each layer silicon rod also increases progressively gradually.In order to keep the homo(io)thermism in reduction furnace 5, the strength of current applied every layer of silicon rod per hour is with the strength of current amplification preset increase.
Concrete, the first strength of current amplification of the 1st layer of silicon rod is 3A/h; Second strength of current amplification of the 2nd layer of silicon rod is 4A/h; 3rd strength of current amplification of the 3rd layer of silicon rod is 6A/h; 4th strength of current amplification of the 4th layer of silicon rod is 8A/h.
Gas mixture carries out in the process of 0-39 hour that reacts in reduction furnace 5, and the electric current amplification evenly applying (X) A/h on each layer silicon rod per hour, X is variable, can set according to the time of reduction reaction and response situation.
If gas mixture is reacted to 40 constantly little in reduction furnace 5, the strength of current that each layer silicon rod applies is Y, when mixed gas is reacted to 41 constantly little in reduction furnace 5, according to above-mentioned setting, 1st layer of silicon rod is applied to the electric current of (Y+3) A/h, 2nd layer of silicon rod is applied to the electric current of (Y+4) A/h, the 3rd layer of silicon rod is applied to the electric current of (Y+6) A/h, the 4th layer of silicon rod is applied to the electric current of (Y+8) A/h; By that analogy, until reduction furnace blowing out.
When the gas mixture of trichlorosilane and hydrogen is reacted to 40h in reduction furnace 5, synchronously reduce the high-temperature tempering flow entering 130 DEG C of feed preheater 2, and open the charging bypass 6 of tail gas heat exchanger, in order to be controlled between 100 DEG C-160 DEG C by temperature of charge.
5-10h before reduction furnace blowing out, by reduction furnace feeding gas mixture mol ratio (H
2: SiHCl
3) be adjusted to 3-5:1, keep in adjustment process temperature-resistant in reduction furnace 5 (900-1100 DEG C), until reduction furnace blowing out.
Embodiment 2
Embodiment 2 is uniformly distributed in the situation in the outside (the circumference place on chassis) of chassis of reducing furnace for tail gas hole.48 pairs of silicon rods are arranged on chassis of reducing furnace, and the 3-6 of chassis of reducing furnace centre is justified (being the 1st layer of silicon rod) to silicon rod as core, and remaining silicon rod is divided into 3 layers (layer 2-4 silicon rods), and each layer silicon rod and this core circle distribute in concentric(al) circles.
In embodiment 2, reduction furnace operation control process is identical with embodiment 1, do not repeat them here, embodiment 2 is with the difference of embodiment 1, the control process adopting point phase current to apply different strength of current to each layer silicon rod is different, in embodiment 2, the control process adopting point phase current to apply different strength of current to each layer silicon rod is as follows:
Because tail gas hole is uniformly distributed in the outside (the circumference place on chassis) of chassis of reducing furnace, the temperature of more closing on the silicon rod in tail gas hole is higher, temperature of thermal field around it is higher, therefore, in order to keep the balanced gentle field of thermal field in reduction furnace 5 balanced, according to the distance with described core circle, according to from the close-by examples to those far off reducing gradually the strength of current that each layer silicon rod applies, and the strength of current amplification that each layer silicon rod applies is successively decreased gradually.In order to keep the homo(io)thermism in reduction furnace 5, the strength of current applied every layer of silicon rod per hour is with the strength of current amplification preset increase.
Concrete, the first strength of current amplification of the 1st layer of silicon rod is 7A/h; Second strength of current amplification of the 2nd layer of silicon rod is 5A/h; 3rd strength of current amplification of the 3rd layer of silicon rod is 4A/h; 4th strength of current amplification of the 4th layer of silicon rod is 3A/h.
In the process of 0-39 hour that mixed gas reacts in reduction furnace 5, the electric current amplification evenly applying (X) A/h on each layer silicon rod per hour, X is variable, can set according to the time of reduction reaction and response situation.
If mixed gas is reacted to 40 constantly little in reduction furnace 5, the electric current that each layer silicon rod applies is Y, when mixed gas is reacted to 41 constantly little in reduction furnace 5, according to above-mentioned setting, 1st layer of silicon rod is applied to the electric current of (Y+7) A/h, 2nd layer of silicon rod is applied to the electric current of (Y+5) A/h, the 3rd layer of silicon rod is applied to the electric current of (Y+4) A/h, the 4th layer of silicon rod is applied to the electric current of (Y+3) A/h; By that analogy, until reduction furnace blowing out.
Every productive capacity that embodiment 1,2 and existing reduction furnace run in Controlling Technology is as shown in table 1.
Table 1
Can be found out by table 1, embodiment 1,2 declines to a great extent in the reduction furnace number of falling stove, excellent rate and cauliflower material occupation rate, especially excellent rate significantly reduces, thus disposable material productive rate is promoted, production cost declines, the labour intensity of employee reduces, and product apparent mass promotes, and also greatly improves job safety coefficient simultaneously.In addition, embodiment 1,2 has and significantly promotes in polysilicon output, thus reduces production cost.The atomization time opening is delayed, thus shortens atomization duration, improves the quality of products.
Compared with prior art, present method is by controlling the pressure of reduction furnace, the flow of temperature and trichlorosilane and hydrogen and proportioning, feeding temperature is controlled by adjustment existing installation, polysilicon hydrogen reduction is reacted can carry out fast well, reduce because of situations such as heterogeneity phantom inequality and excessively high stove, silicon meat exception and the atomizations caused of exhaust temperature.By adjusting process parameter and system control parameters, solve the problem that thermal field in reduction furnace, the problem of gas field distribution and exhaust temperature are too high, ensure heat energy Appropriate application, the proportioning of Optimization of Hydrogen and trichlorosilane, reduce energy consumption, finally make the high-efficiency operation that reduction furnace can be permanently effective under existence conditions.
Be understandable that, the illustrative embodiments that above embodiment is only used to principle of the present invention is described and adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (10)
1. a reduction furnace progress control method, is characterized in that, silicon rod is layer distributed in reduction furnace, said method comprising the steps of:
Original pressure in reduction furnace is set to 0.45-0.6MPa, and initial temperature is set to 1120-1150 DEG C;
Control trichlorosilane and hydrogen continue charging, form gas mixture, and in reduction furnace operational process, are continued to be delivered in reduction furnace by described gas mixture, continue to react to make described gas mixture in reduction furnace;
Described gas mixture is delivered in 0-5 hour of reduction furnace, the temperature in reduction furnace is controlled at 900-1100 DEG C;
When described gas mixture, in reduction furnace, be reacted to 30-60 constantly little, according to the gentle field distribution of heterogeneity phantom in reduction furnace, at interval of the electric current of for some time to layer silicon rod applying varying strength each in reduction furnace, to ensure that in reduction furnace, the balanced gentle field of thermal field is balanced, and the temperature in reduction furnace is remained on 900-1100 DEG C, until reduction furnace blowing out.
2. the method for claim 1, is characterized in that, tail gas hole is arranged in the middle of chassis of reducing furnace, and silicon rod and tail gas hole are concentric(al) circles layer distributed;
Described at interval of the electric current of for some time to layer silicon rod applying varying strength each in reduction furnace, specifically comprise:
Adopt phase-splitting current control, per hour with the strength of current amplification preset, electric current applied to every layer of silicon rod in reduction furnace, and according to the distance apart from tail gas hole from the close-by examples to those far off, the strength of current amplification of each layer silicon rod increases progressively gradually.
3. method as claimed in claim 2, it is characterized in that, the strength of current amplification of described each layer silicon rod is 3-8A/h.
4. the method for claim 1, is characterized in that, tail gas hole is uniformly distributed in the outside of chassis of reducing furnace, using the multipair silicon rod in the middle of chassis of reducing furnace as core circle, and as the first layer, remaining silicon rod layer distributed, and distribute in concentric(al) circles with described core circle;
Described at interval of the electric current of for some time to layer silicon rod applying varying strength each in reduction furnace, specifically comprise:
Adopt phase-splitting current control, per hour with the strength of current amplification preset, electric current is applied to every layer of silicon rod in reduction furnace, and according to the distance with described core circle from the close-by examples to those far off, the strength of current amplification of each layer silicon rod is successively decreased gradually.
5. method as claimed in claim 4, it is characterized in that, the strength of current amplification of described each layer silicon rod is 0-8A/h.
6. the method for claim 1, is characterized in that, when initially described gas mixture being delivered to reduction furnace, in described gas mixture, the mol ratio of hydrogen and trichlorosilane is 2-10:1;
Described method also comprises:
Described gas mixture is delivered in 0-5 hour of reduction furnace, the mol ratio of hydrogen and trichlorosilane in described gas mixture is adjusted to 2-5:1, and keeps this mol ratio;
5-10 hour before reduction furnace blowing out, is adjusted to 3-5:1, until reduction furnace blowing out by the mol ratio of hydrogen and trichlorosilane in the gas mixture being delivered to reduction furnace.
7. method as claimed in claim 6, it is characterized in that, when initially described gas mixture being delivered to reduction furnace, in described gas mixture, the mol ratio of hydrogen and trichlorosilane is 6-8:1.
8. the method as described in any one of claim 1-7, is characterized in that, when described gas mixture, in reduction furnace, be reacted to 30-60 constantly little, and described method also comprises:
Discharge on the high temperature reducing to enter feed preheater, and open the charging bypass of tail gas heat exchanger, the temperature in order to the gas mixture by the trichlorosilane and hydrogen that are delivered to reduction furnace controls at 100 DEG C-160 DEG C.
9. method as claimed in claim 8, it is characterized in that, discharge on the high temperature reducing to enter feed preheater, and open the charging bypass of tail gas heat exchanger, the temperature in order to the gas mixture by the trichlorosilane and hydrogen that are delivered to reduction furnace controls at 120 DEG C-150 DEG C.
10. the method as described in any one of claim 1-7, is characterized in that, the original pressure in reduction furnace is set to 0.55MPa, and initial temperature is set to 1130-1140 DEG C.
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| CN109319787A (en) * | 2018-11-02 | 2019-02-12 | 中国南玻集团股份有限公司 | A kind of reduction apparatus and technique of efficient production polysilicon |
| CN115092932A (en) * | 2022-07-04 | 2022-09-23 | 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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| CN109319787A (en) * | 2018-11-02 | 2019-02-12 | 中国南玻集团股份有限公司 | A kind of reduction apparatus and technique of efficient production polysilicon |
| 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 |
| CN115092932A (en) * | 2022-07-04 | 2022-09-23 | 衡阳凯新特种材料科技有限公司 | Reduction furnace for producing polycrystalline silicon and feeding control method |
| 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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Application publication date: 20150826 Assignee: Xinte silicon based new materials Co.,Ltd. Assignor: XINTE ENERGY Co.,Ltd. Contract record no.: X2023990000586 Denomination of invention: A Method for Controlling the Operation of a Reduction Furnace Granted publication date: 20170707 License type: Common License Record date: 20230605 |
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