WO2024060650A1 - 一种拉晶方法、单晶硅棒和单晶炉 - Google Patents

一种拉晶方法、单晶硅棒和单晶炉 Download PDF

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Publication number
WO2024060650A1
WO2024060650A1 PCT/CN2023/095179 CN2023095179W WO2024060650A1 WO 2024060650 A1 WO2024060650 A1 WO 2024060650A1 CN 2023095179 W CN2023095179 W CN 2023095179W WO 2024060650 A1 WO2024060650 A1 WO 2024060650A1
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gas
time
temperature adjustment
single crystal
crucible
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English (en)
French (fr)
Inventor
王正远
李广砥
郭力
杨正华
张伟建
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Longi Green Energy Technology Co Ltd
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Longi Green Energy Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/20—Controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B27/00—Single-crystal growth under a protective fluid
    • C30B27/02—Single-crystal growth under a protective fluid by pulling from a melt
    • 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

Definitions

  • the present invention relates to the technical field of crystal growth, and in particular to a crystal pulling method, a single crystal silicon rod and a single crystal furnace.
  • the currently commonly used production process for processing silicon materials into single crystal silicon is the Czochralski method.
  • the Czochralski method is mainly divided into processes such as charging, melting, cooling to adjust the seeding temperature, seeding, shoulder placement, shoulder rotation, equal diameter, and finishing.
  • the present invention provides a crystal pulling method, a single crystal silicon rod and a single crystal furnace, aiming to solve the problem that the diameter of the single crystal silicon rod pulled by the existing crystal pulling method fluctuates greatly and the quality of the single crystal silicon rod is poor.
  • a first aspect of the present invention provides a crystal pulling method, the method comprising:
  • Step S in the period from the temperature adjustment start time to the finishing end time, control each moment, the first gas introduced into the single crystal furnace, the first pressure at the crystallization interface, and the temperature adjustment start time, the The absolute value of the difference between the second gas in the single crystal furnace and the second pressure at the crystallization interface is less than or equal to the first preset value.
  • the pressure of the gas flowing into the single crystal furnace at the crystallization interface at different times is approximately equal, and the pressure of the gas flowing into the single crystal furnace at the crystallization interface at the same time is equal to
  • the pressure at the crystal interface at this time that is to say, from the beginning of the temperature adjustment to the end of the temperature adjustment, keeps the pressure at the crystal interface basically stable.
  • the pressure at the crystallization interface will roughly determine the melting point of the silicon material, which will roughly determine the crystallization temperature.
  • the crystallization temperature will roughly determine the crystallization speed, which is macroscopically reflected in the stability of the diameter of the single crystal rod obtained.
  • the pressures of the crystallization interfaces corresponding to different moments are roughly equal, which can ensure that the crystallization temperatures corresponding to different moments are roughly the same in the period from the beginning of the temperature adjustment to the ending time of the finishing. etc., thus ensuring that the crystallization speeds corresponding to different times are approximately equal in the period from the temperature adjustment start time to the finishing end time. Finally, it can ensure that the crystallization speeds corresponding to different times in the period from the temperature adjustment start time to the finishing end time can be guaranteed.
  • the diameters of the rods are roughly equal, so that the diameter fluctuation of the final drawn single crystal rod is small and the stability of the diameter of the crystal rod is high, thereby improving the quality of the crystal rod.
  • the pressure of the crystallization interface will affect the segregation coefficient of the impurities, thereby affecting the concentration distribution of the impurities throughout the crystal rod.
  • the crystallization interface in the period from the temperature adjustment start time to the finishing end time, at different times, the crystallization interface If the pressure is roughly equal, the concentration distribution of the same impurity in the crystal rod will be roughly equal, and the quality uniformity of the crystal rod will be better, which also improves the quality of the crystal rod.
  • step S the method further includes:
  • the step S includes:
  • the difference between the real-time mechanical energy of the first gas at the crystallization interface, except for the pressure potential energy, and the initial mechanical energy is controlled.
  • the absolute value is less than or equal to the second preset value.
  • the first gas is the same as the second gas; based on Bernoulli's principle, the initial mechanical energy of the second gas at the crystallization interface, in addition to pressure potential energy, is obtained, including :
  • the period from the temperature adjustment start time to the finishing end time is based on Bernoulli's principle.
  • the real-time mechanical energy of the first gas at the crystallization interface, except for the pressure potential energy is equal to the real-time mechanical energy of the first gas at the crystallization interface, except for the pressure potential energy.
  • the absolute value of the difference between the starting mechanical energy outside the range is less than or equal to the second preset value, including:
  • the flow rate of the first gas at the crystallization interface at the first time is controlled, and the flow rate of the second gas at the crystallization interface at the temperature adjustment start time is controlled.
  • the absolute value of the difference in flow velocity at is less than or equal to the third preset value.
  • the period from the temperature adjustment start time to the finishing end time is to control the flow rate of the first gas at the crystallization interface at the first time and the flow rate of the second gas at the temperature adjustment time.
  • the absolute value of the difference in flow velocity at the crystallization interface is less than or equal to the third preset value, including:
  • the first moment is obtained from the period after the temperature adjustment start time to the end time of the temperature adjustment.
  • the flow rate from after the first gas flows out from the lower edge of the heat screen to before the first gas is discharged from the single crystal furnace The minimum flow cross-sectional area at each point in the path;
  • the first real-time flow rate of the first gas is introduced into the single crystal furnace.
  • the period from the temperature adjustment start time to the closing end time is to obtain the first time, after the first gas flows out from the lower edge of the heat screen, to the time when the first gas flows out from the single crystal Before the minimum flow cross-sectional area at each point in the flow path before being discharged from the furnace, the method further includes:
  • the minimum flow cross-sectional area at each point in the flow path after the first gas flows out from the lower edge of the heat shield to before the first gas is discharged from the single crystal furnace is obtained in the period from the start time of the temperature adjustment to the end time of the temperature adjustment, including:
  • the minimum flow cross-sectional area corresponding to the first crucible is obtained by querying.
  • the minimum flow cross-sectional area at each point in the flow path is obtained at each crucible position, and the minimum flow cross-sectional area corresponding to the crucible position is stored in the first crucible position area list. , including:
  • each crucible position take the distance between the endpoint of the lower edge of the heat shield close to the crystallization interface and the first centerline of the single crystal furnace as the radius, take the first plane where the endpoint is located and the third The first intersection point of a center line is the center of the circle, forming the first surface area of the side of the cylinder; wherein the first center line is perpendicular to the crystallization interface, and the first plane is parallel to the crystallization interface;
  • each crucible position take the line connecting the upper edge of the inner wall of the crucible and the second point on the R arc of the outer wall of the heat shield as the busbar, and take the first centerline as the centerline to form the third side of the circular cone.
  • the smallest surface area from the first surface area, the second surface area, the third surface area, and the fourth surface area is listed above.
  • the period from the temperature adjustment start time to the finishing end time is to control the flow rate of the first gas at the crystallization interface at the first time and the flow rate of the second gas at the temperature adjustment time.
  • the absolute value of the difference in flow velocity at the crystallization interface is less than or equal to the third preset value, including:
  • the second real-time flow rate of the first gas is introduced into the single crystal furnace.
  • the first time is obtained before the flow cross-sectional area of the first gas at the crystallization interface, and the method further includes:
  • the period from the temperature adjustment start time to the finishing end time is to obtain the first time and the flow cross-sectional area of the first gas at the crystallization interface, including:
  • the flow cross-sectional area corresponding to the first crucible is obtained by querying.
  • the first preset value is: 10pa.
  • the second preset value is: 6J/m 3 .
  • the third preset value is: 2mm/min.
  • the first gas includes a protective gas for the crystal pulling process
  • the second gas includes a protective gas for the crystal pulling process
  • the protective gas includes: nitrogen and/or inert gas.
  • the inert gas includes argon.
  • a second aspect of the present invention further provides a single crystal silicon rod prepared by any of the aforementioned crystal pulling methods.
  • a third aspect of the present invention also provides a single crystal furnace, which is used to pull crystals using any of the aforementioned crystal pulling methods.
  • Figure 1 shows a schematic structural diagram of a single crystal furnace in an embodiment of the present invention
  • Figure 2 shows a step flow chart of a crystal pulling method in an embodiment of the present invention
  • Figure 3 shows a comparative diagram of the diameter fluctuations of the crystal rod in the embodiment of the present invention and the crystal rod in the comparative example.
  • the main reason for the poor quality of the single crystal silicon rod is that the existing crystal pulling method starts from the time of temperature adjustment.
  • the pressure at the crystallization interface is not limited at each moment during the period from the time when the temperature adjustment begins to the time when the temperature adjustment ends, and the pressure at the crystallization interface fluctuates greatly at each moment.
  • the crystallization temperature will roughly determine The crystallization speed is macroscopically reflected in the stability of the diameter of the single crystal rod obtained by drawing. Therefore, in order to solve this problem, the main idea of the present invention is: from the temperature adjustment start time to the finishing time, at each time, the pressure of the gas flowing into the single crystal furnace at the crystallization interface is substantially stable, and at the same time, the pressure of the gas flowing into the single crystal furnace is basically stable.
  • the pressure of the gas entering the single crystal furnace at the crystallization interface is equal to the pressure of the crystallization interface at that moment, which is the period from the beginning of the temperature adjustment to the end of the temperature adjustment.
  • the pressure at the crystallization interface is kept basically stable, thereby making the drawn crystal rod
  • the fluctuation of the diameter is small, and the diameter stability of the single crystal rod obtained by drawing is better.
  • the pressure at the crystallization interface will affect the segregation coefficient of impurities, which in turn affects the concentration distribution of impurities throughout the single crystal rod.
  • the crystallization process occurs at different times. If the pressure at the interface is roughly equal, the concentration distribution of the same impurity in the single crystal rod will be roughly equal, and the quality uniformity of the single crystal rod will be better, which also improves the quality of the single crystal rod.
  • the Czochralski method is mainly divided into processes such as charging, melting, cooling to adjust the seeding temperature, seeding, shoulder placement, shoulder rotation, equal diameter, and finishing.
  • the temperature adjustment start time here is the time when the process of cooling down and adjusting the seeding temperature begins.
  • the first gas is the gas that flows into the single crystal furnace at each moment from the start time of the temperature adjustment to the end time of the finishing. For example, during a certain crystal pulling process in the single crystal furnace A, the start time of the temperature adjustment is October 2021.
  • the first gas is: after 10:13:20 on October 20, 2021, During the time period to 12:13:20 on October 21, 2021, all the gases flowing into the single crystal furnace A at various times.
  • the first gas may be a mixed gas or a single type of gas, which is not specifically limited in the present invention.
  • the first pressure is the pressure of the gas flowing into the single crystal furnace at the crystallization interface at each time from the start time of the temperature adjustment to the end time of the first gas.
  • the first pressure is the pressure flowing into the single crystal furnace A at each time from 10:13:20 on October 20, 2021, to 12:13:20 on October 21, 2021.
  • the first gas and the first pressure here correspond to the same moment.
  • the second gas is: all the gases flowing into the single crystal furnace when the temperature adjustment starts.
  • the second pressure is the pressure at the crystallization interface of the second gas flowing into the single crystal furnace when the temperature adjustment starts.
  • the second pressure at the crystallization interface is: the temperature adjustment start time is October 2021 At 10:13:20 on March 20, the pressure of all the gases flowing into the single crystal furnace A at the crystallization interface.
  • the main factor that affects the pressure at the crystallization interface is the gas flowing into the single crystal furnace.
  • the crystallization process or the ingot drawing process is mainly the period from the beginning of temperature adjustment to the end of finishing. Therefore, the present invention controls the first gas flowing into the single crystal furnace at each time from the time after the temperature adjustment starts to the time when the temperature adjustment ends, the first pressure at the crystallization interface, and the time when the temperature adjustment starts.
  • the absolute value of the difference between the second gas of the single crystal furnace and the second pressure at the crystallization interface is less than or equal to the first preset value. That is to say, it is maintained from the temperature adjustment start time to the finishing end time. During the period, at different times, the pressure of the gas flowing into the single crystal furnace at the crystallization interface remains basically unchanged.
  • the size of the first preset value here is not specifically limited, and is specifically determined by the stability requirements for the diameter of the crystal rod.
  • the present invention maintains is that the pressure of the gas flowing into the single crystal furnace at the crystallization interface is stable during the period from the temperature adjustment start time to the closing end time. Compared with keeping the pressure of the gas at other positions stable, the pressure of the crystallization interface is stable. Stability has the greatest impact on the stability of the diameter of the crystal rod. Therefore, the present invention has a better effect on improving the stability of the diameter of the crystal rod. For example, compared with keeping the pressure of the gas discharged from the single crystal furnace stable, the crystallization temperature and crystallization speed are more and more directly affected by the pressure of the crystallization interface.
  • the pressure of the gas flowing into the single crystal furnace is controlled to be stable at the crystallization interface, and a single crystal rod with a more stable diameter can be obtained.
  • the first preset value is 10pa, that is to say, during the period from the temperature adjustment start time to the finishing end time, the first gas introduced into the single crystal furnace at each time is controlled at the first gas at the crystallization interface.
  • the absolute value of the difference between the pressure p 1 and the second gas flowing into the single crystal furnace at the start of temperature adjustment and the second pressure p 2 at the crystallization interface is less than or equal to 10pa, from the time when temperature adjustment starts In the period to the end of the finishing time, the pressure at the crystal interface is more stable, making the diameter of the single crystal rod obtained by drawing less volatile, and the diameter of the single crystal rod obtained by drawing having better stability.
  • the concentration distribution of the same impurity in the single crystal rod is roughly equal, and the quality uniformity of the single crystal rod is better, which also improves the quality of the single crystal rod.
  • the absolute value of the difference between the second gas of the crystal furnace and the second pressure p 2 at the crystallization interface is 0, 1pa, 1.3pa, 2pa, 5pa, 6pa, 7pa, 8pa, 9pa, 10pa.
  • the first gas includes a protective gas for the crystal pulling process
  • the second gas includes a protective gas for the crystal pulling process.
  • the main function of the protective gas is to avoid the influence of other gases on the crystal pulling process.
  • the protective gas includes nitrogen and/or inert gas.
  • the above protective gases are easy to obtain and have low cost.
  • the inert gas includes argon, which is common, easy to obtain, and low in cost.
  • Figure 1 shows a schematic structural diagram of a single crystal furnace in an embodiment of the present invention.
  • Figure 2 shows a step flow chart of a crystal pulling method in an embodiment of the present invention.
  • the crystal pulling method may include the following steps:
  • Step 101 Based on Bernoulli's principle, obtain the initial mechanical energy of the second gas at the crystallization interface in addition to the pressure potential energy.
  • Bernoulli’s principle for fluids is formula 1: p here is the pressure potential energy of the fluid at a certain location, more specifically, it can be the pressure. It can be mechanical energy other than pressure potential energy in Bernoulli's principle.
  • C is a constant and ⁇ is the density of the fluid.
  • ⁇ is the flow velocity of the fluid at the above-mentioned position
  • g is the gravity acceleration
  • the value can be 9.8N/kg
  • h is the distance between the above-mentioned position and the preset horizontal plane.
  • the preset horizontal plane may be parallel to the crystallization interface, for example, the preset horizontal plane may be sea level.
  • Bernoulli's principle can also be simplified to is a constant. In the present invention, whether Bernoulli's principle is simplified or not is not specifically limited.
  • the initial mechanical energy of the second gas at the crystallization interface in addition to the pressure potential energy, can be: at the start of temperature regulation, the second gas introduced into the single crystal furnace, the initial mechanical energy at the crystallization interface.
  • Kinetic energy parameters and initial gravitational potential energy parameters are: the product of the density of the second gas at the start time of temperature adjustment and the square of the flow rate at the crystallization interface at the start time of temperature adjustment.
  • the initial gravitational potential energy parameter of the second gas is: the product of the temperature adjustment start time, the density of the second gas, the distance between the crystal interface and the preset horizontal plane at the temperature adjustment start time, and the gravity acceleration.
  • the preset horizontal plane only needs to be parallel to the crystal interface, and there is no specific limit on the selection of the preset horizontal plane.
  • the preset horizontal plane can be the sea level, or the preset horizontal plane can be the crystallographic interface, as long as the preset horizontal plane is parallel to the crystallographic interface, and there is no limit to the specific selection of the preset horizontal plane. That is, the initial mechanical energy of the second gas at the crystallization interface in addition to the pressure potential energy is formula 2: ⁇ 1 is the temperature adjustment start time, the second The density of the gas. ⁇ 1 is the flow rate of the second gas at the crystallization interface at the start time of temperature adjustment. h 1 is the distance between the crystallization interface and the preset horizontal plane at the start time of temperature adjustment.
  • the above step 101 is to obtain the starting mechanical energy Q1 of all the gases or the second gas that passed into the single crystal furnace A at 10:13:20 on October 20, 2021, except for the pressure potential energy.
  • Q1 can include the initial kinetic energy parameter and the initial gravitational potential energy parameter.
  • the initial kinetic energy parameter is: the density ⁇ 1 of the second gas introduced into the single crystal furnace A at 10:13:20 on October 20, 2021, and 2021
  • the flow rate of the second gas introduced into the single crystal furnace A at 10:13:20 on October 20, 2019 at the crystallization interface is the product of the square of ⁇ 1 .
  • the starting gravitational potential energy parameters are: the density ⁇ 1 of the second gas introduced into the single crystal furnace A at 10:13:20 on October 20, 2021, and the distance between the crystallization interface and the preset horizontal plane at the start time of temperature adjustment. h 1 , the product of gravity acceleration.
  • Step 102 During the period from the temperature adjustment start time to the finishing end time, based on Bernoulli's principle, the real-time mechanical energy of the first gas at the crystallization interface, except for the pressure potential energy, is equal to the real-time mechanical energy except for the pressure potential energy.
  • the absolute value of the difference in initial mechanical energy is less than or equal to the second preset value.
  • the first gas is everywhere at the crystallization interface during the period from the start of the temperature adjustment to the end of the finish.
  • the real-time mechanical energy other than the pressure potential energy can be: the period from the start of the temperature adjustment to the end of the finish.
  • the real-time kinetic energy parameters and real-time gravitational potential energy parameters of the first gas flowing into the single crystal furnace at the crystallization interface at the first moment, the real-time kinetic energy parameters and real-time gravitational potential energy parameters of the first gas flowing into the single crystal furnace at the crystallization interface.
  • the real-time kinetic energy parameter of the first gas is: the product of the density of the first gas at the first moment and the square of the flow rate at the crystal interface at the first moment during the period from the temperature adjustment start time to the end time.
  • the real-time gravitational potential energy parameter of the first gas is: the product of the density of the first gas at the first moment, the distance between the crystal interface and the aforementioned preset horizontal plane at the first moment, and the gravity acceleration.
  • the preset horizontal plane is the same horizontal plane as the preset horizontal plane in step 101. That is, the real-time mechanical energy of the first gas at the crystallization interface in addition to the pressure potential energy is Formula 3: ⁇ 2 is the density of the first gas at the first moment. ⁇ 2 is the flow rate of the first gas at the crystallization interface at the first moment. g is the acceleration of gravity, and its value can also be 9.8N/kg. h 2 is the distance between the crystallization interface and the preset horizontal plane at the first moment.
  • the real-time mechanical energy Q2 except the pressure potential energy of the first gas at the crystallization interface is controlled, and the initial mechanical energy Q1 except the pressure potential energy is controlled.
  • the absolute value of the difference is less than or equal to the second preset value. That is to say, the real-time mechanical energy Q2 except the pressure potential energy of the first gas at the crystallization interface is basically consistent with the initial mechanical energy Q1 except the pressure potential energy. .
  • p 1 here is the pressure potential energy of the second gas at the crystallization interface at the start time of temperature adjustment, which can be pressure.
  • p 2 here is the period from the temperature adjustment start time to the finishing end time.
  • the pressure potential energy of the first gas at the crystallization interface can be pressure.
  • C in Bernoulli's equation is a constant.
  • this step 102 it may be to control and
  • the absolute value of the difference between the two is less than or equal to the second preset value, which can ensure that the difference between p 1 and p 2 is small.
  • Controlling the pressure of the gas flowing into the single crystal furnace at the crystallization interface is more stable, the operability is stronger, and the control is more precise.
  • the diameter of the single crystal rod is more stable, and the same impurity is more stable in the single crystal rod.
  • the concentration distribution is more uniform everywhere, and the quality uniformity of the single crystal ingot is better, further improving the quality of the single crystal ingot.
  • the above step 102 is to control the time period from 10:13:20 on October 20, 2021 to 12:13:20 on October 21, 2021, to pass into the single crystal furnace at each moment
  • the absolute value of the difference between the real-time mechanical energy Q2 of all gases in A or the first gas except pressure potential energy and the initial mechanical energy Q1 except pressure potential energy is less than or equal to the second preset value, except for pressure potential energy
  • the real-time mechanical energy Q1 outside of the At the first moment the product of the density ⁇ 2 of the first gas flowing into the single crystal furnace A and the square of the flow rate ⁇ 2 of the first gas flowing into the single crystal furnace A at the crystal interface at the first moment.
  • the real-time gravitational potential energy parameter is: the density ⁇ 2 of the first gas flowing into the single crystal furnace A at the first moment, the distance h 2 between the crystal interface and the preset horizontal plane at the first moment, and the gravity acceleration. product.
  • the first moment here is any moment in the period from the temperature adjustment start time to the finishing end time.
  • the aforementioned second preset value can be set according to the stability requirements of the diameter of the single crystal silicon rod that needs to be controlled. The higher the requirement for the stability of the diameter of the single crystal silicon rod, the smaller the second preset value.
  • the second preset value may be 6 J/m 3 . That is, during the period from the start of temperature adjustment to the end of temperature adjustment, the first gas introduced into the single crystal furnace at each time is controlled, and the real-time mechanical energy Q2 at the crystallization interface in addition to the pressure potential energy is controlled to be equal to the second gas introduced into the single crystal furnace at the start of temperature adjustment.
  • the absolute value of the difference between the initial mechanical energy Q1 at the crystallization interface in addition to the pressure potential energy is less than or equal to 6J/m 3.
  • the pressure at the crystallization interface is more stable, which makes the diameter of the pulled single crystal ingot less volatile and the diameter of the pulled single crystal ingot more stable.
  • the concentration distribution of the same impurity at various locations of the single crystal ingot is roughly the same, the quality uniformity of the single crystal ingot is better, and the quality of the single crystal ingot is also improved.
  • the absolute value of the difference between the second gas passed into the single crystal furnace and the starting mechanical energy Q1 in addition to the pressure potential energy at the crystallization interface is 0, 0.2J/m 3 , 1.3J/m 3 , 1.9J /m 3 , 2.5J/m 3 , 3J/m 3 , 4J/m 3 , 5J/m 3 , 5.3J/m 3 , 6J/m 3 .
  • the first gas and the second gas are the same, and the above step 101 may include: obtaining the flow rate of the second gas at the crystallization interface at the start time of the temperature adjustment.
  • the above step 102 may include: controlling the flow rate of the first gas at the crystallization interface at the first moment, and the flow rate of the second gas at the crystallization interface at the temperature adjustment start time during the period from the temperature adjustment start time to the finishing end time.
  • the absolute value of the difference is less than or equal to the third preset value. That is to say, during the period from the temperature adjustment start time to the finishing end time, the composition and type of gas flowing into the single crystal furnace are the same. Then, the density ⁇ 2 of the first gas and the density ⁇ 1 of the second gas are equal.
  • the crucible position is usually changed so that the position of the crystallization interface remains unchanged. That is to say, the position of the crystallization interface remains unchanged from the beginning of the temperature adjustment to the end of the finishing time.
  • h 1 h 2
  • the flow rate ⁇ 1 at the crystallization interface at the beginning of the temperature adjustment, and the flow rate ⁇ 2 of the first gas at the crystallization interface at each time from the start of the temperature adjustment to the end of the finishing time are stable , it can be ensured that the pressure of the gas flowing into the single crystal furnace at the crystallization interface is basically stable at each moment from the beginning of the temperature adjustment to the end of the temperature adjustment. Only by controlling the flow rate of the gas at the crystallization interface, the stability of the diameter of the drawn single crystal silicon rod can be ensured. There are fewer parameters to control, and the process is relatively simple and easy to implement.
  • the aforementioned third preset value can be set according to the stability requirements of the diameter of the single crystal silicon rod that needs to be controlled. The higher the requirement for the stability of the diameter of the single crystal silicon rod, the smaller the third preset value.
  • the third preset value may be 2mm/min. That is to say, in the period from the temperature adjustment start time to the finishing end time, the flow rate ⁇ 2 of the first gas introduced into the single crystal furnace at each moment is controlled at the crystallization interface, and the flow rate ⁇ 2 at the crystallization interface is the same as the temperature adjustment start time, and the flow rate ⁇ 2 introduced into the single crystal furnace.
  • the flow rate of the second gas at the crystallization interface ⁇ 1 is less than or equal to 2mm/min, from the start of temperature adjustment to the end of During the period at the end of the tail, the pressure at the crystal interface is more stable, making the diameter of the single crystal rod obtained by drawing less volatile, and the diameter of the single crystal rod obtained by drawing having better stability.
  • the concentration distribution of the same impurity in the single crystal rod is roughly equal, and the quality uniformity of the single crystal rod is better, which also improves the quality of the single crystal rod.
  • the flow rate ⁇ 2 of the first gas introduced into the single crystal furnace at each time is controlled to be the same as the flow rate ⁇ 2 at the crystallization interface at the start time of temperature adjustment.
  • the flow rate of the second gas at the crystal interface is ⁇ 1 , and the absolute values of the differences between the two are 0, 0.1mm/min, 0.3mm/min, 0.9mm/min, 1.1mm/min, 1.3mm/min, 1.4mm/min, 1.5mm/min, 1.8mm/min, 2mm/min.
  • the above-mentioned period from the start time of temperature adjustment to the end time, controlling the absolute value of the difference between the flow rate of the first gas at the crystallization interface at the first moment and the flow rate of the second gas at the crystallization interface at the start time of temperature adjustment to be less than or equal to the third preset value can include: obtaining the minimum flow cross-sectional area at each point in the flow path from the first moment when the first gas flows out from the lower edge of the heat shield 11 to the first moment when the first gas is discharged from the single crystal furnace during the period from the start time of temperature adjustment to the end time; multiplying the minimum flow cross-sectional area corresponding to the first moment by the flow rate of the first gas at the crystallization interface at the first moment to obtain the first real-time flow rate at the first moment.
  • the first gas of the first real-time flow rate is introduced into the single crystal furnace.
  • the flow rate is easier to measure and control, and converting the flow rate into a flow rate that is easy to measure and control is simpler to operate.
  • the position where the gas is discharged from the single crystal furnace is usually located at the bottom of the single crystal furnace. At different times, the gas flows out from the lower edge of the heat screen to the flow path before the gas is discharged from the single crystal furnace. , the position of the minimum flow cross-sectional area S 1 is different. In this flow path, the minimum flow cross-sectional area can play a key role in determining the flow rate ⁇ of the gas at the crystallization interface.
  • the minimum flow cross-sectional area S 1 of , obtaining the first real-time flow rate can ensure that the pressure at the crystallization interface is more stable during the period from the temperature adjustment start time to the end time, making the single crystal ingot obtained by The fluctuation in diameter is smaller, and the diameter stability of the single crystal rod obtained by drawing is better.
  • the concentration distribution of the same impurity in the single crystal rod is roughly equal, and the quality uniformity of the single crystal rod is better, which also improves the quality of the single crystal rod.
  • the aforementioned period from the temperature adjustment start time to the finishing end time is to obtain the first moment, after the first gas flows out from the lower edge of the heat screen, to the flow path before the first gas is discharged from the single crystal furnace,
  • the method may also include: obtaining each crucible position position, the minimum flow cross-sectional area at each point in the flow path from the lower edge of the heat screen to before the gas is discharged from the single crystal furnace, and the minimum flow cross-sectional area corresponding to the crucible position is stored in the first crucible bit area list.
  • the crucible position is the distance between the upper edge of the crucible 15 and the crystal interface 2 during the crystal pulling process.
  • the minimum flow intersection at each point in the flow path after different gases flow out from the lower edge of the heat screen to before the gas is discharged from the single crystal furnace The areas are equal, that is to say, one crucible position corresponds to a minimum flow cross-sectional area. Therefore, obtaining the minimum flow cross-sectional area corresponding to the crucible position in advance and storing it in the first crucible position area list can reduce repeated work. When the minimum flow cross-sectional area is needed later, you only need to look up the table, which can improve efficiency. .
  • the above-mentioned period from the temperature adjustment start time to the finishing end time is to obtain the first moment, from when the first gas flows out from the lower edge of the heat screen to before the first gas is discharged from the single crystal furnace, the flow path at each point
  • the minimum flow cross-sectional area may include: obtaining the first crucible position corresponding to the first moment, querying the minimum flow cross-sectional area corresponding to the first crucible position from the aforementioned first crucible position area list, and obtaining the minimum flow cross-sectional area corresponding to the first crucible position.
  • the minimum flow cross-sectional area corresponding to the first moment is to obtain the first moment, from when the first gas flows out from the lower edge of the heat screen to before the first gas is discharged from the single crystal furnace, the flow path at each point
  • the minimum flow cross-sectional area may include: obtaining the first crucible position corresponding to the first moment, querying the minimum flow cross-sectional area corresponding to the first crucible position from the aforementioned first
  • the aforementioned method obtains the minimum flow cross-sectional area at each point of each crucible position, from the lower edge of the heat screen to the flow path before the gas is discharged from the single crystal furnace, and sets the minimum flow area corresponding to the crucible position.
  • the cross-sectional area, stored in the first bin area list may include the following sub-steps S1-S5:
  • Sub-step S1 obtain each crucible position, take the distance between the endpoint of the lower edge of the heat screen 11 close to the crystallization interface 2 and the first center line L1 of the single crystal furnace as the radius, take the first plane where the endpoint is located and the distance between the endpoint and the first centerline L1 of the single crystal furnace as the radius.
  • the first intersection point of the first center line L1 is the center of the circle, forming the first surface area of the side of the cylinder.
  • the first center line L1 is perpendicular to the crystal interface 2 , and the first plane is parallel to the crystal interface 2 .
  • Sub-step S2 obtain each crucible position, take the connection line between the upper edge of the inner wall of the crucible 14 and the second point on the R arc 1121 of the outer wall 112 of the heat screen 11 as the bus line, and use the aforementioned first center line L1 as the center line, A second surface area is formed on the sides of the frustum. The second point is located on the line connecting the center of the R arc 1121 of the outer wall 112 of the heat shield 11 and the upper edge of the inner wall of the crucible 14 .
  • Sub-step S3 obtain each crucible position.
  • the line connecting the upper edge of the outer wall of the crucible 15 and the lower edge of the inner wall of the transition plate 12 is the bus line
  • the first center line L1 is the center line. , forming the third surface area of the sides of the circular cone.
  • Sub-step S4 obtain each crucible position, enter the transition plate 12 with the crucible leg 15, the connection line between the upper edge of the outer wall of the crucible leg 15 and the lower edge of the inner wall of the transition plate 12 is the bus line, and the first center line L1 is the center line.
  • Sub-step S5 for the same crucible position, select the smallest surface area from the first surface area, the second surface area, the third surface area, and the fourth surface area as the minimum flow cross-sectional area corresponding to the crucible position, And stored in the first pot area list.
  • the above-mentioned first surface area, second surface area, third surface area, and fourth surface area product are more significant.
  • the four have a greater impact on the pressure of the gas at the crystal interface. Therefore, for the same crucible position, choose from the above four. With the smallest surface area, the calculated flow rate is more accurate.
  • transition plate 12 mainly functions to support the upper insulation tube 17 and, at the same time, plays a transitional role in changing the inner diameters of the middle insulation tube 13 and the upper insulation tube 17 .
  • It can be: first obtain the second crucible position corresponding to the temperature adjustment start time, and then query to obtain the minimum flow cross-sectional area corresponding to the second crucible position from the aforementioned first crucible position area list.
  • the upper edge of a device mentioned in the full text is closer to the furnace cover, the lower edge is further away from the furnace cover, the inner wall is closer to the first center line L1 of the single crystal furnace, and the outer wall is further away from the first center line L1 of the single crystal furnace.
  • the above-mentioned period from the temperature adjustment start time to the finishing end time controls the flow rate of the first gas at the crystallization interface at the first time, and the flow rate of the second gas at the crystallization interface at the temperature adjustment start time.
  • the absolute value of the difference which is less than or equal to the third preset value, may include: obtaining the flow cross-sectional area of the first gas at the crystallization interface at the first moment during the period from the temperature adjustment start time to the finishing end time. S 2 , and then multiply the flow velocity ⁇ of the first gas at the crystal interface at the first moment by the flow cross-sectional area S 2 at the crystal interface corresponding to the first moment, to obtain the second real-time value of the first moment flow.
  • the flow rate is easier to measure and control, and the operation is simpler when the flow rate is converted into a flow rate that is easy to measure and control.
  • the flow rate ⁇ of the first gas at the crystal interface at the first moment is directly related to the flow cross-sectional area S 2 of the first gas at the crystal interface at the first moment.
  • the calculated second real-time flow rate of the flow cross-sectional area S 2 of the first gas at the crystal interface at the first moment has a more direct impact on the stability of the pressure of the first gas at the crystal interface at the first moment.
  • the pressure at the crystal interface is more stable, making the diameter of the drawn single crystal ingot less volatile, and the diameter of the drawn single crystal ingot is smaller. Diameter stability is better.
  • the concentration distribution of the same impurity in the single crystal rod is roughly equal, and the quality uniformity of the single crystal rod is better, which also improves the quality of the single crystal rod.
  • the method may also include: obtaining each The flow cross-sectional area at the crystallization interface at each crucible position is stored in the second crucible position area list.
  • Obtaining the flow cross-sectional area of the first gas at the crystallization interface at the first moment in the aforementioned period from the temperature adjustment start time to the finishing end moment may include: obtaining the first crucible position corresponding to the first moment, and then obtaining the first crucible position from the first moment.
  • the present invention also provides a single crystal silicon rod, which is prepared by any of the foregoing crystal pulling methods.
  • the single crystal silicon rod has the same or similar beneficial effects as any of the foregoing crystal pulling methods. In order to avoid Repeat, will not go into details here.
  • the present invention also provides a single crystal furnace, which is used to pull crystals using any of the aforementioned crystal pulling methods.
  • the single crystal furnace has the same or similar beneficial effects as any of the aforementioned crystal pulling methods. In order to avoid Repeat, will not go into details here.
  • the outer diameter of the outer wall 112 of the heat shield 11 is 614mm
  • the inner diameter of the transition plate 12 is 810mm
  • the outer diameter of the crucible 15 is 740mm
  • the inner diameter of the crucible 14 is 680mm.
  • the crucible 14 can be a quartz crucible.
  • the height difference of the crucible 15 can be 15mm
  • the lid distance is 28mm
  • the heating distance is 72mm
  • the radius of the R arc 1121 of the outer wall 112 of the heat shield 11 is 100mm.
  • the gas flowing into the single crystal furnace is all argon gas, that is, the first gas and the second gas are both argon gas.
  • the flow rate L 0 of argon gas is 70 slpm (stard liter per minute, standard liter per minute).
  • the corresponding crucible position at the beginning of temperature adjustment is -80mm.
  • the flow cross-sectional area at the crystallization interface is 136383.22mm 2 .
  • the crucible position decreases, and the flow rate ⁇ 2 of the argon gas at the crystallization interface at each moment is controlled to be 513.26mm/min.
  • the corresponding crystallization interface at each moment is used.
  • the surface area S 2 ⁇ 2 L t , where L t is the second real-time flow rate of argon gas corresponding to each moment or each crucible position during the period from the temperature adjustment start time to the closing end time.
  • the second real-time flow rate of argon corresponding to that moment or crucible position is passed into the single crystal furnace.
  • the gas flowing into the single crystal furnace is all argon gas, that is, the first gas and the second gas are both argon gas.
  • the flow rate L 0 of argon gas is 70slpm (stard liter per minute, standard liter per minute).
  • the crucible position corresponding to the temperature adjustment start time is -80mm.
  • the smallest surface area is the second surface area, and the second surface area is 136391.97 mm 2
  • the crucible position decreases, and the flow rate ⁇ 2 of the argon gas at the crystallization interface at each moment is controlled to be 513.23mm/min.
  • the minimum surface area corresponding to each moment is used.
  • L t1 is the first real-time flow rate of argon gas corresponding to each moment or each crucible position during the period from the temperature adjustment start time to the closing end time.
  • L t1 is the first real-time flow rate of argon gas corresponding to each moment or each crucible position during the period from the temperature adjustment start time to the closing end time.
  • thermal field is the same as that in Embodiment 1, and will not be described again in order to avoid repetition.
  • the gas flowing into the single crystal furnace is all argon.
  • the flow rate of argon gas is 70slpm.
  • the corresponding crucible position at the start time of temperature adjustment is -80mm.
  • the set diameter of the single crystal ingot in Example 1, Example 2 and Comparative Example is all 300 mm.
  • the silicon materials used in Example 1, Example 2 and Comparative Example are the same. Except for the flow rate of argon gas or the flow rate of argon gas at the crystallization interface, the remaining process parameters in Example 1, Example 2 and Comparative Examples are the same.
  • Figure 3 shows a comparative diagram of the diameter fluctuations of the single crystal ingot 3 in Embodiment 1 of the present invention and the single crystal ingot in the comparative example.
  • the meaning of the numerical representation in Figure 3 is: the deviation of the diameter of the single crystal rod from the set diameter of 300mm.
  • the unit of the value can be mm.
  • the fluctuations in the diameter of the single crystal rods drawn in Example 1 and Comparative Example are shown in Figure 3.
  • the solid line curve in Figure 3 is the fluctuation of the diameter of the single crystal ingot 3 drawn in Example 1
  • the dotted line curve in Figure 3 is the fluctuation in the diameter of the single crystal ingot 3 drawn in the Comparative Example. It can be seen from Figure 3 that the fluctuation in the diameter of the single crystal ingot 3 obtained by drawing in Example 1 is significantly smaller than the fluctuation in the diameter of the single crystal ingot 3 obtained by drawing in the comparative example. Compared with the comparative example in Example 1, the fluctuation in the diameter of the single crystal rod 3 is roughly reduced from ⁇ 1 mm to ⁇ 0.5 mm.
  • Example 1 during the period from the temperature adjustment start time to the finishing end time, the pressure p of the argon gas at the crystallization interface will affect the melting point of the silicon material, roughly determining the crystallization temperature, thereby affecting the crystallization speed, and ultimately affecting the drawn single unit.
  • Example 1 during the period from the temperature adjustment start time to the finishing end time, the pressure p of the argon gas at the crystallization interface remains unchanged, then the crystallization temperature is basically stable, the crystallization speed is basically stable, and the single crystal rod obtained by pulling The fluctuation in the diameter of 3 is small, and the stability of the diameter of the single crystal rod 3 obtained by drawing is better.
  • Example 1 and Example 2 also reduce the usage of argon gas, which can reduce costs. It should be noted that the fluctuation in diameter of the single crystal ingots drawn in Example 2 and Comparative Example is similar to Figure 3, and is not shown in Figure 3 in order to avoid duplication and simplify the illustration.
  • the methods of the above embodiments can be implemented by means of software plus the necessary general hardware platform. Of course, it can also be implemented by hardware, but in many cases the former is better. implementation.
  • the technical solution of the present invention can be embodied in the form of a software product in essence or the part that contributes to the existing technology.
  • the computer software product is stored in a storage medium (such as ROM/RAM, disk, CD), including several instructions to cause a terminal (which can be a mobile phone, a computer, a server, an air conditioner, or a network device, etc.) to execute the methods described in various embodiments of the present invention.
  • the device embodiments described above are only illustrative.
  • the units described as separate components may or may not be physically separated.
  • the components shown as units may or may not be physical units, that is, they may be located in One location, or it can be distributed across multiple network units. Some or all of the modules can be selected according to actual needs to achieve the purpose of the solution of this embodiment. Persons of ordinary skill in the art can understand and implement the method without any creative effort.

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Abstract

本发明提供了一种拉晶方法、单晶硅棒和单晶炉，涉及晶体生长技术领域。拉晶方法包括：从调温开始时刻之后至收尾结束时刻的时段内，控制各个时刻，通入单晶炉的第一气体，在结晶界面处的第一压强，与调温开始时刻，通入所述单晶炉的第二气体，在所述结晶界面处的第二压强，两者的差值的绝对值，小于或等于第一预设值。本发明中，在调温开始时刻至收尾结束时刻的时段中，不同时刻对应的结晶界面的压强大致相等，则不同时刻对应的结晶温度大致相等，不同时刻对应的结晶速度大致相等，不同时刻对应的晶棒直径大致相等，使得最终拉制得到的单晶晶棒的直径波动小较小。同时，同一种杂质在晶棒各处的浓度分布大致相等，晶棒质量均匀性较好。

Description

一种拉晶方法、单晶硅棒和单晶炉
本申请要求在2022年09月20日提交中国专利局、申请号为202211148316.6、名称为“一种拉晶方法、单晶硅棒和单晶炉”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本发明涉及晶体生长技术领域，特别是涉及一种拉晶方法、单晶硅棒和单晶炉。
背景技术
将硅材料加工成单晶硅目前常用的生产工艺为直拉法。直拉法主要分为装料、熔料、降温调整引晶温度、引晶、放肩、转肩、等径、收尾等工序。
然而，现有的拉晶方法拉晶得到的单晶硅棒的直径波动较大，单晶硅棒的质量欠佳。
发明内容
本发明提供一种拉晶方法、单晶硅棒和单晶炉，旨在解决现有的拉晶方法拉晶得到的单晶硅棒的直径波动较大，单晶硅棒的质量欠佳的问题。
本发明的第一方面，提供一种拉晶方法，所述方法包括：
步骤S，从调温开始时刻之后至收尾结束时刻的时段内，控制各个时刻，通入单晶炉的第一气体，在结晶界面处的第一压强，与调温开始时刻，通入所述单晶炉的第二气体，在所述结晶界面处的第二压强，两者的差值的绝对值，小于或等于第一预设值。
本发明中，从调温开始时刻至收尾结束时刻的时段，在不同时刻通入单晶炉的气体在结晶界面的压强大致相等，同一时刻通入单晶炉的气体在结晶界面的压强，等于该时刻结晶界面的压强，就是说，从调温开始时刻至收尾结束时刻的时段，保持结晶界面的压强基本稳定。结晶界面的压强会大致决定硅料的熔点，大致决定结晶温度，结晶温度会大致决定结晶速度，宏观体现在拉制得到的单晶晶棒的直径的稳定性，本发明中，在调温开始时刻至收尾结束时刻的时段中，不同时刻对应的结晶界面的压强大致相等，能够保障在调温开始时刻至收尾结束时刻的时段中，不同时刻对应的结晶温度大致相 等，进而能够保障在调温开始时刻之后至收尾结束时刻的时段中，不同时刻对应的结晶速度大致相等，最终能够保障在调温开始时刻之后至收尾结束时刻的时段中，不同时刻对应的晶棒直径大致相等，使得最终拉制得到的单晶晶棒的直径波动小较小，晶棒的直径的稳定性较高，进而提升了晶棒的质量。同时，结晶界面的压强会影响杂质的分凝系数，进而影响杂质在晶棒各处的浓度分布，本发明中，从调温开始时刻之后至收尾结束时刻的时段中，不同时刻，结晶界面的压强大致相等，则，同一种杂质在晶棒各处的浓度分布大致相等，晶棒质量均匀性较好，同样提升了晶棒的质量。
可选地，所述步骤S之前，所述方法还包括：
基于伯努利原理，获取所述第二气体在所述结晶界面处，除了压力势能之外的起始机械能；
所述步骤S，包括：
从调温开始时刻之后至收尾结束时刻的时段，基于伯努利原理，控制所述第一气体在所述结晶界面处，除了压力势能之外的实时机械能，与所述起始机械能的差值的绝对值，小于或等于第二预设值。
可选地，所述第一气体，与所述第二气体相同；所述基于伯努利原理，获取所述第二气体在所述结晶界面处，除了压力势能之外的起始机械能，包括：
获取所述第二气体，在调温开始时刻，在所述结晶界面处的流速；
所述从调温开始时刻之后至收尾结束时刻的时段，基于伯努利原理，控制所述第一气体在所述结晶界面处，除了压力势能之外的实时机械能，与所述除了压力势能之外的起始机械能的差值的绝对值，小于或等于第二预设值，包括：
从调温开始时刻之后至收尾结束时刻的时段，控制所述第一时刻，所述第一气体，在所述结晶界面处的流速，与所述第二气体，在调温开始时刻，结晶界面处的流速的差值的绝对值，小于或等于第三预设值。
可选地，所述从调温开始时刻之后至收尾结束时刻的时段，控制所述第一时刻，所述第一气体，在所述结晶界面处的流速，与所述第二气体，在调温开始时刻，结晶界面处的流速的差值的绝对值，小于或等于第三预设值，包括：
从调温开始时刻之后至收尾结束时刻的时段，获取所述第一时刻，所述第一气体从热屏下沿流出后，至所述第一气体从所述单晶炉中排出之前的流通路径中，各点处的最小的流通截面积；
用所述第一时刻对应的最小的流通截面积，乘以所述第一时刻，所述第一气体，在结晶界面处的流速，得到所述第一时刻的第一实时流量；
在所述第一时刻，向所述单晶炉内通入所述第一实时流量的所述第一气体。
可选地，所述从调温开始时刻之后至收尾结束时刻的时段，获取所述第一时刻，所述第一气体从热屏下沿流出后，至所述第一气体从所述单晶炉中排出之前的流通路径中，各点处的最小的流通截面积之前，所述方法还包括：
获取各个埚位处，所述流通路径中，各点处的最小的流通截面积，并将所述埚位对应的最小的流通截面积，存储在第一埚位面积列表中；
所述从调温开始时刻之后至收尾结束时刻的时段，获取所述第一时刻，所述第一气体从热屏下沿流出后，至所述第一气体从所述单晶炉中排出之前的流通路径中，各点处的最小的流通截面积，包括：
获取所述第一时刻对应的第一埚位；
从所述第一埚位面积列表中，查询得到所述第一埚位对应的最小的流通截面积。
可选地，所述获取各个埚位处，所述流通路径中，各点处的最小的流通截面积，并将所述埚位对应的最小的流通截面积，存储在第一埚位面积列表中，包括：
获取各个埚位处，以热屏下沿靠近所述结晶界面的端点，与所述单晶炉的第一中线之间的距离，为半径，以所述端点所在的第一平面与所述第一中线的第一交点为圆心，形成的圆柱体的侧面的第一表面积；其中，所述第一中线和所述结晶界面垂直，所述第一平面和所述结晶界面平行；
获取各个埚位处，以坩埚的内壁上沿和所述热屏的外壁的R弧上的第二点的连线为母线，以所述第一中线为中心线，形成的圆台的侧面的第二表面积；其中，所述第二点位于所述热屏的外壁的R弧的圆心，与所述坩埚的内壁上沿的连线上；
获取各个埚位处，以埚帮进入过渡盘前，埚帮的外壁上沿和过渡盘的内 壁下沿两者连线为母线，以所述第一中线为中心线，形成的圆台的侧面的第三表面积；
获取各个埚位处，以埚帮进入过渡盘，埚帮的外壁上沿和过渡盘的内壁下沿两者连线为母线，以所述第一中线为中心线，形成的圆台的侧面的第四表面积；
针对同一埚位处，从所述第一表面积、第二表面积、第三表面积、第四表面积四者中，选择最小的表面积，作为所述埚位对应的最小的流通截面积，并存储在所述第一埚位面积列表中。
可选地，所述从调温开始时刻之后至收尾结束时刻的时段，控制所述第一时刻，所述第一气体，在所述结晶界面处的流速，与所述第二气体，在调温开始时刻，结晶界面处的流速的差值的绝对值，小于或等于第三预设值，包括：
从调温开始时刻之后至收尾结束时刻的时段，获取所述第一时刻，所述第一气体在所述结晶界面处的流通截面积；
用所述第一时刻对应的结晶界面处的流通截面积，乘以所述第一时刻，所述第一气体，在结晶界面处的流速，得到所述第一时刻的第二实时流量；
在所述第一时刻，向所述单晶炉内通入所述第二实时流量的所述第一气体。
可选地，所述从调温开始时刻之后至收尾结束时刻的时段，获取所述第一时刻，所述第一气体在所述结晶界面处的流通截面积之前，所述方法还包括：
获取各个埚位处，所述结晶界面处的流通截面积，并将各个埚位处，所述结晶界面处的流通截面积，存储在第二埚位面积列表中；
所述从调温开始时刻之后至收尾结束时刻的时段，获取所述第一时刻，所述第一气体在所述结晶界面处的流通截面积，包括：
获取所述第一时刻对应的第一埚位；
从所述第二埚位面积列表中，查询得到所述第一埚位对应的流通截面积。
可选地，所述第一预设值为：10pa。
可选地，所述第二预设值为：6J/m3。
可选地，所述第三预设值为：2mm/min。
可选地，所述第一气体包括拉晶过程的保护气体，所述第二气体包括拉晶过程的保护气体。
可选地，所述保护气体包括：氮气，和/或，惰性气体。
可选地，所述惰性气体包括氩气。
本发明的第二方面，还提供一种单晶硅棒，采用任一前述的拉晶方法制备得到。
本发明的第三方面，还提供一种单晶炉，所述单晶炉用于采用任一前述的拉晶方法进行拉晶。
上述说明仅是本申请技术方案的概述，为了能够更清楚了解本申请的技术手段，而可依照说明书的内容予以实施，并且为了让本申请的上述和其它目的、特征和优点能够更明显易懂，以下特举本申请的具体实施方式。
附图说明
为了更清楚地说明本申请实施例或相关技术中的技术方案，下面将对实施例或相关技术描述中所需要使用的附图作一简单地介绍，显而易见地，下面描述中的附图是本申请的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1示出了本发明实施例中的一种单晶炉的结构示意图；
图2示出了本发明实施例中的一种拉晶方法的步骤流程图；
图3示出了本发明实施例中的晶棒与对比例的晶棒的直径波动情况对比图。
附图标记说明：
11-热屏，111-热屏的内壁，112-热屏的外壁，1121-热屏的外壁的R弧，
12-过渡盘，13-中保温筒，14-坩埚，15-埚帮，16-下保温筒，17-上保温筒，2-结晶界面，3-单晶晶棒。
具体实施例
为使本申请实施例的目的、技术方案和优点更加清楚，下面将结合本申请实施例中的附图，对本申请实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本申请一部分实施例，而不是全部的实施例。基于本申请中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获 得的所有其他实施例，都属于本申请保护的范围。
发明人发现，现有的拉晶方法拉晶得到的单晶硅棒的直径波动较大，单晶硅棒的质量欠佳的主要原因在于：现有技术的拉晶方法，从调温开始时刻至收尾结束时刻的时段，在各个时刻，对结晶界面处的压强不作限定，导致从调温开始时刻至收尾结束时刻的时段，在各个时刻，结晶界面处的压强波动较大。同时，发明人创造性的发现，从调温开始时刻至收尾结束时刻的时段，在各个时刻，结晶界面处的压强会大致决定该时刻的硅料的熔点，进而影响结晶温度，结晶温度会大致决定结晶速度，宏观体现在拉制得到的单晶晶棒的直径的稳定性。因此，为了解决该问题，本发明的主要思路在于：从调温开始时刻至收尾结束时刻的时段，在各个时刻，通入单晶炉的气体在位于结晶界面处的压强大致稳定，同一时刻通入单晶炉的气体在结晶界面的压强，等于该时刻结晶界面的压强，就是从调温开始时刻至收尾结束时刻的时段，保持结晶界面的压强基本稳定，进而使得拉制得到的晶棒的直径的波动性较小，拉制得到的单晶晶棒的直径的稳定性较好。同时，结晶界面的压强会影响杂质的分凝系数，进而影响杂质在单晶晶棒各处的浓度分布，本发明中，在调温开始时刻之后至收尾结束时刻的时段中，不同时刻，结晶界面的压强大致相等，则，同一种杂质在单晶晶棒各处的浓度分布大致相等，单晶晶棒质量均匀性较好，同样提升了单晶晶棒的质量。
更为具体的，直拉法主要分为装料、熔料、降温调整引晶温度、引晶、放肩、转肩、等径、收尾等工序。此处的调温开始时刻就是：降温调整引晶温度该工序开始的时刻。第一气体为调温开始时刻之后，至收尾结束时刻的时段内，各个时刻，通入单晶炉的气体，例如，单晶炉A某次拉晶过程中，调温开始时刻为2021年10月20日10:13:20，收尾结束时刻的时刻为：2021年10月21日12:13:20，则，该第一气体即为：2021年10月20日10:13:20之后，至2021年10月21日12:13:20的时间段内，各个时刻通入该单晶炉A的所有气体。该第一气体可以为混合气体或者单一种类的气体，本发明对此不作具体限定。该第一压强就是，第一气体在调温开始时刻之后，至收尾结束时刻的时段内，各个时刻，通入单晶炉的气体在结晶界面的压强。例如，针对上述例子，第一压强就是2021年10月20日10:13:20之后，至2021年10月21日12:13:20的时间段内，各个时刻通入该单晶炉A的所有气体在结晶界面的压强。此处的第一气体和第一压强对应同一时刻。
该第二气体为：调温开始时刻，通入单晶炉的所有气体。该第二压强就是，调温开始时刻，通入该单晶炉的第二气体，在结晶界面处的压强。例如针对上述例子，在结晶界面处的第二压强就是：调温开始时刻为2021年10 月20日10:13:20，通入该单晶炉A的所有气体在结晶界面处的压强。
更为具体的，对结晶界面的压强产生影响的主要因素是通入单晶炉的气体，而且，结晶过程或晶棒拉制过程主要是从调温开始时刻至收尾结束时刻的时段。因此，本发明从调温开始时刻之后至收尾结束时刻的时段内，控制各个时刻，通入单晶炉的第一气体，在结晶界面处的第一压强，与调温开始时刻，通入该单晶炉的第二气体，在结晶界面处的第二压强，两者的差值的绝对值，小于或等于第一预设值，就是说，保持的是从调温开始时刻至收尾结束时刻的时段内，不同时刻，通入单晶炉的气体在结晶界面处的压强基本保持不变。
需要说明的是，此处的第一气体和第二气体的成分是否相同不作具体限定。此处的第一预设值的大小不作具体限定，具体以对晶棒的直径的稳定性要求程度而定。
本发明保持的是，从调温开始时刻至收尾结束时刻的时段内，通入单晶炉的气体在结晶界面的压强稳定，相对于保持气体在其余位置的压强稳定而言，结晶界面的压强稳定，对于晶棒的直径的稳定性的影响最大，因此，本发明对于提升晶棒的直径的稳定性效果更优。例如，相对于保持排出单晶炉的气体的压强稳定而言，结晶温度、结晶速度受到结晶界面的压强的影响更大，更直接，因此，本发明中，从调温开始时刻至收尾结束时刻的时段内，控制通入单晶炉的气体在结晶界面的压强稳定，能够得到直径更稳定的单晶晶棒。
可选地，该第一预设值为10pa，就是说从调温开始时刻之后至收尾结束时刻的时段内，控制各个时刻，通入单晶炉的第一气体，在结晶界面处的第一压强p1，与调温开始时刻，通入单晶炉的第二气体，在结晶界面处的第二压强p2，两者的差值的绝对值，小于或等于10pa，从调温开始时刻至收尾结束时刻的时段内，结晶界面处的压强更为稳定，使得拉制得到的单晶晶棒的直径的波动性更小，拉制得到的单晶晶棒的直径的稳定性更好。同时，同一种杂质在单晶晶棒各处的浓度分布大致相等，单晶晶棒质量均匀性较好，同样提升了单晶晶棒的质量。
例如，从调温开始时刻之后至收尾结束时刻的时段内，控制各个时刻，通入单晶炉的第一气体，在结晶界面处的第一压强p1，与调温开始时刻，通入单晶炉的第二气体，在结晶界面处的第二压强p2，两者的差值的绝对值为0、1pa、1.3pa、2pa、5pa、6pa、7pa、8pa、9pa、10pa。
可选地，第一气体包括拉晶过程的保护气体，第二气体包括拉晶过程的保护气体，保护气体的主要作用在于避免其他气体对于拉晶过程的影响。
可选地，保护气体包括：氮气，和/或，惰性气体。上述保护气体易于获得，成本较低。
可选地，惰性气体包括氩气，氩气较为常见，易于获得，成本较低。
图1示出了本发明实施例中的一种单晶炉的结构示意图。图2示出了本发明实施例中的一种拉晶方法的步骤流程图。
可选地，参照图2所示，该拉晶方法可以包括如下步骤：
步骤101，基于伯努利原理，获取所述第二气体在所述结晶界面处，除了压力势能之外的起始机械能。
流体的伯努利原理为公式一：此处的p为流体在某个位置的压力势能，更为具体的，可以是压强。可以为伯努利原理中，除了压力势能之外的机械能。其中，C为常量，ρ为该流体的密度。υ为流体在上述位置处的流速，g为重力加速度，取值可以为9.8N/kg，h为上述位置处与预设水平面之间的距离。对于拉晶过程中的气体而言，该预设水平面可以和结晶界面平行，例如，该预设水平面可以为海平面。需要说明的是，针对拉晶过程中气体而言，在拉晶过程中，通常是通过改变埚位，使得结晶界面的位置保持不动，也就是说，从调温开始时刻至收尾结束时刻的时段内，结晶界面的位置基本保持不动，则，对于拉晶过程中的气体而言，伯努利原理还可以简化为为常量。在本发明中，伯努利原理是否简化不作具体限定。
例如，基于伯努利原理，第二气体在结晶界面处，除了压力势能之外的起始机械能可以是：调温开始时刻，通入单晶炉的第二气体，在结晶界面处的起始动能参数和起始重力势能参数。第二气体的起始动能参数为：调温开始时刻，该第二气体的密度与其在调温开始时刻，结晶界面处的流速的平方的乘积。第二气体的起始重力势能参数为：调温开始时刻，该第二气体的密度与其在调温开始时刻，结晶界面与预设水平面之间的距离，以及重力加速度三者的乘积。该预设水平面与结晶界面平行即可，对于该预设水平面的选取不作具体限定。例如，该预设水平面可以为海平面，或者，该预设水平面可以为结晶界面，只需保证该预设水平面与结晶界面平行即可，对于该预设水平面的具体选择不作限定。即，第二气体在结晶界面处，除了压力势能之外的起始机械能为公式二：ρ1为调温开始时刻，该第二 气体的密度。υ1为调温开始时刻，该第二气体在结晶界面处的流速。h1为调温开始时刻，结晶界面和预设水平面之间的距离。
针对前述例子，上述步骤101就是，获取2021年10月20日10:13:20通入该单晶炉A的所有气体或第二气体，除了压力势能之外的起始机械能Q1，起始机械能Q1可以包括起始动能参数和起始重力势能参数，该起始动能参数就是：2021年10月20日10:13:20通入该单晶炉A的第二气体的密度ρ1，与2021年10月20日10:13:20通入该单晶炉A的第二气体在结晶界面的流速υ1的平方的乘积。起始重力势能参数就是：2021年10月20日10:13:20通入该单晶炉A的第二气体的密度ρ1、与调温开始时刻，结晶界面与预设水平面之间的距离h1、重力加速度三者的乘积。
步骤102，从调温开始时刻之后至收尾结束时刻的时段，基于伯努利原理，控制所述第一气体在所述结晶界面处，除了压力势能之外的实时机械能，与所述除了压力势能之外的起始机械能的差值的绝对值，小于或等于第二预设值。
基于伯努利原理，从调温开始时刻之后至收尾结束时刻的时段，第一气体在结晶界面处处，除了压力势能之外的实时机械能可以是：从调温开始时刻之后至收尾结束时刻的时段，第一时刻，通入单晶炉的第一气体，在结晶界面处的实时动能参数和实时重力势能参数。第一气体的实时动能参数为：从调温开始时刻之后至收尾结束时刻的时段，第一时刻，该第一气体的密度与其在第一时刻，结晶界面处的流速的平方的乘积。第一气体的实时重力势能参数为：第一时刻，该第一气体的密度与其在第一时刻，结晶界面与前述的预设水平面之间的距离，以及重力加速度三者的乘积。该预设水平面与步骤101中的预设水平面为同一水平面。即，第一气体在结晶界面处，除了压力势能之外的实时机械能为公式三：ρ2为第一时刻，该第一气体的密度。υ2为第一时刻，该第一气体在结晶界面处的流速。g为重力加速度，取值同样可以为9.8N/kg。h2为第一时刻，结晶界面和预设水平面之间的距离。
从调温开始时刻之后至收尾结束时刻的时段，基于伯努利原理，控制第一气体在结晶界面处，除了压力势能之外的实时机械能Q2，与除了压力势能之外的起始机械能Q1的差值的绝对值，小于或等于第二预设值，就是说，控制第一气体在结晶界面处，除了压力势能之外的实时机械能Q2，与除了压力势能之外起始机械能Q1基本保持一致。则，调温开始时刻，第二气体在结晶 界面处的伯努利方程见公式四:此处的p1为调温开始时刻，第二气体在结晶界面处的压力势能，可以是压强。从调温开始时刻之后至收尾结束时刻的时段，各个时刻，第一气体在结晶界面处的伯努利方程见公式五:此处的p2为从调温开始时刻之后至收尾结束时刻的时段，各个时刻，第一气体在结晶界面处的压力势能，可以是压强。伯努利方程中的C为常量。将上述公式四和公式五联立，则，该步骤102中，可以是控制与两者的差值的绝对值，小于或等于第二预设值，进而能够保证p1和p2的差值较小，从更为细致的参数上，从调温开始时刻至收尾结束时刻，控制通入单晶炉的气体在结晶界面处的压强较稳定，可操作性更强，控制更为精准，则，单晶晶棒的直径的稳定性更好，同一种杂质在单晶晶棒各处的浓度分布更均匀，单晶晶棒质量均匀性更好，进一步提升了单晶晶棒的质量。
针对前述例子，上述步骤102就是，控制2021年10月20日10:13:20之后，至2021年10月21日12:13:20的时间段内，每个时刻，通入该单晶炉A的所有气体或第一气体除了压力势能之外的实时机械能Q2，与除了压力势能之外的起始机械能Q1，两者的差值的绝对值小于或等于第二预设值，除了压力势能之外的实时机械能Q1包括实时动能参数和实时重力势能参数，该实时动能参数就是：2021年10月20日10:13:20之后，至2021年10月21日12:13:20的时间段内，第一时刻，通入该单晶炉A的第一气体的密度ρ2，与该第一时刻通入该单晶炉A的第一气体在结晶界面的流速υ2的平方的乘积。实时重力势能参数就是：该第一时刻，通入该单晶炉A的第一气体的密度ρ2、与第一时刻，结晶界面与预设水平面之间的距离h2、重力加速度三者的乘积。
需要说明的是，此处的第一时刻，是从调温开始时刻之后至收尾结束时刻的时段内的任一时刻。
前述的第二预设值可以根据需要控制的单晶硅棒的直径的稳定性的要求进行设定。对于单晶硅棒的直径的稳定性的要求越高，第二预设值越小。
可选地，该第二预设值可以为6J/m3。就是说从调温开始时刻之后至收尾结束时刻的时段内，控制各个时刻，通入单晶炉的第一气体，在结晶界面处除了压力势能之外的实时机械能Q2，与调温开始时刻，通入单晶炉的第二气 体，在结晶界面处除了压力势能之外的起始机械能Q1，两者的差值的绝对值，小于或等于6J/m3，从调温开始时刻至收尾结束时刻的时段内，结晶界面处的压强更为稳定，使得拉制得到的单晶晶棒的直径的波动性更小，拉制得到的单晶晶棒的直径的稳定性更好。同时，同一种杂质在单晶晶棒各处的浓度分布大致相等，单晶晶棒质量均匀性较好，同样提升了单晶晶棒的质量。
例如，从调温开始时刻之后至收尾结束时刻的时段内，控制各个时刻，通入单晶炉的第一气体，在结晶界面处除了压力势能之外的实时机械能Q2，与调温开始时刻，通入单晶炉的第二气体，在结晶界面处除了压力势能之外的起始机械能Q1，两者的差值的绝对值为0、0.2J/m3、1.3J/m3、1.9J/m3、2.5J/m3、3J/m3、4J/m3、5J/m3、5.3J/m3、6J/m3。
可选地，第一气体和第二气体相同，上述步骤101可以包括：获取第二气体，在调温开始时刻，结晶界面处的流速。上述步骤102可以包括：从调温开始时刻之后至收尾结束时刻的时段，控制第一时刻，第一气体，结晶界面处的流速，与第二气体，在调温开始时刻，结晶界面处的流速的差值的绝对值，小于或等于第三预设值。也就是说，从调温开始时刻至收尾结束时刻的时段内，通入单晶炉内的气体成分、种类等相同。则，第一气体的密度ρ2和第二气体的密度ρ1两者相等。同时，在拉晶过程中，通常是通过改变埚位，使得结晶界面的位置保持不动，也就是说，从调温开始时刻至收尾结束时刻的时段内，结晶界面的位置保持不动，则，h1＝h2，则，在该等式中，只需保持第二气体，在调温开始时刻，结晶界面处的流速υ1，和从调温开始时刻之后至收尾结束时刻的时段，各个时刻的第一气体在结晶界面处的流速υ2稳定，就可以保障从调温开始时刻之后至收尾结束时刻的时段，各个时刻，通入单晶炉的气体在结晶界面处的压强基本稳定。仅通过控制气体的在结晶界面处的流速，就可以保障拉制得到的单晶硅棒的直径的稳定性，控制的参数较少，工艺相对简单，易于实现。
需要说明的是，前述的第三预设值可以根据需要控制的单晶硅棒的直径的稳定性的要求进行设定。对于单晶硅棒的直径的稳定性的要求越高，第三预设值越小。
可选地，该第三预设值可以为2mm/min。就是说从调温开始时刻之后至收尾结束时刻的时段内，控制各个时刻，通入单晶炉的第一气体，在结晶界面处的流速υ2，与调温开始时刻，通入单晶炉的第二气体，在结晶界面处的流速υ1，两者的差值的绝对值，小于或等于2mm/min，从调温开始时刻至收 尾结束时刻的时段内，结晶界面处的压强更为稳定，使得拉制得到的单晶晶棒的直径的波动性更小，拉制得到的单晶晶棒的直径的稳定性更好。同时，同一种杂质在单晶晶棒各处的浓度分布大致相等，单晶晶棒质量均匀性较好，同样提升了单晶晶棒的质量。
例如，从调温开始时刻之后至收尾结束时刻的时段内，控制各个时刻，通入单晶炉的第一气体，在结晶界面处的流速υ2，与调温开始时刻，通入单晶炉的第二气体，在结晶界面处的流速υ1，两者的差值的绝对值为0、0.1mm/min、0.3mm/min、0.9mm/min、1.1mm/min、1.3mm/min、1.4mm/min、1.5mm/min、1.8mm/min、2mm/min。
参照图1所示，可选地，上述从调温开始时刻之后至收尾结束时刻的时段，控制该第一时刻，第一气体，结晶界面处的流速，与第二气体，在调温开始时刻，结晶界面处的流速的差值的绝对值，小于或等于第三预设值，可以包括：从调温开始时刻之后至收尾结束时刻的时段，获取该第一时刻，第一气体从热屏11下沿流出后，至该第一气体从单晶炉中排出之前的流通路径中，各点处的最小的流通截面积；用第一时刻对应的最小的流通截面积，乘以该第一时刻，第一气体，在结晶界面处的流速，得到该第一时刻的第一实时流量。在该第一时刻，向单晶炉内通入该第一实时流量的第一气体。通入单晶炉的气体，在结晶界面处的流速υ，可以等于该时刻对应的流量L，除以该时刻该气体从热屏下沿流出后，至该气体从单晶炉中排出之前的流通路径中，各点处的最小的流通截面积S1，即，υ＝L/S1，进而通过逆运算得到该时刻的第一实时流量。通常情况下，流量更容易测量和控制，将流速转换为流量易于测量和控制的流量，操作更简单。
需要说明的是，气体从单晶炉中排出的位置通常位于单晶炉的底部，在不同的时刻，气体从热屏下沿流出后，至该气体从单晶炉中排出之前的流通路径中，最小的流通截面积S1所处的位置不尽相同，该流通路径中，最小的流通截面积，可以对气体在结晶界面处的流速υ起到较为关键的决定作用，因此，采用此处的最小的流通截面积S1，获取该第一实时流量，可以保障从调温开始时刻至收尾结束时刻的时段内，结晶界面处的压强更为稳定，使得拉制得到的单晶晶棒的直径的波动性更小，拉制得到的单晶晶棒的直径的稳定性更好。同时，同一种杂质在单晶晶棒各处的浓度分布大致相等，单晶晶棒质量均匀性较好，同样提升了单晶晶棒的质量。
可选地，前述从调温开始时刻之后至收尾结束时刻的时段，获取第一时刻，第一气体从热屏下沿流出后，至第一气体从单晶炉中排出之前的流通路径中，各点处的最小的流通截面积之前，该方法还可以包括：获取各个埚位 处，从热屏下沿，至该单晶炉的气体排出之前的流通路径中，各点处的最小的流通截面积，并将该埚位对应的最小的流通截面积，存储在第一埚位面积列表中。埚位是拉晶过程中，埚帮15的上沿相对于结晶界面2的距离。在埚位相同的情况下，针对同一个单晶炉或热场，不同气体从热屏下沿流出后，至气体从单晶炉中排出之前的流通路径中，各点处的最小的流通截面积是相等的，就是说，一个埚位对应一个最小的流通截面积。因此，提前获取埚位对应的最小的流通截面积，并存储在第一埚位面积列表中，可以减少重复工作，后续在需要最小的流通截面积时，仅需查表即可，可以提升效率。
上述从调温开始时刻之后至收尾结束时刻的时段，获取第一时刻，第一气体从热屏下沿流出后，至第一气体从单晶炉中排出之前的流通路径中，各点处的最小的流通截面积，可以包括：获取该第一时刻对应的第一埚位，从前述第一埚位面积列表中，查询得到该第一埚位对应的最小的流通截面积，就得到了该第一时刻对应的最小的流通截面积。
可选地，前述获取各个埚位处，从热屏下沿，至从单晶炉中气体排出之前的流通路径中，各点处的最小的流通截面积，并将埚位对应的最小的流通截面积，存储在第一埚位面积列表中，可以包括下述子步骤S1-S5：
子步骤S1，获取各个埚位处，以热屏11下沿靠近结晶界面2的端点，与单晶炉的第一中线L1之间的距离，为半径，以该端点所在的第一平面与该第一中线L1的第一交点为圆心，形成的圆柱体的侧面的第一表面积。其中，该第一中线L1和结晶界面2垂直，第一平面和结晶界面2平行。
子步骤S2，获取各个埚位处，以坩埚14的内壁上沿和热屏11的外壁112的R弧1121上的第二点的连线为母线，以前述的第一中线L1为中心线，形成的圆台的侧面的第二表面积。其中，该第二点位于热屏11的外壁112的R弧1121的圆心，与坩埚14的内壁上沿的连线上。
子步骤S3，获取各个埚位处，以埚帮15进入过渡盘12前，埚帮15的外壁上沿和过渡盘12的内壁下沿两者连线为母线，以第一中线L1为中心线，形成的圆台的侧面的第三表面积。
子步骤S4，获取各个埚位处，以埚帮15进入过渡盘12，埚帮15的外壁上沿和过渡盘12的内壁下沿两者连线为母线，以第一中线L1为中心线，形成的圆台的侧面的第四表面积。
子步骤S5，针对同一埚位处，从所述第一表面积、第二表面积、第三表面积、第四表面积四者中，选择最小的表面积，作为所述埚位对应的最小的流通截面积，并存储在所述第一埚位面积列表中。
更为具体的，上述的第一表面积、第二表面积、第三表面积、第四表面 积，一方面在埚位发生变化时，上述四者的变化较为显著，另一方面，四者对于气体在结晶界面的压强的影响较大，因此，对于同一埚位，从上述四者中选择最小的表面积，计算得到的流速较为准确。
需要说明的是，过渡盘12的作用主要在于：支撑上保温筒17，同时，对于改变中保温筒13和上保温筒17的内径，起到过渡作用。
需要说明的是，对于调温开始时刻，第二气体在结晶界面处的流速υ2的确定，同样是，获取调温开始时刻，第二气体从热屏下沿流出后，至第二气体从所述单晶炉中排出之前的流通路径中，各点处的最小的流通截面积S0。υ2＝L0/S0。L0为调温开始时刻通入单晶炉的第二气体的流量L0。
可选地，获取调温开始时刻，第二气体从热屏下沿流出后，至第二气体从单晶炉中排出之前的流通路径中，各点处的最小的流通截面积S0，同样可以为：先获取调温开始时刻对应的第二埚位，然后从前述的第一埚位面积列表中，查询得到该第二埚位对应的最小的流通截面面积。
需要说明的是，全文所提及的一个器件的上沿更靠近炉盖，下沿更远离炉盖，内壁更靠近单晶炉的第一中线L1，外壁更远离单晶炉的第一中线L1。
可选地，上述从调温开始时刻之后至收尾结束时刻的时段，控制该第一时刻，第一气体，结晶界面处的流速，与第二气体，在调温开始时刻，结晶界面处的流速的差值的绝对值，小于或等于第三预设值，可以包括：从调温开始时刻之后至收尾结束时刻的时段，获取该第一时刻，第一气体在该结晶界面处的流通截面积S2，然后用该第一时刻对应的结晶界面处的流通截面积S2，乘以该第一时刻，该第一气体，在结晶界面处的流速υ，得到该第一时刻的第二实时流量。在该第一时刻，向单晶炉内通入该第二实时流量的第一气体。即，第二实时流量＝υ×S2。通常情况下，流量更容易测量和控制，将流速转换为流量易于测量和控制的流量，操作更简单。
更为具体的，第一时刻，该第一气体，在结晶界面处的流速υ，与该第一时刻，第一气体在该结晶界面处的流通截面积S2的直接相关，采用该第一时刻，第一气体在该结晶界面处的流通截面积S2，计算得到的第二实时流量，对第一时刻，该第一气体，在结晶界面处的压强的稳定性的影响更为直接，进而，从调温开始时刻至收尾结束时刻的时段内，结晶界面处的压强更为稳定，使得拉制得到的单晶晶棒的直径的波动性更小，拉制得到的单晶晶棒的直径的稳定性更好。同时，同一种杂质在单晶晶棒各处的浓度分布大致相等，单晶晶棒质量均匀性较好，同样提升了单晶晶棒的质量。
可选地，前述从调温开始时刻之后至收尾结束时刻的时段，获取第一时刻，第一气体在结晶界面处的流通截面积之前，该方法还可以包括：获取各 个埚位处，结晶界面处的流通截面积，并将各个埚位处，结晶界面处的流通截面积，存储在第二埚位面积列表中。前述从调温开始时刻之后至收尾结束时刻的时段，获取第一时刻，该第一气体在结晶界面处的流通截面积，可以包括：获取该第一时刻对应的第一埚位，然后从第二埚位面积列表中，查询得到该第一埚位对应的流通截面积，可以减少重复工作，后续在需要各个埚位，第一气体在结晶界面的流通截面积时，仅需查表即可，可以提升效率。
本发明还提供一种单晶硅棒，该单晶硅棒采用任一前述的拉晶方法制备得到，该单晶硅棒具有与任一前述的拉晶方法相同或相似的有益效果，为了避免重复，此处不再赘述。
本发明还提供一种单晶炉，该单晶炉用于采用任一前述的拉晶方法进行拉晶，该单晶炉具有与任一前述的拉晶方法相同或相似的有益效果，为了避免重复，此处不再赘述。
下面结合具体的实施例，进一步解释本发明：
实施例1
应用在28吋的热场中。该热场中，热屏11的外壁112的外径为614mm，过渡盘12的内径为810mm，埚帮15的外径为740mm，坩埚14的内径为680mm，坩埚14可以为石英坩埚。坩埚15的高度差可以为15mm，器盖距为28mm，热加距为72mm，热屏11的外壁112的R弧1121的半径为100mm。
从调温开始时刻至收尾结束时刻的时段内，通入单晶炉的气体均为氩气，也就是，第一气体和第二气体相同均为氩气。调温开始时刻，氩气的流量L0为70slpm(stard liter per minute，标准升每分钟)。调温开始时刻对应的埚位为-80mm，调温开始时刻，结晶界面处的流通截面面积为136383.22mm2，则，调温开始时刻，氩气在结晶界面处的流速υ1＝70×106÷136383.22＝513.26mm/min。调温开始时刻之后至收尾结束时刻的时段内，埚位减小，控制每个时刻的氩气在结晶界面处的流速υ2均为513.26mm/min，同时用每个时刻对应的结晶界面处的表面积S2×υ2＝Lt，此处的Lt为调温开始时刻之后至收尾结束时刻的时段内，每个时刻或每个埚位对应的氩气的第二实时流量。在每个时刻或每个埚位，向单晶炉内通入该时刻或该埚位对应的第二实时流量的氩气，则，根据前述的公式： 由于，ρ1＝ρ2，υ1＝υ2，在拉晶过程中，结晶界面保持不变，则h1＝h2，进而保证了，从调温开始时刻至收尾结束时刻的时段内，氩气在结晶界面处的压强p保持不变。
实施例2
也应用在如实施例1所记载的28吋的热场中。该热场与实施例1对应相同，为了避免重复，此处不再赘述。
从调温开始时刻至收尾结束时刻的时段内，通入单晶炉的气体均为氩气，也就是，第一气体和第二气体相同均为氩气。参照下表1，调温开始时刻，氩气的流量L0为70slpm(stard liter per minute，标准升每分钟)。调温开始时刻对应的埚位为-80mm，调温开始时刻，前述第一表面积、第二表面积、第三表面积、第四表面积四者中，最小的表面积为第二表面积，第二表面积为136391.97mm2，则，调温开始时刻，氩气在结晶界面处的流速υ1＝70×106÷136391.97＝513.23mm/min。调温开始时刻之后至收尾结束时刻的时段内，埚位减小，控制每个时刻的氩气在结晶界面处的流速υ2均为513.23mm/min，同时用每个时刻对应的最小的表面积S1S×υ2＝Lt1，此处的Lt1为调温开始时刻之后至收尾结束时刻的时段内，每个时刻或每个埚位对应的氩气的第一实时流量。在每个时刻或每个埚位，向单晶炉内通入该时刻或该埚位对应的第一实时流量的氩气，则，根据前述的公式： 由于，ρ1＝ρ2，υ1＝υ2，在拉晶过程中，结晶界面保持不变，则h1＝h2，进而保证了，从调温开始时刻至收尾结束时刻的时段内，氩气在结晶界面处的压强p保持不变。
表1：实施例中部分拉晶工艺参数表
对比例
也应用在28吋的热场中。该热场与实施例1对应相同，为了避免重复，此处不再赘述。
从调温开始时刻至收尾结束时刻的时段内，通入单晶炉的气体均为氩气。从调温开始时刻至收尾结束时刻的时段内，氩气的流量均为70slpm。调温开始时刻对应的埚位为-80mm。
实施例1、实施例2和对比例中单晶晶棒的设定直径均为300mm。实施例1、实施例2和对比例中所用的硅料相同。实施例1、实施例2和对比例中除了通入氩气的流量或氩气在结晶界面的流速之外其余的工艺参数等均对应相同。图3示出了本发明实施例1中的单晶晶棒3与对比例的单晶晶棒的直径波动情况对比图。图3中数值表征的含义为：单晶晶棒各处的直径与设定直径300mm的偏差大小。数值的单位可以为mm。实施例1和对比例拉制得到的单晶晶棒的直径的波动情况如图3所示。图3中实线曲线为实施例1拉制得到的单晶晶棒3的直径的波动，图3中虚线曲线为对比例拉制得到的单晶晶棒3的直径的波动。从图3中可以得出，实施例1拉制得到的单晶晶棒3的直径的波动，明显小于对比例拉制得到的单晶晶棒的直径的波动。实施例1相对于对比例而言，单晶晶棒3的直径的波动由±1mm，大致缩小至±0.5mm。主要原因在于：从调温开始时刻至收尾结束时刻的时段内，氩气在结晶界面处的压强p会影响硅料的熔点，大致决定结晶温度，进而影响结晶速度，最终影响拉制得到的单晶晶棒3的直径的稳定性。实施例1中，从调温开始时刻至收尾结束时刻的时段内，氩气在结晶界面处的压强p保持不变，则结晶温度基本稳定，结晶速度基本稳定，拉制得到的单晶晶棒3的直径的波动较小，拉制得到的单晶晶棒3的直径的稳定性较好。同时，从调温开始时刻至收尾结束时刻的时段内，氩气在结晶界面处的压强p保持不变，则，同一种杂质在单晶晶棒3各处的浓度分布大致相等，单晶晶棒3质量均匀性较好，同样提升了单晶晶棒3的质量。同时，实施例1和实施例2，相对于对比例而言，还减少了氩气的使用量，可以降低成本。需要说明的是，实施例2和对比例拉制得到的单晶晶棒的直径的波动情况，与图3类似，为了避免重复，且简化图示，未在图3中示出。
需要说明的是，对于方法实施例，为了简单描述，故将其都表述为一系 列的动作组合，但是本领域技术人员应该知悉，本申请实施例并不受所描述的动作顺序的限制，因为依据本申请实施例，某些步骤可以采用其他顺序或者同时进行。其次，本领域技术人员也应该知悉，说明书中所描述的实施例均属于优选实施例，所涉及的动作并不一定都是本申请实施例所必须的。
需要说明的是，在本文中，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者装置不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者装置所固有的要素。在没有更多限制的情况下，由语句“包括一个……”限定的要素，并不排除在包括该要素的过程、方法、物品或者装置中还存在另外的相同要素。
通过以上的实施方式的描述，本领域的技术人员可以清楚地了解到上述实施例方法可借助软件加必需的通用硬件平台的方式来实现，当然也可以通过硬件，但很多情况下前者是更佳的实施方式。基于这样的理解，本发明的技术方案本质上或者说对现有技术做出贡献的部分可以以软件产品的形式体现出来，该计算机软件产品存储在一个存储介质(如ROM/RAM、磁碟、光盘)中，包括若干指令用以使得一台终端(可以是手机，计算机，服务器，空调器，或者网络设备等)执行本发明各个实施例所述的方法。
以上所描述的装置实施例仅仅是示意性的，其中所述作为分离部件说明的单元可以是或者也可以不是物理上分开的，作为单元显示的部件可以是或者也可以不是物理单元，即可以位于一个地方，或者也可以分布到多个网络单元上。可以根据实际的需要选择其中的部分或者全部模块来实现本实施例方案的目的。本领域普通技术人员在不付出创造性的劳动的情况下，即可以理解并实施。
本文中所称的“一个实施例”、“实施例”或者“一个或者多个实施例”意味着，结合实施例描述的特定特征、结构或者特性包括在本申请的至少一个实施例中。此外，请注意，这里“在一个实施例中”的词语例子不一定全指同一个实施例。
在此处所提供的说明书中，说明了大量具体细节。然而，能够理解，本申请的实施例可以在没有这些具体细节的情况下被实践。在一些实例中，并未详细示出公知的方法、结构和技术，以便不模糊对本说明书的理解。
最后应说明的是：以上实施例仅用以说明本申请的技术方案，而非对其限制；尽管参照前述实施例对本申请进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本申请各实施例技术方案的精神和范围。

Claims (16)

  1. 一种拉晶方法，其特征在于，所述方法包括：
    步骤S，从调温开始时刻之后至收尾结束时刻的时段内，控制各个时刻，通入单晶炉的第一气体，在结晶界面处的第一压强，与调温开始时刻，通入所述单晶炉的第二气体，在所述结晶界面处的第二压强，两者的差值的绝对值，小于或等于第一预设值。
  2. 根据权利要求1所述的拉晶方法，其特征在于，所述步骤S之前，所述方法还包括：
    基于伯努利原理，获取所述第二气体在所述结晶界面处，除了压力势能之外的起始机械能；
    所述步骤S，包括：
    从调温开始时刻之后至收尾结束时刻的时段，基于伯努利原理，控制所述第一气体在所述结晶界面处，除了压力势能之外的实时机械能，与所述除了压力势能之外的起始机械能的差值的绝对值，小于或等于第二预设值。
  3. 根据权利要求2所述的拉晶方法，其特征在于，所述第一气体，与所述第二气体相同；所述基于伯努利原理，获取所述第二气体在所述结晶界面处，除了压力势能之外的起始机械能，包括：
    获取所述第二气体，在调温开始时刻，在所述结晶界面处的流速；
    所述从调温开始时刻之后至收尾结束时刻的时段，基于伯努利原理，控制所述第一气体在所述结晶界面处，除了压力势能之外的实时机械能，与所述除了压力势能之外的起始机械能的差值的绝对值，小于或等于第二预设值，包括：
    从调温开始时刻之后至收尾结束时刻的时段，控制所述第一时刻，所述第一气体，在所述结晶界面处的流速，与所述第二气体，在调温开始时刻，结晶界面处的流速的差值的绝对值，小于或等于第三预设值。
  4. 根据权利要求3所述的拉晶方法，其特征在于，所述从调温开始时刻之后至收尾结束时刻的时段，控制所述第一时刻，所述第一气体，在所述结晶界面处的流速，与所述第二气体，在调温开始时刻，结晶界面处的流速的差值的绝对值，小于或等于第三预设值，包括：
    从调温开始时刻之后至收尾结束时刻的时段，获取所述第一时刻，所述第一气体从热屏下沿流出后，至所述第一气体从所述单晶炉中排出之前的流通路径中，各点处的最小的流通截面积；
    用所述第一时刻对应的最小的流通截面积，乘以所述第一时刻，所述第一气体，在结晶界面处的流速，得到所述第一时刻的第一实时流量；
    在所述第一时刻，向所述单晶炉内通入所述第一实时流量的所述第一气体。
  5. 根据权利要求4所述的拉晶方法，其特征在于，所述从调温开始时刻之后至收尾结束时刻的时段，获取所述第一时刻，所述第一气体从热屏下沿流出后，至所述第一气体从所述单晶炉中排出之前的流通路径中，各点处的最小的流通截面积之前，所述方法还包括：
    获取各个埚位处，所述流通路径中，各点处的最小的流通截面积，并将所述埚位对应的最小的流通截面积，存储在第一埚位面积列表中；
    所述从调温开始时刻之后至收尾结束时刻的时段，获取所述第一时刻，所述第一气体从热屏下沿流出后，至所述第一气体从所述单晶炉中排出之前的流通路径中，各点处的最小的流通截面积，包括：
    获取所述第一时刻对应的第一埚位；
    从所述第一埚位面积列表中，查询得到所述第一埚位对应的最小的流通截面积。
  6. 根据权利要求5所述的拉晶方法，其特征在于，所述获取各个埚位处，所述流通路径中，各点处的最小的流通截面积，并将所述埚位对应的最小的流通截面积，存储在第一埚位面积列表中，包括：
    获取各个埚位处，以热屏下沿靠近所述结晶界面的端点，与所述单晶炉的第一中线之间的距离，为半径，以所述端点所在的第一平面与所述第一中线的第一交点为圆心，形成的圆柱体的侧面的第一表面积；其中，所述第一中线和所述结晶界面垂直，所述第一平面和所述结晶界面平行；
    获取各个埚位处，以坩埚的内壁上沿和所述热屏的外壁的R弧上的第二点的连线为母线，以所述第一中线为中心线，形成的圆台的侧面的第二表面积；其中，所述第二点位于所述热屏的外壁的R弧的圆心，与所述坩埚的内壁上沿的连线上；
    获取各个埚位处，以埚帮进入过渡盘前，埚帮的外壁上沿和过渡盘的内壁下沿两者连线为母线，以所述第一中线为中心线，形成的圆台的侧面的第三表面积；
    获取各个埚位处，以埚帮进入过渡盘，埚帮的外壁上沿和过渡盘的内壁下沿两者连线为母线，以所述第一中线为中心线，形成的圆台的侧面的第四表面积；
    针对同一埚位处，从所述第一表面积、第二表面积、第三表面积、第四表面积四者中，选择最小的表面积，作为所述埚位对应的最小的流通截面积，并存储在所述第一埚位面积列表中。
  7. 根据权利要求3所述的拉晶方法，其特征在于，所述从调温开始时刻之后至收尾结束时刻的时段，控制所述第一时刻，所述第一气体，在所述结晶界面处的流速，与所述第二气体，在调温开始时刻，结晶界面处的流速的差值的绝对值，小于或等于第三预设值，包括：
    从调温开始时刻之后至收尾结束时刻的时段，获取所述第一时刻，所述第一气体在所述结晶界面处的流通截面积；
    用所述第一时刻对应的结晶界面处的流通截面积，乘以所述第一时刻，所述第一气体，在结晶界面处的流速，得到所述第一时刻的第二实时流量；
    在所述第一时刻，向所述单晶炉内通入所述第二实时流量的所述第一气体。
  8. 根据权利要求7所述的拉晶方法，其特征在于，所述从调温开始时刻之后至收尾结束时刻的时段，获取所述第一时刻，所述第一气体在所述结晶界面处的流通截面积之前，所述方法还包括：
    获取各个埚位处，所述结晶界面处的流通截面积，并将各个埚位处，所述结晶界面处的流通截面积，存储在第二埚位面积列表中；
    所述从调温开始时刻之后至收尾结束时刻的时段，获取所述第一时刻，所述第一气体在所述结晶界面处的流通截面积，包括：
    获取所述第一时刻对应的第一埚位；
    从所述第二埚位面积列表中，查询得到所述第一埚位对应的流通截面积。
  9. 根据权利要求1至8中任一所述的拉晶方法，其特征在于，所述第一预设值为：10pa。
  10. 根据权利要求2至8中任一所述的拉晶方法，其特征在于，所述第二预设值为：6J/m3。
  11. 根据权利要求3至8中任一所述的拉晶方法，其特征在于，所述第三预设值为：2mm/min。
  12. 根据权利要求1至8中任一所述的拉晶方法，其特征在于，所述第一气体包括拉晶过程的保护气体，所述第二气体包括拉晶过程的保护气体。
  13. 根据权利要求12所述的拉晶方法，其特征在于，所述保护气体包括：氮气，和/或，惰性气体。
  14. 根据权利要求13所述的拉晶方法，其特征在于，所述惰性气体包括氩气。
  15. 一种单晶硅棒，其特征在于，采用如权利要求1至14中任一所述的拉晶方法制备得到。
  16. 一种单晶炉，其特征在于，所述单晶炉用于采用如权利要求1至14中任一所述的拉晶方法进行拉晶。
PCT/CN2023/095179 2022-09-20 2023-05-19 一种拉晶方法、单晶硅棒和单晶炉 Ceased WO2024060650A1 (zh)

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