CN113638037A - Single crystal furnace and preparation method of monocrystalline silicon - Google Patents
Single crystal furnace and preparation method of monocrystalline silicon Download PDFInfo
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- CN113638037A CN113638037A CN202010393429.7A CN202010393429A CN113638037A CN 113638037 A CN113638037 A CN 113638037A CN 202010393429 A CN202010393429 A CN 202010393429A CN 113638037 A CN113638037 A CN 113638037A
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- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims abstract description 147
- 238000003756 stirring Methods 0.000 claims abstract description 91
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 35
- 235000012239 silicon dioxide Nutrition 0.000 claims description 32
- 238000004519 manufacturing process Methods 0.000 claims description 23
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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
- C30B15/14—Heating of the melt or the crystallised materials
-
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/30—Mechanisms for rotating or moving either the melt or the crystal
- C30B15/305—Stirring of the 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
Abstract
The invention provides a single crystal furnace and a preparation method of monocrystalline silicon, the single crystal furnace comprises a furnace body, a crucible supporting assembly is arranged in the furnace body, a crucible is arranged at the upper part of the crucible supporting assembly, a guide cylinder is arranged right above the crucible, a heater is arranged between the inner wall of the furnace body and the periphery of the crucible, a seed crystal lifting mechanism is arranged at the top of the furnace body, the single crystal furnace also comprises: the magnetic field generator is arranged at the periphery of the furnace body and used for generating a magnetic field covering the furnace body; the guide shell driving mechanism is connected with the top of the guide shell and is used for driving the guide shell to do autorotation motion and lifting motion; and the polycrystalline silicon melt stirring device is connected with the bottom of the guide cylinder and can do autorotation motion and lifting motion along with the guide cylinder. According to the single crystal furnace, the heat convection of fluid in the crucible can be retarded, and the crystal performance and uniformity are improved; by additionally arranging the polycrystalline silicon melt stirring device, the melting time of the polycrystalline silicon material can be shortened, and the temperature of the formed melt is more uniform.
Description
Technical Field
The invention relates to the technical field of monocrystalline silicon, in particular to a monocrystalline furnace and a preparation method of monocrystalline silicon.
Background
Polycrystalline silicon is a major raw material for producing solar photovoltaic products and semiconductor products. The Czochralski (Cz) method is one of the most common methods for preparing single crystal silicon, in which a high purity solid polycrystalline silicon raw material is melted in a crucible of a crystal growth furnace (i.e., a single crystal furnace) to form a melt, a seed crystal is lowered by a seed crystal pulling mechanism to be brought into contact with the melt in a molten state in a rotating crucible, and then the seed crystal is pulled out according to a certain process, and the melt is solidified around the seed crystal to form a single crystal silicon rod.
The conventional Cz single crystal furnace requires a lot of complicated work for temperature adjustment before formally pulling, including melting of the polycrystalline silicon material, temperature maintenance, immersion of the seed crystal in the melt bath, observation of the shape and color change of the seed crystal head, neck-down, and the like. Since the exact temperature in the crystal puller and the temperature distribution of the bath are not known, a considerable amount of time is required to wait. These processes are time consuming and labor intensive, and the production time of the silicon single crystal is severely prolonged, which limits the production efficiency of the czochralski silicon. In addition, in the processes of melting polycrystalline silicon materials, maintaining the temperature, immersing seed crystals into a molten pool, observing the shape and color change of a seed crystal head, leading a neck and the like, the manual visual observation of the operation in the furnace is greatly involved, and the manual operation process has high requirements on the technical and experience level of operators. In addition, the visual condition is difficult to describe and cannot be quantified in a plurality of visual observation operations, so that the training period for operators is long, the production cost is increased, and in addition, the risk of drawing failure caused by wrong judgment of the operators exists. In summary, the existing single crystal silicon rod production process has the problems of complicated manual operation, low efficiency, difficult quality control, risk of drawing failure caused by wrong judgment of operators and the like.
Disclosure of Invention
In view of the above, the invention provides a single crystal furnace and a preparation method of single crystal silicon, so as to solve the problems of complicated manual operation, low efficiency, difficult quality control and the like in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
an embodiment of the invention provides a single crystal furnace, which comprises a furnace body, wherein a crucible supporting assembly is arranged in the furnace body, a crucible is arranged at the upper part of the crucible supporting assembly, a guide cylinder is arranged right above the crucible, a heater is arranged between the inner wall of the furnace body and the periphery of the crucible, a seed crystal lifting mechanism is arranged at the top of the furnace body, and the single crystal furnace further comprises:
the magnetic field generator is arranged at the periphery of the furnace body and used for generating a magnetic field covering the furnace body;
the guide shell driving mechanism is connected with the top of the guide shell and is used for driving the guide shell to do autorotation motion and lifting motion;
and the polycrystalline silicon melt stirring device is connected with the bottom of the guide cylinder and can perform autorotation motion and lifting motion along with the guide cylinder.
Optionally, the polycrystalline silicon melt stirring device is ring-shaped.
Optionally, the polycrystalline silicon melt stirring device is made of a silicon dioxide material.
Optionally, the single crystal furnace further comprises:
the crucible driving mechanism is connected with the crucible supporting assembly and used for driving the crucible supporting assembly to do autorotation motion.
Optionally, the single crystal furnace further comprises:
a magnetic field intensity detection unit for detecting the magnetic field intensity in the furnace body;
and the temperature detection unit is used for detecting the temperature in the crucible.
Optionally, the temperature detection unit is a charge coupled device, a plurality of temperature measurement holes are formed in the top of the furnace body, a sealed heat insulation window is arranged in each temperature measurement hole, the temperature detection unit is arranged on the outer side of each window, the magnetic field strength detection unit comprises a plurality of magnetic sensors, and the magnetic sensors are arranged at the bottom of the guide cylinder at intervals.
Optionally, the single crystal furnace further comprises:
a controller, the controller respectively with magnetic field generator temperature detecting element magnetic field intensity detecting element the heater magnetic field generator and draft tube actuating mechanism connects, the controller is used for according to the temperature data control that temperature detecting element detected the heater is adjusted temperature in the crucible, be used for according to the magnetic field intensity data control that magnetic field intensity detecting element detected magnetic field generator adjusts magnetic field intensity in the furnace body and be used for according to the temperature data control that temperature detecting element detected draft tube actuating mechanism drive polycrystalline silicon melt stirring device is right polycrystalline silicon melt in the crucible stirs.
In another aspect, the embodiment of the invention further provides a preparation method of monocrystalline silicon, which is applied to the monocrystalline furnace described in any one of the above, and the method includes:
heating the polycrystalline silicon material in the crucible and applying a magnetic field to the furnace body;
and controlling the guide cylinder driving mechanism to drive a polycrystalline silicon melt stirring device connected with the bottom of the guide cylinder driving mechanism to stir the silicon material in the crucible.
Optionally, the step of controlling the guide shell driving mechanism to drive the polycrystalline silicon melt stirring device connected to the bottom of the guide shell driving mechanism to stir the polycrystalline silicon material in the crucible includes:
acquiring temperature information in the crucible and magnetic field intensity information in the furnace body;
according to the temperature information and the magnetic field intensity information, controlling the depth of the polycrystalline silicon melt stirring device extending into the polycrystalline silicon material and the rotating speed of the polycrystalline silicon melt stirring device, and enabling the average temperature of an annular area with the center of the crucible as the center and the width of 5cm to be equal to any stored temperatureIn the annular region having an area greater than 1cm2The average temperature of the plaques of (a) differs by less than 1 ℃.
Optionally, the method further includes:
and adjusting the magnetic field generator to enable the difference value between the average value of the magnetic field intensity in the furnace body and the preset magnetic field intensity threshold value to be less than 1% of the preset magnetic field intensity threshold value.
The technical scheme of the invention has the following beneficial effects:
according to the single crystal furnace provided by the embodiment of the invention, the magnetic field is applied to the furnace body, so that the heat convection of the fluid in the crucible can be retarded, and the crystal performance and uniformity can be improved; and by additionally arranging the polycrystalline silicon melt stirring device, the time for melting the polycrystalline silicon material can be shortened, and the temperature of the formed melt is more uniform, so that the production time of the monocrystalline silicon is shortened, and the quality of the prepared monocrystalline silicon rod is improved.
Drawings
FIG. 1 is a schematic cross-sectional view of a single crystal furnace according to an embodiment of the present invention before a neck;
FIG. 2 is a second schematic cross-sectional view of a single crystal furnace according to an embodiment of the present invention before a neck;
FIG. 3 is a schematic cross-sectional view of a single crystal furnace according to an embodiment of the present invention during constant diameter growth;
FIG. 4 is a second schematic cross-sectional view of a single crystal furnace according to an embodiment of the present invention during constant diameter growth;
FIG. 5 is a schematic view of an annular polysilicon solution stirring apparatus provided in an embodiment of the present invention;
FIG. 6 is a schematic view of a paddle-shaped polysilicon solution stirring device provided in an embodiment of the present invention;
FIG. 7 is a schematic control diagram of the working process of a single crystal furnace according to an embodiment of the present invention;
fig. 8 is a schematic flow chart of a method for preparing single crystal silicon according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention, are within the scope of the invention.
Polycrystalline silicon is a major raw material for producing solar photovoltaic products and semiconductor products. The Czochralski (Cz) method is one of the most common methods for preparing single crystal silicon, in which a high purity solid polycrystalline silicon raw material is melted in a crucible of a crystal growth furnace (i.e., a single crystal furnace) to form a melt, a seed crystal is lowered by a seed crystal pulling mechanism to be brought into contact with the melt in a molten state in a rotating crucible, and then the seed crystal is pulled out according to a certain process, and the melt is solidified around the seed crystal to form a single crystal silicon rod.
The conventional Cz single crystal furnace requires a lot of complicated work for temperature adjustment before formally pulling, including melting of the polycrystalline silicon material, temperature maintenance, immersion of the seed crystal in the melt bath, observation of the shape and color change of the seed crystal head, neck-down, and the like. Since the exact temperature in the crystal puller and the temperature distribution of the bath are not known, a considerable amount of time is required to wait. These processes are time consuming and labor intensive, and the production time of the silicon single crystal is severely prolonged, which limits the production efficiency of the czochralski silicon. In addition, in the processes of melting polycrystalline silicon materials, maintaining the temperature, immersing seed crystals into a molten pool, observing the shape and color change of a seed crystal head, leading a neck and the like, the manual visual observation of the operation in the furnace is greatly involved, and the manual operation process has high requirements on the technical and experience level of operators. In addition, the visual condition is difficult to describe and cannot be quantified in a plurality of visual observation operations, so that the training period for operators is long, the production cost is increased, and in addition, the risk of drawing failure caused by wrong judgment of the operators exists. In summary, the existing single crystal silicon rod production process has the problems of complicated manual operation, low efficiency, difficult quality control, risk of drawing failure caused by wrong judgment of operators and the like.
Thus, an embodiment of an aspect of the present invention provides a single crystal furnace, as shown in fig. 1 to 4, comprising a furnace body including a main furnace chamber 1, a dome chamber 2 and a pulling chamber 3 arranged in this order from bottom to top, wherein a crucible supporting assembly 71 is arranged inside the main furnace chamber 1, a graphite crucible 72 and a quartz crucible 73 are arranged on the upper portion of the crucible supporting assembly 71, and the quartz crucible 73 is placed inside the graphite crucible 72; the periphery of the graphite crucible 72 is also provided with a side heater 61, the bottom of the graphite crucible 72 is provided with a bottom heater 62, the side heater 61 and the bottom heater 62 surround the graphite crucible 72 and are used for comprehensively heating the polycrystalline silicon material placed in the quartz crucible 73 so as to rapidly melt the polycrystalline silicon material, preferably, the side heater 61 and the bottom heater 62 are independent from each other and can independently heat the polycrystalline silicon material; the top of the furnace body, namely the traction chamber 3, is provided with a seed crystal pulling mechanism 4, the seed crystal pulling mechanism 4 is connected with a seed crystal chuck through a molybdenum wire, a seed crystal 10 is arranged on the seed crystal chuck, and the seed crystal pulling mechanism 4 has power and can drive the seed crystal 10 on the seed crystal chuck to do lifting motion and rotary motion.
In the embodiment of the invention, the single crystal furnace can also comprise a magnetic field generator 5, the magnetic field generator 5 is arranged at the periphery of the furnace body and is used for generating a magnetic field covering the furnace body, the magnetic field intensity and the magnetic field angle of the magnetic field generated by the magnetic field generator 5 can be correspondingly adjusted according to actual production requirements, when the polycrystalline silicon material placed in the quartz crucible 73 is heated and melted to form a melt, as the melt is conductive, and the conductive melt moves and flows in the magnetic field applied by the magnetic field generator 5, current microelements in the melt cut magnetic lines, so that the magnetic field applies ampere force to the melt, and the direction of the current microelements is opposite to the moving direction of the current microelements, so that the heat convection of the fluid can be retarded, and the crystal performance and uniformity are improved.
As shown in fig. 1 to 5, in the embodiment of the present invention, the single crystal furnace may further include a guide cylinder 8 and a guide cylinder driving mechanism 81 connected to a top of the guide cylinder 8, wherein the guide cylinder 8 is disposed right above the quartz crucible 73 and is configured to guide the inert gas into the furnace, and a power output end of the guide cylinder driving mechanism 81 is connected to the top of the guide cylinder 8 and is configured to drive the guide cylinder 8 to perform a rotation motion and a lifting motion, that is, under the driving of the guide cylinder driving mechanism 81, the guide cylinder 8 may be close to a liquid level of the polysilicon material melt, may be far away from the liquid level of the polysilicon material melt, and may perform a self-transmission motion around a central axis of the guide cylinder 8.
Further, in the embodiment of the invention, the single crystal furnace can also comprise a polycrystalline silicon melt stirring device 12, the polysilicon melt stirring device 12 is connected with the bottom of the guide shell 8 and can do autorotation movement and lifting movement along with the guide shell 8, namely, when the guide shell 8 is driven by the guide shell driving mechanism 81 to do autorotation motion and lifting motion, the polysilicon melt stirring device 12 also does synchronous rotation motion and lifting motion, so that the polysilicon melt stirring device 12 can extend into the polysilicon material in the quartz crucible 73 for stirring, the insertion depth and the rotating speed can be adjusted, so that the polycrystalline silicon melt stirring device 12 is used for accelerating the melting process of the polycrystalline silicon material through stirring, and the temperature distribution of the polycrystalline silicon material in the quartz crucible 73 is made more uniform to improve the quality of the produced single crystal silicon rod 11.
As shown in fig. 5, in some embodiments of the present invention, the polysilicon melt stirring device 12 is annular and has a certain height, that is, the polysilicon melt stirring device 12 is a cylindrical structure with a certain height, and when the polysilicon melt is stirred, a part of the polysilicon melt stirring device 12 is immersed into the polysilicon melt; in addition, the polysilicon melt stirring device 12 may be made of a silicon dioxide material, so as to avoid introducing impurities to affect the quality of the prepared single crystal silicon rod 11.
As shown in fig. 6, in some embodiments of the present invention, the polysilicon melt stirring device 12 has a paddle shape, and the paddle-shaped polysilicon melt stirring device 12 can provide a larger stirring amplitude.
In the embodiment of the present invention, the single crystal furnace may further include a crucible driving mechanism (not shown in the figure), a power output end of the crucible driving mechanism is connected to the crucible supporting assembly 71, and is configured to drive the crucible supporting assembly 71 to rotate, so as to drive the graphite crucible 72 and the quartz crucible 73 disposed at the upper portion of the crucible supporting assembly to rotate synchronously, and by controlling the crucible driving mechanism, the rotation speeds of the graphite crucible 72 and the quartz crucible 73 can be conveniently controlled, and then the flow speed of the melt contained therein can be controlled, so as to improve the quality of the prepared single crystal silicon rod.
In other embodiments of the present invention, the single crystal furnace may further include a temperature detecting unit 9 and a magnetic field strength detecting unit 131, wherein the magnetic field strength detecting unit 131 is configured to detect a magnetic field strength in the furnace body, so as to adjust and control the magnetic field generator 5 according to the detected magnetic field strength value, and further control the temperature uniformity of the melt in the quartz crucible 73, since the superconducting magnetic field arranged around the single crystal furnace can generate a magnetic field for inhibiting the free flow of the polysilicon solution inside the single crystal furnace, when the magnetic field in the crystal pulling furnace fluctuates and has poor uniformity and the solution free movement is too strongly controlled, the polysilicon solution in the crucible can be rapidly stirred and rapidly adjusted by using the polysilicon solution stirring device 12 to increase the production efficiency; the temperature detecting unit 9 is used for detecting the temperature in the quartz crucible 73, more specifically, the temperature of the polysilicon material placed in the quartz crucible 73, so as to obtain the specific temperature of each process stage in the production process in real time, thereby adjusting the operating conditions of various components within the single crystal furnace, including, but not limited to, controlling the amount of polysilicon material, the rotational speed of the graphite crucible 72, the rotational speed of the seed crystal 10, and the magnetic field strength, for example, the temperature distribution condition in the quartz crucible 73 in the polycrystalline silicon material melting stage can be obtained in real time, the specific condition of the polycrystalline silicon material melting can be determined, the temperature in the quartz crucible 73 when the seed crystal 10 is immersed in the polycrystalline silicon material in the melting state can also be obtained in real time, further, the time when the neck-drawing process is started is judged, and further, the temperature in the quartz crucible 73 during the shouldering/shouldering process can be obtained in real time, and further, the parameters selected during shouldering/shouldering are selected.
In some embodiments of the present invention, in the production process of the single crystal silicon rod, after the magnetic field strength detection unit 131 obtains the magnetic field strength information in the furnace body, the magnetic field strength information can be fed back to the controller, and at this time, an operator can obtain the magnetic field strength information in the furnace body of the crystal pulling furnace in real time through the controller, and then judge whether to stir the polysilicon solution in the crucible through the polysilicon solution stirring device 12 by combining the real-time magnetic field strength information. In addition, the operator can adjust the depth of immersion of the polysilicon solution stirring device 12 into the surface of the polysilicon solution and the stirring speed of the polysilicon solution stirring device 12 in combination with the magnetic field conditions inside the crystal pulling furnace measured in real time.
In another embodiment of the present invention, after the magnetic field strength detecting unit 131 obtains the magnetic field strength information inside the furnace body, the magnetic field strength information can be fed back to the controller in real time, the controller automatically determines whether the polysilicon solution inside the crucible is stirred by the polysilicon solution stirring device 12 after calculating through a preset optimization algorithm, and if it is determined that the polysilicon solution inside the crucible needs to be stirred by the polysilicon stirring device 12, the controller can output corresponding numerical values to control the depth of the polysilicon solution stirring device 12 immersed into the surface of the polysilicon solution and the stirring speed of the polysilicon solution stirring device 12, so as to achieve automatic control.
During the use of the polysilicon solution stirring device 12, whether the polysilicon solution is stirred by the polysilicon solution stirring device 12 can be determined by combining the temperature condition in the crystal pulling furnace, the pulling intracranial magnetic field condition, the polysilicon melting condition and other corresponding conditions and parameters. The depth of immersion of the polysilicon solution stirring apparatus 12 into the polysilicon solution and the speed of the polysilicon solution stirring apparatus 12 during stirring may also be determined in conjunction with the conditions and parameters listed above. However, the reference conditions are not limited to the three listed above.
In an alternative embodiment of the present invention, the magnetic field strength detecting unit may include a plurality of magnetic sensors spaced at the bottom of the guiding cylinder 8, and since the guiding cylinder 8 is lowered to a position closer to the surface of the melt in the quartz crucible 73 during the pulling of the seed crystal 10, the magnetic sensors may be disposed at the bottom of the guiding cylinder 8 to enable the measured magnetic field strength data to be closer to the magnetic field strength at the melt. At the moment, the magnetic field intensity detection unit is limited by the position of the guide shell and cannot measure at a plurality of space points.
As shown in fig. 5, in another alternative embodiment of the present invention, a magnetic field strength detecting unit 131 is disposed at the bottom end of a lifting rod 133 vertically passing through the dome 2, a plurality of detecting heads 132 are mounted on the magnetic field strength detecting unit 131, and a driving device 134 is disposed outside the dome 2, the driving device 134 being used for driving the lifting rod 133 to move linearly in the vertical direction. The bottom end of the lifting rod 133 can be lowered to a position closer to the surface of the melt in the quartz crucible 73, thereby making the measured magnetic field strength data closer to the magnetic field strength at the melt.
In some embodiments of the present invention, a plurality of temperature measuring holes are formed on the furnace body, specifically, a plurality of temperature measuring holes are formed at the top of the main furnace chamber 1, and the plurality of temperature measuring holes are arranged at intervals, a sealed heat insulation window is arranged in the temperature measuring holes, and the temperature detecting unit 9 is arranged outside the window; preferably, the temperature detecting unit 9 may be a Charge Coupled Device, that is, a CCD camera (Charge Coupled Device), which can change light into charges, store and transfer the charges, and also can take out the stored charges to change the voltage, the CCD camera has the advantages of small volume, light weight, no influence of a magnetic field, strong vibration and impact resistance, etc., and the CCD camera can be used to conveniently obtain a temperature distribution map of the melt in the quartz crucible 73, so that parameters of each process in production can be correspondingly adjusted according to the obtained temperature distribution, and temperature distribution conditions of different areas can be obtained by adjusting the shooting angle of the CCD camera; and the sealed heat insulation window can prevent external air from entering the furnace body to introduce impurities, and can prevent heat in the furnace from being dissipated outwards to influence the heating efficiency. Of course, in practical application, the device for detecting temperature may also be a temperature sensor, and the temperature sensor may be arranged at the bottom of the draft tube, so as to obtain temperature data in the furnace.
In some embodiments of the present invention, when the temperature acquisition unit employs a CCD camera, the controller may further process the received data captured by the CCD camera to further generate a temperature cloud map, and display the temperature cloud map on the display, so that an operator can visually observe the distribution of the temperature in the furnace, thereby performing corresponding operations.
As shown in fig. 7, in the embodiment of the present invention, the single crystal furnace further includes a controller, the controller is respectively connected to the magnetic field generator 5, the temperature detection unit 9, the magnetic field strength detection unit 131, the side heater 61, the bottom heater 62, the seed crystal pulling mechanism 4, the crucible driving mechanism, and the like, and the controller is configured to receive temperature data obtained by real-time detection by the temperature detection unit 9 and magnetic field strength data obtained by real-time detection by the magnetic field strength detection unit 131, so as to control operating parameters of each device in each process according to the temperature data and the magnetic field strength, so as to improve accuracy of control, and further improve quality of the prepared single crystal silicon rod.
Specifically, after the polysilicon material is loaded into the quartz crucible 73, the controller controls the side heater 61 and/or the bottom heater 62 to be turned on to heat and melt the polysilicon material, controls the magnetic field generator 5 to be turned on to apply a magnetic field to the furnace, determines the melting condition of the polysilicon material according to the detected temperature data, finely controls the melting rate and temperature of the polysilicon material, controls the magnetic field intensity and magnetic field angle applied by the magnetic field generator 5 according to the detected magnetic field intensity data, controls the heating power of the side heater 61 and/or the bottom heater 62, the magnetic field intensity and magnetic field angle of the magnetic field generator 5 to make the temperature of the melt reach a preset value and keep constant after the polysilicon material is melted to form a melt, determines the time when the seed crystal 10 is immersed into the polysilicon melt according to the temperature of the melt, the timing for starting the neck-drawing process can be judged, the technological parameters adopted when the shoulder is put on and turned can be determined, and the controller can further control the lifting speed and the rotating speed of the seed crystal lifting mechanism 4, the rotating speed of the quartz crucible 73 and the like according to the detected data in the process of lifting the seed crystal 10. Therefore, operators can judge the working condition in the furnace through a large amount of acquired temperature data and magnetic field intensity data, so that a large amount of waiting time in the traditional method is reduced, the production time of the silicon single crystal rod is shortened, the selected process parameters in each process can be accurately controlled, and the quality of the prepared silicon single crystal rod is effectively improved.
Furthermore, in the process of each stage, the polycrystalline silicon material can be stirred by the polycrystalline silicon melt stirring device 12, the melting of the polycrystalline silicon material can be accelerated by stirring in the melting process, after the polycrystalline silicon material is completely melted, the temperature of each part of the melt formed in the quartz crucible 73 can be uniform by stirring, the difficulty of the processes of leading the neck, shouldering, rotating the shoulder and the like is reduced, the quality of the prepared single crystal silicon rod 11 is ensured, and the purposes of shortening the production time of the single crystal silicon rod and improving the product quality are achieved. More specifically, the temperature uniformity in the quartz crucible 73 can be controlled more precisely by controlling the depth of insertion of the polycrystalline silicon melt stirring device 12 into the polycrystalline silicon material and the rotational speed of the polycrystalline silicon melt stirring device 12.
It should be noted that, when the polycrystalline silicon melt stirring device 12 is used, the temperature of the polycrystalline silicon melt can be more uniform, and the melting speed is accelerated, and meanwhile, the polycrystalline silicon melt is not stable, so that in the embodiment of the present invention, a magnetic field can be applied to the furnace through the magnetic field generator 5, and the thermal convection of the fluid can be retarded by controlling the magnitude of the magnetic field strength and the angle of the magnetic field, so that the surface of the polycrystalline silicon melt is more stable, and the crystal performance and uniformity are improved.
According to the single crystal furnace provided by the embodiment of the invention, the magnetic field is applied to the furnace body, so that the heat convection of the fluid in the crucible can be retarded, and the crystal performance and uniformity can be improved; and by additionally arranging the polycrystalline silicon melt stirring device, the time for melting the polycrystalline silicon material can be shortened, and the temperature of the formed melt is more uniform, so that the production time of the monocrystalline silicon is shortened, and the quality of the prepared monocrystalline silicon rod is improved.
As shown in fig. 8, another embodiment of the present invention further provides a method for preparing single crystal silicon, which is applied to the single crystal furnace described in any one of the above embodiments, and the method includes:
step 801: heating the polycrystalline silicon material in the crucible and applying a magnetic field to the furnace body;
step 802: and controlling the guide cylinder driving mechanism to drive a polycrystalline silicon melt stirring device connected with the bottom of the guide cylinder driving mechanism to stir the silicon material in the crucible.
Specifically, when the single crystal silicon rod is produced by using the single crystal furnace, firstly, a polysilicon material is placed in the quartz crucible 73, then the side heater 61 and/or the bottom heater 62 are controlled to be turned on to heat and melt the polysilicon material, and the magnetic field generator 5 is controlled to be turned on to apply a magnetic field to the furnace, and the polysilicon material is stirred by the polysilicon melt stirring device 12 to accelerate the melting of the polysilicon material, so that the waiting time is saved.
In this embodiment of the present invention, step 802 may specifically include the following steps:
acquiring temperature information in the crucible and magnetic field intensity information in the furnace body;
according to the temperature information and the magnetic field intensity information, the depth of the polycrystalline silicon melt stirring device extending into the polycrystalline silicon material and the rotating speed of the polycrystalline silicon melt stirring device are controlled, so that the average temperature of an annular area with the center of the crucible as the center and the width of 5cm and the area of any one annular area existing in the annular area are larger than 1cm2The average temperature of the plaques of (a) differs by less than 1 ℃.
That is, during the production process, the temperature information in the quartz crucible 73 and the magnetic field strength information in the furnace body can be obtained in real time, specifically, the data information can be detected by the temperature detection unit and the magnetic field strength detection unit 131, and the melting condition of the polysilicon material can be determined according to the detected temperature information and magnetic field strength information, so that the melting rate and temperature of the polysilicon material can be finely controlled by further controlling the depth of the polysilicon melt stirring device 12 inserted into the polysilicon material, the stirring speed and the like; after the polycrystalline silicon material is melted to form a melt, the depth of the polycrystalline silicon melt stirring device 12 inserted into the polycrystalline silicon material and the stirring speed are controlled so that the temperature of the melt reaches a preset value and is kept constant, and the average temperature of an annular area which takes the center of the liquid level of the quartz crucible 73 as the center and has a width of 4-6 cm (namely, the width of the annular area) and the average temperature of any one of the annular areas existing in the annular area are controlledThe area in the field is more than 0.5-1.5 cm2The average temperature difference of the plaques is less than 1 ℃, so that the temperature distribution on the surface of the melt is more uniform, the uniformity is better, and the single crystal silicon rod with high crystal performance and uniformity is further produced; in the above process, further, the heating power of the side heater 61 and/or the bottom heater 62, the magnetic field intensity and the magnetic field angle of the magnetic field generator 5 may be controlled simultaneously to accelerate the adjustment speed.
Moreover, the time when the seed crystal 10 is immersed in the polycrystalline silicon melt can be determined according to the temperature information and the magnetic field intensity information, the time for starting a neck drawing process can be judged, and the technological parameters adopted during shoulder putting and shoulder rotating can be determined, so that the uniform temperature field is favorable for reducing the difficulty of the processes of neck drawing, shoulder putting, shoulder rotating and the like; in pulling up the seed crystal 10, the timing of pulling up the seed crystal pulling mechanism 4, the speed and rotation speed of pulling up, the rotation speed of the quartz crucible 73, and the like can be further controlled based on the above-mentioned detected data.
In other embodiments of the present invention, the method further comprises:
and adjusting the magnetic field generator to enable the difference value between the average value of the magnetic field intensity in the furnace body and the preset magnetic field intensity threshold value to be less than 1% of the preset magnetic field intensity threshold value.
That is, the magnetic field generator 5 can adjust and optimize the environment of the melt in the crucible by using the magnetic field, for example, suppress convection of the melt in the quartz crucible, thereby suppressing elution of oxygen from the quartz crucible, and can suppress the flow of the melt in the quartz crucible by applying the magnetic field, thereby making the surface of the melt more calm and the temperature more uniform, and avoiding the occurrence of unstable liquid level of the polysilicon melt after stirring by using the polysilicon melt stirring device 12; therefore, according to the requirements of the process, the magnetic field strength and the magnetic field angle of the magnetic field generated by the magnetic field generator 5 can be adjusted to meet the preset requirements, that is: the difference value between the average value of the magnetic field intensity in the furnace body and the preset magnetic field intensity threshold value is smaller than 1% of the preset magnetic field intensity threshold value, wherein the preset magnetic field intensity threshold value is a target magnetic field intensity value of a corresponding process, and can be set according to an actual production process and an actual environment. Through the adjustment, the quality of the produced silicon single crystal rod can be effectively improved.
In some embodiments of the present invention, in the production process of the single crystal silicon rod, after the magnetic field strength detection unit 131 obtains the magnetic field strength information in the furnace body, the magnetic field strength information can be fed back to the controller, and at this time, an operator can obtain the magnetic field strength information in the furnace body of the crystal pulling furnace in real time through the controller, and then judge whether to stir the polysilicon solution in the crucible through the polysilicon solution stirring device 12 by combining the real-time magnetic field strength information. In addition, the operator can adjust the depth of immersion of the polysilicon solution stirring device 12 into the surface of the polysilicon solution and the stirring speed of the polysilicon solution stirring device 12 in combination with the magnetic field conditions inside the crystal pulling furnace measured in real time.
In another embodiment of the present invention, after the magnetic field strength detection unit obtains the magnetic field strength information inside the furnace body, the magnetic field strength information can be fed back to the controller in real time, the controller automatically determines whether the polycrystalline silicon solution inside the crucible is stirred by the polycrystalline silicon solution stirring device 12 after calculating through a preset optimization algorithm, and if it is determined that the polycrystalline silicon solution inside the crucible needs to be stirred by the polycrystalline silicon stirring device, the polycrystalline silicon solution stirring device 12 can output corresponding numerical values to control the depth of the polycrystalline silicon solution stirring device 12 immersed into the surface of the polycrystalline silicon solution and the stirring speed of the polycrystalline silicon solution stirring device 12, so that automatic control can be realized.
During the use of the polysilicon solution stirring device 12, whether the polysilicon solution is stirred by the polysilicon solution stirring device 12 can be determined by combining the temperature condition in the crystal pulling furnace, the magnetic field condition in the crystal pulling furnace, the polysilicon melting condition and other corresponding conditions and parameters. The depth of immersion of the polysilicon solution stirring apparatus 12 into the polysilicon solution and the speed of the polysilicon solution stirring apparatus 12 during stirring may also be determined in conjunction with the conditions and parameters listed above. However, the reference conditions are not limited to the three listed above.
According to the preparation method of the monocrystalline silicon, the progress of each process in the production process can be accurately judged by obtaining the temperature information in the crucible and the magnetic field intensity information in the furnace body, and then each device (such as a side heater, a bottom heater, a magnetic field generator and the like) in the monocrystalline furnace is accurately controlled, so that the growth environment of the monocrystalline silicon rod is improved and optimized, and the quality of the produced monocrystalline silicon rod is effectively improved.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The utility model provides a single crystal growing furnace, single crystal growing furnace includes the furnace body, be provided with crucible supporting component in the furnace body, crucible supporting component upper portion is provided with the crucible, be provided with the draft tube directly over the crucible, the inner wall of furnace body with be provided with the heater between the periphery of crucible, the top of furnace body is equipped with the seed crystal and carries and draw the mechanism, its characterized in that, single crystal growing furnace still includes:
the magnetic field generator is arranged at the periphery of the furnace body and used for generating a magnetic field covering the furnace body;
the guide shell driving mechanism is connected with the top of the guide shell and is used for driving the guide shell to do autorotation motion and lifting motion;
and the polycrystalline silicon melt stirring device is connected with the bottom of the guide cylinder and can perform autorotation motion and lifting motion along with the guide cylinder.
2. The single crystal furnace of claim 1, wherein the polycrystalline silicon melt stirring device is annular.
3. The single crystal furnace of claim 1, wherein the polycrystalline silicon melt stirring device is made of a silicon dioxide material.
4. The single crystal furnace of claim 1, further comprising:
the crucible driving mechanism is connected with the crucible supporting assembly and used for driving the crucible supporting assembly to do autorotation motion.
5. The single crystal furnace of claim 1, further comprising:
a magnetic field intensity detection unit for detecting the magnetic field intensity in the furnace body;
and the temperature detection unit is used for detecting the temperature in the crucible.
6. The single crystal furnace according to claim 5, wherein the temperature detection unit is a charge coupled device, a plurality of temperature measurement holes are formed in the top of the furnace body, a sealing and heat insulation window is arranged in each temperature measurement hole, the temperature detection unit is arranged on the outer side of each window, the magnetic field strength detection unit comprises a plurality of magnetic sensors, and the magnetic sensors are arranged at the bottom of the guide shell at intervals.
7. The single crystal furnace of claim 5, further comprising:
a controller, the controller respectively with magnetic field generator temperature detecting element magnetic field intensity detecting element the heater magnetic field generator and draft tube actuating mechanism connects, the controller is used for according to the temperature data control that temperature detecting element detected the heater is adjusted temperature in the crucible, be used for according to the magnetic field intensity data control that magnetic field intensity detecting element detected magnetic field generator adjusts magnetic field intensity in the furnace body and be used for according to the temperature data control that temperature detecting element detected draft tube actuating mechanism drive polycrystalline silicon melt stirring device is right polycrystalline silicon melt in the crucible stirs.
8. A method for manufacturing single crystal silicon, which is applied to the single crystal furnace according to any one of claims 1 to 7, comprising:
heating the polycrystalline silicon material in the crucible and applying a magnetic field to the furnace body;
and controlling the guide cylinder driving mechanism to drive a polycrystalline silicon melt stirring device connected with the bottom of the guide cylinder driving mechanism to stir the silicon material in the crucible.
9. The method for preparing monocrystalline silicon according to claim 8, wherein the step of controlling the guide shell driving mechanism to drive the polycrystalline silicon melt stirring device connected to the bottom of the guide shell to stir the polycrystalline silicon material in the crucible comprises the following steps:
acquiring temperature information in the crucible and magnetic field intensity information in the furnace body;
according to the temperature information and the magnetic field intensity information, the depth of the polycrystalline silicon melt stirring device extending into the polycrystalline silicon material and the rotating speed of the polycrystalline silicon melt stirring device are controlled, so that the average temperature of an annular area with the center of the crucible as the center and the width of 5cm and the area of any one annular area existing in the annular area are larger than 1cm2The average temperature of the plaques of (a) differs by less than 1 ℃.
10. The method for producing single-crystal silicon according to claim 8, characterized by further comprising:
and adjusting the magnetic field generator to enable the difference value between the average value of the magnetic field intensity in the furnace body and the preset magnetic field intensity threshold value to be less than 1% of the preset magnetic field intensity threshold value.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114855284A (en) * | 2022-04-06 | 2022-08-05 | 上海新昇半导体科技有限公司 | Method for growing monocrystalline silicon |
| CN116446048A (en) * | 2023-06-20 | 2023-07-18 | 常州市乐萌压力容器有限公司 | Furnace cover of silicon carbide single crystal furnace and processing technology thereof |
| WO2023179626A1 (en) * | 2022-03-21 | 2023-09-28 | 洛阳长缨新能源科技有限公司 | Artificial crystal furnace, and artificial crystal furnace system comprising artificial crystal furnace |
| CN117385457B (en) * | 2023-10-30 | 2024-05-17 | 昆明理工大学 | Method for delaying seed crystal color change in single crystal furnace |
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2020
- 2020-05-11 CN CN202010393429.7A patent/CN113638037A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023179626A1 (en) * | 2022-03-21 | 2023-09-28 | 洛阳长缨新能源科技有限公司 | Artificial crystal furnace, and artificial crystal furnace system comprising artificial crystal furnace |
| CN114855284A (en) * | 2022-04-06 | 2022-08-05 | 上海新昇半导体科技有限公司 | Method for growing monocrystalline silicon |
| CN116446048A (en) * | 2023-06-20 | 2023-07-18 | 常州市乐萌压力容器有限公司 | Furnace cover of silicon carbide single crystal furnace and processing technology thereof |
| CN117385457B (en) * | 2023-10-30 | 2024-05-17 | 昆明理工大学 | Method for delaying seed crystal color change in single crystal furnace |
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