CN109448800A - Judge the method for refined trichlorosilane quality downslide time - Google Patents
Judge the method for refined trichlorosilane quality downslide time Download PDFInfo
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- CN109448800A CN109448800A CN201811584999.3A CN201811584999A CN109448800A CN 109448800 A CN109448800 A CN 109448800A CN 201811584999 A CN201811584999 A CN 201811584999A CN 109448800 A CN109448800 A CN 109448800A
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- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000005052 trichlorosilane Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 35
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims abstract description 88
- 229920005591 polysilicon Polymers 0.000 claims abstract description 40
- 239000002210 silicon-based material Substances 0.000 claims description 61
- 230000008021 deposition Effects 0.000 claims description 45
- 238000005070 sampling Methods 0.000 claims description 43
- 230000009467 reduction Effects 0.000 claims description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000012535 impurity Substances 0.000 claims description 24
- 229910052710 silicon Inorganic materials 0.000 claims description 24
- 239000010703 silicon Substances 0.000 claims description 24
- 238000004519 manufacturing process Methods 0.000 claims description 23
- 238000004062 sedimentation Methods 0.000 claims description 20
- 238000012544 monitoring process Methods 0.000 claims description 9
- 238000004364 calculation method Methods 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 4
- 210000001161 mammalian embryo Anatomy 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 238000010187 selection method Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000006467 substitution reaction Methods 0.000 claims description 3
- 229910021419 crystalline silicon Inorganic materials 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 4
- 230000033228 biological regulation Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 description 34
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 238000012937 correction Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910052705 radium Inorganic materials 0.000 description 1
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
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Abstract
The invention discloses the methods of judgement refined trichlorosilane quality downslide time a kind of, it can accurately and rapidly determine the time that refined trichlorosilane quality glides, the reason of causing refined trichlorosilane quality to glide for judgement, provides reliable reference, have the advantages that judge that at low cost, computational accuracy is high, it is proven, significant effect, promotional value with higher.The reason of causing refined trichlorosilane quality to glide can be rapidly found out by the method for the invention, and then corresponding regulation measure is taken for the reason, with the quality of fast quick-recovery polysilicon, will because refined trichlorosilane quality glide cause polysilicon quality problems due to bring economic loss minimizes.
Description
Technical field:
The present invention relates to field of polysilicon production, more particularly to the side of judgement refined trichlorosilane quality downslide time a kind of
Method.
Background technique:
Polysilicon is the basic material of electronics industry and solar energy industry, is widely used in semiconductor chip, high-performance
Sensor, optical fiber, solar panel etc..Currently, production of polysilicon technology both domestic and external mostly uses improved Siemens, i.e., it is logical
Cross under the conditions of high temperature by after rectifying trichlorosilane (hereinafter referred to as refined trichlorosilane) and hydrogen be powered in reduction furnace, high temperature silicon
Stick surface occurs chemical vapour deposition reaction and then obtains high purity polycrystalline silicon, as defined in silicon rod diameter gradually rises in furnace
Stick diameter.Since polysilicon is a kind of high purity product, for the quality for ensuring polysilicon product, to the raw material essence trichlorine of production polysilicon
The purity requirement of hydrogen silicon is very high.
In polysilicon production process, although per tour can all be sampled detection to refined trichlorosilane impurity content,
The limitation of the examined frequency, the impurity content for refined trichlorosilane often occur, which is lower than, detects line, and the polycrystalline that final production obtains
The case where siliceous amount but obviously glides；Even if polysilicon quality offset sharper slowdowns, the sampling inspection results of refined trichlorosilane also judge
Refined trichlorosilane quality is glided out, but is limited by the sampling frequency, is still difficult to quickly determine under refined trichlorosilane quality
Sliding correct time cannot rapidly find out the reason of causing refined trichlorosilane quality to glide, seriously affect normal production, give enterprise
Cause serious economic loss.But it can fast and accurately check refined trichlorosilane quality there is no one kind at present to glide the time
The method of point.
Summary of the invention:
In order to find out the reason of causing refined trichlorosilane quality to glide as early as possible, and then corresponding regulation is taken for the reason
Measure will cause polysilicon quality problems due to bring because refined trichlorosilane quality glides with the quality of fast quick-recovery polysilicon
Economic loss minimizes, the time point that the present invention is glided by first determining polysilicon quality, then according under polysilicon quality
Sliding time point determines the time point that refined trichlorosilane quality glides, then arranges near the time point that refined trichlorosilane quality glides
The reason of causing refined trichlorosilane quality to glide is looked into, inexpensive, quick, accurate can lock and refined trichlorosilane quality is caused to glide
The reason of.
Polysilicon production process process specifically includes that trichlorosilane synthesis, (some uses chlorine hydrogen for the heat hydrogenation of silicon tetrachloride
Change), rectifying trichlorosilane and reducing polysilicon, since entire production technology is carried out continuously, the rectifying trichlorine produced
Directly continuously supply reduction furnace uses hydrogen silicon, it is possible to which the time point that polysilicon quality starts to glide is determined as smart trichlorine hydrogen
Siliceous amount starts the time point glided.
That the purpose of the present invention is to provide a kind of computational accuracies is high, at low cost, can fast and accurately judge smart trichlorine hydrogen
The method of siliceous amount downslide time.
The present invention is implemented by following technical solution:
Judge the method for refined trichlorosilane quality downslide time comprising following steps:
Step (1) monitors account according to production of polysilicon, and selection calculates furnace, benchmark furnace one and benchmark furnace two；
Step (2) calculates separately the polycrystalline silicon rod impurity concentration for calculating furnace, benchmark furnace one and benchmark furnace two；
Step (3) determines drafting scale, and according to the ratio of polycrystalline silicon rod diameter and chisel bit, draw calculation furnace
Silicon material sampling figure, and silicon rod deposition radius h is marked in figureEventuallyThe sample position and；
Step (4) calculates the quality normal silicon material of sampling part and the mass ratio of quality downslide silicon material in silicon material sampling figure；
Step (5) utilizes the polysilicon impurity concentration of the calculating furnace, benchmark furnace one and benchmark furnace two, and sampling
The mass ratio of partial quality normal silicon material and quality downslide silicon material determines quality downslide timeline, and samples in the silicon material
Quality downslide timeline is marked out in figure；
Step (6) calculates the corresponding deposition radius h of quality downslide timelineUnder；
Step (7) utilizes the corresponding deposition radius h of quality downslide timelineUnderAnd the production of polysilicon monitoring account note
The data of record calculate the corresponding sedimentation time t of quality downslide timelineUnder, tUnderThe as time of refined trichlorosilane quality downslide.
Further, in the step (1), record has all reduction furnaces corresponding in the production of polysilicon monitoring account
Silicon rod deposits radius hEventually, sedimentation time tEventually, charging situation and the polycrystalline silicon rod resistivity produced of each reduction furnace.
Further, the selection method for calculating furnace, benchmark furnace one and benchmark furnace two specifically:
According to the polycrystalline silicon rod resistivity recorded in production of polysilicon monitoring account, a polycrystalline silicon rod resistance is selected
There is no the reduction furnaces of downslide as benchmark furnace one for rate；
From reduction furnace identical with the benchmark furnace one charging situation, selects a polycrystalline silicon rod resistivity minimum and reach
To stable reduction furnace as benchmark furnace two；
From reduction furnace identical with the benchmark furnace one charging situation, select a polycrystalline silicon rod resistivity between described
Reduction furnace between the polycrystalline silicon rod resistivity corresponding with the benchmark furnace two of benchmark furnace one is as calculating furnace.
Further, in the step (2), the polycrystalline silicon rod impurity for calculating furnace, benchmark furnace one and benchmark furnace two
Concentration is calculated by the following method:
It is respective more that calculating furnace, benchmark furnace one and the benchmark furnace two recorded in account is monitored according to the production of polysilicon
Crystalline silicon rod resistivity calculates separately the mean impurity concentration a for calculating the polycrystalline silicon rod of furnace1, benchmark furnace one polycrystalline silicon rod it is miscellaneous
Matter concentration a2And the impurity concentration a of the polycrystalline silicon rod of benchmark furnace two3。
Further, it in the step (4), calculates in silicon material sampling figure under the quality normal silicon material and quality of sampling part
The mass ratio of sliding silicon material method particularly includes:
Assuming that the quality of sampling part quality downslide silicon material is X, the quality of sampling part quality normal silicon material in step (3)
It is 1, then equation is established according to the impurity gross mass of polycrystalline silicon rod: X*a3+1*a2=(1+X) * a1, X, i.e. sampling portion can be found out
The mass ratio of the quality normal silicon material and quality downslide silicon material divided is 1:X.
Further, in the step (5), quality downslide timeline is determined method particularly includes:
According to the mass ratio 1:X of the quality normal silicon material of the sampling part determined in step (4) and quality downslide silicon material, press
According to for same substance, in the case where contour, mass ratio=volume ratio=area ratio principle obtains the quality of sampling part
The area ratio of normal silicon material and quality downslide silicon material is 1:X, and then determines quality downslide timeline.
Further, in the step (6), the corresponding deposition radius h of quality downslide timeline is calculatedUnderSpecific method
Are as follows: survey calculation furnace silicon material samples figure medium rod core edge at a distance from quality downslide timeline, schemes according to the sampling of furnace silicon material is calculated
Drafting scale, calculate the corresponding deposition radius h of quality downslide timelineUnder。
Further, in the step (7), the corresponding sedimentation time t of quality downslide timeline is calculatedUnderSpecific steps
Are as follows:
Data by detecting the obtained corresponding silicon rod diameter deposition rate of calculating furnace different time points are fitted, and are obtained
To the functional relation of polycrystalline silicon rod radius deposition rate y and sedimentation time t hourly are as follows:
Y=at+b (1)
Wherein, t is the reduction furnace sedimentation time calculated since charging, and a is since temperature change is for deposition rate
Correction factor, a are negative, and b is the embryo deposit rate calculated since charging；In the case where charging electric current is certain, b is fixed
Value can be obtained by measurement；
Then total deposition radius of i-th hour polycrystalline silicon rod is
The silicon rod for calculating furnace is deposited into radius hEventually, sedimentation time tEventuallyIn substitution formula (2), a can be found out；
The corresponding deposition radius h of quality downslide timeline that a is substituted into formula (2), and will be determined in step (5)UnderIt brings into
In formula (2), the corresponding sedimentation time t of mass downslide timeline can be calculatedUnder。
Advantages of the present invention:
The present invention can accurately and rapidly determine the time that refined trichlorosilane quality glides, and lead to refined trichlorosilane for judgement
The reason of quality glides provides reliable reference, has the advantages that judge that at low cost, computational accuracy is high, it has been proved by practice that effect is aobvious
It writes, promotional value with higher.
The reason of causing refined trichlorosilane quality to glide can be rapidly found out by the method for the invention, and then is directed to the reason
Corresponding regulation measure is taken, with the quality of fast quick-recovery polysilicon, polycrystalline is siliceous caused by gliding because of refined trichlorosilane quality
Amount problem and bring economic loss minimizes.
Detailed description of the invention:
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the polycrystalline silicon rod resistivity data that furnace, benchmark furnace one and benchmark furnace two are calculated in the present embodiment；
Fig. 2 is that furnace silicon material sampling figure is calculated in the present embodiment；
Fig. 3 is the fitting a straight line that furnace diameter deposition rate is calculated in the present embodiment.
Specific embodiment:
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1:
Judge the method for refined trichlorosilane quality downslide time comprising following steps:
Step (1) monitors account according to production of polysilicon, and selection calculates furnace, benchmark furnace one and benchmark furnace two；
Step (2) calculates separately the polycrystalline silicon rod impurity concentration for calculating furnace, benchmark furnace one and benchmark furnace two；
Step (3) determines drafting scale, and according to the ratio of polycrystalline silicon rod diameter and chisel bit, according to the reality of sampling
Border situation samples figure using the silicon material of CAD draw calculation furnace, and silicon rod deposition radius h is marked in figureEventuallyAnd sample position, such as
Shown in Fig. 2；
Step (4) calculates the quality normal silicon material of sampling part and the mass ratio of quality downslide silicon material in silicon material sampling figure；
Step (5) utilizes the polysilicon impurity concentration and sampling part for calculating furnace, benchmark furnace one and benchmark furnace two
Quality normal silicon material and quality downslide silicon material mass ratio, determine quality downslide timeline, and mark in silicon material sampling figure
Mass downslide timeline；
Step (6) calculates the corresponding deposition radius h of quality downslide timelineUnder；
Step (7) utilizes the corresponding deposition radius h of quality downslide timelineUnderAnd production of polysilicon monitoring account record
Data calculate the corresponding sedimentation time t of quality downslide timelineUnder, tUnderThe as time of refined trichlorosilane quality downslide.
In step (1), record has the corresponding silicon rod deposition radius h of all reduction furnaces in production of polysilicon monitoring accountEventually, it is heavy
Product time tEventually, charging situation and the polycrystalline silicon rod resistivity produced of each reduction furnace.
The selection method for calculating furnace, benchmark furnace one and benchmark furnace two specifically:
According to the polycrystalline silicon rod resistivity recorded in production of polysilicon monitoring account, a polycrystalline silicon rod resistivity is selected not have
There is the reduction furnace to glide as benchmark furnace one；
From reduction furnace identical with the charging of benchmark furnace one situation, selects a polycrystalline silicon rod resistivity minimum and reach steady
Fixed reduction furnace is as benchmark furnace two；
From reduction furnace identical with the charging of benchmark furnace one situation, select a polycrystalline silicon rod resistivity between benchmark furnace one
Reduction furnace between polycrystalline silicon rod resistivity corresponding with benchmark furnace two is as furnace is calculated, as shown in Figure 1.Due in reduction furnace
Resistivity can intuitively react the quality of polycrystalline silicon rod, therefore, in the present embodiment, resistivity decline is used as and judges polysilicon
The foundation that quality glides.
In step (2), the polycrystalline silicon rod impurity concentration for calculating furnace, benchmark furnace one and benchmark furnace two is counted by the following method
It obtains:
Calculating furnace, benchmark furnace one and the respective polysilicon of benchmark furnace two recorded in account is monitored according to production of polysilicon
Stick resistivity calculates separately the mean impurity concentration a for calculating the polycrystalline silicon rod of furnace according to national standard GB/T 13389-20141, base
The impurity concentration a of the polycrystalline silicon rod of quasi- furnace one2And the impurity concentration a of the polycrystalline silicon rod of benchmark furnace two3.In the present embodiment, prison
The resistivity recorded in control account is to pass through method as defined in national standard GB/T4059-2007 using zone melting furnace and resistance meter
It is molten to carry out area, is determined later using the method that national standard GB/T1551-2009 is required.
In step (4), the quality normal silicon material of sampling part and the quality of quality downslide silicon material in silicon material sampling figure are calculated
Ratio method particularly includes:
Assuming that the quality of sampling part quality downslide silicon material is X, the quality of sampling part quality normal silicon material in step (3)
It is 1, due to gross mass × impurity concentration=impurity gross mass, then equation is established according to the impurity gross mass of polycrystalline silicon rod: X*
a3+1*a2=(1+X) * a1, X can be found out, i.e. the mass ratio of the quality normal silicon material of sampling part and quality downslide silicon material is 1:
X。
In step (5), quality downslide timeline is determined method particularly includes:
According to the mass ratio 1:X of the quality normal silicon material of the sampling part determined in step (4) and quality downslide silicon material, press
According to for same substance, in the case where contour, mass ratio=volume ratio=area ratio principle obtains the quality of sampling part
The area ratio of normal silicon material and quality downslide silicon material is 1:X, try and error method is used, so that in the quality downslide timeline of sampling part
Part and the area ratio outside quality downslide timeline be 1:X, and then determine quality downslide timeline.
In step (6), the corresponding deposition radius h of quality downslide timeline is calculatedUnderMethod particularly includes: survey calculation furnace silicon
Material sampling figure medium rod core edge is at a distance from quality downslide timeline, according to the drafting scale for calculating furnace silicon material sampling figure, meter
Calculate the corresponding deposition radius h of quality downslide timelineUnder。
In step (7), the corresponding sedimentation time t of quality downslide timeline is calculatedUnderSpecific steps are as follows:
Data by detecting the obtained corresponding silicon rod diameter deposition rate of calculating furnace different time points are fitted, and are obtained
To the functional relation of polycrystalline silicon rod radius deposition rate y and sedimentation time t hourly are as follows:
Y=at+b (1)
Wherein, t is the reduction furnace sedimentation time calculated since charging, and a is since temperature change is for deposition rate
Correction factor, a are negative, and b is the embryo deposit rate calculated since charging；In the case where charging electric current is certain, b is fixed
Value can be obtained by measurement；
Then total deposition radius of i-th hour polycrystalline silicon rod is
The silicon rod for calculating furnace is deposited into radius hEventually, sedimentation time tEventuallyIn substitution formula (2), a can be found out；
The corresponding deposition radius h of quality downslide timeline that a is substituted into formula (2), and will be determined in step (5)UnderIt brings into
In formula (2), the corresponding sedimentation time t of mass downslide timeline can be calculatedUnder。
In the present embodiment, by being measured to the corresponding silicon rod diameter deposition rate of calculating furnace different time points, measure
Data are as shown in table 1:
Table 1 calculates the corresponding silicon rod diameter deposition rate of furnace different time points
The data of table 1 are fitted, fig. 3, it is shown that the diameter deposition rate for calculating furnace and time are in line
Sexual intercourse: over time, deposition velocity constantly declines, this is because with the increase of silicon rod deposition radius, silicon rod table
Face temperature gradually declines.By the data tracking to more calculating furnaces and linear fit is carried out, discovery silicon rod electric current in charging
In the case where certain, fitting a straight line slope is different, but intercept (initial diameter deposition rate) is 1.5, this is because initial heavy
Product when, silicon rod deposition be affected by other factors it is smaller, deposition rate only with charging when silicon rod it is current related, therefore, charging when silicon
In the case that stick electric current is certain, initial diameter deposition rate is definite value.Initial diameter deposition rate is 1.5 in the present embodiment, into
One step, initial radium deposition rate is 1.5/2=0.75.Therefore polycrystalline silicon rod radius deposition rate hourly in the present embodiment
Y is
Y=at+0.75
Determining refined trichlorosilane quality downslide time energy ancillary staff judgement leads to smart trichlorine through this embodiment
The reason of siliceous amount of hydrogen glides, for example, the refined trichlorosilane quality determined glides, the time is exactly the time that rectifying column mentions load,
Staff is assured that current rectifying has reached the maximum produce load, and continuing the amount of proposing will cause polysilicon quality fluctuation,
So, corresponding recovery measure is exactly to reduce rectifying column load；If it is determined that refined trichlorosilane quality glide the time be addition
The time of DCS, then staff will no longer add DCS；If it is determined that refined trichlorosilane quality glide the time be some heat exchange
The switching time of equipment needs switchback equipment again then staff will consider this equipment there may be leakage, and to setting
It is standby to open and inspect etc..
The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. judge refined trichlorosilane quality glide the time method, which is characterized in that itself the following steps are included:
Step (1) monitors account according to production of polysilicon, and selection calculates furnace, benchmark furnace one and benchmark furnace two；
Step (2) calculates separately the polycrystalline silicon rod impurity concentration for calculating furnace, benchmark furnace one and benchmark furnace two；
Step (3) determines drafting scale, and according to the ratio of polycrystalline silicon rod diameter and chisel bit, the silicon material of draw calculation furnace
Sampling figure, and silicon rod deposition radius h is marked in figureEventuallyThe sample position and；
Step (4) calculates the quality normal silicon material of sampling part and the mass ratio of quality downslide silicon material in silicon material sampling figure；
Step (5) utilizes the polysilicon impurity concentration and sampling part of the calculating furnace, benchmark furnace one and benchmark furnace two
Quality normal silicon material and quality downslide silicon material mass ratio, determine quality downslide timeline, and in silicon material sampling figure
Mark mass downslide timeline；
Step (6) calculates the corresponding deposition radius h of quality downslide timelineUnder；
Step (7) utilizes the corresponding deposition radius h of quality downslide timelineUnderAnd the production of polysilicon monitoring account record
Data calculate the corresponding sedimentation time t of quality downslide timelineUnder, tUnderThe as time of refined trichlorosilane quality downslide.
2. judging the method for refined trichlorosilane quality downslide time according to claim 1, which is characterized in that the step
(1) in, record has the corresponding silicon rod deposition radius h of all reduction furnaces in the production of polysilicon monitoring accountEventually, sedimentation time
tEventually, charging situation and the polycrystalline silicon rod resistivity produced of each reduction furnace.
3. judging the method for refined trichlorosilane quality downslide time according to claim 2, which is characterized in that the calculating
The selection method of furnace, benchmark furnace one and benchmark furnace two specifically:
According to the polycrystalline silicon rod resistivity recorded in production of polysilicon monitoring account, a polycrystalline silicon rod resistivity is selected not have
There is the reduction furnace to glide as benchmark furnace one；
From reduction furnace identical with the benchmark furnace one charging situation, selects a polycrystalline silicon rod resistivity minimum and reach steady
Fixed reduction furnace is as benchmark furnace two；
From reduction furnace identical with the benchmark furnace one charging situation, select a polycrystalline silicon rod resistivity between the benchmark
Reduction furnace between the polycrystalline silicon rod resistivity corresponding with the benchmark furnace two of furnace one is as calculating furnace.
4. judging the method for refined trichlorosilane quality downslide time according to claim 1, which is characterized in that the step
(2) in, the polycrystalline silicon rod impurity concentration for calculating furnace, benchmark furnace one and benchmark furnace two is calculated by the following method:
Calculating furnace, benchmark furnace one and the respective polysilicon of benchmark furnace two recorded in account is monitored according to the production of polysilicon
Stick resistivity calculates separately the mean impurity concentration a for calculating the polycrystalline silicon rod of furnace1, benchmark furnace one polycrystalline silicon rod impurity it is dense
Spend a2And the impurity concentration a of the polycrystalline silicon rod of benchmark furnace two3。
5. judging the method for refined trichlorosilane quality downslide time according to claim 1, which is characterized in that the step
(4) in, the specific method of the mass ratio of the quality normal silicon material and quality downslide silicon material of sampling part in silicon material sampling figure is calculated
Are as follows:
Assuming that the quality of sampling part quality downslide silicon material is X in step (3), the quality of sampling part quality normal silicon material is 1,
Equation is then established according to the impurity gross mass of polycrystalline silicon rod: X*a3+1*a2=(1+X) * a1, X can be found out, i.e. sampling part
The mass ratio of quality normal silicon material and quality downslide silicon material is 1:X.
6. judging the method for refined trichlorosilane quality downslide time according to claim 5, which is characterized in that the step
(5) in, quality downslide timeline is determined method particularly includes:
According to the mass ratio 1:X of the quality normal silicon material of the sampling part determined in step (4) and quality downslide silicon material, according to right
In same substance, in the case where contour, mass ratio=volume ratio=area ratio principle, the quality for obtaining sampling part is normal
The area ratio of silicon material and quality downslide silicon material is 1:X, and then determines quality downslide timeline.
7. judging the method for refined trichlorosilane quality downslide time according to claim 1, which is characterized in that the step
(6) in, the corresponding deposition radius h of quality downslide timeline is calculatedUnderMethod particularly includes: survey calculation furnace silicon material samples figure medium rod
Core edge is at a distance from quality downslide timeline, according to the drafting scale for calculating furnace silicon material sampling figure, when calculating quality downslide
Between the corresponding deposition radius h of lineUnder。
8. judging the method for refined trichlorosilane quality downslide time according to claim 1, which is characterized in that the step
(7) in, the corresponding sedimentation time t of quality downslide timeline is calculatedUnderSpecific steps are as follows:
Data by detecting the obtained corresponding silicon rod diameter deposition rate of calculating furnace different time points are fitted, and are obtained more
The functional relation of crystalline silicon rod radius deposition rate y and sedimentation time t hourly are as follows:
Y=at+b (1)
Wherein, t is the reduction furnace sedimentation time calculated since charging, and a is the amendment due to temperature change for deposition rate
Coefficient, a are negative, and b is the embryo deposit rate calculated since charging；In the case where charging electric current is certain, b is definite value,
It can be obtained by measurement；
Then total deposition radius of i-th hour polycrystalline silicon rod is
The silicon rod for calculating furnace is deposited into radius hEventually, sedimentation time tEventuallyIn substitution formula (2), a can be found out；
The corresponding deposition radius h of quality downslide timeline that a is substituted into formula (2), and will be determined in step (5)UnderBring formula (2) into
In, the corresponding sedimentation time t of mass downslide timeline can be calculatedUnder。
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|---|---|---|---|---|
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