CN113668046A - Preparation device of monocrystalline silicon and use method thereof - Google Patents

Preparation device of monocrystalline silicon and use method thereof Download PDF

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Publication number
CN113668046A
CN113668046A CN202110907340.2A CN202110907340A CN113668046A CN 113668046 A CN113668046 A CN 113668046A CN 202110907340 A CN202110907340 A CN 202110907340A CN 113668046 A CN113668046 A CN 113668046A
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frequency induction
induction coil
cooled copper
silicon
crucible
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CN113668046B (en
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刘立新
王中然
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Hunan Lixin Silicon Material Technology Co ltd
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Changsha Xinli Silicon Material Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10Crucibles or containers for supporting the melt
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/14Heating of the melt or the crystallised materials
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/06Silicon

Abstract

The invention discloses a preparation device of monocrystalline silicon and a using method thereof, belonging to the technical field of monocrystalline silicon manufacturing, and comprising a vacuum melting chamber; the split water-cooled copper crucible is arranged in the vacuum chamber; the graphite melting rod can extend into the split water-cooled copper crucible; the high-frequency induction coil is arranged outside the split water-cooled copper crucible; the quartz crucible is positioned below the split water-cooled copper crucible; the graphite heater is sleeved outside the quartz crucible; the low-frequency induction coil is sleeved outside the graphite heater; the first lifting mechanism is connected with the low-frequency induction coil and used for providing lifting force of the low-frequency induction coil along the axial direction of the quartz crucible; the cooler is attached to the bottom of the quartz crucible; and the discharging mechanism is used for discharging materials and introducing the split water-cooled copper crucible. The oxygen content of the final silicon crystal can be reduced, and the crystal quality is comprehensively improved.

Description

Preparation device of monocrystalline silicon and use method thereof
Technical Field
The application relates to the technical field of monocrystalline silicon preparation, in particular to a monocrystalline silicon preparation device and a using method thereof.
Background
When the frequency of non-renewable energy sources such as natural gas, coal, petroleum and the like is urgent, the rise of new energy sources and the dominant position of new energy sources in the future are the necessary way for the development of socioeconomic industry. Solar energy is taken as clean energy, and is rapidly developed under the drive of the huge market of the international photovoltaic industry. In the solar photovoltaic power generation industry, monocrystalline silicon becomes a base material serving as a main raw material for preparing a solar cell. At present, Cz method Czochralski single crystal and Fz method float-zone single crystal are the main methods for producing single crystal silicon. Cz method Czochralski single crystal is mainly used for manufacturing solar single crystal silicon, and Fz method zone melting single crystal is mainly used for manufacturing high reaction elements. In the former process, molten silicon is loaded by a quartz crucible, and liquid silicon inevitably contacts oxygen in the quartz crucible; the latter is suspension smelting without crucible, and the suspension of liquid silicon does not contact other materials and has no pollution, but the cost is slightly higher. Reducing the manufacturing cost of the monocrystalline silicon and reducing the oxygen content of the monocrystalline silicon are problems to be solved urgently.
Disclosure of Invention
An object of the embodiments of the present application is to provide a device for preparing single crystal silicon and a method for using the same, so as to solve the problems of high manufacturing cost and high oxygen content of single crystal silicon in the related art.
According to a first aspect of embodiments of the present application, there is provided a manufacturing apparatus of single crystal silicon, including:
a vacuum melting chamber;
the split water-cooled copper crucible is arranged in the vacuum chamber;
the graphite melting rod can extend into the split water-cooled copper crucible;
the high-frequency induction coil is arranged outside the split water-cooled copper crucible;
the quartz crucible is positioned below the split water-cooled copper crucible;
the graphite heater is sleeved outside the quartz crucible;
the low-frequency induction coil is sleeved outside the graphite heater;
the first lifting mechanism is connected with the low-frequency induction coil and is used for providing lifting force of the low-frequency induction coil along the axial direction of the quartz crucible;
a cooler attached to the bottom of the quartz crucible; and
and the discharging of the feeding mechanism is introduced into the split water-cooled copper crucible.
Further, still include:
and the graphite melting rod is arranged on the second lifting mechanism, and after preheating of the split water-cooled copper crucible is completed, the graphite melting rod is pulled out of the split water-cooled copper crucible through the second lifting mechanism.
Furthermore, a high-frequency induction heating power supply is connected to the high-frequency induction coil, and the induction frequency of the high-frequency induction coil is 10 KHz-30 KHz.
Further, a graphite heating power supply is connected to the graphite heater.
Further, a cooling system is connected to the cooler 14.
Furthermore, the low-frequency induction coil is connected with a low-frequency induction coil power supply, and the induction frequency of the low-frequency induction coil is 1 Hz-4 Hz.
Further, in the initial state, the bottom of the low-frequency induction coil and the bottom of the quartz crucible are on the same horizontal line.
Furthermore, a plurality of liquid outlet holes with the diameter of 1mm to 3mm are arranged in the bottom range of the water-cooled copper crucible.
Further, the lifting speed of the first lifting mechanism can be 0.1 mm/min-1.5 mm/min.
According to a second aspect of embodiments of the present application, there is provided a method of using a manufacturing apparatus of single crystal silicon, including:
(1) the feeding mechanism is used for feeding silicon materials into the split type water-cooled copper crucible;
(2) heating the quartz crucible to a predetermined temperature by the graphite heater;
(2) preheating a silicon material in a water-cooled copper crucible to a preset temperature through a graphite melting rod;
(3) heating the silicon material in the water-cooled copper crucible to reach the magnetic conduction temperature through a high-frequency induction coil;
(4) drawing away the graphite melting rod, continuously heating by using the high-frequency induction coil, and after the silicon material is melted, allowing part of silicon liquid to flow into the quartz crucible below from a liquid outlet hole in the water-cooled copper crucible;
(5) the low-frequency induction coil starts to work, the cooler is started, and along with the continuous growth of crystals, the first lifting mechanism gradually moves the low-frequency induction coil upwards by taking the front edge of the solid-liquid interface as the center until the crystal growth is finished.
The technical scheme provided by the embodiment of the application can have the following beneficial effects:
according to the technical scheme, the split water-cooled copper crucible is used for melting silicon in a vacuum state, and the melted silicon flows into the quartz crucible below to grow crystals. In the process of crystal growth, a technical means of low-frequency electromagnetic stirring and bottom cooling is adopted.
Silicon is melted through the water-cooled copper crucible, and crystal growth is started after the silicon flows into the quartz crucible after melting, so that the time for the silicon to contact the quartz crucible is short in the melting-solidification process, and the oxygen content in the silicon crystal is further reduced; through low-frequency stirring of a solid-liquid interface, power is enhanced for fully redistributing solutes in a crystal growth process, impurities are more easily separated from a solidification edge, and the crystal quality is improved; the cooler is involved, so that the solid-liquid interface is horizontal or convex in the process of growing the single crystal, the defect density is greatly reduced, and the crystal quality is ensured.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the application.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present application and together with the description, serve to explain the principles of the application.
Fig. 1 is a schematic configuration diagram showing a manufacturing apparatus of single crystal silicon according to an exemplary embodiment.
The reference numerals in the figures are:
the device comprises a vacuumizing device 1, a vacuum smelting chamber 2, a feeding mechanism 3, a second lifting mechanism 4, a high-frequency induction heating power supply 5, a graphite heating power supply 6, a cooling system 7, a low-frequency induction coil power supply 8, a first lifting mechanism 9, a graphite melting rod 10, a split water-cooled copper crucible 11, a quartz crucible 12, a monocrystalline silicon seed crystal 13, a cooler 14, a low-frequency induction coil 15, a graphite heater 16 and a high-frequency induction coil 17.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present application. Rather, they are merely examples of apparatus and methods consistent with certain aspects of the present application, as detailed in the appended claims.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this application and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any and all possible combinations of one or more of the associated listed items.
It is to be understood that although the terms first, second, third, etc. may be used herein to describe various information, such information should not be limited to these terms. These terms are only used to distinguish one type of information from another. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the present application. The word "if" as used herein may be interpreted as "at … …" or "when … …" or "corresponding to a determination", depending on the context.
Referring to fig. 1, an embodiment of the present invention provides an apparatus for preparing single crystal silicon, which mainly includes: the device comprises a vacuum melting chamber 2, a feeding mechanism 3, a first lifting mechanism 9, a graphite melting rod 10, a split water-cooled copper crucible 11, a quartz crucible 12, a cooler 14, a high-frequency induction coil 17, a low-frequency induction coil 15 and a graphite heater 16, wherein the split water-cooled copper crucible 11 is arranged in the vacuum chamber 2; the graphite melting rod 10 can extend into the split water-cooled copper crucible 11 and is used for preheating the split water-cooled copper crucible 11; the high-frequency induction coil is arranged outside the split water-cooled copper crucible 11; the quartz crucible 12 is positioned below the split water-cooled copper crucible 11; the graphite heater 16 is sleeved outside the quartz crucible 12; the low-frequency induction coil 15 is sleeved outside the graphite heater 16; the first lifting mechanism 9 is connected with the low-frequency induction coil 15 and is used for providing lifting force of the low-frequency induction coil 15 along the axial direction of the quartz crucible 12; the cooler 14 is attached to the bottom of the quartz crucible 12; and discharging of the feeding mechanism 3 is introduced into the split water-cooled copper crucible 11.
According to the technical scheme, the split water-cooled copper crucible is used for melting silicon in a vacuum state, and the melted silicon flows into the quartz crucible below to grow crystals. In the process of crystal growth, a technical means of low-frequency electromagnetic stirring and bottom cooling is adopted. Silicon is melted through the water-cooled copper crucible, and crystal growth is started after the silicon flows into the quartz crucible after melting, so that the time for the silicon to contact the quartz crucible is short in the melting-solidification process, and the oxygen content in the silicon crystal is further reduced; through low-frequency stirring of a solid-liquid interface, power is enhanced for fully redistributing solutes in a crystal growth process, impurities are more easily separated from a solidification edge, and the crystal quality is improved; the cooler is involved, so that the solid-liquid interface is horizontal or convex in the process of growing the single crystal, the defect density is greatly reduced, and the crystal quality is ensured.
In this embodiment, the vacuum melting chamber 2 can be evacuated by the evacuation device 1, and the ultimate vacuum degree is less than 3 Pa. Preferably, the feeding mechanism 3 is also vacuumized, and after the required vacuum degree is achieved, the feeding mechanism 3 feeds silicon materials. The vacuum pumping device 1 can adopt an oil booster pump, a roots pump or a mechanical pump.
Because graphite melts stick 10 mainly used right silicon in the split type water-cooling copper crucible 11 plays melting and restraint effect, and silicon plays melting the back, can pull out it, so corresponding second hoist mechanism 4 has still been designed, specifically, graphite melts stick 10 sets up on the second hoist mechanism 4, works as split type water-cooling copper crucible 11 preheats the back of accomplishing, through second hoist mechanism 4 will graphite melts stick 10 follows pull out in the split type water-cooling copper crucible 11.
The first lifting mechanism 9 and the second lifting mechanism 4 can adopt the existing lifting mechanism, the simplest is that a motor is additionally provided with a rope connected with a motor rotating shaft, and the principle is the same as that of a winch; and a linear motor or a lead screw and nut mechanism and the like can also be directly adopted, which is not described in detail herein. The lifting speed of the first lifting mechanism can be 0.1 mm/min-1.5 mm/min.
In this embodiment, the high-frequency induction coil is connected with a high-frequency induction heating power supply 5, and the induction frequency of the high-frequency induction coil is 10KHz to 30KHz through the high-frequency induction heating power supply 5, so that the silicon in the split water-cooled copper crucible can be melted and restrained at such a frequency.
In this embodiment, the graphite heater 16 is connected to a graphite heating power supply 6, which is a power supply for the graphite heater 16 to work.
In this embodiment, the cooler 14 is connected to the cooling system 7, the cooling system is realized by air cooling (compressed air) and water cooling, the amount of cooling in the early stage of crystal growth is small, gas cooling is applied, and the heat conduction speed in the later stage is slowly converted into water cooling.
In this embodiment, the low-frequency induction coil 15 is connected with a low-frequency induction coil power supply 8, and the low-frequency induction coil power supply 8 enables the induction frequency of the low-frequency induction coil to be 1Hz to 4Hz, so that the front edge of a solid-liquid interface in a crystal growth process can be stirred at such a frequency.
In the embodiment, the graphite heater is arranged in the middle of the vacuum melting chamber, the quartz crucible is placed in the graphite heater, and the central point of the quartz crucible is superposed with the central point of the water-cooled copper crucible; in the initial state, the bottom of the low-frequency induction coil and the bottom of the quartz crucible are on a horizontal line and can move upwards in the crystal pulling process.
In the embodiment, a plurality of liquid outlet holes with the diameter of 1mm to 3mm are formed in the bottom range of the water-cooled copper crucible, so that molten silicon can flow out.
In order to successfully produce a single crystal, a single crystal silicon seed crystal 13 is first produced, and a single silicon single crystal rod is selected, made into a proper size, and then placed at the bottom of a quartz crucible. In order to reduce the defects of pulling the single crystal in the future, the general principle of seed crystal manufacturing can be referred to in various methods such as adjustment of the crystal face of the monocrystalline silicon seed crystal 13, and the invention is not explained.
The main process for preparing the monocrystalline silicon by the device provided by the embodiment of the invention is as follows: the prefabricated seed crystal is placed at the bottom of the quartz crucible, the graphite melting rod 10 is extended into the split type water-cooled copper crucible, and a part of silicon material is added into the split type water-cooled copper crucible. After the vacuum pumping reaches a certain vacuum degree, a graphite heater is started to preheat the quartz crucible. Starting a high-frequency induction heating power supply until silicon in the split water-cooled copper crucible is magnetically conducted, drawing out the graphite melting rod 10, melting part of the silicon in the split water-cooled copper crucible, flowing into the quartz crucible from the bottom hole, gradually feeding by the feeding mechanism 3, and starting the low-frequency induction power supply to continuously stir the silicon liquid after the silicon liquid in the quartz crucible reaches a certain height; and opening the cooler to start to grow the single crystal, wherein the height of the low-frequency induction coil rises along with the rise of the solid-liquid interface until the growth of the single crystal is finished.
Controlling the temperature of the temperature field of the quartz crucible in the graphite heater to melt the surface part of the seed crystal, and ensuring that most of the seed crystal cannot be melted; in the whole process, the silicon melting speed and the crystal growth speed of the water-cooled copper crucible need to be accurately matched by controlling the high-frequency induction heating power supply and the cooler, and the height of silicon liquid in the quartz crucible is kept to be basically consistent within a certain range; the first lifting mechanism is controlled to ensure that the low-frequency induction coil is always positioned at the front edge of a solid-liquid surface of a growing crystal, and the diffusion of useless impurities at a solid-liquid interface is accelerated by stirring the solid-liquid surface; the cooler is controlled accurately, whether the single crystal is pulled into a single crystal or not, the quality of a final single crystal finished product is an important joint, red copper is used as a shell of the cooler, a surrounding red copper pipeline is arranged inside the cooler, low-melting-point and high-boiling-point alloy can be selected as liquid in a cavity, the red copper pipeline can be cooled by air cooling and water cooling, and a cooling inlet is arranged at the central position of the directional solidification cooler, so that a solid-liquid interface is in a horizontal or upward convex trend in the process of growing the single crystal, and the quality of the single crystal is ensured.
Through oxygen-free contact melting of silicon in the water-cooled copper crucible, the silicon liquid is prevented from contacting with oxygen for a long time, and the oxygen content of the final silicon crystal is reduced; in the crystal growth process of the silicon in the quartz crucible, the low-frequency induction magnetic coil is synchronously lifted according to the position of the solid-liquid interface, so that the stirring of the solid-liquid interface is enhanced, the power is enhanced for impurity diffusion, the cooler is simultaneously involved, the shape of the solid-liquid surface is changed, and the crystal quality is comprehensively improved.
Example 1
Placing the prefabricated seed crystal into the bottom of a quartz crucible, wherein the quartz crucible has the size of 255mm by 750mm in diameter; a graphite melting rod 10 with the diameter of 100mm and the length of 400mm is extended into a split type water-cooled copper crucible, the bottom of the water-cooled copper crucible is provided with 30 holes with the diameter of 2mm, and 40Kg of granular silicon material is put into a feeding mechanism 3. Vacuumizing, starting a high-frequency induction heating power supply when the vacuum degree reaches 1Pa, wherein the power of the high-frequency induction heating power supply is 100kw, the frequency of the high-frequency induction heating power supply is 10KHz, and under the frequency, the high-frequency magnetic field has an inward constraint force on silicon liquid to be melted, so that the silicon liquid is in soft contact with the split type water-cooled copper crucible, and the pollution of the quartz crucible to materials is avoided. And starting a graphite heater, heating the inside of the quartz crucible to 1420 ℃, and micro-melting the surface of the seed crystal under the dual actions of the bottom cooler and the graphite heater. It is noted here that the bottom cooler must be turned on, so that the seed crystal is not completely melted, and the micro-molten silicon and the top-run silicon melt are fused together, providing favorable conditions for crystal production. Preheating the silicon material in the split water-cooled copper crucible to 1200 ℃ by the high-purity graphite melting rod, wherein the silicon material becomes a conductor and is completely subjected to induction melting at the temperature, lifting the graphite melting rod 10, increasing high-frequency induction power, and starting to melt the silicon material in the water-cooled copper crucible, wherein part of molten silicon liquid flows into the quartz crucible from the liquid outlet hole along with the melting of the silicon material in the water-cooled copper crucible; along with the continuous process, when the height of the silicon liquid in the quartz crucible reaches about 50mm, the feeding mechanism 3 is started to shake and feed, so that the water cooling is ensuredThe quantity of the silicon materials in the copper crucible can also ensure that the silicon materials are quickly preheated to the conductive temperature after entering; gradually increasing the cooling capacity of the bottom cooler, wherein the air cooling is firstly used, when the crystal growth speed is reduced, the air quantity is increased, the heat taken away can be enhanced, when the increased air quantity cannot meet the crystal growth condition, the water is introduced for cooling, the capacity of the cooler for taking away the heat is fully ensured, the shape of the front edge of a solid-liquid interface for crystal growth can be controlled, and the crystal quality is improved; and starting a low-frequency induction coil power supply 8, wherein the number of turns of the low-frequency induction coil is 1 turn, the frequency is 1Hz, the power is 10kw, and crystal growth is started. After stabilization, the crystal grows at the speed of 0.8mm/min, the low-frequency induction coil synchronously moves upwards at the speed of 0.8mm/min, the position of an induction stirring magnetic field on a solid-liquid surface is ensured, the low-frequency stirring effect is fully exerted, impurities are easier to move to a liquid phase, and the crystal has more power than the traditional diffusion mode. After about 15h of crystal growth process, a silicon rod with the diameter of 250mm x 680mm is obtained. The detection shows that the resistivity of the silicon rod is 1.07-1.0 Ω & cm, the head part of the minority carrier lifetime is 4.22 μ s, the tail part is 3.66 μ s, and the dislocation density is less than 300pcs/cm2And the tail of the interstitial oxygen content is less than 8.12 ppm. Therefore, the single crystal silicon rod crystal manufactured by the device has higher quality, and the dislocation density and the oxygen content are obviously superior to the level of the current CZ Faraday single crystal.
Example 2
Placing the prefabricated seed crystal at the bottom of a quartz crucible, wherein the quartz crucible has the size of 285mm by 650mm in diameter; a graphite melting rod 10 with the diameter of 100mm and the length of 400mm is extended into a split type water-cooled copper crucible, the bottom of the split type water-cooled copper crucible is provided with 50 holes with the diameter of 1mm, and 45Kg of granular silicon material is placed into a feeding mechanism 3. Vacuumizing, starting a high-frequency induction heating power supply when the vacuum degree reaches 1Pa, wherein the power is 100kw, and the frequency is 20 KHz. And starting a graphite heater, heating the inside of the quartz crucible to 1420 ℃, and micro-melting the surface of the seed crystal under the dual actions of the bottom cooler and the graphite heater. It is noted here that the bottom cooler must be turned on, so that the seed crystal is not completely melted, and the micro-molten silicon and the top-run silicon melt are fused together, providing favorable conditions for crystal production. When the graphite melting rod 10 preheats the silicon material in the split water-cooled copper crucible to 1250 ℃, the silicon material becomes a conductor at the temperature and is completely conductedReceiving induction melting, lifting the high-purity graphite rod, increasing high-frequency induction power, and starting to melt silicon materials in the split water-cooled copper crucible, wherein the silicon materials in the split water-cooled copper crucible are melted, and partially melted silicon liquid flows into the quartz crucible from the liquid outlet hole; with the continuous process, when the height of the silicon liquid in the quartz crucible reaches about 60mm, the feeding mechanism 3 is started to feed the silicon liquid spirally, so that the quantity of the silicon material in the split water-cooled copper crucible is ensured, and the silicon material can be quickly preheated to the conductive temperature after entering; gradually increasing the cooling capacity of the bottom cooler, wherein the air cooling is firstly used, when the crystal growth speed is reduced, the air quantity is increased, the heat taken away can be enhanced, when the increased air quantity cannot meet the crystal growth condition, the water is introduced for cooling, the capacity of the cooler for taking away the heat is fully ensured, the shape of the front edge of a solid-liquid interface for crystal growth can be controlled, and the crystal quality is improved; and starting a low-frequency induction coil power supply 8, wherein the number of turns of the low-frequency induction coil is 1 turn, the frequency is 3Hz, the power is 15kw, and crystal growth is started. After stabilization, the crystal grows at the speed of 0.6mm/min, the low-frequency induction coil synchronously moves upwards at the speed of 0.6mm/min, the position of an induction stirring magnetic field on a solid-liquid surface is ensured, the low-frequency stirring effect is fully exerted, impurities are easier to move to a liquid phase, and the crystal has more power than the traditional diffusion mode. After about 15h of crystal growth process, a phi 280mm x 600mm silicon rod is obtained. The detection shows that the resistivity of the silicon rod is 1.04-0.88 Ω & cm, the head part of the minority carrier lifetime is 5.12 μ s, the tail part is 4.36 μ s, and the dislocation density is less than 400pcs/cm2The tail of the interstitial oxygen content is less than 9.12 ppm. Therefore, the single crystal silicon rod crystal manufactured by the device has higher quality, and the dislocation density and the oxygen content are obviously superior to the level of the current CZ Faraday single crystal.
The melting and crystal growth functions are separated, so that the long-time contact between silicon liquid and oxygen in the melting process is avoided, and the oxygen content of the final crystal is reduced; the inherent state of the crystal during growth is changed by the low-frequency electromagnetic stirring and cold zone device technology, and impurities are discharged out of the crystal during the crystal growth process, so that the concentration diffusion and the electromagnetic stirring force are supported; the cooler completely changes the solid-liquid interface from concave to convex, so that the quality of the final crystal is greatly improved.
Specifically, the silicon material is melted in a water-cooled copper crucible, flows into a quartz crucible with a seed crystal arranged below, and starts to melt after a certain amount of liquid is carried in the quartz crucible. In the whole process, the main task of the water-cooled copper crucible is melting, and crystal growth is mainly carried out in the quartz crucible. The two are separated, reducing the contact time of silicon with oxygen in the process. As in example 1, the low-frequency stirring of the 1Hz low-frequency coil is carried out, the synchronization of 0.8mm/min and the crystal growth speed is kept, and the movement rate of impurities on a solid-liquid interface is enhanced; the intervention of the cooler ensures that the back-coating phenomenon does not occur all the time during the growth, keeps the convex trend of the solid-liquid interface and provides powerful guarantee for the final dislocation density and the uniformity of the quality of the whole rod.
Other embodiments of the present application will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the application being indicated by the following claims.
It will be understood that the present application is not limited to the precise arrangements described above and shown in the drawings and that various modifications and changes may be made without departing from the scope thereof. The scope of the application is limited only by the appended claims.

Claims (10)

1. An apparatus for manufacturing single crystal silicon, comprising:
a vacuum melting chamber;
the split water-cooled copper crucible is arranged in the vacuum chamber;
the graphite melting rod can extend into the split water-cooled copper crucible;
the high-frequency induction coil is arranged outside the split water-cooled copper crucible;
the quartz crucible is positioned below the split water-cooled copper crucible;
the graphite heater is sleeved outside the quartz crucible;
the low-frequency induction coil is sleeved outside the graphite heater;
the first lifting mechanism is connected with the low-frequency induction coil and is used for providing lifting force of the low-frequency induction coil along the axial direction of the quartz crucible;
a cooler attached to the bottom of the quartz crucible; and
and the discharging of the feeding mechanism is introduced into the split water-cooled copper crucible.
2. The apparatus for manufacturing single crystal silicon according to claim 1, further comprising:
and the graphite melting rod is arranged on the second lifting mechanism, and after preheating of the split water-cooled copper crucible is completed, the graphite melting rod is pulled out of the split water-cooled copper crucible through the second lifting mechanism.
3. The apparatus according to claim 1, wherein a high-frequency induction heating power supply is connected to the high-frequency induction coil, and an induction frequency of the high-frequency induction coil is 10KHz to 30 KHz.
4. The apparatus for manufacturing a silicon single crystal as claimed in claim 1, wherein a graphite heating power supply is connected to the graphite heater.
5. The apparatus for manufacturing a silicon single crystal as claimed in claim 1, wherein a cooling system is connected to said cooler 14.
6. The apparatus of claim 1, wherein a low frequency induction coil power supply is connected to the low frequency induction coil, and an induction frequency of the low frequency induction coil is 1Hz to 4 Hz.
7. The manufacturing apparatus of a silicon single crystal as set forth in claim 1, wherein the bottom of said low frequency induction coil and the bottom of said quartz crucible are in a horizontal line in an initial state.
8. The apparatus of claim 1, wherein the water-cooled copper crucible has a plurality of outlet holes with a diameter of 1mm to 3mm in the bottom area.
9. The manufacturing apparatus of a silicon single crystal as claimed in claim 1, wherein the lifting speed of said first lifting mechanism is 0.1mm/min to 1.5 mm/min.
10. The method for using a device for manufacturing single crystal silicon according to claim 1, comprising:
(1) the feeding mechanism is used for feeding silicon materials into the split type water-cooled copper crucible;
(2) heating the quartz crucible to a predetermined temperature by the graphite heater;
(2) preheating a silicon material in a water-cooled copper crucible to a preset temperature through a graphite melting rod;
(3) heating the silicon material in the water-cooled copper crucible to reach the magnetic conduction temperature through a high-frequency induction coil;
(4) drawing away the graphite melting rod, continuously heating by using the high-frequency induction coil, and after the silicon material is melted, allowing part of silicon liquid to flow into the quartz crucible below from a liquid outlet hole in the water-cooled copper crucible;
(5) the low-frequency induction coil starts to work, the cooler is started, and along with the continuous growth of crystals, the first lifting mechanism gradually moves the low-frequency induction coil upwards by taking the front edge of the solid-liquid interface as the center until the crystal growth is finished.
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