CN116200806B - Furnace stopping method for producing monocrystalline silicon and monocrystalline furnace - Google Patents
Furnace stopping method for producing monocrystalline silicon and monocrystalline furnace Download PDFInfo
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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
-
- 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
- C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
- C30B15/26—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal using television detectors; using photo or X-ray detectors
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention belongs to the technical field of monocrystalline silicon production, and particularly relates to a furnace stopping method for producing monocrystalline silicon and a monocrystalline furnace, wherein the method comprises the following steps: when the liquid level temperature of the silicon melt is higher than 950-1050 ℃, monitoring the liquid level temperature by adopting a CCD camera; when the liquid level temperature is not higher than 950-1050 ℃, monitoring the temperatures of the surface of the silicon crystal bar and a heating area of a heater in the single crystal furnace by adopting a wide-angle infrared temperature measuring unit, and introducing argon into the single crystal furnace for cooling; the cooling conditions included: the silicon crystal bar and the crucible are respectively rotated; when the temperature of the surface of the silicon crystal bar is reduced to 950-1050 ℃, the silicon crystal bar is lifted for the first time and lifted for the second time, and the crucible is moved downwards; when the temperature of the surface of the silicon crystal bar is reduced to 880-920 ℃, the heat shield is moved upwards, and the crucible is moved downwards; when the temperature of the surface of the silicon crystal bar is reduced to 440-460 ℃, taking out the silicon crystal bar; and when the temperature of the heating area of the heater is reduced to 310-330 ℃, disassembling and/or loading the furnace. The method can improve the production efficiency, avoid accidents, improve the quality of the crystal bar and avoid the ageing of the thermal field component.
Description
Technical Field
The invention belongs to the technical field of monocrystalline silicon production, and particularly relates to a furnace stopping method for producing monocrystalline silicon and a monocrystalline furnace.
Background
Monocrystalline silicon is an important material for preparing solar cells in the photovoltaic industry, monocrystalline silicon is usually produced by adopting a monocrystalline furnace, and after the production of the monocrystalline furnace is finished, in order to avoid the influence on the service life of thermal field components due to the fact that the ageing speed of the thermal field components is increased due to local oxidation of the thermal field components caused by high temperature, the thermal field of the monocrystalline furnace needs to be sufficiently cooled, then the working such as cleaning and furnace restarting can be performed, and at present, the thermal field of the monocrystalline furnace is generally cooled through natural cooling for a fixed period of time. CN109056055B relates to a production method of a single crystal silicon rod, and relates to a furnace stopping operation, in which the crystal rotation of a single crystal furnace is reduced to 5 rotations at a rate of 1 rotation per 3 seconds, the pot rotation of the single crystal furnace is reduced to 0 rotations, the pot position of the single crystal furnace is lowered by 30mm, the pulling rate of the crystal is manually set to 1.5mm/min and kept for 1.5 hours, the argon flow of the single crystal furnace is 60slpm, the opening of a throttle valve of the single crystal furnace is set to 100% for cooling, and the furnace is disassembled after cooling for 6 hours. The fixed cooling time is adopted without considering the influences of the model of the furnace table of the single crystal furnace, the drawing environment, the size of the thermal field and the abnormal conditions in the drawing process of the single crystal furnace on the cooling effect of the thermal field.
However, in the actual operation process, the cooling effect of the thermal field of the single crystal furnace is affected due to the abnormal conditions of the type of the furnace table of the single crystal furnace, the drawing environment, the thermal field size and the drawing process of the single crystal furnace, the thermal field is easy to appear, after the cooling treatment with the same cooling time length is adopted, the temperature of a part of the furnace table is lower, and the temperature of a part of the furnace table is higher, when the temperature of the furnace table is lower, the production efficiency is seriously affected due to overlong cooling time, when the temperature of the furnace table is higher, serious accidents such as cracking of a crystal bar when the crystal bar is subjected to cooling, breakage of a head seed crystal and the like are easy to appear, dislocation at the tail part of the crystal bar is increased, and the thermal field component is partially oxidized due to high temperature so as to accelerate ageing. In addition, before the furnace disassembly, whether the furnace disassembly is carried out in a delayed manner is determined by subjectively observing whether the thermal field in the single crystal furnace is reddened or not by a furnace disassembly person, so that the subjective factors are large, accidents are easy to occur, the quality of the crystal bar is influenced, and the ageing of the thermal field component is accelerated.
Disclosure of Invention
The invention aims to overcome the defects of low production efficiency, easy occurrence of serious accidents such as rapid cracking of a crystal bar when encountering cold, breakage of a head seed crystal, and the like in the prior art, increase of dislocation at the tail of the crystal bar, and accelerated aging of a thermal field component due to local oxidation of the thermal field component caused by high temperature, and provides a furnace shutdown method, a single crystal furnace, electronic equipment and a computer readable storage medium for producing single crystal silicon.
In order to achieve the above object, in a first aspect, the present invention provides a furnace shutdown method for producing single crystal silicon, the method comprising:
when the liquid level temperature of the silicon melt in the single crystal furnace is higher than 950-1050 ℃, monitoring the liquid level temperature by adopting a CCD camera; when the liquid level temperature is not higher than 950-1050 ℃, monitoring the temperatures of the surface of the silicon crystal bar and a heating area of a heater in the single crystal furnace by adopting a wide-angle infrared temperature measuring unit, and introducing argon into the single crystal furnace to cool the silicon crystal bar, the crucible and the heater;
wherein the conditions of the cooling treatment include: the silicon crystal bar rotates at a first preset speed, and the crucible containing silicon melt rotates at a second preset speed; when the temperature of the surface of the silicon crystal bar is reduced to 950-1050 ℃, sequentially carrying out first lifting treatment and second lifting treatment on the silicon crystal bar, and simultaneously downwards moving the position of the crucible; the lifting speed of the first lifting treatment is smaller than that of the second lifting treatment, the tail of the silicon crystal bar is lifted to a first preset position by the first lifting treatment, the vertical distance between the first preset position and the lowest end of a heat shield in the single crystal furnace is 55 mm-65 mm, and the vertical distance between the second preset position and the first preset position is 160 mm-200 mm by the second lifting treatment; when the temperature of the surface of the silicon crystal bar is reduced to 880-920 ℃, the position of the heat shield is moved upwards, the position of the crucible is moved downwards, and the heating area of the heater is exposed; when the temperature of the surface of the silicon crystal bar is reduced to 440-460 ℃, taking out the silicon crystal bar from the single crystal furnace; and when the temperature of the heating area of the heater is reduced to 310-330 ℃, disassembling and/or assembling the furnace.
In some preferred embodiments, the flow rate of the argon is 90L/min-110L/min; and/or the first preset speed and the second preset speed are 2 r/min-5 r/min.
In some preferred embodiments, the first lifting process has a lifting rate of 110mm/h to 130mm/h and the second lifting process has a lifting rate of 320mm/h to 400mm/h; and/or when the temperature of the surface of the silicon crystal bar is reduced to 950-1050 ℃, the position of the crucible is moved down by 90-110 mm.
In some preferred embodiments, when the temperature of the surface of the silicon crystal rod is reduced to 880-920 ℃, the position of the heat shield is moved up to the upper limit position of the heat shield, and the position of the crucible is moved down to the lower limit position of the crucible.
In some preferred embodiments, the conditions of the cooling process further comprise: and stopping introducing argon into the single crystal furnace and detecting air leakage when the temperature of the surface of the silicon crystal bar is reduced to 680-720 ℃.
More preferably, when the temperature of the surface of the silicon crystal rod is reduced to 440-460 ℃, the tail of the silicon crystal rod is lifted to the upper part of a secondary chamber isolation valve of the single crystal furnace, the secondary chamber isolation valve is opened to isolate a main chamber of the single crystal furnace from a secondary chamber of the single crystal furnace, argon is continuously introduced into the secondary chamber until the pressure in the secondary chamber reaches the atmospheric pressure, and then the silicon crystal rod is taken out from the secondary chamber.
More preferably, after the silicon crystal bar is taken out, argon is continuously introduced into a main chamber of the single crystal furnace until the pressure in the main chamber reaches 200 torr~400 torr, and then the pressure is maintained; and continuously introducing argon into the main chamber when the temperature of the heating area of the heater is reduced to 310-330 ℃, and carrying out furnace disassembly and/or furnace loading after the pressure in the main chamber reaches atmospheric pressure.
In a second aspect, the present invention provides a single crystal furnace adopting the furnace shutdown method of the first aspect, the single crystal furnace comprising: the device comprises a crucible, a heater, a heat shield, a CCD camera, a wide-angle infrared temperature measuring unit, an argon gas supply unit, a crystal bar lifting unit and a control unit;
the heater is arranged on the outer side of the crucible in a surrounding mode, the heat shield is arranged above the crucible, and the CCD camera and the wide-angle infrared temperature measuring unit are arranged on a furnace cover of the single crystal furnace;
the control unit is respectively connected with the CCD camera, the wide-angle infrared temperature measuring unit, the argon gas supply unit, the crystal bar lifting unit, the crucible and the heat shield and is used for controlling the actions of the CCD camera and the wide-angle infrared temperature measuring unit, controlling the feeding of argon gas and controlling the positions of the silicon crystal bar, the crucible and the heat shield.
In a third aspect, the present invention provides an electronic device, comprising: a processor, a memory storing machine-readable instructions executable by the processor, which when executed by the processor perform the steps of the method of the first aspect when the electronic device is running.
In a fourth aspect, the present invention provides a computer-readable storage medium having stored thereon a computer program which, when executed by a processor, performs the steps of the method of the first aspect.
According to the invention, when the liquid level temperature of the silicon melt is not higher than 950-1050 ℃, the silicon crystal rod, the crucible and the heater start to be cooled, before the silicon crystal rod is taken out, when the temperature of the surface of the silicon crystal rod is reduced to 950-1050 ℃, the lower lifting speed is adopted, and then the larger lifting speed is adopted to lift the crystal rod, so that the position of the crucible is moved downwards, when the temperature of the surface of the silicon crystal rod is reduced to 880-920 ℃, the position of the heat shield is moved upwards, the position of the crucible is moved downwards, the cooling time can be reduced, the production efficiency is improved, accidents such as explosion and rod dropping of the crystal rod are reduced, the quality of the crystal rod is improved, and the ageing of a thermal field component is inhibited.
When the liquid level temperature of the silicon melt is not higher than 950-1050 ℃, the silicon crystal rod and the heater start to be cooled, and compared with the temperature Wen Tinglu higher than 950-1050 ℃, the operation such as crystal rod rotation, crystal rod lifting, crucible rotation, crucible position descending and the like is performed at a lower temperature, so that the accident of rod frying caused by too fast cooling of the crystal rod can be avoided. When the temperature fluctuation is large in the initial stage of furnace shutdown and the surface temperature of the crystal bar is too fast to reduce, the risk of bar frying accidents is increased, and the cooling operation is controlled according to the temperature of the silicon crystal bar, so that the risk of accidents such as bar frying and the like can be reduced to the greatest extent. When the temperature of the surface of the silicon crystal bar is reduced to 950-1050 ℃, the crystal bar is lifted by adopting a small lifting speed in the first stage, the accidents such as bar frying and the like caused by the fact that the tail temperature of the crystal bar is rapidly reduced and the cooling speed is too high can be prevented, the crystal bar is lifted by adopting a large lifting speed in the second stage, the lifting speed of the crystal bar can be improved, the cooling of the crystal bar is accelerated, the problems that the temperature of a crucible and a heater in a furnace is reduced slowly due to the fact that the stay time of the crystal bar is long and the heat is radiated to the lower part can be controlled, and the shutdown time can be further reduced. When the temperature of the surface of the silicon crystal bar is reduced to 950-1050 ℃, the position of the crucible is moved downwards, the distance between the crystal bar and the crucible can be enlarged, the radiation heating of the crucible to the crystal bar is reduced, in addition, the two high-temperature radiating parts are separated by enlarging the distance between the crystal bar and the crucible, the heat field space of the two parts is enlarged, the uniformity of an internal heat field can be improved, the temperature of the heat field is reduced, the cooling time is shortened, and the furnace shutdown time is shortened. When the temperature of the surface of the silicon crystal bar is reduced to 880-920 ℃, the position of the heat shield is moved upwards, the position of the crucible is moved downwards, the high-temperature heating area of the heater is exposed, namely, the high-temperature heating area of the heater is not shielded by the crucible and the heat shield, heat dissipation of the high-temperature area can be promoted pertinently, the cooling efficiency is improved, the furnace shutdown time is shortened, the heat shield is lifted and the crucible is lowered at a temperature higher than 880-920 ℃, the excessive cooling of the heating body is caused, the defects of temperature change, damage and the like of the heating body occur, the service life is reduced, the heat shield is lifted and the crucible is lowered at a temperature lower than 880-920 ℃, and the effect on reducing the furnace shutdown time is not obvious.
According to the single crystal furnace provided by the invention, the CCD camera and the wide-angle infrared temperature measuring unit are arranged on the furnace cover of the single crystal furnace, so that the temperature of the liquid level of the silicon melt is monitored by the CCD camera during crystal pulling, the smooth crystal pulling process is ensured, and further, the control unit is respectively connected with the CCD camera, the wide-angle infrared temperature measuring unit, the argon supply unit, the crystal bar lifting unit, the crucible and the heat shield by arranging the argon supply unit, the crystal bar lifting unit and the control unit, and the temperature monitoring results of the wide-angle infrared temperature measuring unit on the surface of the silicon crystal bar and the heating area of the heater can be realized during furnace shutdown, and the positions of the silicon crystal bar, the crucible and the heat shield are controlled, so that the furnace shutdown cooling time is shortened, the production efficiency is improved, accidents such as crystal bar explosion and bar dropping are reduced, the quality of the crystal bar is improved, and the ageing of a thermal field component is inhibited.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural view of an embodiment of a single crystal furnace according to the present invention.
Fig. 2 is a block schematic diagram of an electronic device according to an embodiment of the present invention.
Description of the reference numerals
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The inventor of the invention researches and discovers that when the single crystal furnace is shut down and cooled for a fixed period of time, the influence of pulling environment and the like is adopted, and the conditions of higher or lower furnace table temperature after cooling treatment are easy to occur, so that the production efficiency is reduced, dislocation at the tail part of the crystal rod is increased, the thermal field part is aged rapidly, and even accidents such as cracking of the crystal rod when the crystal rod is cooled, and breakage of the head seed crystal occur.
In this regard, in a first aspect, the present invention provides a furnace shutdown method for producing single crystal silicon, the method comprising:
When the liquid level temperature of the silicon melt in the single crystal furnace is higher than 950-1050 ℃, monitoring the liquid level temperature by adopting a CCD camera; when the liquid level temperature is not higher than 950-1050 ℃, monitoring the temperatures of the surface of the silicon crystal bar and a heating area of a heater in the single crystal furnace by adopting a wide-angle infrared temperature measuring unit, and introducing argon into the single crystal furnace to cool the silicon crystal bar, the crucible and the heater;
wherein the conditions of the cooling treatment include: the silicon crystal bar rotates at a first preset speed, and the crucible containing silicon melt rotates at a second preset speed; when the temperature of the surface of the silicon crystal bar is reduced to 950-1050 ℃, sequentially carrying out first lifting treatment and second lifting treatment on the silicon crystal bar, and simultaneously downwards moving the position of the crucible; the lifting speed of the first lifting treatment is smaller than that of the second lifting treatment, the tail of the silicon crystal bar is lifted to a first preset position by the first lifting treatment, the vertical distance between the first preset position and the lowest end of a heat shield in the single crystal furnace is 55 mm-65 mm, and the vertical distance between the second preset position and the first preset position is 160 mm-200 mm by the second lifting treatment; when the temperature of the surface of the silicon crystal bar is reduced to 880-920 ℃, the position of the heat shield is moved upwards, the position of the crucible is moved downwards, and the heating area of the heater is exposed; when the temperature of the surface of the silicon crystal bar is reduced to 440-460 ℃, taking out the silicon crystal bar from the single crystal furnace; and when the temperature of the heating area of the heater is reduced to 310-330 ℃, disassembling and/or assembling the furnace.
According to the invention, when the liquid level temperature of the silicon melt in the single crystal furnace is not higher than 950-1050 ℃, argon is introduced into the single crystal furnace under the premise that the silicon crystal rod rotates at a first preset speed and the crucible containing the silicon melt rotates at a second preset speed, so that the silicon crystal rod, the crucible and the heater are cooled, the silicon crystal rod and the crucible are enabled to rotate respectively, the rotation and the heat dissipation of the silicon crystal rod and the crucible are facilitated, the heat dissipation is more uniform, the heat dissipation can be realized in a flowing argon mode, the heat dissipation can be promoted, the oxide in the single crystal furnace can be driven, the silicon crystal rod, the crucible and the heater are enabled to be cooled when the liquid level temperature of the silicon melt is not higher than 950-1050 ℃, and compared with the temperature of higher Wen Tinglu of 950-1050 ℃, the operations such as crystal rod rotation, crystal rod lifting, crucible rotation, crucible position lowering and the like are carried out at lower temperatures, and the explosion accidents caused by the fact that the crystal rod is cooled too fast can be avoided.
According to the invention, when the liquid level temperature of the silicon melt is reduced to 950-1050 ℃, two-stage cooling treatment is performed according to the surface temperature of the silicon crystal bar, when the surface temperature of the silicon crystal bar is reduced to 950-1050 ℃, the first-stage cooling is performed, and when the surface temperature of the silicon crystal bar is reduced to 880-920 ℃, the second-stage cooling is performed. When the temperature fluctuation is large in the initial stage of furnace shutdown and the surface temperature of the crystal bar is too fast to reduce, the risk of bar frying accidents is increased, and the cooling operation is controlled according to the surface temperature of the silicon crystal bar, so that the risk of accidents such as bar frying and the like can be reduced to the greatest extent.
Specifically, when the surface temperature of the silicon crystal bar is reduced to 950-1050 ℃, the silicon crystal bar is sequentially subjected to first lifting treatment and second lifting treatment, the tail of the silicon crystal bar passes through a heat shield in a single crystal furnace by adopting a small lifting speed in the first lifting treatment, specifically, the tail of the silicon crystal bar is lifted to a first preset position, the vertical distance between the first preset position and the lowest end of the heat shield in the single crystal furnace is 55-65 mm, the tail of the silicon crystal bar is lifted to a second preset position by adopting a large lifting speed in the second lifting treatment, the vertical distance between the second preset position and the first preset position is 160-200 mm, the temperature is cooled and transited by adopting the first lifting treatment with the small lifting speed at a slow speed, the tail of the crystal bar is prevented from being exploded and cracked by the quick low temperature, the tail of the crystal bar is prevented from being damaged by the high distance of the heat shield in the single crystal furnace, the temperature of the crystal bar is prevented from being lifted to be lower than the lowest, the temperature of the crystal bar is further cooled down to the temperature of the crucible, the temperature is further reduced by the temperature of the heat shield, the temperature of the crystal bar is further reduced to be higher than the temperature of the crucible, and the temperature is further reduced to the temperature of the crucible is reduced, and the temperature is further reduced to the temperature of the heat loss is reduced to the heat of the crystal bar is reduced to the temperature of the crystal bar in the furnace, and the temperature is more stable; in addition, when the surface temperature of the silicon crystal rod is reduced to 950-1050 ℃, the position of the crucible is also moved downwards, the distance between the crystal rod and the crucible can be increased, the radiation heating of the crucible to the crystal rod is reduced, in addition, the two high-temperature radiating parts are separated by increasing the distance between the crystal rod and the crucible, the thermal field space of the two parts is enlarged, the uniformity of an internal thermal field can be improved, the temperature of the thermal field is reduced, the cooling time is shortened, and the furnace shutdown time is shortened. If the surface temperature of the silicon ingot is reduced to 950-1050 ℃, the effect of reducing the furnace shutdown time is not obvious by lifting the silicon ingot or moving the crucible downwards, and if the surface temperature of the silicon ingot is reduced to 950-1050 ℃, the situation of rod explosion accidents caused by too fast cooling of the ingot is likely to occur.
Specifically, when the surface temperature of the silicon crystal rod is reduced to 880-920 ℃, the position of the heat shield is moved upwards, the position of the crucible is moved downwards, the heating area of the heater is exposed, the high-temperature heating area of the heater is not shielded by the crucible and the heat shield, the heat dissipation of the high-temperature area can be promoted pertinently, the cooling efficiency is improved, the furnace stopping time is shortened, the heat shield is lifted and the crucible is lowered at the temperature higher than 880-920 ℃, the heating body is excessively cooled, the defects of temperature change damage and the like of the heating body occur, the service life is shortened, the heat shield is lifted and the crucible is lowered at the temperature lower than 880-920 ℃, and the effect of reducing the furnace stopping time is not obvious.
According to the invention, the temperature of different areas can be monitored by using the wide-angle infrared temperature measuring unit, the temperature of the surface of the silicon crystal bar is cooled from 950-1050 ℃ to 440-460 ℃, namely, before the bar is taken out, the wide-angle infrared temperature measuring unit is used for monitoring the temperature of the surface of the silicon crystal bar, after the bar is taken out, the wide-angle infrared temperature measuring unit is used for monitoring the temperature of a heating area of a heater, when the temperature of the heating area of the heater is reduced to 310-330 ℃, the furnace disassembly operation is carried out, the wide-angle infrared temperature measuring unit can be well suitable for the furnace shutdown process of the single crystal furnace, the detection accuracy is high, accidents are avoided while the production efficiency is improved in the furnace shutdown process, the quality of the crystal bar is improved, and the ageing of a thermal field component is avoided.
In the invention, when the temperature of the surface of the silicon crystal bar is reduced to 440-460 ℃, the silicon crystal bar is taken out from the single crystal furnace, and if the temperature of the taken bar is higher than 440-460 ℃, the risk of bar dropping, bar frying or tail dislocation of the crystal bar is increased. When the temperature of the heating area of the heater is reduced to 310-330 ℃, furnace disassembly and/or furnace assembly are carried out, and if the temperature of the furnace disassembly and/or furnace assembly is higher than 310-330 ℃, the risk of ageing of the thermal field part of the single crystal furnace caused by high temperature is increased.
In the invention, the liquid level temperature of the silicon melt refers to the temperature at the highest temperature on the liquid level of the silicon melt, the temperature on the surface of the silicon crystal bar refers to the temperature at the highest temperature on the surface of the silicon crystal bar, and the temperature of the heater heating area refers to the temperature at the highest temperature of the heater heating area in the single crystal furnace.
In some preferred embodiments, the flow rate of the argon gas is 90L/min to 110L/min. The flow rate of argon is more than 90L/min, so that the oxide in the single crystal furnace is more favorably taken away, the cooling rate is improved, the furnace shutdown time is shortened, the flow rate of argon is less than 110L/min, and the problems of crystal bar cracking and bar frying caused by too fast cooling of the crystal bar are more favorably avoided. More preferably, the first preset speed and the second preset speed of the rotation of the silicon crystal rod and the rotation of the crucible containing the silicon melt are 2 r/min-5 r/min, and the heat dissipation uniformity and the cooling effect are improved by enabling the first preset speed and the second preset speed to be 2 r/min-5 r/min. The temperature uniformity of the crystal bar is improved by controlling the heat transfer process by adopting the rotating speed of 2 r/min-5 r/min and the argon flow of 90L/min-110L/min, the temperature deviation of each area on the surface of the crystal bar is reduced as much as possible, the possibility that the abnormal deviation of the temperature of the crystal bar locally occurs at a higher temperature, the occurrence of defects such as cracks and the like of the crystal bar is reduced, and the optimal cooling speed is better facilitated to be obtained, so that the production efficiency is improved on the premise of reducing the defects of cracks and dislocation of the crystal bar.
The argon flow rate in the invention can be, for example, 90L/min, 95L/min, 100L/min, 105L/min and 110L/min, and the first preset speed and the second preset speed can be, for example, 2r/min, 2.5r/min, 3r/min, 3.5r/min, 4r/min, 4.5r/min and 5r/min respectively.
In some preferred embodiments, the first lifting process has a lifting rate of 110mm/h to 130mm/h and the second lifting process has a lifting rate of 320mm/h to 400mm/h. The lifting rate of the first lifting treatment is controlled to be 110mm/h-130mm/h, so that the accidents such as bar frying caused by the fact that the temperature of the crystal bar is rapidly reduced when the crystal bar passes through a heat shield can be prevented, the cooling speed is too high, the lifting rate of the first lifting treatment is controlled to be more than 110mm/h, the radiation heating influence of a crucible and a heater on the crystal bar can be reduced, the cooling effect and the production efficiency can be improved, the lifting rate of the first lifting treatment can be controlled to be less than 130mm/h, and the accidents such as bar frying caused by the fact that the cooling speed is too high can be reduced. The lifting rate of the second lifting treatment is controlled to be 320-400 mm/h, the cooling of the crystal bar is quickened, the influence of radiation heat to the lower part of the long residence time of the crystal bar on cooling of a crucible and a heater in a furnace is restrained, the furnace stopping time is shortened, the lifting rate of the second lifting treatment is controlled to be more than 320mm/h, the cooling effect of the crystal bar, the crucible and the heater is improved, the lifting rate of the second lifting treatment is controlled to be less than 400mm/h, and accidents such as bar frying and bar dropping caused by too fast cooling speed are prevented. More preferably, when the temperature of the surface of the silicon crystal rod is reduced to 950-1050 ℃, the position of the crucible is moved down by 90-110 mm, the radiation heating of the crucible to the crystal rod is reduced by 90-110 mm, the uniformity of an internal thermal field is improved, the temperature of the thermal field is reduced, the cooling time is reduced, the furnace stopping time is shortened, the position of the crucible is controlled to be moved down by more than 90mm, the mutual radiation influence between the crucible and the crystal rod is reduced, the cooling speed is improved, the downward movement distance of the crucible is controlled to be less than 110mm, and the heater is prevented from being damaged due to the too fast cooling speed, so that the heater is aged.
The lifting rate of the first lifting treatment in the invention can be 110mm/h, 115mm/h, 120mm/h, 125mm/h and 130mm/h, and the lifting rate of the second lifting treatment can be 320mm/h, 330mm/h, 340mm/h, 350mm/h, 360mm/h, 370mm/h, 380mm/h, 390mm/h and 400mm/h, and the downward moving distance of the crucible position can be 90mm, 95mm, 100mm, 105mm and 110mm when the temperature of the surface of the silicon crystal bar is reduced to 950-1050 ℃.
In some preferred embodiments, when the temperature of the surface of the silicon crystal rod is reduced to 880-920 ℃, the position of the heat shield is moved up to the upper limit position of the heat shield, and the position of the crucible is moved down to the lower limit position of the crucible.
In some preferred embodiments, the conditions of the cooling process further comprise: and stopping introducing argon into the single crystal furnace and detecting air leakage when the temperature of the surface of the silicon crystal bar is reduced to 680-720 ℃. Under the preferred scheme, the quality of the crystal bar is guaranteed more favorably, the phenomenon that the surface of the silicon crystal bar is whitened due to oxidation of the silicon crystal bar in drawing is seriously caused by air leakage of the single crystal furnace, the crystal bar quality is influenced to increase crystal bar loss, whether the next furnace is opened or not is influenced by the detection result of the step, if the leakage rate is not in the required range, the single crystal furnace is required to be repaired, and the next furnace after the furnace is disassembled after the overhaul is carried out. Preferably, the leak rate of the leak detection is 0 to 30mtorr/hr.
In some preferred embodiments, when the temperature of the surface of the silicon crystal rod is reduced to 440-460 ℃, the tail of the silicon crystal rod is lifted to be above a sub-chamber isolation valve of the single crystal furnace, the sub-chamber isolation valve is opened to isolate a main chamber of the single crystal furnace from a sub-chamber of the single crystal furnace, argon is continuously introduced into the sub-chamber, and after the pressure in the sub-chamber reaches the atmospheric pressure, the silicon crystal rod is taken out from the sub-chamber. Under the preferred scheme, the silicon crystal rod is more beneficial to cooling, and the auxiliary chamber is separated from the main chamber at the moment. Referring to fig. 1, the single crystal furnace of the present invention includes a main chamber and an auxiliary chamber, the main chamber is a region below a furnace cover 3 of the single crystal furnace, where a heat shield 4, a heater 5 and a crucible 6 are located, the auxiliary chamber is a cylindrical structure (not shown in the figure) above the furnace cover 3 of the single crystal furnace, an auxiliary chamber isolation valve is arranged between the auxiliary chamber and the main chamber, the auxiliary chamber isolation valve controls the auxiliary chamber to be spatially communicated with the main chamber, and the diameter of the auxiliary chamber is smaller than that of the main chamber.
In some preferred embodiments, when the wide-angle infrared temperature measurement unit monitors that the surface temperature of the crystal bar is reduced to 440-460 ℃, an alarm is automatically triggered, and argon is continuously introduced into the auxiliary chamber of the single crystal furnace after the manual bar taking confirmation is carried out.
In some preferred embodiments, after the silicon crystal bar is taken out, argon is continuously introduced into a main chamber of the single crystal furnace until the pressure in the main chamber reaches 200-400 torr, and then the pressure is maintained; and continuously introducing argon into the main chamber when the temperature of the heating area of the heater is reduced to 310-330 ℃, and carrying out furnace disassembly and/or furnace loading after the pressure in the main chamber reaches atmospheric pressure. Under this preferred scheme, through going on the pressurize after letting in the argon gas to the main room, more do benefit to fully make heater cooling down, through the pressurize when atmospheric pressure is 200 torr-400 torr, more do benefit to the negative influence of oxygen to thermal field parts such as graphite felt, graphite spare when avoiding the high temperature, can carry out the cooling of thermal field parts temperature under stable environment, negative influence specifically indicates: silicon carbide is generated in the partial area of the reaction of oxygen and graphite at high temperature, the silicon carbide and the graphite have different thermal expansion coefficients, and according to the principle of thermal expansion and contraction, the silicon carbide and the graphite have different expansion and contraction distances, so that stress is generated in the graphite piece to crack.
In some preferred embodiments, when the wide-angle infrared temperature measurement unit monitors that the temperature of the heating area of the heater is reduced to 310-330 ℃, an alarm is automatically triggered, and after the manual furnace opening confirmation is carried out, argon is continuously introduced into the main chamber of the single crystal furnace.
In a second aspect, the present invention provides a single crystal furnace adopting the furnace shutdown method of the first aspect, the single crystal furnace comprising: crucible 6, heater 5, heat shield 4, CCD camera 2, wide-angle infrared temperature measuring unit 1, argon gas supply unit, crystal bar lifting unit and control unit;
the heater 5 is arranged on the outer side of the crucible 6 in a surrounding manner, the heat shield 4 is arranged above the crucible 6, and the CCD camera 2 and the wide-angle infrared temperature measuring unit 1 are arranged on the furnace cover 3 of the single crystal furnace;
the control unit is respectively connected with the CCD camera 2, the wide-angle infrared temperature measuring unit 1, the argon gas supply unit, the crystal bar lifting unit, the crucible 6 and the heat shield 4 and is used for controlling the actions of the CCD camera 2 and the wide-angle infrared temperature measuring unit 1, controlling the feeding of argon gas and controlling the positions of the silicon crystal bar, the crucible 6 and the heat shield 4.
According to the single crystal furnace, the CCD camera 2 and the wide-angle infrared temperature measuring unit 1 are arranged on the furnace cover 3 of the single crystal furnace, and in the crystal pulling stage, the lens of the CCD camera 2 can acquire the liquid level brightness of the silicon melt and then convert the liquid level brightness into the liquid level temperature of the silicon melt, so that the liquid level temperature of the silicon melt is monitored, the crystal pulling process is ensured to be carried out smoothly by adjusting the pulling speed and the like, the crystal quality is improved, and the crystal defects are reduced; the control unit is further connected with the CCD camera 2, the wide-angle infrared temperature measuring unit 1, the argon gas supply unit, the crystal bar lifting unit, the crucible 6 and the heat shield 4 respectively, and in the furnace stopping stage, the feeding of argon gas and the positions of the silicon crystal bar, the crucible 6 and the heat shield 4 can be controlled according to the temperature monitoring results of the wide-angle infrared temperature measuring unit 1 on the surface of the silicon crystal bar and the heating area of the heater 5, so that whether the automatic bar taking, the automatic furnace disassembly and the automatic furnace loading are performed or not is controlled, thereby reducing the furnace stopping cooling time, improving the production efficiency, reducing accidents such as crystal bar explosion and bar dropping, improving the crystal bar quality and inhibiting the ageing of heat field components.
It is to be noted that the single crystal furnace includes a driving mechanism for rotating the silicon ingot and the crucible 6 containing the silicon melt therein.
In a third aspect, the present invention provides an electronic device, referring to fig. 2, the electronic device 200 may include a memory 201, a memory controller 202, a processor 203, a peripheral interface 204, an input-output unit 205, and a display unit 206. It will be appreciated by those of ordinary skill in the art that the configuration shown in fig. 2 is merely illustrative and is not intended to limit the configuration of the electronic device 200. For example, the electronic device 200 may also include more or fewer components than shown in FIG. 2, or have a different configuration than shown in FIG. 2.
The memory 201, the memory controller 202, the processor 203, the peripheral interface 204, the input/output unit 205, and the display unit 206 are electrically connected directly or indirectly to each other, so as to realize data transmission or interaction. For example, the components may be electrically connected to each other via one or more communication buses or signal lines. The processor 203 is configured to execute executable modules stored in the memory 201.
The memory 201 may be, but is not limited to, random access memory, read only memory, programmable read only memory, erasable read only memory, electrically erasable read only memory, etc. The memory 201 is configured to store a program, and the processor 203 executes the program after receiving an execution instruction, and a method executed by the electronic device 200 defined by the process disclosed in any embodiment of the present invention may be applied to the processor 203 or implemented by the processor 203.
The processor 203 may be an integrated circuit chip with signal processing capability. The processor 203 may be a general-purpose processor, including a central processor, a network processor, etc.; but also digital signal processors, application specific integrated circuits, field programmable gate arrays or other programmable logic devices, discrete gate or transistor logic devices, discrete hardware components. Various methods and steps of embodiments of the present invention may be implemented or performed.
The peripheral interface 204 couples various input/output devices to the processor 203 and the memory 201. In some embodiments, the peripheral interface 204, the processor 203, and the memory controller 202 may be implemented in a single chip or separately by separate chips.
The input-output unit 205 is used for providing input data to a user. The input/output unit 205 may be, but is not limited to, a mouse, a keyboard, and the like.
The display unit 206 provides an interactive interface (e.g., a user-operated interface) between the electronic device 200 and a user or is used to display image data to a user reference. In this embodiment, the display unit 206 may be a liquid crystal display or a touch display. In the case of a touch display, the touch display may be a capacitive touch screen or a resistive touch screen, etc. supporting single-point and multi-point touch operations. Supporting single-point and multi-point touch operations means that the touch display can sense touch operations simultaneously generated from one or more positions on the touch display, and the sensed touch operations are passed to the processor for calculation and processing. In this embodiment, the display unit 206 may be used to display the trend of various status data of the silicon melt level, ingot, crucible, and heater during the pulling process and the furnace shutdown cooling process.
In this embodiment, a control program is installed in the electronic device, and the control program may be to control the furnace shutdown system to be equipped with a full-automatic furnace shutdown control system. After the crystal pulling stage is finished, the work of the single crystal furnace is controlled by setting a furnace stopping parameter, and the furnace stopping parameter is sent to a basic automation system for execution. The basic automation system is used for controlling each component in the single crystal furnace so as to realize the cooling control of the furnace shutdown.
The electronic device 200 in the present embodiment may be used to perform each step in each method provided in the embodiment of the present invention.
Furthermore, the embodiment of the invention also provides a computer readable storage medium, and a computer program is stored on the computer readable storage medium, and the computer program is executed by a processor to execute the steps of the furnace shutdown method for producing monocrystalline silicon in the embodiment of the method. A computer program product of a furnace shutdown method for producing single crystal silicon according to an embodiment of the present invention includes a computer readable storage medium storing program code including instructions for executing the steps of the furnace shutdown method for producing single crystal silicon described in the above method embodiment.
The following describes the technical solution in the embodiment of the present invention in detail with reference to the drawings in the embodiment of the present invention.
Example 1
Referring to the single crystal furnace of fig. 1, the method for shutting down the furnace for producing the single crystal furnace in this embodiment adopts a CCD camera to monitor the liquid level temperature of the silicon melt in the single crystal furnace in real time, and when the liquid level temperature of the silicon melt is monitored to be not higher than 1000 ℃, the CCD camera is turned off, a wide-angle infrared temperature measuring unit is turned on, the monitoring angle of the wide-angle infrared temperature measuring unit is adjusted to monitor the temperature of the surface of the silicon ingot, and the temperature at the highest temperature of the surface of the silicon ingot is obtained from the monitoring result, and when the wide-angle infrared temperature measuring unit is turned on, the silicon ingot is rotated at a speed of 3.5r/min through a driving structure in the single crystal furnace, so that a crucible containing the silicon melt is rotated at a speed of 4r/min, and simultaneously argon is introduced into the single crystal furnace through an argon gas supplying unit at a flow of 100L/min, so that the ingot, the crucible and a heater in the single crystal furnace are cooled and oxide in the single crystal furnace is taken away. When the temperature of the highest part of the surface temperature of the silicon crystal bar is monitored by the wide-angle infrared temperature measuring unit to be reduced to 1000 ℃, the silicon crystal bar and the crucible are rotated, the silicon crystal bar is lifted for the first time at the lifting speed of 120mm/h, the tail part of the silicon crystal bar passes through the inner heat shield of the single crystal furnace, specifically, the silicon crystal bar is lifted for the second time at the lifting speed of 360mm/h from the lowest end of the inner heat shield of the single crystal furnace, the silicon crystal bar is lifted for 180mm upwards again continuously, the position of the crucible is moved downwards for the first time, and the position of the crucible is moved downwards for 100mm. Along with the cooling, when the temperature of the highest position of the surface temperature of the silicon crystal rod is monitored to be reduced to 900 ℃ by the wide-angle infrared temperature measuring unit, the position of a heat shield in the crucible is moved upwards for the first time while the silicon crystal rod and the crucible are rotated, the position of the heat shield is moved upwards to the upper limit position of the heat shield, the position of the crucible is moved downwards for the second time, and the position of the crucible is moved downwards to the lower limit position of the crucible. Along with the cooling, when the wide-angle infrared temperature measuring unit monitors that the temperature at the highest position of the surface temperature of the silicon crystal bar is reduced to 700 ℃, argon is stopped from being introduced into the single crystal furnace, namely, argon in a main chamber and an auxiliary chamber of the single crystal furnace is simultaneously closed, the air leakage rate of the single crystal furnace is detected to be 0mtorr/hr-30mtorr/hr, the argon in the main chamber and the auxiliary chamber is kept closed after the air leakage detection is finished, a main valve and a main pump which are introduced with the argon are closed, when the wide-angle infrared temperature measuring unit monitors that the temperature of the surface of the silicon crystal bar is reduced to 450 ℃, a system alarm is triggered, staff performs bar taking confirmation, after the bar taking can be confirmed, the tail part of the silicon crystal bar is lifted to be above an auxiliary chamber isolation valve of the single crystal furnace, the auxiliary chamber isolation valve of the single crystal furnace is opened, the argon is continuously introduced into the auxiliary chamber of the single crystal furnace, and after the air pressure in the auxiliary chamber reaches the atmospheric pressure (600 torr), the method comprises the steps of taking out a crystal bar from a rotating auxiliary chamber, adjusting the monitoring angle of a wide-angle infrared temperature measuring unit after taking out the crystal bar, enabling the temperature inside a heating area of a heater to be monitored, obtaining the temperature at the highest temperature inside the heating area of the heater from a monitoring result, simultaneously opening a main chamber isolation valve, introducing argon into the main chamber, keeping the isolation valves of the main chamber and the auxiliary chamber closed after the air pressure in the main chamber reaches 200-400 torr, keeping the pressure of the main chamber, triggering a system to alarm when the temperature at the highest temperature inside the heating area of the heater is monitored to be reduced to 320 ℃, enabling a worker to open the furnace, opening the main chamber isolation valve after confirming that the furnace opening can be carried out, continuing introducing argon into the main chamber of a single crystal furnace, and unscrewing a furnace cover for disassembling and assembling operation after the air pressure in the main chamber reaches atmospheric pressure (600 torr).
Example 2
The procedure is as in example 1, except that the argon flow is 80L/min.
Example 3
The procedure is as in example 1, except that the argon flow is 120L/min.
Example 4
The procedure was as in example 1, except that the flow rate of the argon gas was 80L/min, the rotation speed of the silicon ingot was 10r/min, and the rotation speed of the crucible was 10r/min.
Example 5
The procedure of example 1 was followed, except that the flow rate of argon gas was 120L/min, the rotation speed of the silicon ingot was 1r/min, and the rotation speed of the crucible was 1r/min.
Example 6
The procedure is as in example 1, except that the first lifting of the silicon ingot is carried out at a lifting rate of 150mm/h.
Example 7
The second lift of the silicon ingot was performed as in example 1, except that the lift rate was 240mm/h.
Example 8
The procedure is as in example 1, except that the position of the crucible is moved down a distance of 60mm for the first time.
Example 9
The process was performed in accordance with example 1, except that the furnace was opened when the temperature of the main chamber was lowered to 320℃and the temperature of the inside of the heating zone was lowered to 320℃by opening the main chamber isolation valve while monitoring the temperature of the inside of the heating zone of the heater by adjusting the wide-angle infrared temperature measuring unit after taking out the ingot without maintaining the pressure of the main chamber to 200to 400 torr.
Comparative example 1
The procedure is as in example 1, except that the position of the crucible is not moved down for the first time.
Comparative example 2
The procedure is as in example 1, except that the position of the crucible is not moved down a second time.
Comparative example 3
The process is performed according to example 1, except that the temperature of the silicon ingot surface at the highest temperature is monitored by the wide-angle infrared temperature measurement unit and is reduced to 900 ℃, and the position of the heat shield in the crucible is not moved upwards for the first time.
Comparative example 4
The process was performed as in example 1, except that when the wide-angle infrared temperature measuring unit monitored that the temperature at the highest temperature of the surface of the silicon ingot was lowered to 920 ℃, the silicon ingot and the crucible were rotated while the silicon ingot was lifted up for the first time and lifted up for the second time, and the position of the crucible was moved down for the first time.
Comparative example 5
The procedure was as in example 1, except that when the wide-angle infrared temperature measurement unit monitored that the temperature at the highest temperature of the surface of the silicon ingot was reduced to 940 c, the position of the heat shield in the crucible was moved up for the first time and the position of the crucible was moved down for the second time while rotating the silicon ingot and the crucible.
Comparative example 6
The procedure was as in example 1, except that when the wide-angle infrared temperature measurement unit monitored that the temperature at the highest temperature of the surface of the silicon ingot was reduced to 850 ℃, the position of the heat shield in the crucible was moved up for the first time and the position of the crucible was moved down for the second time while rotating the silicon ingot and the crucible.
Comparative example 7
The process is performed according to example 1, except that the silicon ingot is taken from the single crystal furnace when the wide-angle infrared temperature measuring unit monitors that the temperature of the surface of the silicon ingot is reduced to 500 ℃.
Comparative example 8
The process is carried out according to the embodiment 1, except that the wide-angle infrared temperature measuring unit is used for disassembling and/or assembling the furnace when the temperature of the heating area of the heater is monitored to be reduced to 380 ℃.
The results of the measurements of the cooling time in the furnace of examples 1 to 9 and comparative examples 1 to 8, the incidence of the falling bar accident, the cracking condition of the ingot, the dislocation condition of the tail portion of the ingot and the aging condition of the thermal field member are shown in Table 1. The condition of the explosion of the crystal bar is that whether the surface of the crystal bar is cracked or not after the crystal bar is taken out in the blowing-out process, the dislocation condition of the tail part of the crystal bar is that whether the end face of the crystal bar is cracked (internally cracked) or not after the crystal bar is normally cut end by end and cut, and the ageing condition of the thermal field component is that whether the thermal field component is cracked or not due to the formation of silicon carbide after the furnace is disassembled, and the abnormal conditions such as slag falling and the like are caused.
TABLE 1
By comparing examples 1-9 with comparative examples 1-8, it can be known that the furnace shutdown time of example 1 is the shortest, the silicon ingot has no ingot falling accident, the end face of the ingot after the tail is normally cut end to end and truncated has no dislocation, and the thermal field piece has no aging failure after furnace disassembly. When the flow of the argon is higher than 90L/min, the reduction of the furnace shutdown cooling time is facilitated, when the flow of the argon is lower than 110L/min, the prevention of cracking of the crystal bar and the control of slight dislocation at the tail part are facilitated, by enabling the flow of the argon to be 90L/min-110L/min, the rotation speed of the silicon crystal bar and the rotation speed of a crucible containing silicon melt to be 2r/min-5r/min, the furnace shutdown cooling time can be reduced to the greatest extent, the cracking of the crystal bar is prevented, the dislocation at the tail part of the crystal bar is reduced, the ageing of a thermal field part is prevented, the cracking of the crystal bar is prevented by enabling the lifting speed of the first lifting treatment to be lower than 130mm/h, the bar falling risk is reduced, the dislocation at the tail part of the crystal bar is reduced, the lifting speed of the second lifting treatment is higher than 320mm/h, and the furnace shutdown time is shortened. When the temperature of the surface of the silicon crystal bar is reduced to 950-1050 ℃, the position of the crucible is moved down by 90-110 mm, which is more beneficial to reducing the cooling time of furnace shutdown. In the cooling process of the furnace, after the air pressure in the main chamber reaches 200-400 torr, pressure maintaining is carried out, so that the ageing of the thermal field component is more favorably inhibited, if the temperature of the surface of the silicon crystal bar is reduced to 950-1050 ℃, the position of the crucible is not moved downwards for the first time, the cooling time of the furnace is prolonged, the ageing of the thermal field component is caused, when the temperature of the surface of the silicon crystal bar is reduced to 880-920 ℃, the position of the crucible is not moved downwards for the second time, the cooling time of the furnace is prolonged, the ageing of the thermal field component is caused, when the temperature of the surface of the silicon crystal bar is reduced to 880-920 ℃, the position of a heat shield in the crucible is not moved upwards for the first time, the cooling time of the furnace is prolonged, the ageing of the thermal field component is caused, and when the temperature of the surface of the silicon crystal bar is reduced to below 950-1050 ℃, the method comprises the steps of lifting a silicon crystal rod for the first time and lifting the silicon crystal rod for the second time, wherein the first time downwards moving the position of the crucible can lead to the prolongation of the cooling time of a shutdown furnace, when the temperature of the surface of the silicon crystal rod is reduced to be higher than 880-920 ℃, the first time upwards moving the position of a heat shield in the crucible can lead to the ageing of a heat field component, when the temperature of the surface of the silicon crystal rod is reduced to be lower than 880-920 ℃, the first time upwards moving the position of the heat shield in the crucible can lead to the second time downwards moving the position of the crucible, the prolongation of the cooling time of the shutdown furnace, the increase of the risk of occurrence of bar dropping accidents when the temperature of a bar is too high, the cracking of the crystal rod is caused, the dislocation of the tail part of the crystal rod is increased, and the obvious ageing of the heat field component is caused when the temperature of the furnace disassembly and/or the furnace assembly is too high.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (6)
1. A furnace shutdown method for producing single crystal silicon, the method comprising:
when the liquid level temperature of the silicon melt in the single crystal furnace is higher than 950-1050 ℃, monitoring the liquid level temperature by adopting a CCD camera; when the liquid level temperature is not higher than 950-1050 ℃, monitoring the temperatures of the surface of the silicon crystal bar and a heating area of a heater in the single crystal furnace by adopting a wide-angle infrared temperature measuring unit, and introducing argon into the single crystal furnace to cool the silicon crystal bar, the crucible and the heater;
wherein the conditions of the cooling treatment include: the silicon crystal bar rotates at a first preset speed, and the crucible containing silicon melt rotates at a second preset speed; when the temperature of the surface of the silicon crystal bar is reduced to 950-1050 ℃, sequentially carrying out first lifting treatment and second lifting treatment on the silicon crystal bar, and simultaneously downwards moving the position of the crucible; the lifting speed of the first lifting treatment is smaller than that of the second lifting treatment, the first lifting treatment enables the tail of the silicon crystal bar to be lifted to a first preset position, the first preset position is located above the lowest end of the heat shield in the single crystal furnace, the vertical distance between the first preset position and the lowest end of the heat shield in the single crystal furnace is 55mm-65mm, the second lifting treatment enables the tail of the silicon crystal bar to be lifted to a second preset position, the second preset position is located above the first preset position, and the vertical distance between the second preset position and the first preset position is 160mm-200mm; when the temperature of the surface of the silicon crystal bar is reduced to 880-920 ℃, the position of the heat shield is moved upwards, the position of the crucible is moved downwards, and the heating area of the heater is exposed; when the temperature of the surface of the silicon crystal bar is reduced to 440-460 ℃, taking out the silicon crystal bar from the single crystal furnace; when the temperature of the heating area of the heater is reduced to 310-330 ℃, disassembling and/or loading the furnace;
The liquid level temperature of the silicon melt refers to the temperature at the highest temperature on the liquid level of the silicon melt, the temperature of the surface of the silicon crystal bar refers to the temperature at the highest temperature on the surface of the silicon crystal bar, and the temperature of the heater heating area refers to the temperature at the highest temperature of the heater heating area in the single crystal furnace;
the flow rate of the argon is 90L/min-110L/min; the first preset speed and the second preset speed are 2 r/min-5 r/min;
the lifting speed of the first lifting treatment is 110-130 mm/h, and the lifting speed of the second lifting treatment is 320-400 mm/h;
when the temperature of the surface of the silicon crystal bar is reduced to 950-1050 ℃, the position of the crucible is moved down by 90-110 mm; when the temperature of the surface of the silicon crystal bar is reduced to 880-920 ℃, the position of the heat shield is moved up to the upper limit position of the heat shield, and the position of the crucible is moved down to the lower limit position of the crucible.
2. The furnace shutdown method of claim 1, wherein the conditions of the cooling process further comprise: and stopping introducing argon into the single crystal furnace and detecting air leakage when the temperature of the surface of the silicon crystal bar is reduced to 680-720 ℃.
3. The method according to claim 2, wherein when the temperature of the surface of the silicon ingot is reduced to 440 ℃ to 460 ℃, the tail of the silicon ingot is raised to above a sub-chamber isolation valve of the single crystal furnace, the sub-chamber isolation valve is opened to isolate a main chamber of the single crystal furnace from a sub-chamber of the single crystal furnace, argon gas is continuously introduced into the sub-chamber, and after the pressure in the sub-chamber reaches atmospheric pressure, the silicon ingot is taken out from the sub-chamber.
4. The method for stopping the furnace according to claim 2, wherein after the silicon crystal rod is taken out, argon is continuously introduced into a main chamber of the single crystal furnace until the pressure in the main chamber reaches 200-400 torr, and then the pressure is maintained; and continuously introducing argon into the main chamber when the temperature of the heating area of the heater is reduced to 310-330 ℃, and carrying out furnace disassembly and/or furnace loading after the pressure in the main chamber reaches atmospheric pressure.
5. An electronic device, comprising: a processor (203), a memory (201), the memory (201) storing machine readable instructions executable by the processor (203) which, when executed by the processor (203), perform the steps of the method of any one of claims 1 to 4.
6. A computer-readable storage medium, characterized in that it has stored thereon a computer program which, when executed by a processor, performs the steps of the method according to any of claims 1 to 4.
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| CN102134739A (en) * | 2011-03-08 | 2011-07-27 | 宁夏日晶新能源装备股份有限公司 | Automatic crystal guide system of single crystal furnace, and automatic crystal guide method |
| CN103266348B (en) * | 2013-05-03 | 2015-12-09 | 江苏海翔化工有限公司 | Fast energy-saving pulling single crystal silicon furnace stopping process |
| CN104213188A (en) * | 2014-08-29 | 2014-12-17 | 江苏拜尔特光电设备有限公司 | Shutdown cooling method for single crystal furnace |
| CN111826707A (en) * | 2020-07-27 | 2020-10-27 | 邢台晶龙新能源有限责任公司 | Method for preventing thermal field damage during shutdown of single crystal furnace |
| CN112760706A (en) * | 2020-12-23 | 2021-05-07 | 西安奕斯伟硅片技术有限公司 | Equal-diameter growth control system and equal-diameter growth control method |
| CN114232080A (en) * | 2021-12-24 | 2022-03-25 | 包头美科硅能源有限公司 | Furnace-closing process of RCZ Czochralski method large thermal field |
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Effective date of registration: 20231226 Address after: 663000 Xiban area of the Industrial Demonstration Park in Guangnan County, Wenshan Zhuang and Miao Autonomous Prefecture, Yunnan Province Patentee after: Yuze Semiconductor (Wenshan) Co.,Ltd. Address before: G3-2401, No. 88, Jinjihu Avenue, Suzhou Industrial Park, Suzhou Pilot Free Trade Zone, China (Jiangsu) 215000 Patentee before: Suzhou Chenhui Intelligent Equipment Co.,Ltd. |