CN113564691A - Heavily arsenic-doped silicon single crystal ending method and device - Google Patents

Heavily arsenic-doped silicon single crystal ending method and device Download PDF

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Publication number
CN113564691A
CN113564691A CN202110794760.4A CN202110794760A CN113564691A CN 113564691 A CN113564691 A CN 113564691A CN 202110794760 A CN202110794760 A CN 202110794760A CN 113564691 A CN113564691 A CN 113564691A
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ending
single crystal
temperature
silicon single
doped silicon
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闫龙
张兴茂
周文辉
李小红
伊冉
王忠保
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Ningxia Zhongxin Wafer Semiconductor Technology Co Ltd
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Ningxia Zhongxin Wafer Semiconductor Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
    • C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20—Controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention provides a method and a device for ending a heavily arsenic-doped silicon single crystal, belonging to the technical field of production of heavily arsenic-doped silicon single crystals. According to the crucible heel ratio after the isodiametric finishing, firstly, a theoretical pulling speed up-regulation proportion X is calculated, and the single crystal pulling speed during ending is regulated according to the theoretical pulling speed up-regulation proportion to carry out ending process. In the ending process, the pulling speed up-regulation proportion X is calculated according to the ending length, and the single crystal pulling speed is gradually increased until ending. Practice shows that the heavily arsenic-doped silicon single crystal ending method provided by the invention can effectively replace manual subjective adjustment, reduce labor intensity and relieve subjective dependence of a terminating process of the heavily arsenic-doped silicon single crystal on technical personnel. Meanwhile, the method for ending the heavily arsenic-doped silicon single crystal can effectively reduce the NG rate of the tail of the heavily arsenic-doped silicon single crystal rod, improve the yield of the heavily arsenic-doped silicon single crystal rod, reduce the NG rate of ending from 45 percent regulated by traditional technicians to 15 percent, reduce the loss of silicon raw materials and reduce the production cost.

Description

Heavily arsenic-doped silicon single crystal ending method and device
Technical Field
The invention belongs to the technical field of production of heavily doped silicon single crystals, and particularly relates to a method and a device for ending a heavily doped arsenic silicon single crystal.
Background
Among heavily doped single crystal polished wafers, heavily doped arsenic silicon single crystal is the most ideal epitaxial substrate material, and the market demand is increasing.
In the process of producing the heavily arsenic-doped silicon single crystal by the Czochralski method, a gas phase doping method is usually adopted, and the specific processes comprise material melting, doping, seeding, shouldering, equal-diameter growth, ending and the like. However, in the actual production and development process, the tail section resistivity of the crystal is sharply reduced due to the low segregation coefficient of arsenic doped with the impurity, and the corresponding impurity concentration in the crystal is rapidly increased. The rapid rise of the impurity concentration causes the lattice distortion in the crystal to be greatly increased, and the tail section of the crystal is subjected to crystal transformation, so that the loss of the qualified rate of the crystal is serious.
Practice shows that the condition that the NG rate of the tail part is high due to crystal change of the tail part of the heavily arsenic-doped silicon single crystal is favorably improved by adjusting the pulling speed and the temperature in the ending process. However, in the prior art, the adjustment of the pulling rate and the temperature in the ending process mostly depends on the experience of technicians, the subjective randomness is large, and the probability of the tail part of the heavily arsenic-doped silicon single crystal generating crystal transformation can not be effectively controlled.
Disclosure of Invention
In view of the above, the present invention provides a method and an apparatus for ending a heavily arsenic-doped silicon single crystal, so as to solve the technical problems in the prior art that the tail of the heavily arsenic-doped silicon single crystal is easy to be subjected to crystal transformation, so that the NG rate of the tail is high, and the yield of the ingot is low.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for ending heavily arsenic-doped silicon single crystal comprises the following steps:
a. obtaining a crucible heel ratio R after the isodiametric finishing;
b. calculating a theoretical pull rate up-regulation ratio X, wherein X is 1/(1+ R);
c. obtaining an adjusting distance delta L, wherein the adjusting distance delta L is set according to production requirements;
d. adjusting the ratio X up according to the theoretical pulling speed, setting the pulling speed of the monocrystalline silicon when the monocrystalline silicon enters the ending process, and entering the monocrystalline ending process;
e. acquiring the current ending length L;
f. obtaining the last adjustment occurring ending length LnAnd the adjusted pull rate up-regulation ratio Xn(ii) a Wherein, the ending length L at the beginning of endingnWhen the pulling speed is adjusted, the pulling speed is adjusted to be 0, and the pulling speed is adjusted to be X;
g. judgment of L-LnWhether Δ L is greater than or equal to Δ L;
h. if L-LnIf the current pull speed is more than or equal to delta L, calculating the current pull speed up-regulation proportion XnWherein X isn＝X+[L/ΔL-1)]A,0<A≤10％；
i. Updating Ln；
And e, repeating the steps e to i until the ending is finished.
Preferably, in step c, the adjustment pitch Δ L is set to 10mm to 30 mm.
Preferably, the method for ending the heavily arsenic-doped silicon single crystal further comprises the following steps:
j. obtaining the ending temperature T at the beginning of ending0A; wherein, 0<a≤0.8℃；
k. Adjusting the tail-out temperature T when the pull rate is adjusted for the first time1A + b; wherein b is more than or equal to 0.5 ℃ and less than or equal to 1.0 ℃;
m. if L-LnIf the temperature is more than or equal to delta L, calculating the current ending temperature TnWherein, Tn＝Tn-1+Tn-2；Tn-1The ending temperature after the last adjustment; t isn-2The final temperature after the last secondary adjustment is obtained;
and n, repeating the step m until the ending.
Preferably, the method for ending the heavily arsenic-doped silicon single crystal further comprises the following steps:
j. obtaining the ending temperature T at the beginning of ending0A; wherein, 0<a≤0.8℃；
If L-LnIf the temperature is more than or equal to delta L, calculating the current ending temperature TnWherein, Tn＝λ1L3+λ2L2+λ3L + a, wherein, λ1、λ2、λ3Is a constant.
Preferably, in step p, λ is obtained by the following steps1、λ2、λ3：
p1., ending according to preset temperature parameters to obtain a successfully ended heavily arsenic-doped silicon single crystal rod;
p2. measuring the ending length of the tail of the monocrystalline ingot heavily doped with arsenic and obtaining the ending temperature corresponding to the mutation;
p3., adjusting the ending temperature of the mutation position, and ending by adopting the adjusted ending temperature;
p4. repeating the steps p2 and p3 until the tail of the heavily arsenic-doped silicon single crystal ingot is smooth;
p5. fitting the adjusted ending temperature and ending length equation to obtain lambda1、λ2、λ3。
A heavily arsenic-doped silicon single crystal ending device is electrically connected with a central controller of a single crystal furnace, and comprises:
the first acquisition module is used for acquiring the crucible heel ratio R after the isodiametric finishing;
a first calculating module, configured to calculate a theoretical pull-up ratio X, where X is 1/(1+ R);
the second acquisition module is used for acquiring an adjustment distance delta L, and the adjustment distance delta L is set according to production requirements;
the pulling speed setting module is used for adjusting the proportion X up according to the theoretical pulling speed, setting the pulling speed of the monocrystalline silicon when the monocrystalline silicon enters the ending process and entering the monocrystalline ending process;
a third obtaining module, configured to obtain a current ending length L;
a fourth obtaining module for obtaining the last adjustment time ending length LnAnd the adjusted pull rate up-regulation ratio Xn(ii) a Wherein, the ending length L at the beginning of endingnWhen the pulling speed is adjusted, the pulling speed is adjusted to be 0, and the pulling speed is adjusted to be X;
a judging module for judging L-LnWhether it is large or notIs equal to or less than Δ L;
a second calculation module if L-LnIf the current pull speed is more than or equal to delta L, calculating the current pull speed up-regulation proportion XnWherein X isn＝X+[L/ΔL-1)]A,0<A≤10％；
Update module, update Ln。
Preferably, the heavily arsenic-doped silicon single crystal ending device further comprises:
a fifth obtaining module, configured to obtain a ending temperature T at the beginning of ending0A; wherein, 0<a≤0.8℃；
A first temperature regulating module for regulating the ending temperature T when the pull rate is regulated for the first time1A + b; wherein b is more than or equal to 0.5 ℃ and less than or equal to 1.0 ℃;
a first ending temperature calculation module for calculating L-LnWhen the temperature is more than or equal to delta L, calculating the current ending temperature TnWherein, Tn＝Tn-1+Tn-2；Tn-1The ending temperature after the last adjustment; t isn-2The final temperature after the last secondary adjustment.
Preferably, the heavily arsenic-doped silicon single crystal ending device further comprises:
a second ending temperature calculation module for calculating L-LnWhen the temperature is more than or equal to delta L, calculating the current ending temperature and calculating the current ending temperature TnWherein, Tn＝λ1L3+λ2L2+λ3L + a, wherein, λ1、λ2、λ3Is a constant.
According to the technical scheme, the invention provides a method and a device for ending heavily arsenic-doped silicon single crystal, which have the beneficial effects that: according to the crucible heel ratio after the isodiametric finishing, firstly, a theoretical pulling speed up-regulation proportion X is calculated, and the single crystal pulling speed during ending is regulated according to the theoretical pulling speed up-regulation proportion to carry out ending process. In the ending process, the pulling speed up-regulation proportion X is calculated according to the ending length, and the single crystal pulling speed is gradually increased until ending. Practice shows that the heavily arsenic-doped silicon single crystal ending method provided by the invention can effectively replace manual subjective adjustment, reduce labor intensity and relieve subjective dependence of a terminating process of the heavily arsenic-doped silicon single crystal on technical personnel. Meanwhile, the method for ending the heavily arsenic-doped silicon single crystal can effectively reduce the NG rate of the tail of the heavily arsenic-doped silicon single crystal rod, improve the yield of the heavily arsenic-doped silicon single crystal rod, reduce the NG rate of ending from 45 percent regulated by traditional technicians to 15 percent, reduce the loss of silicon raw materials and reduce the production cost.
Drawings
FIG. 1 is a block diagram of a process flow of a heavily arsenic-doped silicon single crystal termination apparatus.
FIG. 2 is a schematic view showing the improvement of the shape of the tail of a pre-heavily arsenic-doped silicon single crystal.
FIG. 3 shows an embodiment of an improved tail shape of heavily arsenic-doped silicon single crystal.
FIG. 4 shows a modified tail shape of an arsenic-heavily doped silicon single crystal in yet another embodiment.
Detailed Description
The technical solutions and effects of the embodiments of the present invention will be further described in detail below with reference to the accompanying drawings of the present invention.
Referring to FIG. 1, in one embodiment, a method for ending a heavily arsenic-doped silicon single crystal includes the following steps:
s10, obtaining a crucible heel ratio R after the isodiametric process is finished.
S20, calculating a theoretical pull speed up-regulation ratio X, wherein X is 1/(1+ R).
The crucible-to-crucible ratio R is the ratio of the crucible lifting rate CL (the upward lifting speed of the crucible) to the single crystal pulling rate SL during the single crystal growth process, namely: r ═ CL/SL.
And stopping the crucible speed after the ending process, wherein in order to ensure that the transition from the equal diameter process to the ending process is smooth, the sum of the single crystal pulling speed SL 'when the ending process is carried out and the single crystal pulling speed SL after the equal diameter process and the crucible lifting rate CL is required, namely SL' -SL + CL-X-SL. The theoretical pull rate up-regulation ratio X is calculated as 1/(1+ R).
And S30, obtaining an adjusting interval delta L, wherein the adjusting interval delta L is set according to production requirements.
According to production requirements, setting an adjusting interval delta L, wherein the adjusting interval delta L refers to the distance of every interval delta L, and adjusting the pulling speed and the temperature of the single crystal in the ending process for one time so as to avoid ending failure caused by too frequent adjustment or breakage caused by irregular tail parts due to insufficient adjusting frequency. Preferably, the adjustment pitch Δ L is set to 10mm to 30 mm.
S40, adjusting the ratio X up according to the theoretical pulling speed, setting the pulling speed of the monocrystalline silicon when the monocrystalline silicon is subjected to ending, and performing the working procedure of monocrystalline ending.
S50, obtaining the current ending length L.
S60, acquiring the ending length L when the last adjustment occursnAnd the adjusted pull rate up-regulation ratio Xn(ii) a Wherein, the ending length L at the beginning of endingnThe adjusted pull-up ratio at the beginning of the tail-out is X.
S70, judging L-LnWhether Δ L is greater than or equal to Δ L;
s80. if L-LnIf the current pull speed is more than or equal to delta L, calculating the current pull speed up-regulation proportion XnWherein X isn＝X+[L/ΔL-1)]A,0<A≤10％；
S90, updating Ln；
S100, repeating the steps S50-S90 until the ending.
That is, in the process of single crystal ending, the current ending length L is directly obtained by a single crystal furnace system or obtained by sight glass measurement, the distance delta L is adjusted at intervals according to Xn＝X+[L/ΔL-1)]A,0<A is less than or equal to 10 percent, and the single crystal pulling speed in the current ending process is adjusted once.
It is worth to be noted that the value of a has positive correlation with the adjustment distance Δ L, and the smaller the value of the adjustment distance Δ L is, the smaller the value of a is required; the larger the adjustment distance delta L is, the larger the value A needs to be.
Practice shows that the method for ending the heavily arsenic-doped silicon single crystal realizes automatic control of ending the heavily arsenic-doped silicon single crystal, effectively replaces manual subjective adjustment, reduces labor intensity, and relieves subjective dependence of the ending process of the heavily arsenic-doped silicon single crystal on technical personnel. Meanwhile, the method for ending the heavily arsenic-doped silicon single crystal can effectively reduce the NG rate of the tail of the heavily arsenic-doped silicon single crystal rod, improve the yield of the heavily arsenic-doped silicon single crystal rod, reduce the NG rate of ending from 45 percent regulated by traditional technicians to 15 percent, reduce the loss of silicon raw materials and reduce the production cost.
In order to further reduce the NG rate of the tail of the heavily arsenic-doped silicon single crystal ingot, in an embodiment, the method for ending the heavily arsenic-doped silicon single crystal further includes the following steps:
s110, acquiring ending temperature T at the beginning of ending0A; wherein, 0<a≤0.8℃。
S120, adjusting the ending temperature T when the pulling speed is adjusted for the first time1A + b; wherein b is more than or equal to 0.5 ℃ and less than or equal to 1.0 ℃.
S130. if L-LnIf the temperature is more than or equal to delta L, calculating the current ending temperature TnWherein, Tn＝Tn-1+Tn-2；Tn-1The ending temperature after the last adjustment; t isn-2The final temperature after the last secondary adjustment is obtained;
and S140, repeating the step S130 until the ending is finished.
That is, in the ending process of the monocrystalline ingot heavily doped with arsenic, the ending temperature is adjusted while the pulling speed of the monocrystalline is adjusted. The ending temperature is adjusted according to the following rules: t isn＝Tn-1+Tn-2；Tn-1The ending temperature after the last adjustment; t isn-2The final temperature after the last secondary adjustment. I.e. second adjustment, T2＝T0+T12a + b, at the third adjustment, T3＝T1+T2And 3a +2b, and so on until the end.
Referring to fig. 2 and 3, by adopting the method, the single crystal pulling speed and the ending temperature in the ending process of the heavily arsenic-doped silicon single crystal rod are adjusted simultaneously, so that the automatic control of the ending process of the heavily arsenic-doped silicon single crystal rod is realized, the NG rate of the tail of the heavily arsenic-doped silicon single crystal rod is greatly reduced, the yield of the heavily arsenic-doped silicon single crystal rod is improved, the tail of the obtained heavily arsenic-doped silicon single crystal rod is tapered, the surface is smooth, no obvious bulge or recess exists, and the probability of tail fracture of the heavily arsenic-doped silicon single crystal rod is reduced.
In another embodiment, the method for ending the heavily arsenic-doped silicon single crystal further comprises the following steps:
s110, acquiring ending temperature T at the beginning of ending0A; wherein, 0<a≤0.8℃；
S150. if L-LnIf the temperature is more than or equal to delta L, calculating the current ending temperature TnWherein, Tn＝λ1L3+λ2L2+λ3L + a, wherein, λ1、λ2、λ3Is a constant.
That is, the ending temperature is adjusted in real time by fitting a function curve of ending length and ending temperature and by obtaining the ending length.
Further, in step S150, λ is acquired by the following steps1、λ2、λ3：
S151, ending according to preset temperature parameters to obtain a successfully ended heavily arsenic-doped silicon single crystal rod;
s152, measuring the ending length of the tail part of the heavily arsenic-doped silicon single crystal rod where the mutation occurs, and obtaining the ending temperature corresponding to the mutation;
s153, adjusting the ending temperature of the mutation position, and ending by adopting the adjusted ending temperature;
s154, repeating the steps p2 and p3 until the tail of the heavily arsenic-doped silicon single crystal bar is smooth;
s155, fitting the adjusted ending temperature and ending length equation to obtain lambda1、λ2、λ3。
Referring to fig. 4, by adopting the method, the single crystal pulling speed and the ending temperature in the ending process of the heavily arsenic-doped silicon single crystal rod are adjusted at the same time, so that the automatic control of the ending process of the heavily arsenic-doped silicon single crystal rod is realized, the NG rate of the tail of the heavily arsenic-doped silicon single crystal rod is greatly reduced, the yield of the heavily arsenic-doped silicon single crystal rod is improved, the tail of the obtained heavily arsenic-doped silicon single crystal rod is conical, the surface is smooth, no obvious bulge or recess exists, and the probability of tail fracture of the heavily arsenic-doped silicon single crystal rod is reduced.
In a specific embodiment of the present invention, the heavily arsenic-doped silicon single crystal ending device is electrically connected to the central controller of the single crystal furnace, and is configured to obtain necessary data from the central controller of the single crystal furnace, receive setting data input by a technician, calculate a current pulling rate or ending temperature, and feed the current pulling rate or ending temperature back to the central controller of the single crystal furnace, so as to perform ending operation of the heavily arsenic-doped silicon single crystal.
The heavily arsenic-doped silicon single crystal ending device comprises:
the first acquisition module is used for acquiring the crucible heel ratio R after the isodiametric finishing;
a first calculating module, configured to calculate a theoretical pull-up ratio X, where X is 1/(1+ R);
the second acquisition module is used for acquiring an adjustment distance delta L, and the adjustment distance delta L is set according to production requirements;
the pulling speed setting module is used for adjusting the proportion X up according to the theoretical pulling speed, setting the pulling speed of the monocrystalline silicon when the monocrystalline silicon enters the ending process and entering the monocrystalline ending process;
a third obtaining module, configured to obtain a current ending length L;
a fourth obtaining module for obtaining the last adjustment time ending length LnAnd the adjusted pull rate up-regulation ratio Xn(ii) a Wherein, the ending length L at the beginning of endingnWhen the pulling speed is adjusted, the pulling speed is adjusted to be 0, and the pulling speed is adjusted to be X;
a judging module for judging L-LnWhether Δ L is greater than or equal to Δ L;
a second calculation module if L-LnIf the current pull speed is more than or equal to delta L, calculating the current pull speed up-regulation proportion XnWherein X isn＝X+[L/ΔL-1)]A,0<A≤10％；
Update module, update Ln。
Preferably, the heavily arsenic-doped silicon single crystal ending device further comprises:
a fifth obtaining module, configured to obtain a ending temperature T at the beginning of ending0A; wherein, 0<a≤0.8℃；
A first temperature regulating module for regulating the ending temperature T when the pull rate is regulated for the first time1A + b; wherein b is more than or equal to 0.5 ℃ and less than or equal to 1.0 ℃;
a first ending temperature calculation module for calculating L-LnWhen the temperature is more than or equal to delta L, calculating the current ending temperature TnWherein, Tn＝Tn-1+Tn-2；Tn-1The ending temperature after the last adjustment; t isn-2The final temperature after the last secondary adjustment.
Preferably, the heavily arsenic-doped silicon single crystal ending device further comprises:
a second ending temperature calculation module for calculating L-LnWhen the temperature is more than or equal to delta L, calculating the current ending temperature and calculating the current ending temperature TnWherein, Tn＝λ1L3+λ2L2+λ3L + a, wherein, λ1、λ2、λ3Is a constant.
For the specific definition of the heavily arsenic-doped silicon single crystal ending device, reference may be made to the above definition of the heavily arsenic-doped silicon single crystal ending method, which is not described herein again. All or part of each module in the heavily arsenic-doped silicon single crystal ending device can be realized by software, hardware and a combination thereof. The modules can be embedded in a hardware form or independent from a processor in the computer device, and can also be stored in a memory in the computer device in a software form, so that the processor can call and execute operations corresponding to the modules.
It should be noted that the above-mentioned heavily arsenic-doped silicon single crystal ending device may be an integrated circuit integrated on the controller of the single crystal furnace, or may be a microprocessor arranged in parallel with the controller of the single crystal furnace.
With reference to fig. 2 to 4, the technical solution and the technical effect of the present invention are further described below by specific embodiments. It is worth noting that the following experimental examples all adopt a hanhong 2408SR single crystal furnace to produce 8 inches of heavily arsenic-doped silicon single crystal in a gas phase doping manner. In the experimental examples of the present invention, the process parameters which are not particularly limited are generally parameters which can be obtained by those skilled in the art.
When the adjustment is not enhanced, in the same process of the following experimental examples, 2 batches (i.e. 20 crystal rods pulled in total) are produced by using 10 hanhong 2408SR single crystal furnaces arranged in parallel as the statistical background base.
Comparative example 1
After the constant diameter process is finished, entering a finishing process according to the set single crystal pulling speed and finishing temperature, and manually intervening the single crystal pulling speed and the finishing temperature at intervals, so as to improve the single crystal pulling speed and the finishing temperature until finishing.
By manually intervening the ending process of the heavily arsenic-doped silicon single crystal, not only is great manpower and material resources wasted, but also the probability of NG is about 45% due to crystal transformation of the tail of the heavily arsenic-doped silicon single crystal rod, the tail shape of the obtained arsenic-doped silicon single crystal rod is as shown in figure 2, the tail shape of the crystal rod is not uniform, and the crystal rod has obvious mutation and is easy to break.
Experimental example 1
And after the constant diameter process is finished, acquiring a crucible heel ratio R and a temperature a after the constant diameter process is finished, calculating a theoretical pulling speed up-regulation proportion X, wherein X is 1/(1+ R), up-regulating the pulling speed according to the theoretical pulling speed up-regulation proportion X, and ending.
In the ending process, the ending length (the ending length is generally larger than 1.0 time of the diameter of the crystal bar, for example, 8 inches of the single crystal bar, the ending length is about 210 mm) is detected, the adjustment interval delta L is adjusted once at intervals of 30mm, and the crystal pulling speed is adjusted to SL. XnWherein X isn＝X+[L/ΔL-1)]5%, e.g. for the second adjustment, X2X + 5%, in the third adjustment, X3X +2 · 5%, and so on. Adjusting the temperature to Tn＝Tn-1+Tn-2Wherein, T1＝a，T2＝a+1，T3＝2a+1，T4And 3a +2, and so on until the end.
Through the adjustment, the automatic control of the ending process of the heavily arsenic-doped silicon single crystal is realized, and the crystal change occurs at the tail of the heavily arsenic-doped silicon single crystal rod, so that the NG probability is reduced to about 15%. As shown in FIG. 3, the obtained arsenic-doped silicon single crystal rod has smooth tail, the tail of a plurality of crystal rods has uniform shape, no obvious mutation exists, and the breakage rate of the tail of the heavily arsenic-doped silicon single crystal rod is obviously reduced.
Experimental example two
And after the constant diameter process is finished, acquiring a crucible heel ratio R and a temperature a after the constant diameter process is finished, calculating a theoretical pulling speed up-regulation proportion X, wherein X is 1/(1+ R), up-regulating the pulling speed according to the theoretical pulling speed up-regulation proportion X, and ending.
In the ending process, the ending length (the ending length is generally larger than 1.0 time of the diameter of the crystal bar, for example, 8 inches of the single crystal bar, the ending length is about 210 mm) is detected, the adjustment interval delta L is adjusted once at intervals of 30mm, and the crystal pulling speed is adjusted to SL. XnWherein X isn＝X+[L/ΔL-1)]5%, e.g. for the second adjustment, X2X + 5%, in the third adjustment, X3X +2 · 5%, and so on. Adjusting the ending temperature to T when the single crystal pulling speed is adjustedn＝0.00001L3+0.0014L2+0.15L + a until the end of the run-out.
Through the adjustment, the automatic control of the ending process of the heavily arsenic-doped silicon single crystal is realized, and the crystal change occurs at the tail of the heavily arsenic-doped silicon single crystal rod, so that the NG probability is reduced to about 15%. As shown in FIG. 4, the obtained arsenic-doped silicon single crystal rod has smooth tail, the tail of a plurality of crystal rods has uniform shape, no obvious mutation exists, and the breakage rate of the tail of the heavily arsenic-doped silicon single crystal rod is obviously reduced.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.

Claims (8)

1. A method for ending heavily arsenic-doped silicon single crystal is characterized by comprising the following steps:
a. obtaining a crucible heel ratio R after the isodiametric finishing;
b. calculating a theoretical pull rate up-regulation ratio X, wherein X is 1/(1+ R);
c. obtaining an adjusting distance delta L, wherein the adjusting distance delta L is set according to production requirements;
d. adjusting the ratio X up according to the theoretical pulling speed, setting the pulling speed of the monocrystalline silicon when the monocrystalline silicon enters the ending process, and entering the monocrystalline ending process;
e. acquiring the current ending length L;
f. obtaining the last adjustment occurring ending length LnAnd the adjusted pull rate up-regulation ratio Xn(ii) a Wherein, the ending length L at the beginning of endingnWhen the pulling speed is adjusted, the pulling speed is adjusted to be 0, and the pulling speed is adjusted to be X;
g. judgment of L-LnWhether Δ L is greater than or equal to Δ L;
h. if L-LnIf the current pull speed is more than or equal to delta L, calculating the current pull speed up-regulation proportion XnWherein X isn＝X+[L/ΔL-1)]A,0<A≤10％；
i. Updating Ln；
And e, repeating the steps e to i until the ending is finished.
2. The method according to claim 1, wherein in step c, the adjustment distance Δ L is set to 10mm to 30 mm.
3. The method of claim 2, further comprising the steps of:
j. obtaining the ending temperature T at the beginning of ending0A; wherein, 0<a≤0.8℃；
k. Adjusting the tail-out temperature T when the pull rate is adjusted for the first time1A + b; wherein b is more than or equal to 0.5 ℃ and less than or equal to 1.0 ℃;
m. if L-LnIf the temperature is more than or equal to delta L, calculating the current ending temperature TnWherein, Tn＝Tn-1+Tn-2；Tn-1The ending temperature after the last adjustment; t isn-2The final temperature after the last secondary adjustment is obtained;
and n, repeating the step m until the ending.
4. The method of claim 2, further comprising the steps of: j. obtaining the ending temperature T at the beginning of ending0A; wherein, 0<a≤0.8℃；
If L-LnIf the temperature is more than or equal to delta L, calculating the current ending temperature TnWherein, Tn＝λ1L3+λ2L2+λ3L + a, wherein, λ1、λ2、λ3Is a constant.
5. The method of claim 4, wherein in step p λ is obtained by1、λ2、λ3：
p1., ending according to preset temperature parameters to obtain a successfully ended heavily arsenic-doped silicon single crystal rod;
p2. measuring the ending length of the tail of the monocrystalline ingot heavily doped with arsenic and obtaining the ending temperature corresponding to the mutation;
p3., adjusting the ending temperature of the mutation position, and ending by adopting the adjusted ending temperature;
p4. repeating the steps p2 and p3 until the tail of the heavily arsenic-doped silicon single crystal ingot is smooth;
p5. fitting the adjusted ending temperature and ending length equation to obtain lambda1、λ2、λ3。
6. The utility model provides a heavily mix arsenic silicon single crystal ending device, the central controller of single crystal growing furnace is connected to the electrical behavior, its characterized in that includes:
the first acquisition module is used for acquiring the crucible heel ratio R after the isodiametric finishing;
a first calculating module, configured to calculate a theoretical pull-up ratio X, where X is 1/(1+ R);
the second acquisition module is used for acquiring an adjustment distance delta L, and the adjustment distance delta L is set according to production requirements;
the pulling speed setting module is used for adjusting the proportion X up according to the theoretical pulling speed, setting the pulling speed of the monocrystalline silicon when the monocrystalline silicon enters the ending process and entering the monocrystalline ending process;
a third obtaining module, configured to obtain a current ending length L;
a fourth obtaining module for obtaining the latest toneLength of tail in the whole generationnAnd the adjusted pull rate up-regulation ratio Xn(ii) a Wherein, the ending length L at the beginning of endingnWhen the pulling speed is adjusted, the pulling speed is adjusted to be 0, and the pulling speed is adjusted to be X;
a judging module for judging L-LnWhether Δ L is greater than or equal to Δ L;
a second calculation module if L-LnIf the current pull speed is more than or equal to delta L, calculating the current pull speed up-regulation proportion XnWherein X isn＝X+[L/ΔL-1)]A,0<A≤10％；
Update module, update Ln。
7. The heavily arsenic-doped silicon single crystal termination apparatus of claim 6, further comprising:
a fifth obtaining module, configured to obtain a ending temperature T at the beginning of ending0A; wherein, 0<a≤0.8℃；
A first temperature regulating module for regulating the ending temperature T when the pull rate is regulated for the first time1A + b; wherein b is more than or equal to 0.5 ℃ and less than or equal to 1.0 ℃;
a first ending temperature calculation module for calculating L-LnWhen the temperature is more than or equal to delta L, calculating the current ending temperature TnWherein, Tn＝Tn-1+Tn-2；Tn-1The ending temperature after the last adjustment; t isn-2The final temperature after the last secondary adjustment.
8. The heavily arsenic-doped silicon single crystal termination apparatus of claim 6, further comprising:
a second ending temperature calculation module for calculating L-LnWhen the temperature is more than or equal to delta L, calculating the current ending temperature and calculating the current ending temperature TnWherein, Tn＝λ1L3+λ2L2+λ3L + a, wherein, λ1、λ2、λ3Is a constant.
CN202110794760.4A 2021-07-14 2021-07-14 Heavily arsenic-doped silicon single crystal ending method and device Pending CN113564691A (en)

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CN113073382A (en) * 2021-03-30 2021-07-06 广东高景太阳能科技有限公司 Drawing and ending process of 12-inch single crystal silicon rod

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Application publication date: 20211029