CN109448800B - Method for judging mass gliding time of refined trichlorosilane - Google Patents

Method for judging mass gliding time of refined trichlorosilane Download PDF

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CN109448800B
CN109448800B CN201811584999.3A CN201811584999A CN109448800B CN 109448800 B CN109448800 B CN 109448800B CN 201811584999 A CN201811584999 A CN 201811584999A CN 109448800 B CN109448800 B CN 109448800B
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杨媛丽
吴锋
曹忠
姜海明
宗凤云
贺珍俊
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Orisi Silicon Co ltd
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Abstract

The invention discloses a method for judging the quality downslide time of refined trichlorosilane, which can accurately and quickly determine the quality downslide time of the refined trichlorosilane, provides reliable reference for judging reasons causing the quality downslide of the refined trichlorosilane, and has the advantages of low judgment cost and high calculation precision. The method can quickly find out the reason causing the quality of the refined trichlorosilane to slide down, and further adopts corresponding regulation and control measures aiming at the reason to quickly recover the quality of the polycrystalline silicon, so that the economic loss caused by the quality problem of the polycrystalline silicon caused by the quality of the refined trichlorosilane to slide down is reduced to the minimum.

Description

Method for judging mass gliding time of refined trichlorosilane
The technical field is as follows:
the invention relates to the field of polycrystalline silicon production, in particular to a method for judging the mass gliding time of refined trichlorosilane.
The background art comprises the following steps:
polycrystalline silicon is a basic raw material for the electronic industry and the solar industry, and is widely applied to semiconductor chips, high-performance sensors, optical fibers, solar panels and the like. At present, the polysilicon production technology at home and abroad mostly adopts an improved siemens method, namely, rectified trichlorosilane (hereinafter referred to as refined trichlorosilane) and hydrogen are electrified in a reduction furnace under the high-temperature condition, and chemical vapor deposition reaction is carried out on the surface of a high-temperature silicon rod to obtain high-purity polysilicon until the diameter of the silicon rod in the furnace is gradually increased to the specified rod diameter. Because the polycrystalline silicon is a high-purity product, the requirement on the purity of the raw material fine trichlorosilane for producing the polycrystalline silicon is very high in order to ensure the quality of the polycrystalline silicon product.
In the production process of polycrystalline silicon, although the content of the fine trichlorosilane is sampled and detected every shift, the content of the fine trichlorosilane is lower than a detection line due to the limitation of detection frequency, and the quality of the polycrystalline silicon finally produced obviously slides down; even if the quality of the polysilicon slips down seriously, the sampling detection result of the fine trichlorosilane also judges that the quality of the fine trichlorosilane slips down, but the accurate time of the quality of the fine trichlorosilane is still difficult to determine quickly due to the limitation of sampling frequency, the reason for causing the quality of the fine trichlorosilane to slip down cannot be found out quickly, the normal production is seriously influenced, and serious economic loss is caused to enterprises. But no method for rapidly and accurately checking the mass slip-down time point of the refined trichlorosilane exists at present.
The invention content is as follows:
in order to find out the reason causing the downward sliding of the quality of the fine trichlorosilane as soon as possible and further take corresponding regulation and control measures aiming at the reason so as to quickly recover the quality of the polycrystalline silicon and reduce the economic loss caused by the problem of the quality of the polycrystalline silicon caused by the downward sliding of the quality of the fine trichlorosilane to the minimum.
The production process flow of the polycrystalline silicon mainly comprises the following steps: the whole production process is continuously carried out, and the produced rectified trichlorosilane is directly and continuously supplied to a reduction furnace for use, so that the time point when the quality of the polycrystalline silicon begins to slide down can be determined as the time point when the quality of the rectified trichlorosilane begins to slide down.
The invention aims to provide a method for rapidly and accurately judging the mass slip-down time of refined trichlorosilane, which has high calculation precision and low cost.
The invention is implemented by the following technical scheme:
the method for judging the mass gliding time of the refined trichlorosilane comprises the following steps:
step (1), selecting a calculating furnace, a first reference furnace and a second reference furnace according to a polycrystalline silicon production monitoring machine account;
step (2), respectively calculating the impurity concentrations of the polycrystalline silicon rods of the calculation furnace, the first reference furnace and the second reference furnace;
step (3), determining a drawing scale, drawing a silicon material sampling drawing of the calculating furnace according to the ratio of the diameter of the polycrystalline silicon rod to the sampling drill bit, and marking the deposition radius h of the silicon rod in the drawing Final (a Chinese character of 'gan') And a sampling location;
step (4), calculating the mass ratio of the normal silicon material to the gliding silicon material in the mass of the sampling part in the silicon material sampling graph;
step (5), determining a mass glide time line by using the impurity concentrations of the polycrystalline silicon rods of the calculating furnace, the reference furnace I and the reference furnace II and the mass ratio of the normal-quality silicon material to the mass glide silicon material of the sampling part, and marking the mass glide time line in the silicon material sampling graph;
step (6) calculating the deposition radius h corresponding to the mass gliding time line Lower part
Step (7) utilizing the deposition radius h corresponding to the mass gliding time line Lower part And the data of the polysilicon production monitoring ledger record is used for calculating the deposition time t corresponding to the quality glide time line Lower part ,t Lower part Namely the mass gliding time of the refined trichlorosilane.
Further, in the step (1), the polysilicon production monitoring ledger records deposition radiuses h of silicon rods corresponding to all reduction furnaces Final (a Chinese character of 'gan') Deposition time t Final (a Chinese character of 'gan') The feeding condition and the resistivity of the polycrystalline silicon rod produced by each reducing furnace.
Further, the selection method of the calculating furnace, the first reference furnace and the second reference furnace specifically comprises the following steps:
selecting a reduction furnace without the downward sliding of the resistivity of the polycrystalline silicon rod as a first reference furnace according to the resistivity of the polycrystalline silicon rod recorded in the polycrystalline silicon production monitoring ledger;
selecting a reduction furnace with the lowest resistivity and reaching stability of the polycrystalline silicon rod from the reduction furnaces with the same feeding condition as the reference furnace I as a reference furnace II;
and selecting a reducing furnace with the resistivity of the polycrystalline silicon rod between the resistivity of the polycrystalline silicon rods corresponding to the first reference furnace and the second reference furnace from the reducing furnaces with the same feeding condition as the first reference furnace as a calculating furnace.
Further, in the step (2), the impurity concentrations of the polycrystalline silicon rods in the calculation furnace, the first reference furnace and the second reference furnace are calculated by the following method:
respectively calculating the average impurity concentration a of the polycrystalline silicon rods of the calculation furnace according to the respective polycrystalline silicon rod resistivities of the calculation furnace, the first reference furnace and the second reference furnace recorded in the polycrystalline silicon production monitoring ledger 1 Impurity concentration a of polycrystalline silicon rod of reference furnace I 2 And the impurity concentration a of the polycrystalline silicon rod in the second reference furnace 3
Further, in the step (4), the specific method for calculating the mass ratio of the normal silicon material to the gliding silicon material in mass at the sampling part in the silicon material sampling diagram comprises the following steps:
assuming that the mass of the silicon material sliding down from the sampling part mass in the step (3) is X and the mass of the silicon material with the normal sampling part mass is 1, establishing an equation according to the total mass of impurities of the polycrystalline silicon rod: x a 3 +1*a 2 =(1+X)*a 1 And obtaining X, namely the mass ratio of the mass normal silicon material to the mass sliding silicon material of the sampling part is 1.
Further, in the step (5), a specific method for determining the quality glide time line is as follows:
according to the mass ratio 1X of the normal-mass silicon material to the gliding-mass silicon material of the sampling part determined in the step (4), obtaining that the area ratio of the normal-mass silicon material to the gliding-mass silicon material of the sampling part is 1X according to the principle that the mass ratio = the volume ratio = the area ratio under the equal altitude condition for the same material, and further determining a mass gliding time line.
Further, in the step (6), a deposition radius h corresponding to the mass glide time line is calculated Lower part The specific method comprises the following steps: measuring and calculating the distance between the rod core edge and the mass glide time line in the furnace silicon material sampling diagram, and calculating the deposition radius h corresponding to the mass glide time line according to the drawing scale of the furnace silicon material sampling diagram Lower part
Further, in the step (7), a deposition time t corresponding to the mass glide time line is calculated Lower part The method comprises the following specific steps:
fitting is carried out through data of the silicon rod diameter deposition rates corresponding to different time points of the calculated furnace, and the function relation of the radius deposition rate y of the polycrystalline silicon rod per hour and the deposition time t is obtained as follows:
y=at+b (1)
wherein t is the deposition time of the reduction furnace calculated from the beginning of the feeding, a is a correction coefficient for the deposition rate due to temperature change, a is a negative number, and b is the initial deposition rate calculated from the beginning of the feeding; under the condition of a certain feeding current, b is a fixed value and can be obtained by measurement;
the total deposition radius of the i-th polycrystalline silicon rod is
Figure GDA0003150632920000051
The deposition radius h of the silicon rod of the furnace is calculated Terminal Deposition time t Terminal Substituting in formula (2) to obtain a;
substituting a into the formula (2), and determining the deposition radius h corresponding to the mass gliding timeline determined in the step (5) Lower part In the formula (2), the deposition time t corresponding to the mass gliding time line can be calculated Lower part
The invention has the advantages that:
the method can accurately and quickly determine the mass downslide time of the refined trichlorosilane, provides reliable reference for judging the reason of the mass downslide of the refined trichlorosilane, has the advantages of low judgment cost and high calculation precision, and has obvious effect and higher popularization value proved by practice.
By the method, the reason causing the quality of the refined trichlorosilane to slide down can be quickly found out, and corresponding regulation and control measures are taken aiming at the reason so as to quickly recover the quality of the polycrystalline silicon and minimize the economic loss caused by the quality problem of the polycrystalline silicon caused by the quality slide down of the refined trichlorosilane.
Description of the drawings:
in order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a graph showing resistivity data of polysilicon rods in a calculation furnace, a first reference furnace and a second reference furnace according to the present embodiment;
FIG. 2 is a silicon material sampling diagram of the furnace in this embodiment;
FIG. 3 is a fitted line of calculated furnace diameter deposition rates in this example.
The specific implementation mode is as follows:
the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the method for judging the mass gliding time of the refined trichlorosilane comprises the following steps:
step (1), selecting a calculating furnace, a first reference furnace and a second reference furnace according to a polycrystalline silicon production monitoring ledger;
step (2), respectively calculating the impurity concentrations of the polycrystalline silicon rods of the calculation furnace, the first reference furnace and the second reference furnace;
step (3), determining a drawing scale, drawing a silicon material sampling drawing of the calculating furnace by using a CAD (computer aided design) according to the ratio of the diameter of the polycrystalline silicon rod to the sampling drill bit and the actual sampling condition, and marking the deposition radius h of the silicon rod on the drawing Final (a Chinese character of 'gan') And a sampling position, as shown in FIG. 2;
step (4), calculating the mass ratio of the normal silicon material to the gliding silicon material in the mass of the sampling part in the silicon material sampling graph;
determining a mass gliding time line by utilizing the impurity concentrations of the polycrystalline silicon rods of the calculating furnace, the first reference furnace and the second reference furnace and the mass ratio of the normal-quality silicon material to the mass gliding silicon material of the sampling part, and marking the mass gliding time line on a silicon material sampling graph;
step (6) calculating the deposition radius h corresponding to the mass gliding time line Lower part
Step (7) utilizing the deposition radius h corresponding to the mass gliding time line Lower part And data of the monitoring ledger records of the polysilicon production, and calculating the deposition time t corresponding to the quality glide time line Lower part ,t Lower part Namely the mass gliding time of the refined trichlorosilane.
In the step (1), the deposition radiuses h of the silicon rods corresponding to all the reduction furnaces are recorded in a polysilicon production monitoring ledger Final (a Chinese character of 'gan') Deposition time t Final (a Chinese character of 'gan') The feeding condition and the resistivity of the polycrystalline silicon rod produced by each reducing furnace.
The selection method of the calculating furnace, the first reference furnace and the second reference furnace specifically comprises the following steps:
selecting a reduction furnace without the downward sliding of the resistivity of the polycrystalline silicon rod as a first reference furnace according to the resistivity of the polycrystalline silicon rod recorded in the polycrystalline silicon production monitoring ledger;
selecting a reduction furnace with the lowest resistivity and stability of the polycrystalline silicon rod from the reduction furnaces with the same feeding condition as the reference furnace I as a reference furnace II;
from among the reduction furnaces fed in the same manner as the reference furnace one, a reduction furnace having a resistivity of the polycrystalline silicon rod between the resistivities of the polycrystalline silicon rods corresponding to the reference furnace one and the reference furnace two was selected as a calculation furnace, as shown in fig. 1. Since the resistivity in the reduction furnace can intuitively reflect the quality of the polysilicon rod, in this embodiment, the decrease in resistivity is used as a basis for determining the slip-down of the polysilicon quality.
In the step (2), the impurity concentrations of the polycrystalline silicon rods of the calculating furnace, the first reference furnace and the second reference furnace are calculated by the following method:
according to polysilicon production monitoringThe resistivity of the polycrystalline silicon rod of the calculation furnace, the resistivity of the polycrystalline silicon rod of the reference furnace I and the resistivity of the polycrystalline silicon rod of the reference furnace II recorded in the ledger are respectively calculated according to the national standard GB/T13389-2014 1 Impurity concentration a of polycrystalline silicon rod of reference furnace I 2 And the impurity concentration a of the polycrystalline silicon rod in the second reference furnace 3 . In this embodiment, the resistivity recorded in the monitoring ledger is determined by using a zone-melting furnace and a resistance tester, performing zone-melting by using a method specified in the national standard GB/T4059-2007, and then using a method required by the national standard GB/T1551-2009.
In the step (4), the specific method for calculating the mass ratio of the normal silicon material to the gliding silicon material in mass at the sampling part in the silicon material sampling diagram comprises the following steps:
assuming that the mass of the silicon material sliding down from the sampling part mass in the step (3) is X and the mass of the silicon material normal to the sampling part mass is 1, an equation is established according to the total mass of the impurities of the polycrystalline silicon rod as the total mass X the impurity concentration = the total mass of the impurities: x a 3 +1*a 2 =(1+X)*a 1 And (4) calculating X, namely the mass ratio of the normal silicon material to the gliding silicon material in mass of the sampling part is 1.
In the step (5), the specific method for determining the quality glide time line comprises the following steps:
according to the mass ratio 1 x of the normal-quality silicon material to the gliding-quality silicon material of the sampling part determined in the step (4), obtaining that the area ratio of the normal-quality silicon material to the gliding-quality silicon material of the sampling part is 1 x according to the principle that the mass ratio = volume ratio = area ratio under the condition of equal height for the same substance, and determining the mass gliding time line by adopting a trial and error method to make the area ratio of the part in the mass gliding time line of the sampling part to the part outside the mass gliding time line be 1 x.
In the step (6), the deposition radius h corresponding to the mass gliding time line is calculated Lower part The specific method comprises the following steps: measuring and calculating the distance between the rod core edge and the mass glide time line in the furnace silicon material sampling diagram, and calculating the deposition radius h corresponding to the mass glide time line according to the drawing scale of the furnace silicon material sampling diagram Lower part
In step (7), countingCalculating the deposition time t corresponding to the mass glide time line Lower part The method comprises the following specific steps:
fitting is carried out through the detected data of the silicon rod diameter deposition rate corresponding to different time points of the calculated furnace, and the function relation of the radius deposition rate y of the polycrystalline silicon rod per hour and the deposition time t is obtained as follows:
y=at+b (1)
wherein t is the deposition time of the reduction furnace calculated from the beginning of the feeding, a is a correction coefficient for the deposition rate due to temperature change, a is a negative number, and b is the initial deposition rate calculated from the beginning of the feeding; under the condition of a certain feeding current, b is a fixed value and can be obtained by measurement;
the total deposition radius of the i-th polycrystalline silicon rod is
Figure GDA0003150632920000091
Calculating the deposition radius h of the silicon rod of the furnace Terminal Deposition time t Terminal Substituting in formula (2) to obtain a;
substituting a into the formula (2), and determining the deposition radius h corresponding to the mass gliding timeline determined in the step (5) Lower part In the formula (2), the deposition time t corresponding to the mass glide time line can be calculated Lower part
In this embodiment, the silicon rod diameter deposition rates corresponding to different time points of the furnace are measured, and the measurement data is shown in table 1:
TABLE 1 calculation of silicon rod diameter deposition rates at different time points of the furnace
Figure GDA0003150632920000101
Fitting the data of table 1, as shown in fig. 3, it can be seen that the calculated furnace diameter deposition rate is linear with time: the deposition rate decreases continuously with the passage of time, because the surface temperature of the silicon rod gradually decreases as the deposition radius of the silicon rod increases. Through data tracking and linear fitting of a plurality of calculating furnaces, the slope of a fitting straight line is different under the condition that the silicon rod current is constant during feeding, but the intercept (initial diameter deposition rate) is 1.5, because the silicon rod deposition is less influenced by other factors during initial deposition, the deposition rate is only related to the silicon rod current during feeding, and therefore, the initial diameter deposition rate is a constant value under the condition that the silicon rod current is constant during feeding. In the present example, the initial diameter deposition rate was 1.5, and further, the initial radius deposition rate was 1.5/2=0.75. Therefore, in this example, the deposition rate y per hour of the polycrystalline silicon rod is
y=at+0.75
The determined downward sliding time of the quality of the refined trichlorosilane can assist workers in judging the reason for the downward sliding of the quality of the refined trichlorosilane, for example, the determined downward sliding time of the quality of the refined trichlorosilane is just the time for lifting the load of a rectifying tower, the workers can determine that the current rectification reaches the maximum production load, and the continuous lifting amount can cause the fluctuation of the quality of polycrystalline silicon, so that the corresponding recovery measure is to reduce the load of the rectifying tower; if the determined mass slip time of the refined trichlorosilane is the time for adding DCS, the staff does not add DCS any more; if the determined mass gliding time of the refined trichlorosilane is the switching time of a certain heat exchange device, the worker considers that the device is likely to leak, needs to switch back the device again, and carries out disassembly and inspection on the device.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. The method for judging the mass gliding time of the refined trichlorosilane is characterized by comprising the following steps of:
step (1), selecting a calculating furnace, a first reference furnace and a second reference furnace according to a polycrystalline silicon production monitoring machine account;
step (2), respectively calculating the impurity concentrations of the polycrystalline silicon rods of the calculating furnace, the first reference furnace and the second reference furnace;
step (3) determining a drawing scale, drawing a silicon material sampling drawing of the calculating furnace according to the ratio of the diameter of the polycrystalline silicon rod to the sampling drill bit, and marking the deposition radius h of the silicon rod in the drawing Terminal And a sampling location;
step (4), calculating the mass ratio of the normal silicon material to the gliding silicon material in the mass of the sampling part in the silicon material sampling graph;
determining a mass glide time line by using the impurity concentrations of the polycrystalline silicon rods of the calculating furnace, the first reference furnace and the second reference furnace and the mass ratio of the normal-quality silicon material to the mass glide silicon material of the sampling part, and marking the mass glide time line in the silicon material sampling diagram;
step (6) calculating the deposition radius h corresponding to the mass gliding time line Lower part
Step (7) utilizing the deposition radius h corresponding to the mass gliding time line Lower part And calculating the deposition time t corresponding to the mass gliding time line according to the data recorded by the polysilicon production monitoring ledger Lower part ,t Lower part Namely the mass gliding time of the refined trichlorosilane.
2. The method for judging the mass downslide time of refined trichlorosilane according to claim 1, wherein in the step (1), the deposition radius h of the silicon rod corresponding to all the reduction furnaces is recorded in the monitoring ledger of polysilicon production Final (a Chinese character of 'gan') Deposition time t Final (a Chinese character of 'gan') The feeding condition and the resistivity of the polycrystalline silicon rod produced by each reduction furnace.
3. The method for judging the mass downslide time of refined trichlorosilane according to claim 2, wherein the selection method of the calculation furnace, the first reference furnace and the second reference furnace is as follows:
selecting a reduction furnace without the downward sliding of the resistivity of the polycrystalline silicon rod as a first reference furnace according to the resistivity of the polycrystalline silicon rod recorded in the polycrystalline silicon production monitoring ledger;
selecting a reduction furnace with the lowest resistivity and stability of the polycrystalline silicon rod from the reduction furnaces with the same feeding condition as the reference furnace I as a reference furnace II;
and selecting a reducing furnace with the resistivity of the polycrystalline silicon rod between the resistivity of the polycrystalline silicon rods corresponding to the first reference furnace and the second reference furnace from the reducing furnaces with the same feeding condition as the first reference furnace as a calculating furnace.
4. The method for judging the mass downslide time of refined trichlorosilane according to claim 1, wherein in the step (2), the impurity concentrations of the polycrystalline silicon rods of the calculation furnace, the first reference furnace and the second reference furnace are calculated by the following method:
respectively calculating the average impurity concentration a of the polycrystalline silicon rods of the calculation furnace according to the respective polycrystalline silicon rod resistivities of the calculation furnace, the first reference furnace and the second reference furnace recorded in the polycrystalline silicon production monitoring ledger 1 Impurity concentration a of polycrystalline silicon rod of reference furnace one 2 And the impurity concentration a of the polycrystalline silicon rod in the second reference furnace 3
5. The method for judging the mass gliding time of the refined trichlorosilane, as set forth in claim 4, wherein the specific method for calculating the mass ratio of the normal silicon material to the gliding silicon material in mass at the sampling part in the silicon material sampling graph in the step (4) is as follows:
assuming that the mass of the silicon material sliding down from the sampling part mass in the step (3) is X and the mass of the silicon material with the normal sampling part mass is 1, establishing an equation according to the total mass of impurities of the polycrystalline silicon rod: x a 3 +1*a 2 =(1+X)*a 1 And obtaining X, namely the mass ratio of the mass normal silicon material to the mass sliding silicon material of the sampling part is 1.
6. The method for judging the mass downslide time of refined trichlorosilane according to claim 5, wherein in the step (5), the specific method for determining the mass downslide time line is as follows:
according to the mass ratio 1X of the normal-mass silicon material to the gliding-mass silicon material of the sampling part determined in the step (4), obtaining that the area ratio of the normal-mass silicon material to the gliding-mass silicon material of the sampling part is 1X according to the principle that the mass ratio = the volume ratio = the area ratio under the equal altitude condition for the same material, and further determining a mass gliding time line.
7. The method for judging quality downslide time of refined trichlorosilane according to claim 1, wherein in the step (6), a deposition radius h corresponding to a quality downslide time line is calculated Lower part The specific method comprises the following steps: measuring and calculating the distance between the rod core edge and the mass glide time line in the furnace silicon material sampling graph, and calculating the deposition radius h corresponding to the mass glide time line according to the drawing scale of the furnace silicon material sampling graph Lower part
8. The method for judging the mass downslide time of refined trichlorosilane according to claim 1, wherein in the step (7), the deposition time t corresponding to the mass downslide time line is calculated Lower part The method comprises the following specific steps:
fitting is carried out through data of the silicon rod diameter deposition rates corresponding to different time points of the calculated furnace, and the function relation of the radius deposition rate y of the polycrystalline silicon rod per hour and the deposition time t is obtained as follows:
y=at+b (1)
wherein t is the deposition time of the reduction furnace calculated from the beginning of the feeding, a is a correction coefficient for the deposition rate due to temperature change, a is a negative number, and b is the initial deposition rate calculated from the beginning of the feeding; under the condition of a certain feeding current, b is a fixed value and can be obtained by measurement;
the total deposition radius of the i-th polycrystalline silicon rod is
Figure FDA0003150632910000041
Calculating the deposition radius h of the silicon rod of the furnace Final (a Chinese character of 'gan') Deposition time t Terminal Substituting in formula (2) to obtain a;
substituting a into the formula (2), and corresponding to the quality slide-down time line determined in the step (5)Radius of deposition h Lower part In the formula (2), the deposition time t corresponding to the mass gliding time line can be calculated Lower part
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