CN115491753A - Drawing process for controlling resistivity of gallium-doped single crystal according to furnace pressure - Google Patents
Drawing process for controlling resistivity of gallium-doped single crystal according to furnace pressure Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 599
- 238000000034 method Methods 0.000 title claims abstract description 44
- 230000008569 process Effects 0.000 title claims abstract description 42
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 47
- 239000000956 alloy Substances 0.000 claims abstract description 47
- 230000009467 reduction Effects 0.000 claims description 18
- 230000008859 change Effects 0.000 claims description 13
- 239000007789 gas Substances 0.000 description 24
- 230000001681 protective effect Effects 0.000 description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 15
- 229910052710 silicon Inorganic materials 0.000 description 15
- 239000010703 silicon Substances 0.000 description 15
- 239000007788 liquid Substances 0.000 description 13
- 230000001276 controlling effect Effects 0.000 description 11
- 229910000807 Ga alloy Inorganic materials 0.000 description 8
- 239000007791 liquid phase Substances 0.000 description 7
- 238000010899 nucleation Methods 0.000 description 4
- 238000005204 segregation Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- RZJQYRCNDBMIAG-UHFFFAOYSA-N [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] Chemical class [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] RZJQYRCNDBMIAG-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 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
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- 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
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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
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- C—CHEMISTRY; METALLURGY
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- 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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Abstract
The invention provides a drawing process for controlling the resistivity of a gallium-doped single crystal according to furnace pressure. The method has the advantages that the furnace pressure of the single crystal furnace is reduced along with the increase of the single crystal pulling length in the equal diameter stage, different furnace gas flow scenes are manufactured in the single crystal pulling process, the alloy volatilization rate at the later stage of the pulling of the gallium-doped single crystal is increased, the alloy concentration is reduced, the control precision of the circumferential resistivity of the gallium-doped single crystal is improved, and the pulling length of the gallium-doped single crystal is improved.
Description
Technical Field
The invention belongs to the technical field of solar photovoltaic materials, and particularly relates to a drawing process for controlling the resistivity of a gallium-doped single crystal according to furnace pressure.
Background
The competition in the industry is increasingly intense, and the demand of the single crystal battery component on the low light attenuation silicon chip is increasing. The single crystal is pulled by adding gallium alloy, so that the light attenuation of the silicon single crystal can be reduced, and the gallium-doped single crystal is manufactured in the single crystal silicon industry at present. Because the segregation coefficient of gallium is only 0.08, is far lower than the segregation coefficient of boron by 0.8, and the difference is 100 times, the control of the axial resistivity of the gallium-doped single crystal is difficult, the drawing length cannot be well matched with the existing single crystal furnace, and the resistivity reduction amplitude is larger than the theoretical calculation value. In the process of pulling the gallium-doped single crystal, the ratio of gallium alloy entering a solid phase interface to liquid phase is very small, and the ratio of the gallium alloy and the liquid phase is only 0.08, so that an alloy enrichment area is formed on one side of the liquid phase of a solid-liquid interface, the actual alloy concentration of the solid-liquid interface at the later stage of pulling the single crystal is higher than that calculated theoretically due to the formation of the area, the alloy entering the single crystal is increased, the resistance is reduced to the target lower limit, and the crystal pulling cannot be continued. For the reasons mentioned above, the axial resistivity of gallium-doped single crystals is difficult to control, and the pulling length is often less than 2500mm. The concentration of liquid phase alloy outside a solid-liquid interface can be reduced by increasing volatilization in the process of pulling the single crystal, the concentration reduction speed of an alloy enrichment area is increased, but in the equal diameter stage, the volatilization interface of silicon liquid is reduced, so that the volatilization speed is reduced.
Disclosure of Invention
In view of the above, the present invention provides a drawing process for controlling the resistivity of a gallium-doped single crystal according to the furnace pressure, so as to solve the above or other former problems in the prior art.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a process for controlling the resistivity of gallium-doped monocrystal by furnace pressure includes such steps as regulating the furnace pressure of monocrystal furnace according to the variation of monocrystal pulling length, controlling the furnace pressure of monocrystal furnace and controlling the volatilization rate of alloy.
Further, in the equal diameter stage, the furnace pressure of the single crystal furnace is gradually reduced, and the furnace pressure of the single crystal furnace is adjusted within the range of 12-5torr.
Further, in the initial stage of the equal diameter, the furnace pressure of the single crystal furnace is the first furnace pressure;
the ratio of the length variation of the single crystal pulling to the furnace pressure variation of the single crystal furnace reduction is 250-1200 as the pulling length of the single crystal increases;
when the pulling length of the single crystal is the first length, the furnace pressure of the single crystal furnace is the second furnace pressure, and the furnace pressure of the single crystal furnace is kept unchanged until the single crystal pulling in the equal diameter stage is completed.
Further, the ratio of the length variation of the single crystal pulling to the furnace pressure variation of the single crystal furnace reduction is 400 to 800.
Furthermore, the length variation is 400-600mm.
Further, the first furnace pressure is 11-13torr.
Further, the second furnace pressure is 4-6torr.
Further, the first length is 2800-3200mm.
Further, the furnace pressure variation is 0.5to 1.5torr.
By adopting the technical scheme, the furnace pressure of the single crystal furnace is adjusted according to the change of the pulling length of the single crystal when the Czochralski single crystal enters the equal diameter stage, so that the furnace pressure of the single crystal furnace is reduced along with the increase of the pulling length of the single crystal in the equal diameter stage, different gas flowing scenes in the furnace are manufactured in the single crystal pulling process, the alloy volatilization rate in the later stage of pulling the gallium-doped single crystal is increased, the alloy concentration is reduced, the control precision of the circumferential resistivity of the gallium-doped single crystal is improved, and the pulling length of the gallium-doped single crystal is improved; the resistivity of the head of the single crystal is reduced, the resistivity of the tail of the single crystal is improved, the later resistivity of the gallium-doped single crystal is improved, the pulling length of the single crystal is increased within the target resistance range, the output of a single gallium-doped single crystal furnace is improved, and the competitiveness of a gallium-doped product is enhanced.
Detailed Description
The present invention will be further described with reference to the following examples.
The invention relates to a drawing process for controlling the resistivity of a gallium-doped single crystal according to furnace pressure, which is mainly used for controlling the furnace pressure of a single crystal furnace in the constant diameter process of pulling the single crystal, further controlling the volatilization efficiency of alloy to improve the consistency of the resistivity of the single crystal, reducing the control difficulty of the resistivity of the single crystal, reducing the attenuation rate from the resistivity of the head to the resistivity of the tail of the single crystal, keeping the earlier stage of the constant diameter stage using larger furnace pressure, reducing the gas flow rate in the single crystal furnace, ensuring less volatilization of the alloy, reducing the head resistivity of the single crystal exceeding the specification caused by overlarge volatilization, reducing the furnace pressure of the single crystal furnace in the constant diameter process, increasing the gas flow rate in the single crystal furnace, accelerating the volatilization speed of the alloy and making up the insufficient volatilization of the alloy caused by the reduction of the volatilization area of silicon liquid.
The drawing process for controlling the resistivity of the gallium-doped single crystal according to the furnace pressure is suitable for alloys with extremely small segregation coefficient, such as gallium alloy single crystals, the gallium-doped single crystal is drawn by the process, the volatilization rate of the head of the single crystal is reduced, the head resistance of the single crystal is reduced, the head resistivity of the single crystal can be lower, the target resistivity is improved, the use of the alloys is reduced, a foundation is laid for drawing longer single crystals, sufficient volatilization effect can be ensured at the later stage of single crystal drawing, the alloy concentration in silicon liquid is reduced, the condition that the alloy content in solid silicon exceeds the specification to cause too low resistance is avoided, the single drawing length of the gallium-doped single crystal is further increased, the single furnace output is improved, and the product competitiveness is increased.
A pulling process for controlling the resistivity of a gallium-doped single crystal according to furnace pressure is characterized in that in the process of pulling a single crystal, the furnace pressure of a single crystal furnace is controlled in an equal diameter stage, due to the difference between actual resistivity and theoretical resistivity, the furnace pressure of the single crystal furnace is adjusted according to the change of the pulling length of the single crystal, the volatilization rate of alloy is controlled, the consistency of the axial resistivity of the single crystal is improved, the control difficulty of the resistivity is reduced, and the control precision of the resistivity of the gallium-doped single crystal is improved.
In the equal diameter stage, in view of the fact that when the single crystal is pulled by the existing process, the difference between the actual resistivity and the theoretical resistivity is large, the resistivity of the head of the single crystal is large, the resistivity of the tail of the single crystal is small, and the attenuation rate of the resistivity of the single crystal is high, after the single crystal enters the equal diameter stage, the furnace pressure of the single crystal furnace is adjusted along with the increase of the pulling length of the single crystal, the furnace pressure of the single crystal furnace is gradually reduced, and in the equal diameter stage, the furnace pressure of the single crystal furnace is reduced from the large furnace pressure to the small furnace pressure to adjust the flowing speed of the protective gas so as to adjust the volatilization rate of the alloy. In the initial stage of the isometric stage, the volatilization interface of the silicon solution is changed from a larger volatilization liquid level during seeding to a smaller volatilization liquid level during the isometric stage, and the volatilization liquid level of the silicon solution is reduced after the isometric stage, so that the flowing speed of protective gas is changed by adjusting the furnace pressure of the single crystal furnace, the volatilization rate of the silicon solution is further changed, the alloy entering the single crystal is reduced, and the resistivity of the tail part of the single crystal is improved. Here, the furnace pressure of the single crystal furnace is adjusted within a range of 12to 5torr, and the furnace pressure of the single crystal furnace at each stage is selected as each stage of the increase of the single crystal pulling length.
At the initial stage of the equal diameter stage, at the moment, the alloy concentration of the alloy enrichment area is smaller, the volatilization interface of the silicon solution is reduced from a larger area during seeding to a smaller area during equal diameter, the volatilization rate of the alloy is higher, at the moment, the furnace pressure of the single crystal furnace is higher, the gas flow rate in the single crystal furnace is reduced, less volatilization of the alloy is ensured, and the head resistivity of the single crystal caused by the larger volatilization of the alloy is reduced to exceed the specification; along with the process of single crystal pulling in the equal diameter stage, the area of a silicon solution volatilization interface is kept unchanged, but the alloy concentration of an alloy enrichment area is gradually increased along with the process of single crystal pulling, at the moment, the furnace pressure of a single crystal furnace is gradually reduced, the air exhaust rate of an air exhaust pump is increased, the gas flow speed in the single crystal furnace is increased, the volatilization speed is accelerated, the insufficient volatilization of the alloy caused by the small volatilization area of the silicon solution is made up, the alloy entering the single crystal is reduced, the resistivity of the tail part of the single crystal is increased, the attenuation rate of the resistivity of the head and the tail of the single crystal is reduced, the resistivity of the tail part of the single crystal is improved, and due to the improvement of the alloy volatilization rate, the resistivity of the tail part of the single crystal is on the target lower limit, the pulling time in the equal diameter stage is prolonged, the pulling length of the single crystal is increased, and the yield of the single crystal furnace is improved.
Specifically, in the equal diameter stage, the furnace pressure of the single crystal furnace is adjusted according to the change of the pulling length of the single crystal, and the furnace pressure of the single crystal furnace is adjusted along with the increase of the pulling length of the single crystal, so that the furnace pressure of the single crystal furnace is reduced along with the increase of the length of the single crystal, the gas flow rate in the single crystal furnace is increased, the volatilization speed of an alloy is accelerated, the resistivity of the head of the single crystal is reduced, the use of the alloy is reduced, the longer pulling of the single crystal is convenient to realize, the sufficient volatilization effect in the later stage of pulling the single crystal can be ensured, the alloy concentration in a silicon solution is reduced, the phenomenon that the resistance is too low due to the fact that the alloy content at the tail of the single crystal exceeds the specification is avoided, and the single pulling length of the gallium-doped single crystal is increased.
In the initial stage of the equal diameter, the furnace pressure of the single crystal furnace is the first furnace pressure; the first furnace pressure is 11-13torr, and is selected according to actual requirements.
In the initial stage, the silicon liquid volatilization interface is changed from a larger area during seeding to a smaller area during equal diameter, because the flow rate of the protective gas in the seeding stage is larger, at the moment, the alloy concentration in the liquid phase of the solid-liquid interface of the silicon solution is smaller, and because of the volatile characteristic of the gallium alloy, the volatilized gallium alloy is taken away under the flow action of the protective gas, the alloy concentration in the liquid phase outside the solid-liquid interface can be reduced, at the moment, the volatilized gallium alloy can be taken away by adopting the protective gas flow with smaller flow, the volatilization rate of the gallium alloy is increased, the alloy concentration in the liquid phase outside the solid-liquid interface is reduced, the alloy entering the single crystal is reduced, and the resistivity of the head of the single crystal is reduced; because the furnace pressure of the single crystal furnace is larger, the furnace pressure of the single crystal furnace is kept within the specified process value range, the flow rate of the protective gas in the single crystal furnace can be increased, and the volatilization rate of the alloy can be increased.
The ratio of the length variation of single crystal pulling to the furnace pressure variation of the single crystal furnace is 250-1200 along with the increase of the pulling length of the single crystal, the furnace pressure of the single crystal furnace is reduced along with the increase of the pulling length of the single crystal, the furnace pressure reduction of the single crystal furnace and the increase of the length of the single crystal are changed according to a certain proportion, the furnace pressure of the single crystal furnace is gradually reduced, the flow rate of protective gas in the single crystal furnace is increased, the volatilization of alloy is accelerated, and the tail resistivity of the single crystal is improved.
When the furnace pressure of the single crystal furnace is adjusted according to equidistant increase of the pulling length of the single crystal, the furnace pressure of the single crystal furnace is proportionally reduced along with the increase of the pulling length of the single crystal, the pulling length of the single crystal is increased along with the increase of the pulling time in the equal diameter stage, the alloy concentration is gradually increased, the pulling length of the single crystal is gradually increased, the furnace pressure of the single crystal furnace is gradually reduced according to a proportion of 250-1200, the flow rate of the protective gas in the single crystal furnace is gradually increased, the volatilization rate of the alloy is increased, the alloy concentration is reduced, the alloy entering the single crystal in the later period of the equal diameter stage is reduced, and the resistivity of the tail part of the single crystal is improved.
Furthermore, the ratio of the length variation of the single crystal pulling to the furnace pressure variation reduced by the single crystal furnace is 400-800, and the length variation is selected according to actual requirements without specific requirements.
The length variation is 400-600mm, the furnace pressure variation is 0.5-1.5torr, and the selection is carried out according to actual requirements, and no specific requirements are made here.
With the process of single crystal pulling, when the pulling length of the single crystal is a first length, the furnace pressure of the single crystal furnace is a second furnace pressure, the furnace pressure of the single crystal furnace is kept unchanged until the single crystal pulling in the equal diameter stage is finished, at the moment, the pulling of the single crystal enters the final stage of the equal diameter stage, the furnace pressure of the single crystal furnace is unchanged, namely, the ending stage can be entered, the first length is 2800-3200mm, the second furnace pressure is 4-6torr, and the method is selected according to actual requirements and does not need to be specifically required.
In the process of pulling the single crystal, the length variation of the pulling of the single crystal can be increased equidistantly or non-equidistantly, and is selected according to actual requirements.
The protective gas is an inert gas, and preferably, the protective gas is argon.
The following examples are given for illustrative purposes.
Example one
In this embodiment, the ratio of the variation in length of single crystal pulling to the variation in furnace pressure reduction of the single crystal furnace is 400, the variation in increase in single crystal pulling length is 400mm, and the variation in furnace pressure reduction of the single crystal furnace is 1torr, then:
in the initial stage of constant diameter, the pulling length of the single crystal is 0mm, and at the moment, the furnace pressure of a single crystal furnace is 12torr, so that the single crystal is pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 400mm, the furnace pressure of the single crystal furnace is kept unchanged, the furnace pressure of the single crystal furnace is 12torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 800mm, the furnace pressure of the single crystal furnace is slowly reduced from 12torr to 11torr in the process of increasing the pulling length of the single crystal by 400mm, the furnace pressure of the single crystal furnace is 11torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 1200mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 10torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 1600mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 9torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 2000mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 8torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 2400mm, the single crystal enters the end section of the equal-diameter stage, the furnace pressure of the single crystal furnace is slowly reduced, the speed of an evacuation pump is increased, the flow rate of protective gas in the single crystal furnace is increased, the furnace pressure of the single crystal furnace is 7torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 2800mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 6torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 3200mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 3600mm, the furnace pressure of the single crystal furnace is kept at 5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 4000mm, the furnace pressure of the single crystal furnace is kept at 5torr, and the drawing of the single crystal in the equal-diameter stage is completed to be ended.
The single crystal is pulled by adopting the process in the equal diameter stage, and after the single crystal is pulled, the resistivity parameters of each section of the single crystal are as follows:
therefore, the resistivity of the tail part of the single crystal is obviously improved, the resistivity of the head part of the single crystal is slightly reduced, and the attenuation rate of the axial resistivity of the single crystal is reduced.
Example two
In this embodiment, the ratio of the variation in length of single crystal pulling to the variation in furnace pressure reduction of the single crystal furnace is 500, the variation in increase in single crystal pulling length is 500mm, and the variation in furnace pressure reduction of the single crystal furnace is 1torr, then:
in the initial stage of the constant diameter, the pulling length of the single crystal is 0mm, at the moment, the furnace pressure of a single crystal furnace is 11torr, and the single crystal is pulled;
when the length of the single crystal is increased by 500mm, the length of the single crystal is 500mm, the furnace pressure of the single crystal furnace is kept unchanged, the furnace pressure of the single crystal furnace is 12torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 500mm, the length of the single crystal is 1000mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 11torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 500mm, the length of the single crystal is 1500mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 10torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 500mm, the length of the single crystal is 2000mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 9torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 500mm, the length of the single crystal is 2500mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 8torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 500mm, the length of the single crystal is 3000mm, the single crystal enters the end section of the equal diameter stage, the furnace pressure of the single crystal furnace is slowly reduced, the speed of an evacuation pump is increased, the flow rate of protective gas in the single crystal furnace is increased, the furnace pressure of the single crystal furnace is 7torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 500mm, the length of the single crystal is 3500mm, the furnace pressure is kept, the furnace pressure of the single crystal furnace is 6.2torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 500mm, the length of the single crystal is 4000mm, the furnace pressure of the single crystal furnace is kept at the moment, the furnace pressure of the single crystal furnace is 7torr, the single crystal is continuously pulled until the pulling of the single crystal in the equal diameter stage is finished, and the ending is carried out.
The single crystal at the equal diameter stage is pulled by adopting the process, and after the single crystal is pulled, the resistivity parameters of each section of the single crystal are as follows:
therefore, the resistivity of the tail part of the single crystal is obviously improved, the resistivity of the head part of the single crystal is slightly reduced, and the decay rate of the axial resistivity of the single crystal is reduced.
EXAMPLE III
In this embodiment, the ratio of the variation in length of single crystal pulling to the variation in furnace pressure reduction of the single crystal furnace is 800, the variation in increase in single crystal pulling length is 400mm, and the variation in furnace pressure reduction of the single crystal furnace is 0.5torr, then:
in the initial stage of constant diameter, the pulling length of the single crystal is 0mm, and at the moment, the furnace pressure of a single crystal furnace is 12torr, so that the single crystal is pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 400mm, the furnace pressure of the single crystal furnace is kept unchanged, the furnace pressure of the single crystal furnace is 12torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 800mm, the furnace pressure of the single crystal furnace is slowly reduced to 11.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 1200mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 11torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 1600mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 10.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 2000mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 10torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 2400mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 9torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 2800mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 9torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 3200mm, the single crystal enters the end of an equal-diameter stage, the furnace pressure of a single crystal furnace is slowly reduced, the speed of an evacuation pump is increased, the flow rate of protective gas in the single crystal furnace is increased, the furnace pressure of the single crystal furnace is 8.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 3600mm, the furnace pressure of the single crystal furnace is kept at 8.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 4000mm, the furnace pressure of the single crystal furnace is kept at 8.5torr, and the drawing of the single crystal in the equal diameter stage is completed and the ending is carried out.
The single crystal at the equal diameter stage is pulled by adopting the process, and after the single crystal is pulled, the resistivity parameters of each section of the single crystal are as follows:
therefore, the resistivity of the tail part of the single crystal is obviously improved, the resistivity of the head part of the single crystal is slightly reduced, and the attenuation rate of the axial resistivity of the single crystal is reduced.
Example four
In this example, the ratio of the amount of change in the length of the single crystal pulling to the amount of change in the furnace pressure reduced by the single crystal furnace was 266, and the amount of change in the increase in the length of the single crystal pulling was 400mm, then the amount of change in the furnace pressure reduction by the single crystal furnace was 1.5torr, then:
in the initial stage of the equal diameter, the pulling length of the single crystal is 0mm, at the moment, the furnace pressure of a single crystal furnace is 12torr, and the single crystal is pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 400mm, the furnace pressure of the single crystal furnace is kept unchanged, the furnace pressure of the single crystal furnace is 12torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 800mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 10.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 1200mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 9torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 1600mm, the furnace pressure of the single crystal furnace is slowly reduced to 7.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 2000mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 6torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 2400mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 4.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 2800mm, the furnace pressure of the single crystal furnace is kept at 4.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 3200mm, the single crystal enters the end of an equal-diameter stage, the furnace pressure of a single crystal furnace is slowly reduced, the speed of an evacuation pump is increased, the flow rate of protective gas in the single crystal furnace is increased, the furnace pressure of the single crystal furnace is 4.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 3600mm, the furnace pressure of the single crystal furnace is kept at 4.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 4000mm, the furnace pressure of the single crystal furnace is kept at 4.5torr, and the drawing of the single crystal in the equal diameter stage is completed and the ending is carried out.
The single crystal at the equal diameter stage is pulled by adopting the process, and after the single crystal is pulled, the resistivity parameters of each section of the single crystal are as follows:
therefore, the resistivity of the tail part of the single crystal is obviously improved, the resistivity of the head part of the single crystal is slightly reduced, and the decay rate of the axial resistivity of the single crystal is reduced.
EXAMPLE five
In this embodiment, the ratio of the amount of change in the length of the single crystal pulling to the amount of change in the furnace pressure reduced by the single crystal furnace is 1200, and the amount of change in the increase in the length of the single crystal pulling is 600mm, then the amount of change in the furnace pressure reduction by the single crystal furnace is 0.5torr, then:
in the initial stage of the equal diameter, the pulling length of the single crystal is 0mm, the furnace pressure of a single crystal furnace is 12torr at the moment, and the single crystal is pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 600mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 11.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 1200mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 11torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 1800mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 10.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 2400mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 10torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 3000mm, the single crystal enters the end section of the equal diameter stage, the furnace pressure of the single crystal furnace is slowly reduced, the speed of an evacuation pump is increased, the flow rate of protective gas in the single crystal furnace is increased, the furnace pressure of the single crystal furnace is 9.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 3600mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 9torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 4200mm, the furnace pressure of the single crystal furnace is slowly reduced to 8.5torr, the single crystal is continuously pulled, the pulling of the single crystal in the equal diameter stage is completed, and the ending is carried out.
The single crystal at the equal diameter stage is pulled by adopting the process, and after the single crystal is pulled, the resistivity parameters of each section of the single crystal are as follows:
therefore, the resistivity of the tail part of the single crystal is obviously improved, the resistivity of the head part of the single crystal is slightly reduced, and the attenuation rate of the axial resistivity of the single crystal is reduced.
Example six
In this embodiment, the ratio of the variation in length of single crystal pulling to the variation in furnace pressure reduction of the single crystal furnace is 400, the variation in increase in single crystal pulling length is 600mm, and the variation in furnace pressure reduction of the single crystal furnace is 1.5torr, then:
in the initial stage of constant diameter, the pulling length of the single crystal is 0mm, and at the moment, the furnace pressure of a single crystal furnace is 12torr, so that the single crystal is pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 600mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 10.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 1200mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 9torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 1800mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 7.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 2400mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 6torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 3000mm, the single crystal enters the end section of the equal diameter stage, the furnace pressure of the single crystal furnace is slowly reduced, the speed of an evacuation pump is increased, the flow rate of protective gas in the single crystal furnace is increased, the furnace pressure of the single crystal furnace is 4.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 3600mm, the furnace pressure of the single crystal furnace is kept at the moment, the furnace pressure of the single crystal furnace is 4.5torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 600mm, the length of the single crystal is 4200mm, the furnace pressure of the single crystal furnace is kept at 4.5torr, the single crystal is continuously pulled, the pulling of the single crystal in the equal diameter stage is completed, and the ending is carried out.
The single crystal at the equal diameter stage is pulled by adopting the process, and after the single crystal is pulled, the resistivity parameters of each section of the single crystal are as follows:
therefore, the resistivity of the tail part of the single crystal is obviously improved, the resistivity of the head part of the single crystal is slightly reduced, and the attenuation rate of the axial resistivity of the single crystal is reduced.
EXAMPLE seven
In this embodiment, the ratio of the variation of the length of the single crystal pulling to the variation of the furnace pressure reduced by the single crystal furnace is 500, and the variation of the increase of the single crystal pulling length is a non-equidistant increase, and the variation of the furnace pressure reduction by the single crystal furnace is a non-constant value, then:
in the initial stage of constant diameter, the pulling length of the single crystal is 0mm, and at the moment, the furnace pressure of a single crystal furnace is 12torr, so that the single crystal is pulled;
when the length of the single crystal is increased by 300mm, the length of the single crystal is 300mm, the furnace pressure of the single crystal furnace is kept at 12torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 700mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 11.2torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 500mm, the length of the single crystal is 1200mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 10.2torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 500mm, the length of the single crystal is 1700mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 9.2torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 300mm, the length of the single crystal is 2000mm, the furnace pressure of the single crystal furnace is slowly reduced at the moment, the furnace pressure of the single crystal furnace is 8.4torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 500mm, the length of the single crystal is 2500mm, the furnace pressure of the single crystal furnace is slowly reduced, the furnace pressure of the single crystal furnace is 7.4torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 500mm, the length of the single crystal is 3000mm, the single crystal enters the end of the equal-diameter stage, the furnace pressure of the single crystal furnace is slowly reduced, the speed of an air pump is increased, the flow rate of protective gas in the single crystal furnace is increased, the furnace pressure of the single crystal furnace is 6.4torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 200mm, the length of the single crystal is 3200mm, the furnace pressure of the single crystal furnace is kept at the moment, the furnace pressure of the single crystal furnace is 6.4torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm, the length of the single crystal is 3600mm, the furnace pressure of the single crystal furnace is kept at 6.4torr, and the single crystal is continuously pulled;
when the length of the single crystal is increased by 400mm and the length of the single crystal is 4000mm, maintaining the furnace pressure of the single crystal furnace at the moment, keeping the furnace pressure of the single crystal furnace at 6.4torr, continuously drawing the single crystal, finishing the drawing of the single crystal at the equal diameter stage, and ending.
The single crystal at the equal diameter stage is pulled by adopting the process, and after the single crystal is pulled, the resistivity parameters of each section of the single crystal are as follows:
therefore, the resistivity of the tail part of the single crystal is obviously improved, the resistivity of the head part of the single crystal is slightly reduced, and the decay rate of the axial resistivity of the single crystal is reduced.
By adopting the technical scheme, the furnace pressure of the single crystal furnace is adjusted according to the change of the pulling length of the single crystal when the Czochralski single crystal enters the equal diameter stage, so that the furnace pressure of the single crystal furnace is reduced along with the increase of the pulling length of the single crystal in the equal diameter stage, different gas flowing scenes in the furnace are manufactured in the single crystal pulling process, the alloy volatilization rate in the later stage of pulling the gallium-doped single crystal is increased, the alloy concentration is reduced, the control precision of the circumferential resistivity of the gallium-doped single crystal is improved, and the pulling length of the gallium-doped single crystal is improved; the resistivity of the head of the single crystal is reduced, the resistivity of the tail of the single crystal is improved, the later resistivity of the gallium-doped single crystal is improved, the pulling length of a single crystal is increased within the range of target resistance, the yield of a single gallium-doped single crystal furnace is improved, and the competitiveness of gallium-doped products is improved.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (9)
1. A drawing process for controlling the resistivity of a gallium-doped single crystal according to furnace pressure is characterized in that: in the process of pulling the single crystal, the furnace pressure of the single crystal furnace is adjusted according to the change of the pulling length of the single crystal in the equal diameter stage, the furnace pressure of the single crystal furnace is controlled, and the volatilization rate of the alloy is controlled.
2. A pulling process for controlling the resistivity of a gallium-doped single crystal according to the furnace pressure as recited in claim 1, wherein: in the equal diameter stage, the furnace pressure of the single crystal furnace is gradually reduced, and the furnace pressure of the single crystal furnace is adjusted within the range of 12-5torr.
3. A pulling process for controlling the resistivity of a gallium-doped single crystal according to the furnace pressure as claimed in claim 1 or 2, characterized in that: in the initial stage of the equal diameter, the furnace pressure of the single crystal furnace is a first furnace pressure;
the ratio of the length variation of the single crystal pulling to the furnace pressure variation of the single crystal furnace reduction is 250-1200 as the pulling length of the single crystal increases;
and when the pulling length of the single crystal is the first length, the furnace pressure of the single crystal furnace is the second furnace pressure, and the furnace pressure of the single crystal furnace is kept unchanged until the single crystal pulling in the equal diameter stage is finished.
4. A pulling process for controlling the resistivity of a gallium-doped single crystal as recited in claim 3, wherein: the ratio of the length variation of the single crystal pulling to the furnace pressure variation of the single crystal furnace is 400-800.
5. A pulling process for controlling the resistivity of a gallium-doped single crystal as recited in claim 4, wherein the resistivity of the gallium-doped single crystal is controlled based on the furnace pressure by: the length variation is 400-600mm.
6. A pulling process for controlling the resistivity of a gallium-doped single crystal according to the furnace pressure as claimed in claim 4 or 5, wherein: the first furnace pressure is 11-13torr.
7. A pulling process for controlling the resistivity of a gallium-doped single crystal according to the furnace pressure as recited in claim 6, wherein: the second furnace pressure is 4-6torr.
8. A pulling process for controlling the resistivity of a gallium-doped single crystal as recited in claim 7, wherein: the first length is 2800-3200mm.
9. A pulling process for controlling the resistivity of a gallium-doped single crystal according to the furnace pressure as claimed in claim 7 or 8, wherein: the furnace pressure variation is 0.5-1.5torr.
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Citations (5)
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|---|---|---|---|---|
| JPS59190292A (en) * | 1983-04-08 | 1984-10-29 | Shin Etsu Handotai Co Ltd | Method for controlling resistivity of semiconductor silicon single crystal |
| CN1455028A (en) * | 2002-12-30 | 2003-11-12 | 天津市环欧半导体材料技术有限公司 | Gas-phase doping-area fused silicon monocrystal production method |
| CN102162124A (en) * | 2011-04-06 | 2011-08-24 | 天津市环欧半导体材料技术有限公司 | Method for improving axial resistivity uniformity of single crystal with heavily doped Ar |
| CN102345155A (en) * | 2011-08-14 | 2012-02-08 | 上海合晶硅材料有限公司 | Pulling method for overweight As-doped crystal bar |
| CN105019017A (en) * | 2015-06-30 | 2015-11-04 | 内蒙古中环光伏材料有限公司 | Method used for reducing oxygen content of czochralski silicon |
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2021
- 2021-06-17 CN CN202110672611.0A patent/CN115491753A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS59190292A (en) * | 1983-04-08 | 1984-10-29 | Shin Etsu Handotai Co Ltd | Method for controlling resistivity of semiconductor silicon single crystal |
| CN1455028A (en) * | 2002-12-30 | 2003-11-12 | 天津市环欧半导体材料技术有限公司 | Gas-phase doping-area fused silicon monocrystal production method |
| CN102162124A (en) * | 2011-04-06 | 2011-08-24 | 天津市环欧半导体材料技术有限公司 | Method for improving axial resistivity uniformity of single crystal with heavily doped Ar |
| CN102345155A (en) * | 2011-08-14 | 2012-02-08 | 上海合晶硅材料有限公司 | Pulling method for overweight As-doped crystal bar |
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