CN114545865A - Polycrystalline silicon growth control method - Google Patents
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 51
- 230000009467 reduction Effects 0.000 claims abstract description 60
- 238000004519 manufacturing process Methods 0.000 claims abstract description 41
- 229920005591 polysilicon Polymers 0.000 claims abstract description 33
- 238000013178 mathematical model Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims description 62
- 239000001257 hydrogen Substances 0.000 claims description 46
- 229910052739 hydrogen Inorganic materials 0.000 claims description 46
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 43
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 38
- 229910052710 silicon Inorganic materials 0.000 claims description 37
- 239000010703 silicon Substances 0.000 claims description 37
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 29
- 239000005052 trichlorosilane Substances 0.000 claims description 29
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- G05B19/00—Programme-control systems
- G05B19/02—Programme-control systems electric
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- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
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Abstract
The invention discloses a polycrystalline silicon growth control method, which comprises the following steps: establishing a rapid fusing control curve and writing the rapid fusing control curve into a DCS (distributed control system); acquiring a U-I standard curve by establishing a mathematical model, and writing the U-I standard curve into a DCS; a reference feeding table is formulated and set on a DCS, real-time data of the operating current and voltage of the reduction furnace are collected based on the DCS 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 producing the polycrystalline silicon product with uniform quality according to the final control curve. The invention can avoid the electrical fault caused by overload operation of the reducing furnace and obtain the polysilicon product with uniform quality.
Description
Technical Field
The invention belongs to the technical field of polycrystalline silicon, and particularly relates to a polycrystalline silicon growth control method.
Background
At present, most of polysilicon enterprises in China adopt basically the same production process control mode during polysilicon production, high-value polysilicon products are produced by controlling material quantity ratio and current mainly based on diameter calculation or temperature measurement setting of polysilicon rods, and a constant temperature control technology linear feeding control mode is mainly adopted abroad. In the control modes, temperature measurement or diameter measurement is carried out by means of external equipment through a sight glass, the complexity of a flow field and a temperature field of a large-diameter reduction furnace is considered, point temperature is generally adopted to represent the overall temperature or the diameter of a single polycrystalline silicon rod is generally adopted to represent the diameter of the overall polycrystalline silicon rod, the shape changes along with the increase of the diameter of the silicon rod growing in the production process and the increase of reaction silicon powder, errors are necessarily caused in the measurement mode, and if the deviation of a control value cannot be timely corrected, the situation that the control of a production process deviates from the actual growth condition is inevitably caused, and a series of production or quality problems are caused.
However, in the actual growth process of 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, namely, the silicon rod grows to have deviation, so that the voltage drop under the current is not equal to the allowable value of a production system, the current is higher under the operation condition when the large 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 is reduced after the temperature is increased, the fuse is fused due to slight fluctuation of the current, the method has great influence on the safe and stable operation of a power supply control cabinet of a polycrystalline silicon production system, and if the long-term overload operation can cause serious damage to the electric operation, the production of a reduction furnace can be seriously influenced. At present, when the silicon rod in the reduction furnace has a growth deviation, almost all the silicon rod depends on the experience of workers in the process of optimizing process control parameters, the silicon rod is pre-judged according to the temperature and the operation condition of the furnace, and each parameter is adjusted, so that the adjustment process is complicated and long, and the effect is very little.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art, and provides a polycrystalline silicon growth control method, which can timely correct the deviation of the growth process of polycrystalline silicon in a reduction furnace, avoid electrical faults caused by overload of the reduction furnace, obtain a growth mode with stable and controllable growth rate of the polycrystalline silicon, and is beneficial to obtaining polycrystalline silicon products with uniform quality.
The technical scheme for solving the technical problems is as follows:
a polysilicon growth control method comprises the following steps:
s1, establishing a fast fusing control curve according to the transformer controlled silicon fast fusing parameters of the power supply control system matched with the reducing furnace, and writing the fast fusing control curve into a DCS (distributed control system);
s2, establishing a mathematical model through collected current and voltage data of the furnace reaching the expected index performance in the previous operation of the reduction furnace, acquiring a U-I standard curve, and writing the U-I standard curve into a DCS;
s3, making a reference feeding table, setting various parameter values in the reference feeding table on a DCS, realizing real-time data interaction between the DCS and a power supply control system of the reduction furnace through a network and a corresponding communication protocol, acquiring real-time data of the operation current and voltage of the reduction furnace based on the DCS in the production process, and obtaining a U-I real-time curve;
s4, comparing the U-I real-time curve with the U-I standard curve, and correcting the parameter value in the 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, and obtaining a final control curve and producing the polysilicon product with uniform quality according to the final control curve.
Preferably, the step S2 is to obtain the U-I standard curve by establishing a mathematical model through the 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 previous polysilicon production heat, a heat with the silicon rod growth rate, the power consumption and the washing-free material/cauliflower material/coral material ratio reaching the expected indexes is selected, a mathematical model is established according to the actual voltage and current data of the selected heat in the production process, and the U-I standard curve is obtained through fitting, wherein the equation of the U-I standard curve is as follows:
U＝aI6+bI5+cI4+dI3+eI2+fI+K
wherein a, b, c, d, e and f are respectively control coefficients generated by fitting, and a, b, c, d, e and f are not zero at the same time; k is a constant; i is greater than 0.
Preferably, when the growth rate and the power consumption of the silicon rod and the ratio of the washing-free material/the cauliflower material/the coral material reach the expected indexes, the method comprises the following steps: 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 washing-free material/the cauliflower material/the coral material is more than 80%.
Preferably, the standard voltage in the U-I standard curve is less than or equal to the fast fusing voltage in the fast fusing 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 values in the established reference feed table according to the comparison result between the actual voltage in the U-I real-time curve and the standard voltage in the U-I standard curve, including:
every period t1Comparing the actual voltage with the standard voltage for one time to obtain an actual voltage deviation value delta U;
comparing the absolute value of the actual voltage deviation value delta U with a preset voltage operation deviation set value delta U0, and triggering a current/hydrogen/trichlorosilane adjustment mechanism by the DCS when the absolute value of the actual voltage deviation value delta U is larger than the preset voltage operation deviation set value delta U0 and the time for keeping the actual voltage deviation value delta U reaches the voltage deviation judgment time t 2.
Preferably, the period t is1For 5-10 min;
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 rapid fusing control curve;
the voltage deviation judgment time is 5-10min and is not less than the period t1。
Preferably, a U-I standard curve is respectively determined for polysilicon production furnaces with different silicon rod growth rates, power consumption and washing-free material/cauliflower material/coral material ratios;
and the same reduction furnace type adopts the same U-I standard curve.
Preferably, for different reduction furnace barrels, a U-I standard curve is respectively established;
and the silicon rod in each reducing furnace is divided into a plurality of phases to be arranged, and the actual voltage and the actual current of each phase are respectively and independently collected in real time to respectively obtain the U-I standard curves of different phases.
Preferably, the method further comprises:
s5 uses the final control curve of the previous polysilicon producing heat as a correction curve of the next polysilicon producing heat.
The method for controlling the growth of the polycrystalline silicon is based on real-time data interaction of a whole-process DCS (distributed computer control system) control and power supply control system, uses voltage drop as a key control point in the reduction production process, adopts automatic adjustment to counteract the influence of interference factor fluctuation, and establishes a U-I (voltage-current) standard curve control mode, so that the voltage is stably reduced, and further, the overload electrical fault of operation is avoided; and the material-washing-free rapid growth is realized by adopting a control mode combining flow field simulation (simulation by POLYSIM software) and a volt-ampere characteristic curve (namely a U-I curve), the automatic independent control of the process of a single reduction furnace can be realized, a growth mode with stable and controllable growth speed and a power consumption reduction control mode are obtained, and the method is favorable for obtaining a low-cost high-quality polycrystalline silicon product.
Drawings
FIG. 1 is a flow chart illustrating the steps of a method for controlling the growth of polysilicon according to an embodiment of the present invention;
FIG. 2 is a schematic illustration of various curves in an embodiment of the present invention;
FIG. 3 is a graph showing a control curve of rapid fusing of thyristor in a transformer of an electronic control system associated with 36 pairs of rod reduction furnaces in an embodiment of the present invention;
FIG. 4 is a comparison of a fast fusing control curve and a U-I real-time curve for each phase in an embodiment of the present invention.
In the figure: 1-fast fusing control curve; 2-U-I real-time curve; 3-U-I standard curve.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is obvious that the described embodiments are a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, belong to the scope of the present invention.
In the description of the present invention, it is to be understood that the directional terms as used herein are used in a specific orientation or positional relationship shown in the drawings, and are used for convenience in describing the present invention and for simplicity in description, but do not indicate or imply that the device or element so referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be considered as limiting the present invention.
Example 1
As shown in fig. 1, the present embodiment discloses a method for controlling polysilicon growth, which includes:
s1, establishing a fast fusing control curve according to the transformer thyristor fast fusing parameters (namely the voltage parameters of the fast fusing fuse in the transformer which need to be corresponding under different current parameters) of the power supply control system matched with the reducing furnace, and writing the fast fusing control curve into a DCS (distributed control system);
s2, establishing a mathematical model through collected current and voltage data of the furnace reaching the expected index performance in the previous operation of the reduction furnace, acquiring a U-I standard curve, and writing the U-I standard curve into a DCS;
s3, a reference feeding table (including parameters such as growth running time, trichlorosilane/hydrogen feeding amount, silicon rods and current of each phase of silicon rod) is set, each parameter value in the reference feeding table is set on a DCS, real-time data interaction between the DCS and a power supply control system of the reduction furnace is realized through a network and a corresponding communication protocol (such as a PROFIBUS communication protocol), real-time data of the running current and voltage of the reduction furnace are collected based on the DCS 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 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 that the actual voltage reaches the standard voltage when the actual current reaches the standard current (namely, the voltage drop is controlled, the voltage drop reflects the actual growth state of the silicon rod in the reduction furnace, is the comprehensive feedback of the diameter, the surface temperature and the temperature condition in the furnace, the voltage of each phase of the silicon rod can be fed back in real time, the lower the voltage drop, the higher the deposition rate, the lower the power consumption), thereby controlling the reduction furnace to operate stably, and obtaining the final control curve and the polycrystalline silicon product with uniform quality produced according to the final control curve.
In this embodiment, the step S2 is to establish a mathematical model by using collected current and voltage data of a heat reaching an expected index performance in the previous operation of the reduction furnace, and obtain a U-I standard curve, including the following steps:
in the traditional polysilicon production heat, a heat with the silicon rod growth rate, the power consumption and the washing-free material (namely, the polysilicon product with compact, uniform and good appearance and capable of meeting the direct use requirement) and the ratio of the cauliflower material to the coral material reaching the expected index (namely, the power consumption is reduced or the washing-free material ratio is improved as the optimization target) is selected, a mathematical model is established according to the actual voltage and the actual current data of the selected heat in the production process, the U-I standard curve is obtained by fitting, and repeated verification is carried out for many times. The equation of the above obtained U-I standard curve is:
U＝aI6+bI5+cI4+dI3+eI2+fI+K
wherein a, b, c, d, e and f are respectively control coefficients generated by fitting, and a, b, c, d, e and f are not zero at the same time; k is a constant; i is more than 0 (not including the actual current in the blowing-out current reduction stage), and the deviation of the U-I standard curve obtained by linear fitting is R2≥0.9998。
It should be noted that, since the current for each growth time is constant and the current corresponds to the time one by one, the U-I standard curve can also be represented by fitting the growth time to the variation of the voltage with the growth time (T), that is, the above obtained U-I standard curve can also be represented as U-gT6+hT5+jT4+kT3+mT2+ nT + K (where g, h, j, K, m, n are control coefficients generated by fitting, respectively, and g, h, j, K, m, n are not zero at the same time), so as 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 wash-free/cauliflower/coral material ratio reaching the desired criteria are: the growth rate of the silicon rod is more than 80Kg/h, for example, more than 90 Kg/h; the power consumption is < 50KWh/kg, for example < 49 KWh/kg; the total proportion range of the washing-free material/the cauliflower material/the coral material is more than 80 percent.
In some embodiments, the standard voltage in the U-I standard curve is equal to or less than the fast fusing voltage in the fast fusing control curve at the same current, i.e. the U-I standard curve is confirmed to be controlled under the fast fusing control curve (as shown in fig. 2) to avoid the electrical fault caused by voltage overload.
In this embodiment, the step S4 of comparing the U-I real-time curve with the U-I standard curve and modifying the parameters in the established reference feeding table according to the comparison result between the actual voltage in the U-I real-time curve and the standard voltage in the U-I standard curve includes the following steps:
(4-1) every time period t1The actual voltage and the standard are comparedComparing the voltages for one time to obtain an actual voltage deviation value delta U;
(4-2) comparing the absolute value of the actual voltage deviation value delta U with a preset voltage operation deviation set value delta U0Comparing, and when the absolute value of the actual voltage deviation value delta U is larger than the preset voltage operation deviation set value delta U0And keeping the time of the actual voltage deviation value delta U to reach the voltage deviation judgment time t2And triggering a current/hydrogen/trichlorosilane adjustment mechanism by the DCS. The principle of the current/hydrogen/trichlorosilane adjustment mechanism is as follows: the voltage drop reflects the actual growth state of the silicon rod in the reduction furnace, the diameter, the surface temperature and the temperature condition in the furnace are comprehensively fed back, 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 power consumption is, the hydrogen amount or the trichlorosilane amount is adjusted, namely, the material amount ratio is changed, the temperature in the furnace and the surface temperature of the silicon rod are changed, the voltage drop of the silicon rod is further influenced, the growth speed of the silicon rod is further influenced, and therefore, the voltage drop of the silicon rod can be adjusted by adjusting the hydrogen amount or the trichlorosilane amount.
In some embodiments, the period t1The voltage comparison is performed every 5-10min for 5-10 min. Voltage operation deviation set value delta U0The difference value of the voltage of the fast fusing parameter on the corresponding standard voltage and the corresponding fast fusing control curve is 5-10 percent; the voltage deviation judgment time is 5-10min and is not less than the period t1So as to determine whether the actual voltage deviates from the standard voltage by the required regulating degree, and avoid over regulation.
Specifically, the time period t of voltage parameter comparison is set on the DCS system1Every time period t1The actual voltage is compared with the standard voltage once, and a deviation allowable range of the actual voltage and the standard voltage is set on the DCS system, namely a voltage allowable deviation set value delta U is set0. In the running process of the reducing furnace, according to a set time period t1Calculating the difference between the current actual voltage and the standard voltage to obtain the actual voltage deviation value delta U, and a period t1An actual deviation value deltau is calculated.Operating the deviation set value delta U by using the actual deviation value delta U and the voltage0And (3) comparison:
if the absolute value of the actual voltage deviation value delta U is smaller than the allowable voltage deviation set value delta U0Then, the reduction furnace is kept to continue to operate according to the corresponding parameters in the reference feeding table without additional adjustment;
if the absolute value of the actual voltage deviation value delta U is larger than the allowable voltage deviation set value delta U0Calculating the corresponding voltage deviation judgment time by using a start timer on the DCS system, and when the voltage deviation judgment time t is reached2Then, the absolute value of the actual voltage deviation value delta U is still larger than the allowable voltage deviation set value delta U0Then the DCS triggers a current/hydrogen/trichlorosilane adjustment mechanism; when the voltage deviation time does not reach the set voltage deviation judgment time t2Then, the absolute value of the actual voltage deviation value delta U is changed to be smaller than the allowable voltage deviation set value delta U0And then the current/hydrogen/trichlorosilane regulation mechanism is not triggered.
The trigger current/hydrogen/trichlorosilane adjustment mechanism comprises two conditions of positive voltage deviation (shown in the upper part of a curve 2 shown in figure 2 and above a curve 3) and negative voltage deviation (shown in the lower part of the curve 2 shown in figure 2 and below the curve 3), and the specific adjustment process is as follows:
first hydrogen adjustment amount, second hydrogen adjustment amount, trichlorosilane adjustment amount and adjusted hydrogen variation amplitude are preset on a DCS (distributed control system), wherein the first hydrogen adjustment amount and the second hydrogen adjustment amount are 5-10% of hydrogen value parameters in a corresponding reference feeding table, the first hydrogen adjustment amount is preferably 5%, the second hydrogen adjustment amount is preferably 10%, the trichlorosilane adjustment amount is 5-10% of the trichlorosilane parameters in the corresponding reference feeding table, and the adjusted hydrogen variation amplitude is the slope of voltage variation of a corresponding U-I standard curve;
when the condition of positive voltage deviation is satisfied, namely the actual voltage-standard voltage > the voltage allowable deviation set value delta U0Firstly, according to the preset first hydrogen regulation quantity (for example, according to 5% of hydrogen value parameter in correspondent reference feeding table) making hydrogen quantity reduction process, and making the hydrogen quantity reduction process implementThe hydrogen change is carried out according to the preset adjusted hydrogen change amplitude, and simultaneously, a timer is started to start timing and reaches three periods t during timing1Then judging whether the voltage positive deviation condition is satisfied, if not, the absolute value of the actual voltage deviation delta U is less than the allowable deviation set value delta U0Continuing to operate 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 time reaches three periods t1If the positive deviation condition of the voltage is still met, then reducing the hydrogen according to a preset second hydrogen regulating quantity (for example, according to 10% of the hydrogen value parameter in the corresponding reference feeding table), starting the timer again to start timing, and reaching three periods t when the timing is up to1Then, whether the voltage positive deviation condition is met is judged again, if the voltage positive deviation condition is not met, the absolute value of the actual voltage deviation delta U is smaller than the voltage allowable deviation set value delta U0Continuing to operate 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 three periods t are provided1And then, if the voltage positive deviation condition is still met, keeping the given value of the current trichlorosilane/current/hydrogen regulating quantity unchanged, and sending a system early warning signal to prompt an operator to check and perform manual intervention until the actual voltage deviation delta U is recovered to the voltage allowable deviation set value delta U0And after the alarm is over, early warning is eliminated.
When the negative deviation condition of the voltage is satisfied, namely the standard voltage-actual voltage > the voltage allowable deviation set value delta U0During the process, because the influence of hydrogen on a thermal field and a gas field in the reducing furnace is large, and the amount of the hydrogen cannot be too large, so as to prevent the growth condition of the whole polycrystalline silicon rod from seriously deviating, when the negative voltage deviation exists, the adjustment is preferentially carried out by adjusting the amount of the hydrogen, if the negative voltage deviation still exists, namely the expected effect is not achieved after the adjustment of the amount of the hydrogen, the atomization condition existing in the reducing furnace is not controlled, at the moment, the reference amount of the corresponding trichlorosilane is too large, and the amount of the trichlorosilane needs to be reduced to control the atomization, and the specific process is as follows: according to the presetPerforming hydrogen increasing on the first hydrogen adjusting amount (for example, 5% of the hydrogen value parameter in the corresponding reference feeding table), and enabling the hydrogen change in the hydrogen increasing process to be performed according to the preset adjusted hydrogen change amplitude, namely, adjusting by increasing the hydrogen amount; at the same time, starting a timer to start timing, and reaching three periods t when the timing is finished1Then judging whether the negative deviation condition of the voltage is satisfied, if not, the absolute value of the actual voltage deviation delta U is less than the set value delta U of the allowable deviation0Continuing to operate the reduction furnace according to the parameters of the corresponding time points in the reference material supply table, namely recovering the parameters of the reference work material table of the corresponding time points, and if the timing reaches three periods t1If the negative bias condition of the voltage is still met, reducing the trichlorosilane according to a preset trichlorosilane adjustment amount (for example, according to 10 percent of the trichlorosilane parameter in a corresponding reference feeding table), namely, reducing the amount of the trichlorosilane for adjustment; meanwhile, the timer is started again to start timing, and the timing reaches three periods t1Then, whether the negative deviation condition of the voltage is satisfied is judged again, if the negative deviation condition of the voltage is not satisfied, the absolute value of the actual voltage deviation delta U is smaller than the set value delta U of the allowable voltage deviation0Continuing to operate 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 three periods t are provided1And then, the negative voltage deviation condition is still met, namely, the expected effect is not achieved after the quantity of the trichlorosilane is reduced, and the abnormal growth of the polycrystalline silicon rod is proved to be caused by the problems of hydrogen, the purity of the trichlorosilane material and the like possibly existing in the reduction furnace, the current regulating quantity/current/hydrogen set value is kept unchanged, and a system early warning signal is sent out to prompt an operator to check and perform manual intervention until the actual voltage deviation delta U is recovered to the voltage allowable deviation set value delta U0And after the alarm is over, early warning is eliminated.
In some embodiments, the U-I standard curve is determined for polysilicon production runs with different quality indicators, such as silicon rod growth rate, power consumption, and wash-free material/cauliflower material/coral material ratio. And the same U-I standard curve can be adopted for the same reduction furnace type.
In some embodiments, the U-I standard curve is established for different reduction furnace cartridges to offset the influence of cooling water on the thermal balance of the cartridges, taking into account the difference in thermal radiation of the respective reduction furnace cartridges. The silicon rod in each reducing furnace is divided into a plurality of phases to be arranged, the actual voltage and the actual current of each phase are respectively and independently collected in real time, and the U-I standard curves of different phases are respectively obtained. Specifically, 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 controlled in a split-phase way, i.e. by a multiple of 3, for example, a reduction furnace with 36 pairs of rods, possibly in 6 phases, 6 pairs of rods per phase, for electrical control, in addition, 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 collected independently, the three phases on the same ring can use the same or similar two values of the three phases as judgment conditions, namely, the inner ring and the outer ring can execute an automatic adjustment program by taking the voltage value 'two out of three' as a judgment condition, so that excessive adjustment is avoided, and the complexity of controlling the gas field and the temperature field in the reduction furnace, particularly the large-scale reduction furnace, is favorably controlled.
In some embodiments, the method further comprises:
s5 uses the final control curve of the previous polysilicon production heat as the correction curve (i.e., U-I standard curve) of the next polysilicon production heat, and compares the U-I standard curve U-aI obtained by the loop closure verification (i.e., once comparing the U-I standard curve of the previous heat with the U-I standard curve of the next heat every time the production of one heat is completed)6+bI5+cI4+dI3+eI2And whether the control parameter of + gI + K is stable or not, and simultaneously, the uniformity of the quality of the controlled produced polycrystalline silicon product is verified according to the indexes of discharging power consumption/deposition rate/no-clean material and the like.
In some embodiments, the reference feed meter adopts a control mode of 'atomization critical point' with large material quantity and high current, namely, a stable gas field and a temperature field are quickly established at the initial growth stage of polycrystalline silicon to reach a state close to atomization, at the moment, the deposition speed is the fastest, and the complicated working conditions of the gas field and the temperature field in the furnace are simulated by using polycrystalline silicon growth trend simulation software (such as POLYSIM software), so that the establishment of a stable flow field for polycrystalline silicon growth is ensured, and the stable flow field is the basis for uniform growth of the silicon rod, so that the quick and uniform deposition of the polycrystalline silicon is realized.
The polysilicon growth control method of the present embodiment is described in detail in two directions of reducing power consumption and increasing the wash-free material ratio, taking a 36-pair rod furnace type as an example, according to the production profit requirement:
preparation example 1
The method for controlling the growth of the polycrystalline silicon comprises the following steps:
establishing a fast fusing control curve according to the fast fusing parameters of the transformer thyristor of an electric control system matched with the 36 pairs of rod reduction furnaces, as shown in figure 3 (wherein 4P represents phases of 4 pairs of rods, and 8P represents phases of 8 pairs of rods), and writing the fast fusing control curve into a DCS (distributed control system);
selecting a heat with the growth rate of the silicon rod more than 90Kg/h, the power consumption less than 49KWh/Kg and the ratio of the non-washing material to the cauliflower material more than 80% in the previous production as a 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-4E through data fitting-16I6-3E-12I5+1E-08I4-2E-05I3+0.0186I2-10.288I+3965.8(R20.9998), the U-I standard curve can be fitted with the growth time to the variation of voltage with growth time (T) in order to compare the difference between the actual voltage and the voltage to be controlled at a certain time, i.e. the above obtained U-I standard curve can be expressed as U-8E-9T6-5E-6T5+0.0009T4-0.0809T3+3.7961T2-105.22T+2306.7(R20.9998). Comparing the U-I standard curve with the fast fusing control curve, and confirming that the U-I standard curve is controlled below the fast fusing control curve to avoid electrical faults caused by voltage overload;
under the same material supply and auxiliary material conditions, reducing furnaces with expected quality indexes such as the proportion of the washing-free materials in the prior production but high power consumption are selected, and the average power consumption of the reducing furnaces (marked as an experimental furnace 1) and the quality indexes such as the proportion of the washing-free materials are recorded as a comparative example 1 and are detailed in a table 2. Writing the determined U-I standard curve into a DCS of the experimental furnace 1;
setting a reference feeding table, as shown in table 1, setting each parameter value in the reference feeding table on a DCS, realizing real-time data interaction between the DCS and a power supply control system of a reduction furnace through a network and a corresponding communication protocol (such as a PROFIBUS communication protocol), automatically controlling the operation of the reduction furnace by the DCS according to the set reference feeding table when polycrystalline silicon is produced, acquiring real-time data of the operation current and voltage of the reduction furnace based on the DCS in the production process, and obtaining a U-I real-time curve of each phase;
table 1 preparative 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 molar 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 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 control the reduction furnace to stably operate, so that the actual voltage reaches the standard voltage when the actual current reaches the standard current, and a final control curve and a polycrystalline silicon product with uniform quality produced according to the final control curve are obtained. Wherein the allowable deviation of voltage DeltaU0Setting the difference value of the corresponding standard voltage and the voltage on the corresponding rapid fusing control curve to be 5%; period t1Setting for 5 min; voltage deviation determination time t2Set to 10 min. In the operation process of the reduction furnace, comparing the current actual voltage with the standard according to the set voltage parameter comparison period t1Calculating the difference value of the voltage to obtain an actual deviation value delta U, calculating an actual deviation value in each comparison period, and calculating the actual deviation value delta U and a voltage operation deviation set value delta U0And comparing, and automatically controlling the voltage to stably drop by the DCS according to the set current/hydrogen/trichlorosilane adjustment mechanism according to the comparison result, so as to obtain the polycrystalline silicon product with uniform quality.
A comparison graph of the fast fusing control curve of the preparation example and the real-time U-I curves of the phases is shown in fig. 4, and the change of the voltage along with the current in the production process of the polysilicon 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, the actual voltage is greater than the corresponding standard voltage) is judged, so that the actual voltage in the process can be further optimized and reduced in the subsequent production.
Under the same conditions as described above, a plurality of production runs were carried out for each test furnace 1 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 parameters of preparation example 1
As can be seen from Table 2, compared with the conventional method (i.e., comparative example 1), the method of the present invention has the advantages that the power consumption is reduced from 55.5kwh/kg to 45.8kwh/kg, the output per furnace is increased from 7.65 tons to 8.77 tons, and the quality indexes such as the no-clean material ratio and the like are still kept on the polysilicon product prepared by the conventional method, i.e., 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 of the key stage, gradually and stably reduce the power consumption, and can perform the reproduction production on other reduction furnaces.
Preparation example 2
The method for controlling the growth of the polycrystalline silicon comprises the following steps:
similarly, a fast fusing control curve is established according to the fast fusing parameters of the transformer controlled silicon of the electric control system matched with the 36 pairs of rod reduction furnaces, as shown in fig. 3, and is written into a DCS system;
selecting the heat with the washing-free material ratio more than 65% and the power consumption less than 49KWh/kg in the previous 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 fitting data to obtain a U-I standard curve U-3E-16I6-3E-12I5+1E-08I4-2E-05I3+0.0194I2-11.191I+4123.9(R20.9998), the U-I standard curve can be represented again as U-8E in order to facilitate comparison of the difference between the actual voltage and the voltage to be controlled at a certain time-8T6-3E-5T5+0.0033T4-0.2171T3+7.7277T2163.2T + 2636.1. Comparing the U-I standard curve with the fast fusing control curve, and confirming that the U-I standard curve is controlled below the fast fusing control curve to avoid electrical faults caused by voltage overload;
under the same material supply and auxiliary material conditions, reducing furnaces with lower power consumption in the prior art but with quality indexes such as the washing-free material ratio which are still to be improved are selected, and the average power consumption of the reducing furnaces (marked as the experimental furnace 2) and the quality indexes such as the washing-free material ratio are recorded as a comparative example 2 and are detailed in table 4. Writing the determined U-I standard curve into a DCS of the experimental furnace 2;
setting a reference feeding table, as shown in table 3, setting each parameter value in the reference feeding table on a DCS, realizing real-time data interaction between the DCS and a power supply control system of a reduction furnace through a network and a corresponding communication protocol (such as a PROFIBUS communication protocol), automatically controlling the operation of the reduction furnace by the DCS according to the set reference feeding table when polycrystalline silicon is produced, acquiring real-time data of the operation current and voltage of the reduction furnace based on the DCS in the production process, and obtaining a U-I real-time curve of each phase;
table 3 preparative 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 molar 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 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 control the reduction furnace to stably operate, so that the actual voltage reaches the standard voltage when the actual current reaches the standard current, and a final control curve and a polycrystalline silicon product with uniform quality produced according to the final control curve are obtained. Wherein the allowable deviation of voltage DeltaU0Setting the difference value of the corresponding standard voltage and the voltage on the corresponding rapid fusing control curve to be 5%; period t1Setting for 5 min; voltage deviation determination time t2Set to 10 min. In the running process of the reduction furnace, comparing the period t according to the set voltage parameter1Calculating the difference value between the current actual voltage and the standard voltage to obtain an actual deviation value delta U, calculating an actual deviation value in each comparison period, and calculating the actual deviation value delta U and a voltage operation deviation set value delta U0And comparing, and automatically controlling the voltage to stably drop by the DCS according to the set current/hydrogen/trichlorosilane adjustment mechanism according to the comparison result, so as to obtain the polycrystalline silicon product with uniform quality.
Under the same conditions as described above, a plurality of production runs were carried out for each experimental furnace 2 in accordance with the procedure of preparation example 2, and the average index produced in accordance with preparation example 2 was recorded as shown in Table 4.
TABLE 2 average index parameters of preparation example 2
| Index (I) | Comparative example 2 | Preparation example 2 |
| Deposition time (h) | / | 95 |
| Energy production per furnace (ton) | 7.65 | 8.714 |
| Deposition Rate (Kg/h) | / | 91.73 |
| Electric power consumption of single furnace (KWh/kg) | 46 | 48.4 |
| Trichlorosilane Primary conversion (%) | / | 11.04 |
| Proportion of non-washing material (%) | 57 | 68.99 |
| Percentage of vegetable flower material (%) | 18.8 | 13.71 |
| Coral material ratio (%) | 15.3 | 7.24 |
As can be seen from Table 2, compared with the conventional method (i.e., comparative example 2), the content of the no-clean material in the polysilicon product produced by the method of the present invention is increased from 57% to 68.99%, the content of the cauliflower is decreased from 18.8% to 13.71%, the content of the coral is decreased from 15.3% to 7.24%, and the comprehensive quality index is still maintained on the polysilicon product prepared by the conventional method. That is, the quality of the polysilicon product can be effectively improved by adopting the polysilicon growth control method of the invention.
The method for controlling the growth of the polycrystalline silicon is based on real-time data interaction of a full-process DCS control and power supply control system, the voltage drop is used as a key control point in the reduction production process, the influence of interference factor fluctuation is counteracted by automatic adjustment, and a U-I standard curve control mode is established, so that the voltage is stably reduced, and further, the overload electrical fault during operation is avoided; and the control mode combining flow field simulation and volt-ampere characteristic curve is adopted to realize the rapid growth of the washing-free material, the automatic independent control of the process of a single reduction furnace can be realized, the growth mode with stable and controllable growth speed and the control mode of reducing power consumption are obtained, and the method is favorable for obtaining the polycrystalline silicon product with low cost and high quality.
It will be understood that the above embodiments are merely exemplary embodiments taken to illustrate the principles of the present invention, which is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.
Claims (9)
1. A polysilicon growth control method comprises the following steps:
s1, establishing a fast fusing control curve according to the transformer controlled silicon fast fusing parameters of the power supply control system matched with the reducing furnace, and writing the fast fusing control curve into a DCS (distributed control system);
s2, establishing a mathematical model through collected current and voltage data of the furnace reaching the expected index performance in the previous operation of the reduction furnace, acquiring a U-I standard curve, and writing the U-I standard curve into a DCS;
s3, a reference feeding table is set, each parameter value in the reference feeding table is set on a DCS, real-time data interaction between the DCS and a power supply control system of the reduction furnace is achieved through a network and a corresponding communication protocol, real-time data of the operation current and voltage of the reduction furnace are collected based on the DCS 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 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, and obtaining a final control curve and producing the polysilicon product with uniform quality according to the final control curve.
2. The method for controlling the growth of polycrystalline silicon according to claim 1, wherein the step S2 is to establish a mathematical model by collecting current and voltage data of a heat reaching a desired index performance in the past operation of the reduction furnace, to obtain a U-I standard curve, and specifically comprises the steps of:
in the previous polysilicon production heat, a heat with the silicon rod growth rate, the power consumption and the washing-free material/cauliflower material/coral material ratio reaching the expected indexes is selected, a mathematical model is established according to the actual voltage and current data of the selected heat in the production process, and the U-I standard curve is obtained through fitting, wherein the equation of the U-I standard curve is as follows:
U＝aI6+bI5+cI4+dI3+eI2+fI+K
wherein a, b, c, d, e and f are respectively control coefficients generated by fitting, and a, b, c, d, e and f are not zero at the same time; k is a constant; i is greater than 0.
3. The method for controlling the growth of polycrystalline silicon according to claim 2, wherein the silicon rod growth rate, the power consumption and the washing-free material/cauliflower material/coral material ratio reaching the expected indexes are as follows: 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 non-washing material/the cauliflower material/the coral material is more than 80%.
4. The method of claim 1, wherein the standard voltage in the U-I standard curve is less than or equal to the fast fusing voltage in the fast fusing control curve at the same current.
5. The method as claimed in claim 1, wherein the step S4 compares the U-I real-time curve with the U-I standard curve, and corrects the parameter values in the established reference feed table according to the comparison result between the actual voltage in the U-I real-time curve and the standard voltage in the U-I standard curve, comprising:
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 and a preset voltage operation deviation set value delta U are compared0Comparing, and when the absolute value of the actual voltage deviation value delta U is larger than the preset voltage operation deviation set value delta U0And when the time for keeping the actual voltage deviation value delta U reaches the voltage deviation judgment time t2, triggering a current/hydrogen/trichlorosilane adjustment mechanism by the DCS.
6. The method for controlling the growth of the polycrystalline silicon as claimed in claim 5, wherein the period t1 is 5-10 min;
the voltage operation deviation set value delta U0The difference value of the corresponding standard voltage and the voltage on the corresponding rapid fusing control curve is 5% -10%;
the voltage deviation judgment time is 5-10min and is more than or equal to the period t 1.
7. The method for controlling the growth of polycrystalline silicon according to any one of claims 1 to 6, wherein a U-I standard curve is determined for different silicon rod growth rates, power consumption, and polycrystalline silicon production heat times of a washing-free material/a cauliflower material/a coral material ratio, respectively;
and the same U-I standard curve is adopted for the same reduction furnace type.
8. The method for controlling the growth of polycrystalline silicon according to any one of claims 1 to 6, wherein for different reduction furnace barrels, a U-I standard curve is respectively established;
and the silicon rod in each reducing furnace is divided into a plurality of phases to be arranged, and the actual voltage and the actual current of each phase are respectively and independently collected in real time to respectively obtain the U-I standard curves of different phases.
9. The polysilicon growth control method according to any one of claims 1 to 6, further comprising:
s5 uses the final control curve of the previous polysilicon producing heat as a correction curve of the next polysilicon producing heat.
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