CN102608913B - System and method for controlling blowing out of reduction furnace in production of polycrystalline silicon - Google Patents
System and method for controlling blowing out of reduction furnace in production of polycrystalline silicon Download PDFInfo
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Abstract
The invention relates to a system and a method for controlling blowing out of a reduction furnace in the production of polycrystalline silicon. The blowing out control system comprises a magnetic force calculation module, a stress calculation module, a blowing out optimizing module and a control module, wherein the magnetic force calculation module is used for calculating maximum magnetic force when a silicon rod completely grows; the stress calculation module is used for calculating a minimum release stress when the silicon rod completely grows; the blowing out optimizing module is used for calculating blowing out optimizing time and blowing out optimizing temperature based on the maximum magnetic force that the silicon rod is suffered, and the minimum release stress of the silicon rod by utilizing an optimization algorithm; and the control module is used for controlling blowing out of the reduction furnace based on the calculated blowing out optimizing time and blowing out optimizing temperature. The system and the method for controlling blowing out provided by the invention can be used for shortening the time needs by material dropping and temperature lowering in the blowing out process, saving the cost, and improving the safety and stability of producing the polycrystalline silicon.
Description
Technical field
The present invention relates to a kind of polysilicon producing and reducing furnace blowing out control system and method thereof.
Background technology
Polysilicon, as a kind of semiconductor material, can be used as important photovoltaic material at present, and photovoltaic material can be directly changed into electric energy by sun power, for example solar cell.One of main method of producing polysilicon is at present improved Siemens.Improved Siemens produces rod-like polycrystal silicon by vapour deposition process.
Siemens Method reduction production well known in the prior art is: the trichlorosilane of vaporization mixes introducing polycrystalline silicon reducing furnace by a certain percentage with carrier gas hydrogen; Bar-like silicon core two ends in being positioned over reduction furnace are voltage in addition; Under certain temperature and pressure, at high temperature silicon wicking surface, trichlorosilane reacts generting element silicon with hydrogen mixed gas, and is deposited on silicon wicking surface, generate gradually the polycrystalline silicon rod of required specification, produce the accessory substances such as silicon tetrachloride, dichloro-dihydro silicon, hydrogen chloride simultaneously.
After polysilicon producing and reducing furnace start-up is moving, in the body of heater that reaction feed (being trichlorosilane and hydrogen mixed gas) enters reduction furnace by draft tube, with electrode pair silicon core energising heating, produce high temperature, conventionally temperature of reaction is controlled to approximately 1000 ℃ to 1200 ℃, be preferably 1100 ℃ of left and right.The trichlorosilane passing into and hydrogen carry out vapor deposition reaction generting element silicon at silicon wicking surface.The tail gas that reaction is produced is discharged by exhaust pipe from the center of stove cylinder bottom.Along with being deposited on the silicon of silicon wicking surface, increase, silicon rod is chap gradually, finally grows up to the polycrystalline silicon rod of required size.Silicon rod grows into after required size, and for example the size of 2.0 to 2.8 meters of length, 40 to 200 millimeters of final diameters, needs to carry out blowing out processing.
Reduction furnace blowing out is the important stage in reduction furnace production run, and the harmony of the Yield and quality of polysilicon, cost and whole production system, stability, security are played to immeasurable effect.
In original furnace stopping process, the stopping process conventionally adopting is at present: first evenly fall material 1 ~ 3 hour, the mixture of trichlorosilane and hydrogen is down to 0Nm
3/ h(standard cube m/h), falling in material process is still well-defined reaction temp by regulating electric current to keep silicon rod surface temperature; After falling and having expected, switch to after pure hydrogen displacement, start evenly to reduce flow through the electric current of electrode and continue 1～3 hour, until electric current is reduced to after 0A, power-off has also completed blowing out operation.
Above-mentioned original furnace stopping process used time is longer, and in furnace shutting down process because curent change produces magnetic field, the effect that the silicon rod of energising is subject to magnetic force produces moment, causes silicon rod root loosening; Because the crystal form of polycrystalline is different, its local electrical resistance is also different, reduces identical electric current again, and the variation of silicon rod local temperature is also different, because the degree difference of thermal shrinkage is slowly split silicon rod; Again because polysilicon is semiconductor, the reduction of its electrical resistance temperature and increasing, evenly falls electric current and can make silicon rod temperature variation is in the same time not different, causes its stress evenly not discharge; Thereby initiation silicon rod short texture, local fracture, the adverse consequencess such as stove of falling.
Summary of the invention
In order to overcome the above-mentioned shortcoming of existing stopping process, one of object of the present invention is to provide a kind of improved polysilicon producing and reducing furnace blowing out control system and control method, this blowing out control system and method thereof can shorten the blowing out time used, save cost and reduce the excellent rate of falling of polycrystalline silicon rod.
In one aspect of the invention, the invention provides a kind of polysilicon producing and reducing furnace blowing out control system, described reduction furnace comprises the silicon rod being arranged on chassis, and described blowing out control system comprises: calculation of magnetic force module, the maximum magnetic force being subject to for calculating the silicon rod of having grown; Stress calculation module, discharges stress for calculating the minimum of the silicon rod of having grown; Module is optimized in blowing out, discharges stress utilize optimized algorithm to calculate to optimize furnace outage time and optimize blowing out temperature for the minimum of the maximum magnetic force that is subject to based on this silicon rod and silicon rod; And control module, the optimization furnace outage time based on calculating and optimization blowing out temperature are controlled the blowing out of reduction furnace.
In other features of the present invention, control module is controlled the inlet amount of trichlorosilane and hydrogen mixed gas, after blowing out is started, in optimizing furnace outage time, inlet amount is evenly down to zero.
In other features of the present invention, control module is controlled by the electric current of silicon rod, and after blowing out is started, silicon rod temperature evenly declines.
In other features of the present invention, control system also comprises Current calculation module, and this Current calculation module is based on optimizing furnace outage time and optimizing blowing out thermometer and calculate curent change curve in furnace shutting down process.And the curent change curve controlled of described control module based on calculating by the electric current of silicon rod, evenly declines silicon rod temperature in optimizing furnace outage time.
In other features of the present invention, after blowing out starts through optimization furnace outage time, inlet amount be down to zero and silicon rod temperature be down to while optimizing blowing out temperature, control system is cut off the power supply to reduction furnace.
In other features of the present invention, described optimized algorithm can be genetic algorithm.
In other features of the present invention, optimization furnace outage time is the scope of approximately 10 minutes to 1.3 hours, can be preferably 30 minutes.Optimizing blowing out temperature is between approximately 750 to 970 ℃, preferably can be 878 ℃.
In a second aspect of the present invention, a kind of polysilicon producing and reducing furnace blowing out control method is provided, comprise the following steps: the maximum magnetic force that the silicon rod that calculating has been grown is subject to; The minimum of estimating this silicon rod discharges stress; The maximum magnetic force being subject to based on this silicon rod and the minimum of silicon rod discharge stress and utilize optimized algorithm to calculate optimization furnace outage time and optimize blowing out temperature; With the optimization furnace outage time and the blowing out of optimizing blowing out temperature control reduction furnace based on calculating.
In other features of the present invention, the step of controlling the blowing out of reduction furnace further comprises: control the inlet amount of trichlorosilane and hydrogen mixed gas, after blowing out is started, in optimizing furnace outage time, inlet amount is evenly down to zero.
In other features of the present invention, the step of the blowing out of described control reduction furnace further comprises: in the time of with reduction inlet amount, control by the electric current of silicon rod, after blowing out is started, silicon rod temperature evenly declines.
In other features of the present invention, described method also comprises based on optimizing furnace outage time and optimizing the step that blowing out thermometer is calculated current reduction speed in furnace shutting down process.And the step of the blowing out of described control reduction furnace further comprises: the current reduction speed based on calculating is controlled to be optimized in furnace outage time by the electric current of silicon rod, and silicon rod temperature is evenly declined.
In other features of the present invention, described method also comprises based on optimizing fracture, power-off point, calculates inlet amount changing down and the alive changing down of silicon rod in furnace shutting down process.
In other features of the present invention, described method also comprises: after blowing out starts, through optimization furnace outage time or while having reached optimization blowing out temperature, cut off the power supply to reduction furnace.
The more areas of the present invention's application become more apparent by the detailed description by below given.Should be appreciated that specific descriptions and specific examples are only with laying down a definition and understanding object, but should not be used to limit the scope of the invention.
Accompanying drawing explanation
By the detailed description and the accompanying drawings, will understand more completely the present invention, wherein:
Fig. 1 is the simplified schematic diagram of polysilicon producing and reducing furnace of the present invention.
Fig. 2 is according to the block schematic diagram of the first embodiment of blowing out control system of the present invention.
Fig. 3 is according to the block schematic diagram of the second embodiment of blowing out control system of the present invention.
Fig. 4 is according to the optimization calculation flow chart of best fracture of the present invention, power-off point.
Fig. 5 shows the process flow diagram of the furnace stopping process of optimization of the present invention.
Embodiment
The detailed description and the accompanying drawings are below described and are shown various embodiment of the present invention.These are described and accompanying drawing is used for enabling those skilled in the art to manufacturing and using the present invention, are not to limit the scope of the invention by any way.About disclosed method, described step is in fact schematically, therefore not necessarily necessary or crucial.
Fig. 1 shows the structural representation of the polysilicon producing and reducing furnace of the present invention's employing.As shown in Figure 1, reduction furnace mainly comprises stove cylinder 1, is positioned at the stone or metal plate for standing a stove on as a precaution against fire 2 of stove cylinder inner bottom part, a plurality of electrode 3(that are arranged on stone or metal plate for standing a stove on as a precaution against fire only illustrate two), combination gas draft tube 5, exhaust pipe 6, cooling water inlet pipe and rising pipe 7,8.A plurality of bar-like silicon cores 4, for example diameter is that 7～10 millimeters, length are 2.0 to 2.8 meters, is evenly arranged on stone or metal plate for standing a stove on as a precaution against fire 2, and is electrically connected to electrode 3.On stove barrel, visor hole 9 be can also be provided with, temperature or silicon rod temperature in stove are convenient to monitor, to control temperature of reaction.
Because of differences such as reduction furnace structure, polysilicon product height, diameter, quality, processing parameter, production cycles, all can exert an influence to blowing out.A plurality of exemplary embodiments are described below and set forth the present invention.Required silicon rod specification is for example in the scope of 2.0 to 2.8 meters of length, 40 to 200 millimeters of diameters.Start polysilicon producing and reducing furnace, by combination gas draft tube 5, to the combination gas that passes into trichlorosilane and hydrogen in reduction furnace, utilize 3 pairs of silicon cores energising heating of electrode to produce polysilicon to carry out vapor deposition reaction on the surface of bar-like silicon core 4.Along with continuous generation the deposition of polysilicon, grow the silicon rod of required specification.After having obtained the polycrystalline silicon rod of required specification, start blowing out and process.
In furnace shutting down process, as mentioned above, the silicon rod of substantially grow can be subject to electric current simultaneously and reduce the stress causing due to thermal shrinkage in the magnetic force that caused by electromagnetic field variation in process and temperature-fall period.Particularly, after blowing out starts, need to reduce gradually the electric current by silicon rod, curent change produces magnetic field, and the silicon rod of energising is subject to magnetic force.Silicon rod, under the effect of magnetic force, can produce and rock, and serious situation can make silicon rod fracture, and rod even occurs.On the other hand, because silicon rod can produce temperature variation in furnace shutting down process, in temperature-fall period, meeting produces certain contraction and causes thermal stress.If do not discharge certain stress, also can produce silicon rod cracking, increase and fall excellent probability.
In order to optimize furnace stopping process, wish that magnetic force and stress that silicon rod is subject to all tries one's best little and can reduce as early as possible, thereby prevent down rod.Yet the maximum suffered magnetic force of silicon rod and the minimum release of silicon rod stress are conflicting.This be because, in furnace shutting down process, the electric current I by silicon rod evenly reduces gradually, magnetic induction density also reduces with electric current and reduces gradually.So, the magnetic field force that silicon rod is subject to reduces gradually along with current reduction.The maximum magnetic force that silicon rod is subject to occurs in the incipient time period of blowing out.If do not consider stress factors, when blowing out is processed, wish to reduce rapidly electric current, can eliminate as early as possible the impact of magnetic force on silicon rod like this.But it is directly related that the suffered thermal stress of silicon rod and the temperature of silicon rod reduce caused drawdown deformation, it is faster that temperature reduces, and caused thermal stress is larger.Therefore, between them, there is contradiction.
Consider above-mentioned factor, the present invention calculates the maximum suffered magnetic force of silicon rod and the minimum stress that discharges of silicon rod, and based on these two factors, the best fracture, the power-off point that utilize the blowing out of optimized algorithm optimization to process, to obtain optimized furnace shutting down process.
The maximum suffered magnetic force of silicon rod can calculate by flowing through the momentary current of silicon rod.The stress that silicon rod is subject to can be calculated according to mechanics parameter, constraint condition and the loadometer of the silicon arranging by Stress calculation module.Then, the maximum suffered magnetic force of silicon rod based on calculating and the minimum stress that discharges of silicon rod, utilize optimized algorithm to calculate best fracture, power-off point, i.e. best blowing out temperature and required time of best blowing out.In best blowing out temperature, the suffered thermal stress of silicon rod is considered to substantially discharge.That is to say, at this below temperature, then continue cooling, silicon rod shrinks that the stress causing is very little maybe can be left in the basket and disregard, and can not produce down excellent.According to the scope of the best fracture of above-mentioned blowing out control method optimization of the present invention, power-off point generally between approximately 10 minutes to approximately 1.3 hours and approximately 750 degree between 970 degree.So greatly shortened the required time of blowing out, and saved reduction furnace and produced required electric energy.
In prior art, conventionally material process will first be fallen: need evenly to fall for 1-3 hour material to zero; Fall after material process finishes, then carry out temperature-fall period: through 1-3 hour, electric current is down to zero.
Unlike the prior art, in furnace stopping process of the present invention, reduce charging (combination gas) and reduce the suffered electric current of silicon rod and carry out simultaneously.That is to say, after polycrystalline silicon rod growth finishes, start the blowing out stage, start to fall material, in best furnace outage time by the even near 0Nm of the inlet amount of trichlorosilane and hydrogen mixed gas
3after/h.When falling material, start cooling, in this best furnace outage time, silicon rod temperature is evenly down to best blowing out temperature simultaneously, then power-off, furnace shutting down process finishes.
Compared to existing technology, one of beneficial effect of the present invention is: shorten reduction furnace and fall the material time, and shorten reduction furnace temperature fall time, and fall material process and temperature-fall period carries out simultaneously, thereby greatly shortened required T.T. of reduction furnace blowing out, and greatly reduced inlet amount and the required energy consumption consuming in furnace shutting down process.
The first preferred embodiment of reduction furnace blowing out control system of the present invention or control device 10 is described below in conjunction with accompanying drawing 2.Control system 10 mainly comprises calculation of magnetic force module 20, Stress calculation module 30, blowing out optimization module 40 and control module 60.
Calculation of magnetic force module 20 calculates the suffered maximum magnetic force of silicon rod by flowing through the momentary current of silicon rod.Stress calculation module 30 estimates the minimum stress that discharges of silicon rod according to mechanics parameter, constraint condition and the load of the silicon of setting.Module 40 connections of communicate by letter with Stress calculation module 30 with calculation of magnetic force module 20 optimized in blowing out, and from calculation of magnetic force module 20 and Stress calculation module 30, receives the silicon rod suffered magnetic force of maximum and the silicon rod minimum release stress of calculating respectively.Then blowing out is optimized module 40 based on the maximum suffered magnetic force of silicon rod and the minimum stress that discharges of silicon rod, utilizes optimized algorithm, and genetic algorithm is for example calculated the furnace outage time P of optimization (the best)
optimaland optimization (the best) blowing out temperature T
optimal, optimize fracture, the power-off point of (the best).Control module 60 is configured for the whole process that blowing out is processed of controlling.Module 40 connections of communicate by letter optimized in control module 60 and blowing out, and from the blowing out optimization module 40 best furnace outage time of reception and best blowing out temperature.Control module 60 is controlled the temperature of silicon rod in furnace shutting down process, makes silicon rod temperature in best furnace outage time, evenly be down to best blowing out temperature T
optimal.Meanwhile, control module 60 is also controlled and is entered the trichlorosilane of reduction furnace and the inlet amount of hydrogen mixed gas evenly reduces gradually, makes through after best furnace outage time, and this inlet amount is down to 0Nm
3/ h.At the best furnace outage time P of process
optimalafterwards, silicon rod temperature will be down to best blowing out temperature T
optimal, and inlet amount is zero, now control module 60 is cut off the power supply to reduction furnace immediately, cuts off by the electric current of electrode 3, thereby complete blowing out, controls.Afterwards, be converted to hydrogen exchange.
The second preferred embodiment of reduction furnace blowing out control system of the present invention or control device 10 ' is described below in conjunction with accompanying drawing 3.Similar to the first preferred embodiment, control system 10 ' comprises calculation of magnetic force module 20 ', Stress calculation module 30 ', blowing out optimization module 40 ', control module 60 '.In the second preferred embodiment, control system 10 ' also preferably includes Current calculation module 50.Current calculation module 50 is designed to according to best furnace outage time P
optimalwith best blowing out temperature T
optimal, calculate in furnace shutting down process to the required curent change applying of silicon rod, to realize the furnace stopping process of above-mentioned optimization.
Further combined with Current calculation module 50, be described in the Current Control to silicon rod energising in furnace shutting down process of the present invention below.
In the furnace shutting down process of prior art, employing reduces electric current equably conventionally.Because polysilicon is semiconductor, the reduction of its electrical resistance temperature and increasing, therefore, evenly falling electric current can make silicon rod temperature variation in the same time be not different, that is to say, electric current decline uniformly can cause inhomogeneous temperature to reduce, thereby causes the suffered stress of silicon rod evenly not discharge.
In order to overcome above-mentioned shortcoming, the present invention, by control the electric current fall off rate changing in furnace shutting down process, can evenly reduce silicon rod temperature.First, size, material parameter and temperature according to generating silicon rod, estimate the temperature variant resistance value R of silicon rod.The temperature variant resistance value of silicon rod also can be by rule of thumb or various laboratory facilities and obtaining.In order to make silicon rod temperature evenly be reduced to best blowing out temperature from temperature of reaction, according to thermodynamic equilibrium principle, utilize Joule law according to the silicon rod resistance value R changing, calculate by the value of silicon rod electric current I.
According to above-mentioned result of calculation, in furnace shutting down process, the value of electric current I is controlled as, and current reduction speed reduces gradually, that is, along with the process of time, in time per unit, the slippage of electric current reduces.Such Current Control not only can be optimized the suffered stress of silicon rod in furnace shutting down process, and can also reduce quickly in the early stage in blowing out stage electric current, therefore in the early stage in blowing out stage, just magnetic force is reduced largely to the acting force of silicon rod.In blowing out, start t
0time, current value used when current value I is substantially equal to production of polysilicon.As time goes on, electric current I reduces unevenly with above-mentioned current reduction speed, and silicon rod temperature can evenly be declined.When blowing out finishes t
1time, while cutting off electric current, silicon rod temperature reaches best blowing out temperature.
In a second embodiment, module 40 ' connections of communicate by letter optimized in Current calculation module 50 and blowing out, from optimizing the best furnace outage time P of module 40 ' reception optimization
optimalwith best blowing out temperature T
optimal.According to thermodynamic equilibrium, Current calculation module 50 can be based on best furnace outage time and best blowing out temperature, according to the temperature variant resistance value R of silicon rod, calculate the current value of optimization or the current reduction speed of optimization of silicon rod energising in furnace shutting down process, in the furnace outage time that makes to optimize, silicon rod temperature can reduce equably, thereby has reduced the thermal stress of the required release of silicon rod.
Control module 60 ' is configured for the whole process that blowing out is processed of controlling.Module 40 ' the connection of communicating by letter with Current calculation module 50 is optimized in control module 60 ' and blowing out, and receive best furnace outage time and/or best blowing out temperature from blowing out optimization module 40 ', from Current calculation module 50, receive the current value of optimization or the current reduction speed of optimization.Control module 60 ' current value based on optimizing or lower speed and control by the size of current of silicon rod in furnace shutting down process, makes silicon rod temperature evenly be down to best blowing out temperature T
optimal.Meanwhile, control module 60 ' also evenly reduces to enter the inlet amount of trichlorosilane and the hydrogen mixed gas of reduction furnace gradually, makes through after best furnace outage time, and this inlet amount is down to 0Nm
3/ h.At the best furnace outage time P of process
optimalafterwards, silicon rod temperature will be down to best blowing out temperature T
optimal, and inlet amount is zero, the power supply that now control module 60 ' is cut off reduction furnace, cuts off by the electric current of electrode 3, thereby complete blowing out, controls.Afterwards, be converted to hydrogen exchange.
The configuration and function that module 40 ' is optimized in calculation of magnetic force module 20 ' in the second embodiment, Stress calculation module 30 ' and blowing out is identical with the first embodiment substantially, at this, needn't repeat.In this embodiment, Current calculation module 50 is configured to independent module, yet as required, Current calculation module 50 also can be integrated into a module of formation in control module 60 '.
In addition, the control system described in the first embodiment and the second embodiment or device 10,10 ' can also comprise inlet amount computing module (not shown).This inlet amount computing module can be optimized module 40, the 40 ' connection of communicating by letter with blowing out, and from blowing out, optimizes module and receive best furnace outage time.Initial mixing gas inlet amount when inlet amount computing module is arranged to according to the best furnace outage time receiving and reduction furnace blowing out, calculates uniform inlet amount changing down in furnace shutting down process.Then, the inlet amount computing module connection of communicating by letter with control module 60,60 ', and the inlet amount changing down calculating is offered to control module, reduces and controls for the charging of furnace shutting down process.One skilled in the art will appreciate that inlet amount computing module can be configured to independent module; Or as required, inlet amount computing module also can be integrated into and form a module in control module 60,60 '.Alternatively, also can omit inlet amount computing module, and realize the inlet amount calculating of furnace shutting down process and control by control module.
Below in conjunction with attached Figure 4 and 5, reduction furnace blowing out control method of the present invention is described.Fig. 4 is according to the optimization calculation flow chart of best fracture of the present invention, power-off point.Fig. 5 shows according to optimizing as shown in Figure 4 the best fracture calculating, the process flow diagram that power-off point carries out the furnace stopping process of optimization of the present invention.
As shown in Figure 4, at step S10, calculate the minimum stress that discharges of the suffered maximum magnetic force of silicon rod and silicon rod.Control advances to step S20, and the minimum stress that discharges of the suffered maximum magnetic force of silicon rod based on calculating and silicon rod, utilizes optimized algorithm to calculate optimized furnace outage time and blowing out temperature (fracture of optimization, power-off point).Optimized algorithm can be for example genetic algorithm.In step S30, according to optimized furnace outage time and blowing out temperature, the current value of the current reduction speed in calculating furnace shutting down process or the variation of optimization, makes temperature in described optimum furnace outage time can evenly be reduced to optimum blowing out temperature.In step S40, the initial charge amount during according to optimized furnace outage time and reduction furnace blowing out, calculates inlet amount changing down constant in furnace shutting down process, makes inlet amount in described optimum furnace outage time, evenly be down to zero.
As shown in Figure 5, in step S100, after polycrystalline silicon rod growth finishes, start polycrystalline silicon reducing furnace blowing out and process.In step S110, the furnace outage time of the optimization based on calculating in step S20 and blowing out temperature, carry out furnace shutting down process control.Material falls in control, during the furnace outage time of this optimization by the even near 0Nm of the inlet amount of trichlorosilane and hydrogen mixed gas
3/ h.When falling material, start cooling, silicon rod temperature is evenly down to substantially to the blowing out temperature of optimization in the furnace outage time of optimizing.
Preferably, in step S110, the inlet amount changing down that control method can calculate according to step S40 is evenly down to 0Nm by inlet amount
3/ h, meanwhile, the current value of the current reduction speed calculating according to step S30 or the variation of optimization, controls by the decline of the electric current of silicon rod, makes silicon rod temperature can evenly be down to optimized blowing out temperature.
In step S120, control method judges whether to have reached optimum fracture, power-off point, namely judge whether to have passed through optimum furnace outage time, or whether silicon rod temperature has declined and reach optimum blowing out temperature.If be judged as "Yes" in step S120, that is, passed through optimized furnace outage time or reached optimum blowing out temperature, so in step S130, power-off blowing out, furnace shutting down process finishes.If be judged as "No" in step S120, control and turn back to step S110.
By above-mentioned control procedure, the present invention can make polycrystalline silicon reducing furnace blowing out process optimization, prevented silicon rod short texture, local fracture and fallen excellent probability, greatly shortened simultaneously furnace stopping process required material time and temperature fall time fall, and saved electric power.
Example 1
In example 1, the silicon core of 24 pairs of silicon rods, 2 meters of length is set on the stone or metal plate for standing a stove on as a precaution against fire 2 of polysilicon producing and reducing furnace, 1150 ℃ of temperature of reaction in production run, the growth cycle of silicon rod are 72 hours.The required specification of polycrystalline silicon rod is 125 millimeters of diameters, approximately 2 meters of length.
Adopt the as above growth course of processing parameter, in reduction furnace, produce the polycrystalline silicon rod of 125 millimeters of diameters, approximately 2 meters of specifications of length.After polycrystalline silicon rod growth finishes, control module 60 or 60 ' beginning blowing out processing.Start blowing out, start to fall material, in 30 minutes by the even near 0Nm of the inlet amount of trichlorosilane and hydrogen mixed gas
3after/h, switch to replacing hydrogen.When falling material, start cooling, in 30 minutes, silicon rod temperature is evenly down to after 878 ℃ to power-off blowing out.
Example 2
In example 2, the silicon core of 24 pairs of silicon rods, 2 meters of length is set on the stone or metal plate for standing a stove on as a precaution against fire 2 of polysilicon producing and reducing furnace, the required specification of polycrystalline silicon rod is: 40 millimeters of diameters, approximately 2 meters of length.Temperature of reaction in production run and growth cycle are identical with example 1.
After polycrystalline silicon rod growth finishes, control module 60 or 60 ' beginning blowing out processing.Start blowing out, start to fall material, in approximately 10 minutes by the even near 0Nm of the inlet amount of trichlorosilane and hydrogen mixed gas
3after/h, switch to replacing hydrogen.When falling material, start cooling, in approximately 10 minutes, silicon rod temperature is evenly down to after 970 ℃ to power-off blowing out.
Example 3
In example 3, the silicon core of 24 pairs of silicon rods, 2.5 meters of length is set on the stone or metal plate for standing a stove on as a precaution against fire 2 of polysilicon producing and reducing furnace, the required specification of polycrystalline silicon rod is: 125 millimeters of diameters, approximately 2.5 meters of length.Temperature of reaction in production run and growth cycle are identical with example 1.
Move calculation of magnetic force module of the present invention, Stress calculation module, blowing out and optimize module to calculate best fracture, the power-off point of furnace stopping process, best blowing out required time is that 38 minutes, best blowing out temperature are 871 ℃.
After polycrystalline silicon rod growth finishes, control module 60 or 60 ' beginning blowing out processing.Start blowing out, start to fall material, in 38 minutes by the even near 0Nm of the inlet amount of trichlorosilane and hydrogen mixed gas
3after/h, switch to replacing hydrogen.When falling material, start cooling, in 38 minutes, silicon rod temperature is evenly down to after 871 ℃ to power-off blowing out.
Example 4
In example 4, the silicon core of 24 pairs of silicon rods, 2.8 meters of length is set on the stone or metal plate for standing a stove on as a precaution against fire 2 of polysilicon producing and reducing furnace, the required specification of polycrystalline silicon rod is: 180 millimeters of diameters, approximately 2.8 meters of length.Temperature of reaction in production run and growth cycle are identical with example 1.
Move calculation of magnetic force module of the present invention, Stress calculation module, blowing out and optimize module to obtain best fracture, the power-off point of furnace stopping process, best blowing out required time is that approximately 1 hour, best blowing out temperature are approximately 800 ℃.
After polycrystalline silicon rod growth finishes, control module 60 or 60 ' beginning blowing out processing.Start blowing out, start to fall material, in approximately 1 hour by the even near 0Nm of the inlet amount of trichlorosilane and hydrogen mixed gas
3after/h, switch to replacing hydrogen.When falling material, start cooling, in approximately 1 hour, silicon rod temperature is evenly down to after approximately 800 ℃ to power-off blowing out.
Each above example has provided the blowing out Optimization Technology under different manufacturing parameters.It will be appreciated by those skilled in the art that according to different reduction furnace processing parameters, different required silicon rod specification etc., by method of the present invention, can obtain different optimization fractures, power-off point.Within the scope of the common working condition of polysilicon producing and reducing furnace, according to the present invention, the best fracture of furnace stopping process optimization, the scope of power-off point are generally: the scope of best furnace outage time between 10 minutes to approximately 1.3 hours, the scope of best blowing out temperature between 750 degree to 970 degree.The silicon rod growing into more carefully, shorter, required release stress is fewer, the optimization power-off time of furnace shutting down process is faster, optimizes power-off temperature relatively higher.
Many-sided technology such as comprehensive electromagnetic of the present invention, mechanics, thermodynamics are improved traditional stopping process.Compare with original furnace stopping process, the invention has the beneficial effects as follows: shortened furnace stopping process required time, reduced the excellent rate of falling in polycrystalline silicon rod blowing out stage, improved product quality, reduce a material consumption of chlorosilane approximately 1.5% ~ 2.35%, reduce approximately 7 ~ 11kwh/kg-si of polysilicon list power consumption, reduce approximately 17 ~ 26kwh/kg-si of the comprehensive power consumption of polysilicon, reduce tail gas recycle load and then improve polysilicon output approximately 5.56 %, and having improved harmony, security and the stability between reduction and two systems of tail gas recycle.
Although for the ease of understanding better the present invention, invention has been described according to preferred embodiment, be to be understood that, in the situation that not deviating from principle of the present invention, the present invention can implement with multitude of different ways.Therefore, the present invention is appreciated that and comprises all possible embodiment implementing and distortion in the situation that not deviating from scope of the present invention.
Claims (21)
1. a polysilicon producing and reducing furnace blowing out control system, described reduction furnace comprises the silicon rod being arranged on chassis, described blowing out control system comprises:
Calculation of magnetic force module, the maximum magnetic force being subject to for calculating the silicon rod of having grown;
Stress calculation module, discharges stress for calculating the minimum of the silicon rod of having grown;
Module is optimized in blowing out, discharges stress utilize optimized algorithm to calculate to optimize furnace outage time and optimize blowing out temperature for the minimum of the maximum magnetic force that is subject to based on this silicon rod and silicon rod; With
Control module, the optimization furnace outage time based on calculating and optimization blowing out temperature are controlled the blowing out of reduction furnace.
2. control system according to claim 1, is characterized in that, control module is controlled the inlet amount of trichlorosilane and hydrogen mixed gas, after blowing out is started, in optimizing furnace outage time, inlet amount is evenly down to zero.
3. control system according to claim 2, is characterized in that, described control module is controlled by the electric current of silicon rod, and after blowing out is started, silicon rod temperature evenly declines.
4. control system according to claim 2, it is characterized in that, also comprise Current calculation module, this Current calculation module is based on optimizing furnace outage time and optimizing blowing out thermometer and calculate curent change curve in furnace shutting down process, and, the curent change curve controlled of described control module based on calculating by the electric current of silicon rod, evenly declines silicon rod temperature in optimizing furnace outage time.
5. according to the control system described in any one in claim 1-4, it is characterized in that, after blowing out starts through optimization furnace outage time, inlet amount be down to zero and silicon rod temperature be down to while optimizing blowing out temperature, control system is cut off the power supply to reduction furnace.
6. control system according to claim 1, is characterized in that, described optimized algorithm is genetic algorithm.
7. control system according to claim 1, is characterized in that, optimization furnace outage time is the scope of 10 minutes to 1.3 hours.
8. control system according to claim 7, is characterized in that, optimizing furnace outage time is 30 minutes.
9. control system according to claim 1, is characterized in that, optimizing blowing out temperature is 750 to 970 ℃.
10. control system according to claim 9, is characterized in that, optimizing blowing out temperature is 878 ℃.
11. 1 kinds of polysilicon producing and reducing furnace blowing out control methods, comprise the following steps:
The maximum magnetic force that the silicon rod that calculating has been grown is subject to;
The minimum of estimating this silicon rod discharges stress;
The maximum magnetic force being subject to based on this silicon rod and the minimum of silicon rod discharge stress and utilize optimized algorithm to calculate optimization furnace outage time and optimize blowing out temperature; With
Optimization furnace outage time based on calculating and optimization blowing out temperature are controlled the blowing out of reduction furnace.
12. control methods according to claim 11, it is characterized in that, the step of the blowing out of described control reduction furnace further comprises: control the inlet amount of trichlorosilane and hydrogen mixed gas, after blowing out is started, in optimizing furnace outage time, inlet amount is evenly down to zero.
13. control methods according to claim 12, is characterized in that, the step of the blowing out of described control reduction furnace further comprises: in the time of with reduction inlet amount, control by the electric current of silicon rod, after blowing out is started, silicon rod temperature evenly declines.
14. control methods according to claim 12, is characterized in that, described method also comprises the step of calculating current reduction speed in furnace shutting down process based on optimization furnace outage time and optimization blowing out thermometer, and,
The step of the blowing out of described control reduction furnace further comprises: the current reduction speed based on calculating is controlled to be optimized in furnace outage time by the electric current of silicon rod, and silicon rod temperature is evenly declined.
15. control methods according to claim 11, is characterized in that, described method also comprises based on described optimization furnace outage time and optimizes blowing out temperature, calculates inlet amount changing down and the alive changing down of silicon rod in furnace shutting down process.
16. according to the control method described in any one in claim 11-15, it is characterized in that, described method also comprises: after blowing out starts, through optimization furnace outage time or while having reached optimization blowing out temperature, cut off the power supply to reduction furnace.
17. control methods according to claim 11, is characterized in that, described optimized algorithm is genetic algorithm.
18. control methods according to claim 11, is characterized in that, optimization furnace outage time is the scope of 10 minutes to 1.3 hours.
19. control methods according to claim 18, is characterized in that, optimizing furnace outage time is 30 minutes.
20. control methods according to claim 11, is characterized in that, optimizing blowing out temperature is 750 to 970 ℃.
21. control methods according to claim 20, is characterized in that, optimizing blowing out temperature is 878 ℃.
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| CN108394905B (en) * | 2017-02-08 | 2019-12-31 | 新特能源股份有限公司 | Full-automatic stable operation method for reduction furnace |
| CN109448800B (en) * | 2018-12-24 | 2022-12-06 | 内蒙古神舟硅业有限责任公司 | Method for judging mass gliding time of refined trichlorosilane |
| CN112110449B (en) * | 2019-06-21 | 2022-06-28 | 新特能源股份有限公司 | Polycrystalline silicon production method and system |
| CN113741599B (en) * | 2021-09-26 | 2022-05-31 | 四川永祥新能源有限公司 | Blowing-out control process for reduction furnace, system thereof and computer readable storage medium |
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