CN115341268A - Method for automatically controlling resistivity of monocrystalline silicon - Google Patents
Method for automatically controlling resistivity of monocrystalline silicon Download PDFInfo
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- CN115341268A CN115341268A CN202110522365.0A CN202110522365A CN115341268A CN 115341268 A CN115341268 A CN 115341268A CN 202110522365 A CN202110522365 A CN 202110522365A CN 115341268 A CN115341268 A CN 115341268A
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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
- 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
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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
- 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
Abstract
The invention provides a method for automatically controlling the resistivity of monocrystalline silicon, which carries out gas doping in the process of pulling the monocrystalline silicon and comprises the following steps: setting a gas doping opening node and gas flow; carrying out single crystal pulling; in the process of pulling the single crystal, obtaining the contact voltage of the melt in the crucible, and automatically calculating the resistivity of the single crystal according to the contact voltage; judging the single crystal pulling process, and controlling gas to be input into the single crystal furnace for doping if the set gas doping starting node condition is met; meanwhile, controlling the flow change of the gas according to the calculated single crystal resistivity, and controlling the single crystal axial resistivity; otherwise, the pulling of the single crystal is continued. The invention has the advantages that the automatic ventilation system is additionally arranged, the condition of doping gas for starting doping is set, the control system controls the automatic ventilation system to act, the doping gas is introduced, the resistivity of the single crystal is obtained according to the contact voltage of the single crystal and melts with different weights in the crucible, the flow change of the doping gas is automatically controlled, and the axial attenuation of the resistivity of the single crystal is controlled.
Description
Technical Field
The invention belongs to the technical field of photovoltaics, and particularly relates to a method for automatically controlling the resistivity of monocrystalline silicon.
Background
In the prior art, gallium-doped single crystals have the advantage of low light attenuation compared with boron-doped single crystals, so that the market demand on gallium-doped single crystals is promoted, but because the segregation coefficient of Ga is extremely small (Ga: 0.008, B. At present, the doping is carried out by a solid phase doping mode commonly used in the industry, and the doping compensation method can not meet the requirement of single crystal quality in the crystal pulling process and can not realize automatic continuous compensation.
Disclosure of Invention
In view of the above problems, the present invention provides a method for automatically controlling resistivity of single crystal silicon, so as to solve at least one of the above or other former problems of the prior art.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for automatically controlling the resistivity of single crystal silicon during gas doping in a Czochralski single crystal pulling process, comprising:
setting a gas doping opening node and gas flow;
carrying out single crystal pulling;
in the process of pulling the single crystal, obtaining the contact voltage of a melt in a crucible, and automatically calculating the resistivity of the single crystal according to the contact voltage;
judging the process of single crystal pulling, and controlling gas to be input into the single crystal furnace for doping if the set gas doping starting node condition is met; meanwhile, controlling the flow change of the gas according to the calculated single crystal resistivity, and controlling the single crystal axial resistivity;
otherwise, no gas is fed into the single crystal furnace.
Furthermore, the gas doping opening node is a stage of pulling the single crystal to enter a shoulder expanding stage or an equal diameter stage.
Further, the gas flow is 0-1L/min.
Further, the gas is a mixed gas of phosphine and argon.
Further, controlling the change in the flow rate of the gas based on the calculated resistivity of the single crystal comprises:
the flow rate of the gas is gradually increased along with the reduction of the resistivity of the single crystal, and the flow rate of the gas is increased by a flow rate change amount every time the resistivity of the single crystal is reduced by a resistivity change amount, so that the attenuation of the axial resistivity of the single crystal is controlled.
Furthermore, the resistivity variation is 0-1 omega cm/m, and the gas flow variation is 0-1L/min.
Further, the gas is mixed by argon and the first gas according to a certain flow ratio.
Further, the flow ratio of argon to the first gas is 2:1-10.
Further, the first gas is a mixed gas of argon and phosphine.
By adopting the technical scheme, in the crystal pulling process procedure of the czochralski single crystal, the condition that the doping gas starts to dope is set, meanwhile, an automatic ventilation system is additionally arranged in the crystal pulling equipment of the single crystal furnace, and when the set condition is met in the process of czochralski single crystal pulling, the control system controls the automatic ventilation system to act, and the doping gas is introduced into the single crystal furnace; calculating the resistivity of the single crystal at different periods according to the contact voltage of the single crystal and the melt with different weights in the crucible, and automatically controlling the flow change of the introduced doping gas according to the change of the resistivity of the single crystal, so as to control the axial attenuation of the resistivity of the single crystal and slow the attenuation of the axial resistivity of the single crystal; the axial resistivity of the single crystal can be automatically controlled, the resistivity of the head is automatically measured and calculated, and the axial attenuation of the resistivity of the single crystal is automatically controlled according to the resistivity of the head; the resistivity of the single crystal is controlled according to the axial attenuation law of the resistivity of the single crystal, and the distribution range of the resistivity of the single crystal can be customized according to requirements.
Drawings
Fig. 1 is a schematic diagram of an automatic ventilation system according to an embodiment of the present invention.
In the figure:
1. first flow rate detection device 2, first switch 3, and second switch
4. Second flow rate detection device 5, pressure regulation device 6 and proportioning device
7. Single crystal furnace
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
The embodiment of the invention relates to a method for automatically controlling the resistivity of single crystal silicon, which is used for carrying out phosphorus gas phase doping on gallium-doped single crystal in the drawing process, inhibiting the attenuation of the resistivity of the single crystal, controlling the axial resistivity of the single crystal, realizing the automatic control of the axial resistivity of the single crystal, automatically measuring and calculating the resistivity of a head in the drawing process of the single crystal, controlling the introduction flow of doping gas according to the resistivity of the head, automatically controlling the axial attenuation of the resistivity, and having the advantages of easy development of an automatic ventilation system, low investment cost, customized axial distribution range of the resistivity of the single crystal, no manual intervention of personnel in the crystal drawing process, automatic control in the whole process and high automation degree.
A method for automatically controlling the resistivity of monocrystalline silicon, gas doping is carried out in the process of pulling monocrystalline silicon, particularly, phosphorus element doping is carried out in the process of pulling gallium-doped monocrystalline silicon, the segregation speed of gallium element is controlled, the attenuation of the axial resistivity of monocrystalline silicon is controlled, and the distribution range of the axial resistivity of monocrystalline silicon is controlled, specifically, the method for automatically controlling the resistivity of monocrystalline silicon comprises the following steps:
setting a gas doping opening node and gas flow: presetting a single crystal pulling process in a control system for pulling the single crystal, pulling the single crystal according to the pulling process, setting a doping gas doping starting node in the single crystal pulling process, controlling the starting time of doping gas doping in the crystal pulling process, controlling the gas flow when the doping gas starts to dope, and starting doping gas doping; the gas doping opening node is a single crystal pulling stage or a shoulder expanding stage or an equal diameter stage, is selected according to actual requirements, and does not make specific requirements; the gas flow is 0-1L/min, and the gas flow can be 0.1L/min, 0.3L/min, 0.5L/min, 0.7L/min, 0.9L/min or 1L/min, and is selected according to actual requirements, and no specific requirement is made here.
Carrying out single crystal pulling: pulling the single crystal according to a crystal pulling process preset by a control system, presetting a doping opening node and gas flow of doping gas in the crystal pulling process, and judging conditions in the crystal pulling process to determine whether doping gas is introduced or not;
in the process of pulling the single crystal, obtaining the contact voltage of the melt in the crucible, and automatically calculating the resistivity of the single crystal according to the contact voltage: during the process of pulling the single crystal, the weight of a melt in a crucible is continuously reduced, different voltage changes can occur when the single crystal is contacted with melts with different weights, a control system measures different voltages, the resistivity of the single crystal at different periods is calculated according to the measured different voltages, and the control system measures the resistivity of the single crystal at each period in the process of pulling the single crystal at any time, so that the resistivity of the single crystal can be detected at any time;
judging the process of pulling the single crystal, controlling gas to be input into the single crystal furnace for doping if the set gas doping starting node condition is met, and controlling the axial resistivity of the single crystal according to the calculated resistivity of the single crystal and the flow change of the gas. Controlling the change in the flow rate of the gas based on the calculated resistivity of the single crystal comprises:
the flow rate of the gas is gradually increased with the decrease of the resistivity of the single crystal, the resistivity of the single crystal is decreased by a resistivity variation amount, the flow rate of the gas is increased by a flow rate variation amount, and the attenuation of the resistivity of the single crystal in the axial direction is controlled, the resistivity variation amount is 0 to 1 Ω · cm/m, and the resistivity variation amount may be 0.05 Ω · cm/m, 0.1 Ω · cm/m, 0.15 Ω · cm/m, 0.2 Ω · cm/m, 0.25 Ω · cm/m, 0.3 Ω · cm/m, 0.35 Ω · cm/m, 0.4 Ω · cm/m, 0.45 Ω · cm/m, 0.5 Ω · cm/m, 0.55 Ω · cm/m, 0.6 Ω · cm/m, 0.65 Ω · cm/m, 0.7 Ω · cm/m, 0.75 Ω · cm/m, 0.8 Ω · cm/m, 0.85 · cm/m, 0.9 · cm/m, 0.95 Ω · cm/m, or 1.95 Ω · cm/m, and the specific requirements are not specifically selected herein; the flow rate of the gas is varied by 0-1L/min, and the flow rate of the gas can be varied by 0.01L/min, 0.02L/min, 0.03L/min, 0.04L/min, 0.06L/min, 0.08L/min, 0.1L/min, 0.15L/min, 0.2L/min, 0.25L/min, 0.3L/min, 0.35L/min, 0.4L/min, 0.45L/min, 0.5L/min, 0.55L/min, 0.6L/min, 0.65L/min, 0.7L/min, 0.75L/min, 0.8L/min, 0.85L/min, 0.9L/min, 0.95L/min or 1L/min, and the gas is selected according to actual needs, and is not specifically required.
The gas is a mixed gas of phosphine and argon, the concentration of the gas is 1000-10000ppm, and the concentration of the gas can be 1000ppm, 2000ppm, 3000ppm, 4000ppm, 5000ppm, 6000ppm, 7000ppm, 8000ppm, 9000ppm or 10000ppm, and the gas is selected according to actual requirements and is not specifically required here.
In order to realize the automatic gas phase doping of the phosphorus element in the Czochralski single crystal process, an automatic ventilation system is added in the Czochralski single crystal system, so that the mixed gas containing the phosphorus element acts according to a preset program under the action of the automatic ventilation system, the introduction time and the introduction time of the mixed gas containing the phosphorus element are controlled, and the automatic gas phase doping is carried out on the Czochralski single crystal.
Specifically, as shown in fig. 1, the automatic ventilation system includes a first gas path, a second gas path and a proportioning device 6, wherein the first gas path and the second gas path are respectively communicated with the proportioning device 6, the first gas path is used for controlling the introduction of argon gas, and the second gas path is used for introducing first gas; one end of the first gas path is connected with the proportioning device 6, the other end of the first gas path is connected with the argon storage device, so that the argon storage device flows out of the argon storage device under the action of the first gas path and enters the proportioning device 6, one end of the second gas path is connected with the proportioning device 6, and the other end of the second gas path is connected with the first gas storage device, so that the first gas flows out of the first gas storage device under the action of the second gas path and enters the proportioning device 6; the arrangement of the first gas path and the second gas path can realize the directional flow of argon and the first gas, can realize the continuous input of the argon and the first gas into the single crystal furnace 7, and inputs the doping gas while inputting the protective gas in the crystal pulling process to carry out gas phase doping on the single crystal.
The proportioning device 6 is used for proportioning the flow of argon gas and the flow of first gas, and the end of giving vent to anger of proportioning device 6 communicates with single crystal growing furnace 7, lets in the gas after the ratio single crystal growing furnace 7 in, and the argon gas that flows out in the first gas circuit mixes with the first gas that flows out in the second gas circuit carries out the ratio in proportioning device 6 to in importing the gas after mixing single crystal growing furnace 7, carry out doping gas and protective gas's continuous input. Here, the mixed gas formed by mixing the argon gas and the first gas in proportion by the proportioning device 6 is the doping gas. When the proportioning device 6 mixes and proportiones the argon and the first gas, the ratio of the flow of the argon to the flow of the first gas is 2:1-10, the ratio of the flow of the argon to the flow of the first gas can be 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, 8:1, 9:1 or 10, and the ratio is selected according to actual needs, and is not specifically required here.
Specifically, the first gas circuit comprises a first pipeline, a first switch 2 and a first flow detection device 1, the first switch 2 and the first flow detection device 1 are arranged on the first pipeline to control the opening and closing of the first gas circuit and the gas flow, the arrangement of the first pipeline is convenient for guiding the flow of argon, so that the argon flows along the direction of the first pipeline and enters the proportioning device 6, and the first pipeline is a connecting pipeline, is a low-temperature-resistant and high-pressure-resistant connecting pipeline and can convey the argon; the first switch 2 is arranged to control the opening and closing of the first gas path, when the first switch 2 is opened, argon can flow out from the storage device of the argon along the first pipeline and flow into the proportioning device 6, when the first switch 2 is closed, the argon can flow out from the storage device of the argon, the argon cannot flow along the first pipeline and flow into the proportioning device 6, the first pipeline is in a closed state, the first switch 2 can be a stop valve, an electromagnetic valve or other valves capable of opening and closing pipelines, and selection is performed according to actual requirements, wherein specific requirements are not made.
The first flow detecting device 1 is used for detecting the flow rate of the argon gas in the first pipeline, and the first flow detecting device 1 is a flow meter, preferably, in this embodiment, the first flow detecting device 1 is a mass flow meter, and is a commercially available product, and is selected according to actual requirements, which is not specifically required here.
In the present embodiment, it is preferable that the first switch 2 and the first flow rate detection device 1 are provided in this order along the flow direction of the argon gas.
The second gas circuit comprises a second pipeline, a pressure adjusting device 5, a second switch 3 and a second flow detecting device 4, the pressure adjusting device 5, the second switch 3 and the second flow detecting device 4 are arranged on the second pipeline, the pressure, the flow, the opening and the closing of the second gas circuit are controlled, the second pipeline is arranged, first gas can flow out of the first gas storage device and flows along the direction of the second pipeline, the first gas flows into the proportioning device 6, the flow of the first gas is guided, the second pipeline is a connecting pipeline and is a low-temperature-resistant and high-pressure-resistant pipeline, and the selection is carried out according to actual requirements, and no specific requirements are made here.
The second switch 3 is configured to control opening and closing of the second air path, when the second switch 3 is opened, the first gas can flow out from the storage device of the first gas along the second pipeline and flow into the proportioning device 6, when the second switch 3 is closed, the first gas can flow out from the storage device of the first gas, the first gas cannot flow along the second pipeline and flow into the proportioning device 6, at this time, the second pipeline is in a closed state, the second switch 3 may be a stop valve, or a solenoid valve, or another valve capable of opening and closing the pipeline, and is selected according to actual needs, where no specific requirements are made.
The second flow rate detecting device 4 is used for detecting the flow rate of the first gas in the second pipeline, the second flow rate detecting device 4 is a flow meter, preferably, in this embodiment, the second flow rate detecting device 4 is a mass flow meter, and is a commercially available product, and is selected according to actual requirements, which is not specifically required here.
The pressure regulating device 5 is used for regulating the pressure of the first gas flowing out of the first gas storage device, in this embodiment, the pressure of the first gas in the first gas storage device is large, and the first gas flowing out of the device needs to be decompressed, so that the pressure of the first gas in the second pipeline is less than 0.5MPa, therefore, the pressure regulating device 5 is preferably a pressure reducing valve, and the first gas flowing out of the first gas storage device is decompressed, so that the decompressed first gas flows along the second pipeline, the pressure reducing valve is a commercially available product, and is selected according to actual needs, and no specific requirement is made here.
The first gas is a mixed gas of phosphine and argon.
In the present embodiment, it is preferable that the pressure adjusting device 5, the second flow rate detecting device 4, and the second switch 3 are provided in this order along the flow direction of the first gas.
When the automatic ventilation system is used, the first flow detection device 1, the first switch 2, the second switch 3, the second flow detection device 4 and the pressure regulation device 5 are all connected with a control system of a single crystal furnace, single crystal is drawn according to a drawing process of the single crystal, the control system controls the first switch 2 to act, the first gas circuit is opened, argon is continuously introduced into the single crystal furnace in the drawing process of the single crystal, the argon is used as protective gas, and impurities are removed in the crystal pulling process; when doping gas needs to be introduced, the control system controls the pressure adjusting device 5 and the second switch 3 to act, so that first gas containing phosphine and argon is introduced, the flow of the argon in the first gas path and the flow of the first gas in the second gas path are respectively measured through the first flow detection device 1 and the second flow detection device 4, the control system controls the first switch 2 and the second switch 3 to act according to the detection results of the first flow detection device 1 and the second flow detection device 4, and controls the flow of the argon and the flow of the first gas, so that the argon and the first gas are proportioned in the proportioning device 6 according to the required flow, the proportioned gas flows out of the proportioning device 6 and enters the single crystal furnace for meteorological doping, and meanwhile, the flow of protective gas argon is also kept introduced, so that the smooth drawing of the single crystal is ensured; after the first gas flows out of the first gas storage device, the pressure of the first gas is reduced under the action of the pressure regulating device 5, the pressure of the first gas is reduced, and the reduced first gas flows in the second gas path; the control system controls the flow of the dopant gas in accordance with a single crystal pulling process such that the flow of the dopant gas increases with a decay in the resistivity of the single crystal during the pulling of the single crystal, and controls the decay in the axial resistivity of the single crystal.
The following is a description of a specific example.
In the Czochralski single crystal pulling process, a crystal pulling process program is preset and edited in a control system, and a gas doping opening node and gas flow are set in the program, in the embodiment, doping gas is introduced when the doping gas doping opening node enters a constant diameter stage, and the flow of the doping gas is 0.6L/min when the doping gas starts to be introduced;
pulling a single crystal according to a crystal pulling process procedure, wherein the control system controls a first air path of an automatic ventilation system to keep a ventilation state, and continuously introduces protective gas argon into the single crystal furnace to take away impurities generated in the process of pulling the single crystal; when the Czochralski single crystal enters an equal-diameter stage, the control system judges that the preset doping gas starting node and flow conditions are met, the control system controls the automatic ventilation action, the second gas path keeps the ventilation state, the mixed gas of phosphine and argon is continuously introduced into the single crystal furnace, and the Czochralski single crystal is doped with phosphorus;
in the process of introducing the phosphine and argon mixed gas, the axial resistivity of the single crystal is gradually attenuated along with the increase of the length of the single crystal, the flow of the phosphine and argon mixed gas is controlled to be gradually increased according to the attenuation rule of the axial resistivity of the single crystal, the attenuation speed of the axial resistivity of the single crystal is inhibited, and particularly,
measuring the contact voltage between the single crystal and the melt in the crucible, and calculating the resistivity of the single crystal according to the relation between the contact voltage and the resistivity of the single crystal, wherein,
when the axial resistivity of the single crystal is 0.8 omega cm/m, the flow of the mixed gas of phosphine and argon is 0.12L/min;
when the axial resistivity of the single crystal is reduced to 0.7 omega cm/m, the flow of the mixed gas of phosphine and argon is increased to 0.16L/min;
when the axial resistivity of the single crystal is reduced to 0.65 Ω · cm/m, the flow rate of the mixed gas of phosphine and argon is increased to 0.20L/min;
when the axial resistivity of the single crystal is reduced to 0.6 omega cm/m, the flow of the mixed gas of phosphine and argon is increased to 0.24L/min;
when the axial resistivity of the single crystal was reduced to 0.54. Omega. Cm/m, the flow rate of the mixed gas of phosphine and argon was increased to 0.28L/min;
when the axial resistivity of the single crystal is reduced to 0.5 omega cm/m, the flow of the mixed gas of phosphine and argon is increased to 0.32L/min;
when the axial resistivity of the single crystal was reduced to 0.43. Omega. Cm/m, the flow rate of the mixed gas of phosphine and argon was increased to 0.36L/min;
when the axial resistivity of the single crystal is reduced to 0.4 omega cm/m, the flow of the mixed gas of phosphine and argon is increased to 0.40L/min;
after the equal diameter stage is finished, continuously introducing mixed gas of phosphine and argon, wherein the flow of the mixed gas is the mixed flow at the end of the equal diameter stage, the flow is maintained to be introduced until the end of the ending stage, and the introduction of the mixed gas of phosphine and argon is finished;
the pulling of the single crystal continues until the pulling of the single crystal is completed.
The change in the flow rate of the mixed gas of phosphine and argon and the axial resistivity of the single crystal were analyzed as shown in the following table:
analyzing the data to know that in the process of pulling the gallium-doped single crystal, mixed gas containing phosphorus elements is introduced into the single crystal furnace as doping gas, and the resistivity of the single crystal is calculated according to the contact voltage of the single crystal and melts with different weights in the crucible, so that the attenuation law of the axial resistivity of the single crystal is known; in a Czochralski single crystal pulling system of a single crystal furnace, an automatic doping gas introducing system is added, the node and the flow rate of the doping gas which is introduced are set in the crystal pulling process, when the starting condition is met, the automatic introducing system is controlled to control the automatic introduction of the doping gas, the flow rate of the doping gas is controlled, the doping gas is automatically doped, the attenuation speed of the axial resistivity of the single crystal is inhibited, and compared with the existing doping without the doping gas, the attenuation speed of the axial resistivity of the single crystal is slowed down and effectively controlled.
By adopting the technical scheme, in the crystal pulling process procedure of the czochralski single crystal, the condition that the doping gas starts to dope is set, meanwhile, an automatic ventilation system is additionally arranged in the crystal pulling equipment of the single crystal furnace, and when the set condition is met in the process of czochralski single crystal pulling, the control system controls the automatic ventilation system to act, and the doping gas is introduced into the single crystal furnace; calculating the resistivity of the single crystal at different periods according to the contact voltage of the single crystal and the melt with different weights in the crucible, and automatically controlling the flow change of the introduced doping gas according to the change of the resistivity of the single crystal, so as to control the axial attenuation of the resistivity of the single crystal and slow the attenuation of the axial resistivity of the single crystal; the axial resistivity of the single crystal can be automatically controlled, the head resistivity is automatically measured and calculated, and the axial attenuation of the single crystal resistivity is automatically controlled according to the head resistivity; the automatic ventilation system has simple structure, is easy to develop, does not modify the structure of crystal pulling equipment of the single crystal furnace, and has low input cost; the resistivity of the single crystal is controlled according to the axial attenuation law of the resistivity of the single crystal, and the distribution range of the resistivity of the single crystal can be customized according to requirements.
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 (10)
1. A method for automatically controlling the resistivity of monocrystalline silicon is characterized in that: gas doping is carried out in a Czochralski single crystal process, comprising:
setting a gas doping opening node and gas flow;
performing single crystal pulling, acquiring the contact voltage of a melt in a crucible in the single crystal pulling process, and automatically calculating the resistivity of the single crystal according to the contact voltage;
judging the single crystal pulling process, and controlling gas to be input into the single crystal furnace for doping if the set gas doping starting node condition is met; meanwhile, controlling the flow change of the gas according to the calculated single crystal resistivity, and controlling the single crystal axial resistivity;
otherwise, no gas is fed into the single crystal furnace.
2. A method of automatically controlling resistivity of single crystal silicon as claimed in claim 1 wherein: the gas doping opening node is a stage of pulling the single crystal to enter a shoulder expanding stage or an equal diameter stage.
3. A method of automatically controlling resistivity of single crystal silicon as claimed in claim 2 wherein: the gas flow is 0-1L/min.
4. A method of automatically controlling the resistivity of single crystal silicon as claimed in claim 1, wherein: the gas is a mixed gas of phosphine and argon.
5. A method of automatically controlling the resistivity of single crystal silicon as claimed in any one of claims 1 to 4 wherein: the controlling the flow rate variation of the gas according to the calculated resistivity of the single crystal comprises:
the flow rate of the gas is gradually increased along with the decrease of the resistivity of the single crystal, and the flow rate of the gas is increased by a flow rate change amount every time the resistivity of the single crystal is decreased by a resistivity change amount so as to control the attenuation of the axial resistivity of the single crystal.
6. A method of automatically controlling resistivity of single crystal silicon as claimed in claim 5 wherein: the resistivity variation is 0-1 omega cm/m, and the flow variation of the gas is 0-1L/min.
7. A method of automatically controlling the resistivity of single crystal silicon as claimed in any one of claims 1 to 4 and 6 wherein: the concentration of the gas is 1000-10000ppm.
8. A method of automatically controlling resistivity of single crystal silicon as claimed in claim 1 wherein: the gas is mixed by argon and a first gas according to a certain flow ratio.
9. A method of automatically controlling resistivity of single crystal silicon as claimed in claim 8 wherein: the flow ratio of the argon gas to the first gas is 2:1-10.
10. The method of automatically controlling resistivity of single crystal silicon as claimed in claim 8 or 9, wherein: the first gas is a mixed gas of argon and phosphine.
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