CN114545865B - Polycrystalline silicon growth control method - Google Patents

Polycrystalline silicon growth control method Download PDF

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CN114545865B
CN114545865B CN202011336534.3A CN202011336534A CN114545865B CN 114545865 B CN114545865 B CN 114545865B CN 202011336534 A CN202011336534 A CN 202011336534A CN 114545865 B CN114545865 B CN 114545865B
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voltage
curve
standard
time
actual
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CN114545865A (en
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刘长圣
李大伟
刘丹丹
李伟
吕海花
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Xinte Energy Co Ltd
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Xinte Energy Co Ltd
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    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05BCONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
    • G05B19/00Programme-control systems
    • G05B19/02Programme-control systems electric
    • G05B19/418Total factory control, i.e. centrally controlling a plurality of machines, e.g. direct or distributed numerical control [DNC], flexible manufacturing systems [FMS], integrated manufacturing systems [IMS], computer integrated manufacturing [CIM]
    • G05B19/41835Total factory control, i.e. centrally controlling a plurality of machines, e.g. direct or distributed numerical control [DNC], flexible manufacturing systems [FMS], integrated manufacturing systems [IMS], computer integrated manufacturing [CIM] characterised by programme execution
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/02Silicon
    • C01B33/021Preparation
    • C01B33/027Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/035Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P90/00Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
    • Y02P90/02Total factory control, e.g. smart factories, flexible manufacturing systems [FMS] or integrated manufacturing systems [IMS]

Abstract

The invention discloses a polysilicon growth control method, which comprises the following steps: establishing a quick fusing control curve and writing the quick fusing control curve into a DCS; acquiring a U-I standard curve by establishing a mathematical model, and writing the U-I standard curve into a DCS (distributed control system); a reference feeding table is formulated and set on a DCS system, real-time data of the running current and the running voltage of the reduction furnace are collected based on the DCS system in the production process, and a U-I real-time curve is obtained; and comparing the U-I real-time curve with the U-I standard curve, and correcting the parameters in the established reference feeding table according to the comparison result of the actual voltage in the U-I real-time curve and the standard voltage in the U-I standard curve so as to enable the actual voltage to reach the standard voltage when the actual current reaches the standard current, thereby obtaining a final control curve and a polysilicon product with uniform quality, wherein the polysilicon product is produced according to the final control curve. The invention can avoid the electrical faults caused by overload of the operation of the reduction furnace and obtain the polysilicon products with uniform quality.

Description

Polycrystalline silicon growth control method
Technical Field
The invention belongs to the technical field of polysilicon, and particularly relates to a polysilicon growth control method.
Background
At present, most of domestic polysilicon enterprises adopt basically the same production process control mode during the production of polysilicon, mainly the control of the material quantity proportion and the current is set on the basis of the diameter calculation or the temperature measurement of polysilicon rods so as to produce the polysilicon product with high value, and the foreign use of the constant temperature control technology is mainly the linear feeding control mode. In the control modes, the temperature measurement or the diameter measurement is carried out by means of an external device through a sight glass, and in consideration of the complexity of the flow field and the temperature field of the large-diameter reduction furnace, the measurement is generally carried out in a mode that the point temperature represents the whole temperature or the diameter of a single polycrystalline silicon rod represents the diameter of the whole polycrystalline silicon rod, and as the diameter of the silicon rod growing in the production process is increased, the shape is changed and the silicon powder is increased, errors necessarily occur in the measurement mode, and if the control value cannot be corrected in time, the deviation of the production process control from the actual growth condition inevitably occurs, so that a series of production or quality problems are brought.
However, in the actual growth process of the polysilicon, due to the complexity of the flow field and the temperature field of the large-diameter reduction furnace, the phenomenon that the growth rate of the silicon rod is not matched with the U-I curve designed by the power supply system often occurs, for example, after the current is increased, the silicon rod does not actually grow to the expected size, i.e. the silicon rod growth is deviated, the voltage drop under the current is not lower than the allowable value of the production system, under the operation condition, the current is higher when the given current is accelerated, the overload phenomenon of the fast-melting fuse is easily caused, the fast-melting temperature is increased, the actual current carrying value of the fuse becomes smaller after the temperature is increased, the fuse is fused due to slight fluctuation of the current, and the safe and stable operation of the power supply control cabinet of the polysilicon production system is greatly influenced, for example, the long-term overload operation can cause serious damage to the electric operation, and the production of the reduction furnace is seriously influenced. At present, when the growth of a silicon rod in a reduction furnace deviates, in the process of optimizing process control parameters, the silicon rod is almost completely dependent on the experience of staff, the silicon rod is prejudged according to the mild running condition of the furnace and each parameter is adjusted, the adjustment process is complicated and long, and the effect is very little.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the polycrystalline silicon growth control method, which can timely correct and regulate the growth process of polycrystalline silicon in a reducing furnace, avoid electrical faults caused by overload of the reducing furnace, obtain a growth mode with stable and controllable polycrystalline silicon growth rate and is beneficial to obtaining polycrystalline silicon products with uniform quality.
The technical scheme for solving the technical problems is as follows:
a method of polysilicon growth control comprising:
s1, establishing a rapid fusing control curve according to a transformer thyristor rapid fusing parameter of a power supply control system matched with a reduction furnace, and writing the rapid fusing control curve into a DCS (distributed control system);
s2, establishing a mathematical model through collected current and voltage data of a furnace number reaching expected index performance in the past operation of the reduction furnace, obtaining a U-I standard curve, and writing the U-I standard curve into a DCS system;
s3, a reference feed table is established, parameter values in the reference feed table are set on a DCS system, real-time data interaction is realized between the DCS system and a power supply control system of the reduction furnace through a network and a corresponding communication protocol, real-time data of running current and voltage of the reduction furnace are acquired based on the DCS system in the production process, and a U-I real-time curve is obtained;
s4, comparing the U-I real-time curve with the U-I standard curve, and correcting the parameter value in the formulated reference feeding table according to the comparison result of the actual voltage in the U-I real-time curve and the standard voltage in the U-I standard curve so as to enable the actual voltage to reach the standard voltage when the actual current reaches the standard current, thereby obtaining a final control curve and a polysilicon product with uniform quality, wherein the polysilicon product is produced according to the final control curve.
Preferably, the step S2 obtains a U-I standard curve by establishing a mathematical model from collected current and voltage data of the heat reaching the expected index performance in the previous operation of the reduction furnace, and specifically includes the following steps:
in the prior art, selecting a furnace number with a silicon rod growth rate, power consumption and a washing-free material/vegetable flower material/coral material ratio reaching expected indexes, and establishing a mathematical model according to actual voltage and current data of the selected furnace number in the production process to fit to obtain the U-I standard curve, wherein the equation of the U-I standard curve is as follows:
U=aI 6 +bI 5 +cI 4 +dI 3 +eI 2 +fI+K
wherein a, b, c, d, e, f are control coefficients generated by fitting, respectively, and a, b, c, d, e, f are not zero at the same time; k is a constant; i > 0.
Preferably, the silicon rod growth rate, electricity consumption and no-wash material/vegetable flower material/coral material ratio reach the expected indexes: the growth rate of the silicon rod is more than 80Kg/h, the power consumption is less than 50KWh/Kg, and the ratio of the no-clean material to the cauliflower material to the coral material is more than 80 percent.
Preferably, the standard voltage in the U-I standard curve is less than or equal to the fuse voltage in the fuse control curve at the same current.
Preferably, the step S4 compares the U-I real-time curve with the U-I standard curve, and corrects the parameter value in the formulated reference feeding table according to the comparison result of the actual voltage in the U-I real-time curve and the standard voltage in the U-I standard curve, including:
every other period t 1 Comparing the actual voltage with the standard voltage for one time to obtain a voltage actual deviation value delta U;
comparing the absolute value of the voltage actual deviation value delta U with a preset voltage operation deviation set value delta U0, and triggering a current/hydrogen/trichlorosilane adjusting mechanism by the DCS when the absolute value of the voltage actual deviation value delta U is larger than the preset voltage operation deviation set value delta U0 and the time for keeping the voltage actual deviation value delta U reaches a voltage deviation judging time t 2.
Preferably, the period t 1 For 5-10min;
the voltage operation deviation set value delta U0 is 5% -10% of the difference value between the corresponding standard voltage and the voltage on the corresponding quick-fusing control curve;
the voltage deviation judging time is 5-10min, and is more than or equal to the period t 1
Preferably, the U-I standard curve is respectively determined for polysilicon production heats with different silicon rod growth rates, power consumption and no-clean material/vegetable flower material/coral material ratios;
and the same U-I standard curve is adopted for the same furnace type of the reduction furnace.
Preferably, for different reduction furnace barrels, respectively establishing a U-I standard curve;
and the silicon rod in each reduction furnace is divided into a plurality of phases for arrangement, and the actual voltage and the actual current of each phase are respectively and independently collected in real time to respectively obtain U-I standard curves of different phases.
Preferably, the method further comprises:
s5, using the final control curve of the last polysilicon production furnace as a correction curve of the next polysilicon production furnace.
According to the polysilicon growth control method, based on real-time data interaction between DCS (distributed computer control system) control and a power supply control system in the whole process, voltage drop is used as a key control point in the reduction production process, the influence of disturbance factor fluctuation is offset by adopting automatic adjustment, and a U-I (voltage-current) standard curve control mode is established, so that the voltage is stably reduced, and further overload electric faults during operation are avoided; and the control mode of combining flow field simulation (simulated by POLYSIM software) and volt-ampere characteristic curve (namely U-I curve) is adopted to realize the rapid growth of the no-clean material, the automatic independent control of a single reduction furnace process can be realized, the growth mode with stable and controllable growth speed and the power consumption reduction control mode are obtained, and the low-cost high-quality polysilicon product is obtained.
Drawings
FIG. 1 is a flow chart showing steps of a method for controlling growth of polysilicon according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of various curves in an embodiment of the present invention;
FIG. 3 is a graph showing a fast-fusing control of a thyristor of a transformer of an electronic control system matched with a 36-pair rod reduction furnace in an embodiment of the invention;
FIG. 4 is a graph comparing a fast blow control curve with a U-I real-time curve for each phase in an embodiment of the present invention.
In the figure: 1-a fast blow control curve; 2-U-I real-time curve; 3-U-I standard curve.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, a clear and complete description of the technical solutions of the present invention will be provided below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
In the description of the present invention, it should be understood that the orientation or positional relationship indicated by the directional terms is based on the orientation or positional relationship shown in the drawings, and is merely for convenience of description and simplicity of description, and does not indicate or imply that the apparatus or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the invention.
Example 1
As shown in fig. 1, this embodiment discloses a polysilicon growth control method, which includes:
s1, establishing a rapid-melting control curve according to the rapid-melting parameters of a transformer thyristor of a power supply control system matched with a reduction furnace (namely, the rapid-melting fuses in the transformer are under different current parameters and need to correspond to voltage parameters), and writing the rapid-melting control curve into a DCS (distributed control system);
s2, establishing a mathematical model through collected current and voltage data of a furnace number reaching expected index performance in the past operation of the reduction furnace, obtaining a U-I standard curve, and writing the U-I standard curve into a DCS system;
s3, a reference feed table (comprising parameters such as growth running time, trichlorosilane/hydrogen feed amount, silicon rod, current of each phase of silicon rod and the like) is formulated, each parameter value in the reference feed table is set on a DCS system, the DCS system and a power supply control system of a reduction furnace realize real-time data interaction through a network and a corresponding communication protocol (such as PROFIBUS communication protocol), real-time data of running current and voltage of the reduction furnace are acquired based on the DCS system in the production process, and a U-I real-time curve is obtained;
s4, comparing the U-I real-time curve with the U-I standard curve, and correcting parameters in the formulated reference feeding table according to the comparison result of the actual voltage in the U-I real-time curve and the standard voltage in the U-I standard curve, so that the actual voltage reaches the standard voltage when the actual current reaches the standard current (namely, the voltage drop reflects the actual growth state of the silicon rod in the reduction furnace and is the comprehensive feedback of the diameter, the surface temperature and the temperature condition in the furnace of the silicon rod), the voltage of each phase of the silicon rod can be fed back in real time, the lower the voltage drop is, the higher the deposition rate is, the lower the electricity consumption is, and the reduction furnace is controlled to stably operate, so that a final control curve and a polysilicon product with uniform quality produced according to the final control curve are obtained.
In this embodiment, the step S2 establishes a mathematical model by collecting current and voltage data of the heat reaching the expected index performance in the previous operation of the reduction furnace, and obtains a U-I standard curve, which includes the following steps:
in the prior art, a silicon rod growth rate, electricity consumption and a washing-free material (namely, the appearance is compact, uniform and good, the polycrystalline silicon product which is required by direct use can be met without cleaning or other treatment) are selected in the prior art, the heat with the ratio of the vegetable flower material to the coral material reaching the expected index (namely, the electricity consumption is reduced or the washing-free material ratio is lifted as an optimization target), a mathematical model is built according to the actual voltage and actual current data of the selected heat in the production process, the U-I standard curve is obtained through fitting, and repeated verification is carried out for a plurality of times. The equation of the obtained U-I standard curve is as follows:
U=aI 6 +bI 5 +cI 4 +dI 3 +eI 2 +fI+K
wherein a, b, c, d, e, f are control coefficients generated by fitting, respectively, and a, b, c, d, e, f are not zero at the same time; k is a constant; i > 0 (excluding the actual current during the down-current phase of the furnace), the deviation of the U-I standard curve obtained by linear fitting is R 2 ≥0.9998。
It should be noted that since each of the studentsThe current is constant for a long time and corresponds to the time one by one, so the U-I standard curve can be expressed by fitting the change of the voltage with the growth time (T) through the growth time, namely the obtained U-I standard curve can be expressed as U=gT 6 +hT 5 +jT 4 +kT 3 +mT 2 +nt+k (where g, h, j, K, m, n is the control coefficient generated by the fitting and g, h, j, K, m, n is not zero at the same time), respectively), in order to compare the difference between the actual voltage and the voltage to be controlled at a certain time.
In some embodiments, the silicon rod growth rate, power consumption, and leave-on/cauliflower/coral material ratio reaching the desired level are: the growth rate of the silicon rod is more than 80Kg/h, for example, more than 90Kg/h; the electricity consumption is less than 50KWh/kg, for example, less than 49KWh/kg; the total proportion of the washing-free material, the cauliflower material and the coral material is more than 80 percent.
In some embodiments, at the same current, the standard voltage in the U-I standard curve is less than or equal to the fuse voltage in the fast-fuse control curve, i.e., the U-I standard curve is confirmed to be controlled below the fast-fuse control curve (as shown in fig. 2) to avoid electrical faults caused by voltage overload.
In this embodiment, step S4 compares the U-I real-time curve with the U-I standard curve, and corrects the parameters in the formulated reference feeding table according to the comparison result of the actual voltage in the U-I real-time curve and the standard voltage in the U-I standard curve, including the following steps:
(4-1) every time period t 1 Comparing the actual voltage with the standard voltage for one time to obtain a voltage actual deviation value delta U;
(4-2) comparing the absolute value of the actual voltage deviation value DeltaU with the preset voltage operation deviation set value DeltaU 0 Comparing, and when the absolute value of the actual voltage deviation value DeltaU is larger than the preset voltage operation deviation set value DeltaU 0 And the time for maintaining the actual voltage deviation value DeltaU reaches the voltage deviation judging time t 2 When the DCS system triggers a current/hydrogen/trichlorosilane adjustment mechanism. Principle of current/hydrogen/trichlorosilane tuning mechanism: voltage drop reflects reduction ofThe actual growth state of the silicon rod in the furnace is the comprehensive feedback of the diameter, the surface temperature and the temperature condition in the furnace, the voltage of each phase of silicon rod can be fed back in real time, the lower the voltage drop is, the higher the deposition rate is, the lower the electricity consumption is, the amount of hydrogen or the amount of trichlorosilane is regulated, namely, the material amount ratio is changed, the temperature in the furnace and the surface temperature of the silicon rod can be changed, the voltage drop of the silicon rod is further influenced, and the growth speed of the silicon rod is further influenced, so the voltage drop of the silicon rod can be regulated by regulating the amount of hydrogen or the amount of trichlorosilane.
In some embodiments, period t 1 The voltage comparison is performed every 5-10min, i.e. every 5-10 min. Voltage operating deviation setpoint Δu 0 5% -10% of the difference between the corresponding standard voltage and the voltage of the fast fusing parameter on the corresponding fast fusing control curve; the voltage deviation judging time is 5-10min, and is more than or equal to the period t 1 To determine if the actual voltage deviates from the standard voltage by an amount that is to be adjusted to avoid over-adjustment.
Specifically, a time period t for comparing voltage parameters is set on the DCS system 1 Every time period t 1 The actual voltage and the standard voltage are compared once, and the allowable deviation range of the actual voltage and the standard voltage, namely the allowable deviation set value DeltaU of the voltage is set on the DCS system 0 . During the operation of the reduction furnace, according to a set time period t 1 Calculating the difference between the current actual voltage and the standard voltage to obtain the actual voltage deviation value delta U, one period t 1 An actual deviation value deltau is calculated. By actual deviation value DeltaU and voltage operation deviation set value DeltaU 0 Comparison was performed:
if the absolute value of the actual voltage deviation value DeltaU is smaller than the voltage allowable deviation set value DeltaU 0 Keeping the reduction furnace continuously operated according to the corresponding parameters in the reference feed table without additional adjustment;
if the absolute value of the actual voltage deviation value DeltaU is greater than the voltage allowable deviation set value DeltaU 0 The corresponding voltage deviation judging time is calculated by a starting timer on the DCS system, and when the voltage deviation judging time is reachedInterval t 2 After that, the absolute value of the actual voltage deviation value DeltaU is still larger than the voltage allowable deviation set value DeltaU 0 The DCS system triggers the current/hydrogen/trichlorosilane adjustment mechanism; when the voltage deviation time does not reach the set voltage deviation judging time t 2 When the absolute value of the actual voltage deviation value DeltaU is changed to be smaller than the voltage allowable deviation set value DeltaU 0 The current/hydrogen/trichlorosilane tuning mechanism is not triggered.
The trigger current/hydrogen/trichlorosilane adjustment mechanism comprises two cases of voltage positive deviation (see the upper part of the curve 2 shown in fig. 2 and the curve 3) and voltage negative deviation (see the lower part of the curve 2 shown in fig. 2 and the curve 3), and the specific adjustment process is as follows:
the method comprises the steps that a first hydrogen adjusting amount, a second hydrogen adjusting amount, trichlorosilane adjusting amount and an adjusted hydrogen change amplitude are preset on a DCS, wherein the first hydrogen adjusting amount and the second hydrogen adjusting amount are 5-10% of hydrogen value parameters in a corresponding reference feed table, the first hydrogen adjusting amount is preferably 5%, the second hydrogen adjusting amount is preferably 10%, the trichlorosilane adjusting amount is 5-10% of trichlorosilane parameters in the corresponding reference feed table, and the adjusted hydrogen change amplitude is the slope of voltage change of a corresponding U-I standard curve;
(1) when the positive voltage deviation condition is satisfied, i.e. the actual voltage-standard voltage > the voltage allowable deviation set value DeltaU 0 When the hydrogen reducing amount is carried out according to a preset first hydrogen adjusting amount (for example, 5 percent of hydrogen value parameter in a corresponding reference feeding table), the hydrogen change in the hydrogen reducing process is carried out according to a preset adjusted hydrogen change amplitude, and simultaneously, a timer is started to start timing, and the timing reaches three periods t 1 Then judging whether the voltage positive deviation condition is satisfied, if not, the absolute value of the actual voltage deviation DeltaU is smaller than the allowable deviation set value DeltaU 0 Continuously operating the reduction furnace according to the parameters of the corresponding time points in the reference feeding table, namely recovering the parameter quantity of the reference work material table of the corresponding time points, and if the timing reaches three periods t 1 After that, the positive voltage deviation condition is still satisfied, thenReducing hydrogen according to a preset second hydrogen regulating quantity (such as 10% of hydrogen value parameters in a corresponding reference feeding table), starting a timer again to start timing, and reaching three periods t 1 Then judging whether the voltage positive deviation condition is satisfied again, if not, the absolute value of the actual voltage deviation DeltaU is smaller than the voltage allowable deviation set value DeltaU 0 Continuously operating the reduction furnace according to the parameters of the corresponding time points in the reference feeding table, namely recovering the parameters of the reference work material table of the corresponding time points, if the parameters of the reference work material table of the corresponding time points are three periods t 1 After the voltage positive deviation condition is still met, the given value of the current trichlorosilane/current/hydrogen regulating quantity is kept unchanged, and a system early warning signal is sent out to prompt an operator to check and intervene manually until the actual voltage deviation delta U is recovered to the voltage allowable deviation set value delta U 0 And after that, early warning is eliminated.
(2) When the negative voltage deviation condition is satisfied, i.e. standard voltage-actual voltage > voltage allowable deviation set value DeltaU 0 When the hydrogen gas affects the thermal field and the air field in the reduction furnace greatly, and the hydrogen gas amount cannot be excessively large so as to prevent the growth condition of the whole polysilicon rod from seriously deviating, therefore, when the voltage is negatively deviated, the hydrogen gas amount is preferentially regulated, if the voltage is negatively deviated, that is, the expected effect is not achieved after the hydrogen gas amount is regulated, the atomization condition in the reduction furnace is not controlled, and at the moment, the corresponding reference amount of trichlorosilane is excessively large, and the reduction is needed to be carried out so as to control the atomization, and the specific process is as follows: carrying out hydrogen lift according to a preset first hydrogen regulation quantity (for example, 5% of hydrogen value parameters in a corresponding reference feed table), and carrying out hydrogen change in the hydrogen lift process according to a preset regulated hydrogen change amplitude, namely, regulating by lifting the hydrogen; at the same time, a timer is started to start timing, and the timing reaches three periods t 1 Then judging whether the voltage negative deviation condition is satisfied, if not, the absolute value of the actual voltage deviation DeltaU is smaller than the allowable deviation set value DeltaU 0 According to the parameters of the corresponding time points in the reference feeding tableContinuously operating the reduction furnace, i.e. recovering the parameter of the reference work material table at the corresponding time point, if the timing reaches three periods t 1 After that, the negative voltage deviation condition is still met, and then the trichlorosilane is reduced according to the preset trichlorosilane regulating quantity (for example, 10 percent of the trichlorosilane parameters in the corresponding reference feeding table), namely, the quantity of the trichlorosilane is reduced; at the same time, the timer is started again to start timing, and the timing reaches three periods t 1 Then judging whether the voltage negative deviation condition is satisfied again, if not, the absolute value of the actual voltage deviation DeltaU is smaller than the voltage allowable deviation set value DeltaU 0 Continuously operating the reduction furnace according to the parameters of the corresponding time points in the reference feeding table, namely recovering the parameters of the reference work material table of the corresponding time points, if the parameters of the reference work material table of the corresponding time points are three periods t 1 After that, the negative voltage deviation condition is still met, namely the expected effect is not achieved after the quantity of the trichlorosilane is reduced, which means that the problem of abnormal growth of the polysilicon rod caused by the problems of hydrogen, purity of the trichlorosilane material and the like possibly exists in the reducing furnace, the current trichlorosilane regulating quantity/current/hydrogen given value is kept unchanged, and a system early warning signal is sent out to prompt an operator to check and manually intervene until the actual voltage deviation delta U is recovered to the voltage allowable deviation set value delta U 0 And after that, early warning is eliminated.
In some embodiments, the U-I standard curve is determined for different polysilicon production runs for different silicon rod growth rates, power consumption, and quality indicators such as no-wash material/flowering material/coral material ratio. And the same U-I standard curve can be adopted for the same furnace type of the reduction furnace.
In some embodiments, the U-I standard curve is established for different reduction furnace barrels respectively to offset the influence of the furnace barrel cooling water on the heat balance, in consideration of the difference of heat radiation of the reduction furnace barrels. The silicon rod in each reduction furnace is divided into a plurality of phases for arrangement, and the actual voltage and the actual current of each phase are respectively and independently collected in real time to respectively obtain U-I standard curves of different phases. In particular, the power supply of the reduction furnace adopts a three-phase power supply, in order to ensure the balance of three-phase power transmission, the power supply system of the reduction furnace is correspondingly split into three phases, namely, a reduction furnace is divided into 36 pairs of bars, for example, each phase of the reduction furnace can be divided into 6 pairs of bars so as to be electrically controlled, the 6 phases can be divided into an inner ring and an outer ring according to the layout, the inner ring 3 phases and the outer ring 3 phases, the thermal fields of the phases at different positions under the same current are slightly different, the current and voltage data of each phase can be acquired independently, the three phases on the same ring can take the same or similar two values of the three phases as judging conditions, namely, the inner ring and the outer ring can both take the voltage value of three or two as judging conditions to execute an automatic adjustment program, so that excessive adjustment is avoided, and the complexity of the gas field and the temperature field in the reduction furnace, especially the large-scale reduction furnace, is beneficial to control.
In some embodiments, the method further comprises:
s5, using the final control curve of the last polysilicon production furnace as a correction curve (namely, U-I standard curve) of the next polysilicon production furnace, and comparing, by comparison, the loop closure verification (namely, comparing the U-I standard curve of the last furnace with the U-I standard curve of the next furnace once every time the production of one furnace is completed) to obtain a U-I standard curve U=aI 6 +bI 5 +cI 4 +dI 3 +eI 2 And (3) whether the control parameters of +gI and K are stable or not, and verifying the uniformity of the quality of the controlled produced polycrystalline silicon product according to indexes such as the power consumption of the discharging furnace, the deposition rate, the washing-free material and the like.
In some embodiments, the reference feeding table adopts a large amount of high-current 'atomization critical point' control mode, namely, a stable gas field and a stable temperature field are quickly established at the initial growth stage of the polysilicon to reach a state close to atomization, at this time, the deposition speed is fastest, and the complex working conditions of the gas field and the temperature field in the furnace are simulated by utilizing polysilicon growth trend simulation software (such as POLYSIM software), so that the establishment of a stable flow field for polysilicon growth is ensured, and the stable flow field is the basis for uniform growth of silicon rods, thereby realizing the rapid and uniform deposition of the polysilicon.
The following takes 36 pairs of rod furnace type as an example, and the polysilicon growth control method of the embodiment is described in detail from two directions of reducing power consumption and improving the cleaning-free material ratio according to the production profit requirement:
preparation example 1
The polysilicon growth control method of the preparation example comprises the following steps:
establishing a rapid-fusing control curve according to the rapid-fusing parameters of a transformer thyristor of an electric control system matched with a 36-pair rod reduction furnace, as shown in fig. 3 (wherein 4P represents 4 pairs of rod phases and 8P represents 8 pairs of rod phases), and writing into a DCS system;
the furnace times with the silicon rod growth rate of more than 90Kg/h, the power consumption of less than 49KWh/Kg and the ratio of no-clean material to vegetable flower material of more than 80% in the previous production are selected as the furnace times reaching the expected indexes, mathematical models are built according to the current and voltage parameters of the selected furnace times in the actual production operation, and a U-I standard curve U=4E is obtained through data fitting -16 I 6 -3E -12 I 5 +1E -08 I 4 -2E -05 I 3 +0.0186I 2 -10.288I+3965.8(R 2 =0.9998), the U-I standard curve can be fitted again with the growth time to the change of the voltage with the growth time (T), i.e. the U-I standard curve obtained above can be expressed again as u=8e -9 T 6 -5E -6 T 5 +0.0009T 4 -0.0809T 3 +3.7961T 2 -105.22T+2306.7(R 2 =0.9998). Comparing the U-I standard curve with the quick-fusing control curve, and confirming that the U-I standard curve is controlled below the quick-fusing control curve so as to avoid electrical faults caused by voltage overload;
under the same material supply and auxiliary material conditions, a reduction furnace with expected quality indexes such as the ratio of the no-clean material in the prior production and higher power consumption is selected, and the average power consumption of the reduction furnaces (recorded as an experiment furnace 1) and the quality indexes such as the ratio of the no-clean material are recorded as a comparative example 1, and are shown in Table 2 in detail. Writing the determined U-I standard curve into a DCS system of the experimental furnace 1;
establishing a reference feed table, as shown in table 1, setting each parameter value on a DCS system, realizing real-time data interaction between the DCS system and a power supply control system of a reduction furnace through a network and a corresponding communication protocol (such as PROFIBUS communication protocol), automatically controlling the operation of the reduction furnace by the DCS system according to the established reference feed table when polycrystalline silicon is produced, acquiring real-time data of the operation current and voltage of the reduction furnace based on the DCS system in the production process, and obtaining U-I real-time curves of each phase;
table 1 preparation example 1 reference feed table
Wherein TCS is trichlorosilane, a1, b1, c1, a2, b2 and c2 respectively represent different phases, and the proportion is the mole ratio of hydrogen to trichlorosilane.
And comparing the U-I real-time curve with the U-I standard curve, and correcting the parameters in the formulated reference feeding table according to the comparison result of the actual voltage in the U-I real-time curve and the standard voltage in the U-I standard curve so as to control the reduction furnace to stably run, so that the actual voltage reaches the standard voltage when the actual current reaches the standard current, and a final control curve and a polysilicon product with uniform quality produced according to the final control curve are obtained. Wherein the voltage tolerance DeltaU 0 Setting to be 5% of the difference between the corresponding standard voltage and the voltage on the corresponding fast fuse control curve; period t 1 Setting for 5min; time t for determining voltage deviation 2 Set to 10min. In the running process of the reduction furnace, the current actual voltage and the standard voltage are subjected to difference calculation according to a set voltage parameter comparison period t1 to obtain an actual deviation value delta U, each comparison period calculates an actual deviation value, and the actual deviation value delta U and a voltage running deviation set value delta U are calculated 0 And comparing, automatically controlling voltage stability to be reduced by the DCS according to the set current/hydrogen/trichlorosilane adjustment mechanism according to the comparison result, thereby obtaining a polysilicon product with uniform quality.
The comparison between the fast fusing control curve of the preparation example and the real-time U-I real-time curve of each phase is shown in fig. 4, and the change condition of the voltage along with the current in the polysilicon production process of the heat can be conveniently known through fig. 4, and whether the process is overloaded (namely, the voltage is overloaded when the actual current reaches the standard current and the actual voltage is greater than the corresponding standard voltage) can be judged, so that the actual voltage of the process can be further optimized and reduced in the subsequent production.
Under the same conditions as above, each experimental furnace 1 was subjected to multi-pass production in accordance with the procedure of preparation example 1, and the average index of production in accordance with preparation example 1 was recorded as shown in table 2.
TABLE 2 average index parameter for PREPARATION EXAMPLE 1
As can be seen from Table 2, compared with the conventional method (i.e., comparative example 1), the power consumption of the method of the present invention was reduced from 55.5kwh/kg to 45.8kwh/kg, the single furnace yield was increased from 7.65 tons to 8.77 tons, and the quality indexes such as the no-clean material ratio remained above the polysilicon product prepared by the conventional method, that is, the polysilicon growth control method of the present invention can realize a low power consumption mode by controlling the voltage drop, gradually reduce the overall voltage and the voltage at the key stage, gradually and stably reduce the power consumption, and can perform the replication production on other reduction furnaces.
Preparation example 2
The polysilicon growth control method of the preparation example comprises the following steps:
a fast fusing control curve is built according to the fast fusing parameters of the transformer controlled silicon of the 36-pair rod reduction furnace matched electric control system, as shown in figure 3, and the fast fusing control curve is written into a DCS system;
selecting the heat with the washing-free material ratio of more than 65% and the electricity consumption of less than 49KWh/kg in the past production as the heat reaching the expected index, establishing a mathematical model according to the current and voltage parameters of the selected heat in the actual production operation, and obtaining a U-I standard curve U=3E through data fitting -16 I 6 -3E -12 I 5 +1E -08 I 4 -2E -05 I 3 +0.0194I 2 -11.191I+4123.9(R 2 =0.9998), the U-I standard curve can be expressed as u=8e again in order to facilitate comparison of the difference between the actual voltage and the voltage to be controlled at a certain time -8 T 6 -3E -5 T 5 +0.0033T 4 -0.2171T 3 +7.7277T 2 -163.2t+2636.1. Comparing the U-I standard curve with the quick-fusing control curve, and confirming that the U-I standard curve is controlled below the quick-fusing control curve so as to avoid electrical faults caused by voltage overload;
under the same material supply and auxiliary material conditions, a reduction furnace with lower electricity consumption but no-clean material ratio and other quality indexes to be lifted in the prior production is selected, and the average electricity consumption, no-clean material ratio and other quality indexes of the reduction furnaces (recorded as an experiment furnace 2) are recorded as a comparative example 2, and are shown in Table 4 in detail. Writing the determined U-I standard curve into a DCS system of the experimental furnace 2;
establishing a reference feed table, as shown in table 3, setting each parameter value on a DCS system, realizing real-time data interaction between the DCS system and a power supply control system of a reduction furnace through a network and a corresponding communication protocol (such as PROFIBUS communication protocol), automatically controlling the operation of the reduction furnace by the DCS system according to the established reference feed table when polycrystalline silicon is produced, acquiring real-time data of the operation current and voltage of the reduction furnace based on the DCS system in the production process, and obtaining U-I real-time curves of each phase;
table 3 preparation example 2 reference feed table
Wherein TCS is trichlorosilane, a1, b1, c1, a2, b2 and c2 respectively represent different phases, and the proportion is the mole ratio of hydrogen to trichlorosilane.
Comparing the U-I real-time curve with the U-I standard curve, and according to the actual voltage in the U-I real-time curve and the U-I standard curveAnd (3) correcting parameters in the established reference feed table to control the reduction furnace to stably run, so that the actual voltage reaches the standard voltage when the actual current reaches the standard current, and a final control curve and a polysilicon product with uniform quality produced according to the final control curve are obtained. Wherein the voltage tolerance DeltaU 0 Setting to be 5% of the difference between the corresponding standard voltage and the voltage on the corresponding fast fuse control curve; period t 1 Setting for 5min; time t for determining voltage deviation 2 Set to 10min. In the running process of the reduction furnace, comparing the period t according to the set voltage parameter 1 Calculating the difference between the current actual voltage and the standard voltage to obtain an actual deviation value DeltaU, calculating an actual deviation value in each comparison period, and setting the actual deviation value DeltaU and the voltage operation deviation value DeltaU 0 And comparing, automatically controlling voltage stability to be reduced by the DCS according to the set current/hydrogen/trichlorosilane adjustment mechanism according to the comparison result, thereby obtaining a polysilicon product with uniform quality.
Under the same conditions as above, each experimental furnace 2 was subjected to multi-pass production in accordance with the procedure of preparation example 2, and the average index of production in accordance with preparation example 2 was recorded as shown in table 4.
Table 2 average index parameter of preparation example 2
Index (I) Comparative example 2 Preparation example 2
Deposition time (h) / 95
Single furnaceCapacity (ton) 7.65 8.714
Deposition Rate (Kg/h) / 91.73
Single furnace power consumption (KWh/kg) 46 48.4
Trichlorosilane once conversion (%) / 11.04
Leave-in material ratio (%) 57 68.99
Vegetable flower material ratio (%) 18.8 13.71
Ratio of coral material (%) 15.3 7.24
As can be seen from Table 2, compared with the conventional method (i.e. comparative example 2), the washing-free material ratio of the polysilicon product produced by the method of the invention is improved from 57% to 68.99%, the cauliflower ratio is reduced from 18.8% to 13.71%, the coral ratio is reduced from 15.3% to 7.24%, and the comprehensive quality index is maintained on the polysilicon product prepared by the conventional method. That is, the polysilicon growth control method of the invention can effectively improve the quality of polysilicon products.
According to the polysilicon growth control method, based on real-time data interaction between DCS control and a power supply control system in the whole process, voltage drop is used as a key control point in the reduction production process, the influence of disturbance factor fluctuation is offset by adopting automatic adjustment, and a U-I standard curve control mode is established, so that the voltage is stably reduced, and further overload electric faults during operation are avoided; and the control mode of combining flow field simulation and volt-ampere characteristic curve is adopted to realize the rapid growth of the no-clean material, the automatic independent control of a single reduction furnace process can be realized, the growth mode with stable and controllable growth speed and the power consumption reduction control mode are obtained, and the method is favorable for obtaining the low-cost high-quality polysilicon product.
It is to be understood that the above embodiments are merely illustrative of the application of the principles of the present invention, but not in limitation thereof. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the invention, and are also considered to be within the scope of the invention.

Claims (8)

1. A method of polysilicon growth control comprising:
s1, establishing a rapid fusing control curve according to a transformer thyristor rapid fusing parameter of a power supply control system matched with a reduction furnace, and writing the rapid fusing control curve into a DCS (distributed control system);
s2, establishing a mathematical model through collected current and voltage data of a furnace number reaching expected index performance in the past operation of the reduction furnace, obtaining a U-I standard curve, and writing the U-I standard curve into a DCS system;
s3, a reference feed table is established, parameter values in the reference feed table are set on a DCS system, real-time data interaction is realized between the DCS system and a power supply control system of the reduction furnace through a network and a corresponding communication protocol, real-time data of running current and voltage of the reduction furnace are acquired based on the DCS system in the production process, and a U-I real-time curve is obtained;
s4, comparing the U-I real-time curve with the U-I standard curve, and correcting the parameter value in the formulated reference feeding table according to the comparison result of the actual voltage in the U-I real-time curve and the standard voltage in the U-I standard curve so as to enable the actual voltage to reach the standard voltage when the actual current reaches the standard current, thereby obtaining a final control curve and a polysilicon product with uniform quality, wherein the polysilicon product is produced according to the final control curve;
and step S4 is to compare the U-I real-time curve with the U-I standard curve, and correct the parameter value in the formulated reference feeding table according to the comparison result of the actual voltage in the U-I real-time curve and the standard voltage in the U-I standard curve, and comprises the following steps:
comparing the actual voltage with the standard voltage once every period t1 to obtain an actual voltage deviation value delta U;
the absolute value of the actual voltage deviation value delta U is compared with a preset voltage operation deviation set value delta U 0 Comparing, and when the absolute value of the actual voltage deviation value DeltaU is larger than the preset voltage operation deviation set value DeltaU 0 And when the time for keeping the actual voltage deviation value delta U reaches the voltage deviation judging time t2, the DCS system triggers a current/hydrogen/trichlorosilane adjusting mechanism.
2. The method according to claim 1, wherein the step S2 is to build a mathematical model by collecting current and voltage data of a heat reaching an expected index performance in a previous operation of the reduction furnace, and obtain a U-I standard curve, and specifically comprises the steps of:
in the prior art, selecting a furnace number with a silicon rod growth rate, power consumption and a washing-free material/vegetable flower material/coral material ratio reaching expected indexes, and establishing a mathematical model according to actual voltage and current data of the selected furnace number in the production process to fit to obtain the U-I standard curve, wherein the equation of the U-I standard curve is as follows:
U=aI 6 +bI 5 +cI 4 +dI 3 +eI 2 +fI+K
wherein a, b, c, d, e, f are control coefficients generated by fitting, respectively, and a, b, c, d, e, f are not zero at the same time; k is a constant; i > 0.
3. The method of claim 2, wherein the silicon rod growth rate, power consumption, and wash-free/flowering/coral material ratio reaching the desired level are: the growth rate of the silicon rod is more than 80Kg/h, the power consumption is less than 50KWh/Kg, and the ratio of the no-clean material to the cauliflower material to the coral material is more than 80 percent.
4. The method of claim 1, wherein the standard voltage in the U-I standard curve is less than or equal to the fuse voltage in the fuse control curve at the same current.
5. The method of claim 1, wherein the period t1 is 5-10min;
the voltage operation deviation set value delta U 0 5% -10% of the difference between the corresponding standard voltage and the voltage on the corresponding fast fuse control curve;
the voltage deviation judging time is 5-10min, and is more than or equal to the period t1.
6. The method according to any one of claims 1 to 5, wherein the U-I standard curves are determined for different silicon rod growth rates, power consumption, and polysilicon production runs of no-wash/cauliflower/coral ratios, respectively;
and the same U-I standard curve is adopted for the same furnace type of the reduction furnace.
7. The method for controlling growth of polycrystalline silicon according to any one of claims 1 to 5, wherein a U-I standard curve is established for different reduction furnace barrels, respectively;
and the silicon rod in each reduction furnace is divided into a plurality of phases for arrangement, and the actual voltage and the actual current of each phase are respectively and independently collected in real time to respectively obtain U-I standard curves of different phases.
8. The method of any one of claims 1-5, further comprising:
s5, using the final control curve of the last polysilicon production furnace as a correction curve of the next polysilicon production furnace.
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