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WO2023143298A1 - Device for manufacturing silicon carbide crystal and method for manufacturing silicon carbide crystal - Google Patents

Device for manufacturing silicon carbide crystal and method for manufacturing silicon carbide crystal Download PDF

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Publication number
WO2023143298A1
WO2023143298A1 PCT/CN2023/072843 CN2023072843W WO2023143298A1 WO 2023143298 A1 WO2023143298 A1 WO 2023143298A1 CN 2023072843 W CN2023072843 W CN 2023072843W WO 2023143298 A1 WO2023143298 A1 WO 2023143298A1
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WIPO (PCT)
Prior art keywords
silicon carbide
crucible
graphite
assembly
seed crystal
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Ceased
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PCT/CN2023/072843
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French (fr)
Chinese (zh)
Inventor
郭超
母凤文
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Innovative Semiconductor Substrate Technology Co Ltd
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Innovative Semiconductor Substrate Technology Co Ltd
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Publication of WO2023143298A1 publication Critical patent/WO2023143298A1/en
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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
    • C30B27/00Single-crystal growth under a protective fluid
    • C30B27/02Single-crystal growth under a protective fluid by pulling from a 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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/36Carbides

Definitions

  • the present application relates to the technical field of silicon carbide manufacturing, for example, to a device for manufacturing silicon carbide crystals and a method for manufacturing silicon carbide crystals.
  • Silicon carbide is a wide bandgap semiconductor material. Devices made of silicon carbide substrates have the advantages of high temperature resistance, high voltage resistance, high frequency, high power, radiation resistance, and high efficiency. They have important roles in radio frequency, new energy vehicles and other fields. Value.
  • the physical vapor transport method is a common silicon carbide crystal growth method. It heats silicon carbide powder by induction heating in a vacuum environment to sublimate it to produce reaction gases containing different gas phase components such as Si, Si2C, and SiC2. Silicon carbide single crystals are produced by solid-gas reactions. The single crystal produced by this method contains many defects such as micropipes and dislocations, which have a negative impact on the performance of silicon carbide devices.
  • the crystal growth of the liquid phase method is closer to the thermodynamic equilibrium conditions, which can produce higher quality silicon carbide crystals.
  • the basic principle of the liquid phase method is: put the silicon-containing co-solvent in the graphite crucible, melt the co-solvent by induction heating, and dissolve the carbon in the graphite crucible into the co-solvent; then place the silicon carbide seed crystal in the co-solvent At the liquid level, due to the supercooling of the seed crystal, carbon precipitates on the solid-liquid interface of the seed crystal, and combines with silicon in the co-solvent to form silicon carbide crystals.
  • the present application proposes a device for manufacturing silicon carbide crystals.
  • the present application proposes a method of manufacturing silicon carbide crystals.
  • the present application discloses a device for manufacturing silicon carbide crystals, comprising: a housing, the housing defines an accommodating cavity; a crucible assembly, the crucible assembly includes a graphite crucible and a non-graphite crucible disposed in the graphite crucible, The non-graphite crucible is used to carry the co-solvent solution; the seed crystal assembly, the seed crystal assembly can be lifted and fitted in the housing, and one end of the seed crystal assembly extends into the crucible assembly, the seed crystal assembly The assembly is used to carry the silicon carbide crystal; the heating element is arranged in the accommodating chamber and surrounds the crucible assembly; One end of the piece is immersed in the co-solvent solution.
  • the present application also discloses a method for manufacturing silicon carbide crystals.
  • the method for manufacturing silicon carbide crystals is carried out by using the device for manufacturing silicon carbide crystals described above.
  • the method for manufacturing silicon carbide crystals includes:
  • the seed crystal assembly is pulled to achieve silicon carbide crystal growth.
  • Fig. 1 is a schematic structural diagram of a device for manufacturing silicon carbide crystals according to an embodiment of the present application
  • Fig. 2 is the structural representation of a kind of graphite part of the embodiment of the present application.
  • Fig. 3 is the structural representation of another kind of graphite part of the embodiment of the present application.
  • Fig. 4 is a schematic flowchart of a method for manufacturing a silicon carbide crystal according to an embodiment of the present application.
  • the graphite crucible is not only a container for a solvent, but also a source of carbon. As the growth progresses, the graphite crucible will continue to dissolve and corrode. At the same time, it is prone to cracks due to thermal shock, resulting in a limited number of cycles, or even one-time use.
  • the cost of high-purity graphite crucible is relatively high, which is one of the main cost components of liquid phase crystal growth.
  • Graphite crucibles have a limited number of cycles, resulting in high crystal manufacturing costs.
  • embodiments of the present application provide a device for manufacturing silicon carbide crystals and a method for manufacturing silicon carbide crystals.
  • connection should be understood in a broad sense, for example, it can be a fixed connection or a detachable connection. Connected, or integrally connected; it can be mechanically connected or electrically connected; it can be directly connected or indirectly connected through an intermediary, and it can be the internal communication of two components. Those of ordinary skill in the art can understand the specific meanings of the above terms in this application in specific situations.
  • the crucible assembly 2 includes a graphite crucible 21 and a non-graphite crucible 22 disposed in the graphite crucible 21, the non-graphite crucible 22 is used to carry the cosolvent solution, the seed crystal assembly 3 can be lifted and fitted in the housing 1, and One end of the seed crystal assembly 3 extends into the crucible assembly 2, the seed crystal assembly 3 is used to carry the silicon carbide crystal, the heating element 4 is arranged in the accommodation chamber 11 and is arranged around the crucible assembly 2, and the graphite element 5 can be raised and lowered to fit in the housing 1, one end of the graphite piece 5 is immersed in the co-solvent solution.
  • the seed crystal assembly 3 and the graphite component 5 are lowered to a position in contact with the co-solvent solution.
  • the carbon in piece 5 dissolves into the co-solvent solution, and due to the supercooling of the seed crystal component 3, the carbon precipitates on the lower surface of the seed crystal component 3, and combines with the silicon in the co-solvent solution to form silicon carbide crystals.
  • the crucible assembly 2 of the present embodiment includes a graphite crucible 21 and a non-graphite crucible 22 disposed in the graphite crucible 21, during the entire reaction process, the graphite crucible 21 will not undergo dissolution and corrosion, and due to the barrier of the non-graphite crucible 22 , there will be no cold and heat shock in the graphite crucible 21, which reduces the probability of cracks in the graphite crucible 21, prolongs the service life of the graphite crucible 21, thereby prolonging the replacement cycle of the graphite crucible 21 and reducing the manufacturing cost of silicon carbide crystals .
  • the melting point of the non-graphite crucible 22 is slightly higher than the temperature of the co-solvent solution, and as the crystal growth time increases, the non-graphite crucible 22 may soften and deform. Therefore, if the non-graphite crucible 22 is placed in the graphite crucible 21, the shape of the graphite crucible 21 is stable at a high temperature, and the shape of the non-graphite crucible 22 can be effectively maintained, thereby avoiding the serious deformation of the non-graphite crucible 22 that cannot produce silicon carbide crystals smoothly. phenomenon occurs.
  • the non-graphite crucible 22 in this embodiment refers to a crucible with a lower cost than high-purity graphite.
  • a quartz crucible is used, and the melting point of quartz is about 1750°C, slightly higher than the temperature of the co-solvent.
  • the temperature of the co-solvent is about 1800°C, and a corundum crucible is used, and the melting point of corundum is about 2000°C, which is slightly higher than the temperature of the co-solvent.
  • the non-graphite crucible 22 in this embodiment can also be made of high-melting-point metal materials such as tungsten and molybdenum that do not chemically react with the co-solvent.
  • the accommodating chamber 11 has at least one air suction port and is connected to a vacuum obtaining device, which can reduce the air pressure in the accommodating chamber 11 to a desired value.
  • the containing chamber 11 has at least one gas filling port, which can be filled with nitrogen, argon, helium or other inert gases.
  • the containing chamber 11 is connected to at least one vacuum gauge.
  • the experimenter can intuitively observe the vacuum degree in the accommodation chamber 11 .
  • the co-solvent solution may also include Ti, Cr, Sc, Ni, Al, Co, Mn, Mg, Ge, As, P, N, O, B, One or more elements of Dy, Y, Nb, Nd, and Fe can be selected according to actual needs.
  • the device for making silicon carbide crystals further includes a support rod 6 , the support rod 6 is passed through the housing 1 , and one end of the support rod 6 extends into the housing 1 and connects with the graphite piece 5 connected, and the other end protrudes from the casing 1 and is connected with the external drive mechanism.
  • the driving member that drives the support rod 6 is set as an external drive mechanism located outside the housing 1, so that the graphite member 5 will not be driven under the premise of ensuring stable crystallization.
  • the driving parts are in a high temperature working environment, thus prolonging their service life.
  • FIG. 2 schematically shows a section of a part of the graphite member 5 .
  • the graphite piece 5 is ring-shaped, and the inner or outer wall of the graphite piece 5 is provided with a hole structure 51 . It can be understood that the graphite part 5 is ring-shaped and the inner and/or outer walls are provided with a hole structure 51, which can increase the contact area between the graphite part 5 and the cosolvent solution, improve the dissolution efficiency of the graphite part 5, and thereby improve the silicon carbide. manufacturing efficiency.
  • the hole structure 51 includes a plurality of grooves, the plurality of grooves are arranged at intervals along the axial and/or circumferential directions of the graphite member 5, and each groove is arranged along the graphite The circumferential or axial extension of the member 5 is set.
  • the hole structure 51 can be processed more conveniently, which reduces the processing difficulty of the graphite piece 5 .
  • the graphite member 5 may also be formed in a porous structure or in a shape with other hollow structures, and is not limited to the ring shape in this embodiment.
  • the seed assembly 3 includes a seed rod 31 and a seed holder 32, the seed rod 31 is passed through the housing 1, and one end of the seed rod 31 protrudes from the housing 1 and is connected to an external drive mechanism , the other end extends into the crucible assembly 2, and the seed crystal support 32 is provided at one end of the seed rod 31 protruding into the crucible assembly 2, and the seed crystal support 32 is used to carry the growing silicon carbide crystal. It can be understood that since the interior of the chamber 11 is always at a relatively high temperature during the entire growth process, if the driver for driving the seed crystal assembly 3 is placed in the chamber 11 , the driver may be easily damaged.
  • the driving member for driving the seed crystal assembly 3 is set outside the housing cavity 11 to form an external driving structure.
  • the drive will not The driving part of the seed crystal assembly 3 is in a high-temperature working environment, thereby prolonging the service life of the driving part.
  • the seed crystal holder 32 in this embodiment may be a graphite holder or other high-temperature-resistant metal holders, which may be selected according to actual needs.
  • the external drive mechanism can also drive the seed rod 31 to rotate when driving the seed rod 31 up and down, so that the liquid in the crucible assembly 2 will be stirred, thereby better improving the crystallization effect.
  • the external drive mechanism can choose any structure that can realize linear drive and rotational drive, such as a motor driving a ball screw, a cylinder, or an electric push rod, according to actual needs, and the external drive mechanism is not limited here.
  • the seed crystal assembly 3 further includes a seed wafer 33 disposed on the seed crystal support 32 , and the seed wafer 33 is used to support the growing silicon carbide crystal. It can be understood that setting the seed wafer 33 on the seed crystal support 32 can make the crystal form of the generated silicon carbide crystal consistent with the seed wafer, and at the same time, it is more convenient to peel the generated silicon carbide crystal from the seed crystal assembly 3 .
  • the device for manufacturing silicon carbide crystals further includes a crucible holder 7, the crucible holder 7 is pierced on the housing 1, one end of the crucible holder 7 protrudes from the housing 1 and is connected to an external drive mechanism, and the other end is connected to the graphite
  • the crucibles 21 are connected. It can be understood that, since the inside of the containing chamber 11 is always at a relatively high temperature during the whole growth process, if the driving part for driving the crucible assembly 2 is arranged in the containing chamber 11, the driving part may be easily damaged.
  • the driving part used for the crucible assembly 2 is arranged outside the containing chamber 11, under the premise of ensuring stable crystallization, the driving part will not be placed in a high-temperature working environment, thereby The service life of the drives of the crucible assembly 2 is extended.
  • the external drive mechanism can also drive the graphite crucible 21 to rotate when driving the graphite crucible 21 up and down, so that the liquid in the graphite crucible 21 will be stirred, thereby better improving the crystallization effect.
  • the external drive mechanism can choose any structure that can realize linear drive and rotational drive, such as a motor driving a ball screw, a cylinder, or an electric push rod, according to actual needs, and the external drive mechanism is not limited here.
  • the heating element 4 comprises an induction heating coil formed in a helical shape. It can be understood that the induction heating coil is used for heating. During the working process, the induction heating coil passes an alternating current, An alternating magnetic field is generated, thereby generating an induced current in the graphite crucible 21 to realize heating of the graphite crucible 21, and then the heat is conducted from the graphite crucible 21 to the non-graphite crucible 22, so that the cosolvent in the non-graphite crucible 22 melts and heats up to the required temperature.
  • the induction heating coil is used for heating, the heating temperature is higher, the utilization rate of electric energy is higher, and the liquid in the graphite crucible 2 can be electromagnetically stirred.
  • the induction heating coil is a helical tube with equal pitch, that is, the distance between two adjacent turns is a fixed value. This can improve the heating uniformity of the induction heating coil.
  • the number of turns of the induction heating coil can be selected as 10-20 turns according to actual needs, and of course other turns can also be used.
  • the longitudinal section of the induction heating coil is a circular ring or a rectangular ring, that is, the induction heating coil is a hollow structure, so that the induction heating coil can be cooled by water to avoid overheating of the induction heating coil.
  • the induction heating coil passes through a flexible circuit and a water circuit, and a vacuum feedthrough provided on the housing 1 , and the vacuum feedthrough is then connected to a power source and a circulating water source outside the chamber.
  • the vacuum feedthrough can be set as a plug structure according to actual needs, which is convenient for installation and disassembly.
  • the current frequency of the induction heating coil is 1-100 kHz.
  • the device for manufacturing silicon carbide crystals further includes a heat insulating layer 8 , and the heat insulating layer 8 is disposed between the heating element 4 and the graphite crucible 21 and is disposed around the graphite crucible 21 .
  • the setting of the heat insulating layer 8 can avoid the heat loss of the graphite crucible 21 .
  • the insulating layer material is graphite felt with low thermal conductivity.
  • the device for manufacturing silicon carbide crystals includes a housing 1, a crucible assembly 2, a seed crystal assembly 3, a graphite piece 5, a support rod 6, a crucible holder 7 and a thermal insulation layer 8, and the housing 1 defines a housing
  • the crucible assembly 2 includes a graphite crucible 21 and a non-graphite crucible 22 arranged in the graphite crucible 21, the non-graphite crucible 22 is used to carry a cosolvent solution
  • the support rod 6 is installed on the shell 1, and one end of the support rod 6 It extends into the casing 1 and connects with the graphite piece 5, and the other end extends out of the casing 1 and connects with the external drive mechanism.
  • the graphite part 5 is a ring structure, and the outer or inner peripheral wall of the graphite part 5 is provided with a plurality of grooves, and the plurality of grooves are spaced along the axial and/or circumferential direction of the graphite part 5 Each groove is set along the circumferential or axial extension of the graphite member 5 .
  • the seed crystal assembly 3 includes a seed crystal rod 31 and a seed crystal holder 32, the seed crystal rod 31 is penetrated on the housing 1, and one end of the seed crystal rod 31 protrudes from the housing 1 and is connected with an external drive mechanism, and can be driven externally Driven by the mechanism to lift and rotate, the other end of the seed rod 31 extends into the crucible assembly 2, the seed holder 32 is set at the end where the seed rod 31 extends into the crucible assembly 2, and the seed wafer 33 is located at the end of the seed holder 32. At one end of the crucible assembly 2, the seed wafer 33 is used to support the growing silicon carbide crystal.
  • the heating element 4 is arranged in the accommodating chamber 11 and includes Included is an induction heating coil formed in a helical shape.
  • the crucible holder 7 is mounted on the casing 1 , one end of the crucible holder 7 protrudes from the casing 1 and is connected with an external driving mechanism, and the other end is connected with a graphite crucible 21 .
  • the heat insulation layer 8 is arranged between the heating element 4 and the graphite crucible 21 and is arranged around the graphite crucible 21 .
  • the present application also discloses a method for manufacturing silicon carbide crystals.
  • the method for manufacturing silicon carbide crystals is carried out by using the aforementioned device for manufacturing silicon carbide crystals.
  • the method for manufacturing silicon carbide crystals includes:
  • a vacuum device For example, first use a vacuum device to evacuate the chamber 11, so that the pressure in the chamber 11 drops to a set value, and then fill the chamber 11 with nitrogen, argon, helium or other inert gases, so that The pressure rises to the set value.
  • nitrogen, argon, helium or other inert gases so that The pressure rises to the set value.
  • Both the suction pressure and the inflation pressure can be selected according to actual needs, and the set pressure values are not limited here.
  • a non-contact heating element 4 (such as an induction heating coil) can be used to heat the graphite crucible 21 by an alternating current in the induction heating coil, and the heat of the graphite crucible 21 can be transferred to the non-graphite crucible 22 to make the non-graphite crucible 22
  • the co-solvent solution in it reaches the specified temperature.
  • the temperature of the co-solvent solution can be detected by using an existing detection device, and there is no need to limit how to detect and control it here;
  • the lower surface of the seed crystal assembly 3 can just touch the liquid level of the co-solvent solution, and can also be immersed in a certain depth of the liquid level, so that supercooling can be better realized and carbon is precipitated, thereby being compatible with the co-solvent solution.
  • the silicon combines to form silicon carbide crystals.
  • the carbon in the graphite piece 5 will dissolve into the co-solvent.
  • silicon carbide crystals can continuously grow on the lower surface of the seed crystal assembly 3 .
  • the graphite piece 5 needs to be lifted and separated from the co-solvent solution to avoid waste of the graphite piece 5 . And at the same time turn off the heating element 4, and wait for the auxiliary solvent to cool down to the set safe temperature.
  • lowering the seed crystal assembly 3 can also lift the seed crystal assembly 3 so that the lower surface of the seed crystal assembly 3 is above the liquid level of the co-solvent solution, so that the seed crystal assembly 3 can be pulled out Partial co-solvent solution. It can be understood that, in this way, the lower surface of the seed crystal assembly 3 can be located Above the liquid level, due to the effect of surface tension, a part of the solution is lifted to form a meniscus, which helps the formation of silicon carbide crystals.
  • the distance between the lower surface of the seed crystal assembly 3 and the liquid surface of the co-solvent is 0.1 mm-3 mm.
  • the seed crystal assembly 3 when the seed crystal assembly 3 is pulled, the seed crystal assembly 3 can be driven to rotate and the crucible assembly 2 can be driven to rotate at the same time. As a result, the co-solvent solution can be shaken, thereby contributing to the formation of silicon carbide crystals.
  • the graphite part 5 when the seed crystal assembly 3 is pulled, the graphite part 5 is driven down to maintain the liquid level of the cosolvent solution constant, and the depth at which the graphite part 5 is immersed in the cosolvent solution is increased, so that the liquid level of the cosolvent solution The height remains basically unchanged during the whole process of crystal growth, thereby ensuring the stability and consistency of the formation of silicon carbide crystals.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

A device for manufacturing a silicon carbide crystal and a method for manufacturing a silicon carbide crystal, the device for manufacturing a silicon carbide crystal comprising a housing (1), a crucible assembly (2), a seed crystal assembly (3), a heater (4), and a graphite member (5), wherein the housing (1) defines an accommodating cavity (11), the crucible assembly (2) comprises a graphite crucible (21) and a non-graphite crucible (22), which is arranged inside the graphite crucible (21), the non-graphite crucible (22) is configured for containing a cosolvent solution, the seed crystal assembly (3) is liftably fitted in the housing (1), one end of the seed crystal assembly (3) extends into the crucible assembly (2), the seed crystal assembly (3) is configured for containing the silicon carbide crystal, the heater (4) is arranged inside the accommodating cavity (11) and around the crucible assembly (2), the graphite member (5) is liftably fitted in the housing (1), and one end of the graphite member (5) is immersed in the cosolvent solution.

Description

制造碳化硅晶体的装置及制造碳化硅晶体的方法Device for producing silicon carbide crystal and method for producing silicon carbide crystal

本申请要求在2022年01月27日提交中国专利局、申请号为202210102342.9的中国专利申请的优先权,以上申请的全部内容通过引用结合在本申请中。This application claims the priority of the Chinese patent application with application number 202210102342.9 submitted to the China Patent Office on January 27, 2022, and the entire content of the above application is incorporated in this application by reference.

技术领域technical field

本申请涉及碳化硅制造技术领域,例如涉及一种制造碳化硅晶体的装置及制造碳化硅晶体的方法。The present application relates to the technical field of silicon carbide manufacturing, for example, to a device for manufacturing silicon carbide crystals and a method for manufacturing silicon carbide crystals.

背景技术Background technique

碳化硅是一种宽禁带半导体材料,以碳化硅衬底制作的器件具有耐高温、耐高压、高频、大功率、抗辐射、效率高等优势,在射频、新能源汽车等领域具有重要的应用价值。Silicon carbide is a wide bandgap semiconductor material. Devices made of silicon carbide substrates have the advantages of high temperature resistance, high voltage resistance, high frequency, high power, radiation resistance, and high efficiency. They have important roles in radio frequency, new energy vehicles and other fields. Value.

物理气相传输法是一种常见的碳化硅晶体生长方法,其在真空环境下通过感应加热的方式加热碳化硅粉料,使其升华产生包含Si、Si2C、SiC2等不同气相组分的反应气体,通过固-气反应产生碳化硅单晶。该方法制造的单晶含有较多微管、位错等缺陷,给碳化硅器件的性能带来负面影响。The physical vapor transport method is a common silicon carbide crystal growth method. It heats silicon carbide powder by induction heating in a vacuum environment to sublimate it to produce reaction gases containing different gas phase components such as Si, Si2C, and SiC2. Silicon carbide single crystals are produced by solid-gas reactions. The single crystal produced by this method contains many defects such as micropipes and dislocations, which have a negative impact on the performance of silicon carbide devices.

液相法的晶体生长更接近热力学平衡条件,可以制造更高质量的碳化硅晶体。液相法的基本原理是:将含硅助溶剂置于石墨坩埚中,利用感应加热的方式熔化助溶剂,石墨坩埚中的碳溶解到助溶剂中;然后将碳化硅籽晶置于助溶剂的液面,由于籽晶处过冷,碳在籽晶的固液界面上析出,并和助溶剂中的硅结合形成碳化硅晶体。The crystal growth of the liquid phase method is closer to the thermodynamic equilibrium conditions, which can produce higher quality silicon carbide crystals. The basic principle of the liquid phase method is: put the silicon-containing co-solvent in the graphite crucible, melt the co-solvent by induction heating, and dissolve the carbon in the graphite crucible into the co-solvent; then place the silicon carbide seed crystal in the co-solvent At the liquid level, due to the supercooling of the seed crystal, carbon precipitates on the solid-liquid interface of the seed crystal, and combines with silicon in the co-solvent to form silicon carbide crystals.

发明内容Contents of the invention

本申请提出一种制造碳化硅晶体的装置。The present application proposes a device for manufacturing silicon carbide crystals.

本申请提出一种制造碳化硅晶体的方法。The present application proposes a method of manufacturing silicon carbide crystals.

本申请公开了一种制造碳化硅晶体的装置,包括:壳体,所述壳体限定出容纳腔;坩埚组件,所述坩埚组件包括石墨坩埚和设在所述石墨坩埚内的非石墨坩埚,所述非石墨坩埚用于承载助溶剂溶液;籽晶组件,所述籽晶组件可升降配合在所述壳体内,且所述籽晶组件的一端伸入所述坩埚组件内,所述籽晶组件用于承载碳化硅晶体;加热件,所述加热件设在所述容纳腔内且环绕所述坩埚组件设置;石墨件,所述石墨件可升降地配合在所述壳体内,所述石墨件的一端浸入所述助溶剂溶液内。 The present application discloses a device for manufacturing silicon carbide crystals, comprising: a housing, the housing defines an accommodating cavity; a crucible assembly, the crucible assembly includes a graphite crucible and a non-graphite crucible disposed in the graphite crucible, The non-graphite crucible is used to carry the co-solvent solution; the seed crystal assembly, the seed crystal assembly can be lifted and fitted in the housing, and one end of the seed crystal assembly extends into the crucible assembly, the seed crystal assembly The assembly is used to carry the silicon carbide crystal; the heating element is arranged in the accommodating chamber and surrounds the crucible assembly; One end of the piece is immersed in the co-solvent solution.

本申请还公开了一种制造碳化硅晶体的方法,所述制造碳化硅晶体的方法采用前文所述的制造碳化硅晶体的装置进行,所述制造碳化硅晶体的方法包括:The present application also discloses a method for manufacturing silicon carbide crystals. The method for manufacturing silicon carbide crystals is carried out by using the device for manufacturing silicon carbide crystals described above. The method for manufacturing silicon carbide crystals includes:

利用真空装置对容纳腔进行抽气并且注入惰性气体;Use a vacuum device to evacuate the chamber and inject inert gas;

启动加热件使得助溶剂熔化并且使得助溶剂溶液到达指定温度;Start the heating element to melt the co-solvent and bring the co-solvent solution to a specified temperature;

降低籽晶组件使得所述籽晶组件的下表面接触所述助溶剂溶液;lowering the seed assembly such that the lower surface of the seed assembly contacts the co-solvent solution;

降低石墨件使得所述石墨件浸入所述助溶剂溶液;lowering the graphite member such that the graphite member is immersed in the co-solvent solution;

提拉所述籽晶组件实现碳化硅晶体生长。The seed crystal assembly is pulled to achieve silicon carbide crystal growth.

本申请的附加方面和优点将在下面的描述中部分给出,部分将从下面的描述中变得明显,或通过本申请的实践了解到。Additional aspects and advantages of the application will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the application.

附图说明Description of drawings

图1是本申请实施例的制造碳化硅晶体的装置的结构示意图;Fig. 1 is a schematic structural diagram of a device for manufacturing silicon carbide crystals according to an embodiment of the present application;

图2是本申请实施例的一种石墨件的结构示意图;Fig. 2 is the structural representation of a kind of graphite part of the embodiment of the present application;

图3是本申请实施例的另一种石墨件的结构示意图;Fig. 3 is the structural representation of another kind of graphite part of the embodiment of the present application;

图4是本申请实施例的制造碳化硅晶体的方法的流程示意图。Fig. 4 is a schematic flowchart of a method for manufacturing a silicon carbide crystal according to an embodiment of the present application.

附图标记:Reference signs:

1、壳体;11、容纳腔;2、坩埚组件;21、石墨坩埚;22、非石墨坩埚;3、籽晶组件;31、籽晶杆;32、籽晶托;33、籽晶片;4、加热件;5、石墨件;51、孔槽结构;6、支撑杆;7、坩埚托;8、隔热层。1. Shell; 11. Accommodating cavity; 2. Crucible assembly; 21. Graphite crucible; 22. Non-graphite crucible; 3. Seed crystal assembly; 31. Seed crystal rod; , heating element; 5, graphite element; 51, hole structure; 6, support rod; 7, crucible holder; 8, heat insulation layer.

具体实施方式Detailed ways

相关技术中的液相法晶体生长装置中,石墨坩埚既是助溶剂的容器,也是碳的来源。随着生长进行,石墨坩埚不断溶解腐蚀,同时伴随着冷热冲击,容易产生裂纹,导致循环使用的次数有限,甚至只能一次性使用。高纯度的石墨坩埚造价较高,是液相法晶体生长的主要成本组成之一。石墨坩埚的循环使用次数有限,导致晶体的制造成本居高不下。In the liquid phase method crystal growth device in the related art, the graphite crucible is not only a container for a solvent, but also a source of carbon. As the growth progresses, the graphite crucible will continue to dissolve and corrode. At the same time, it is prone to cracks due to thermal shock, resulting in a limited number of cycles, or even one-time use. The cost of high-purity graphite crucible is relatively high, which is one of the main cost components of liquid phase crystal growth. Graphite crucibles have a limited number of cycles, resulting in high crystal manufacturing costs.

针对上述情况,本申请实施例提供一种制造碳化硅晶体的装置及制造碳化硅晶体的方法。In view of the above situation, embodiments of the present application provide a device for manufacturing silicon carbide crystals and a method for manufacturing silicon carbide crystals.

下面结合附图并通过具体实施方式来说明本申请的实施例。Embodiments of the present application will be described below in conjunction with the accompanying drawings and through specific implementation methods.

在本申请的描述中,需要理解的是,术语“中心”、“纵向”、“横向”、“长度”、“宽度”、“厚度”、“上”、“下”、“前”、“后”、“左”、“右”、“竖直”、“水平”、“顶”、“底”、“内”、“外”、“顺时针”、“逆时针”、“轴向”、“周向”等指 示的方位或位置关系为基于附图所示的方位或位置关系,仅是为了便于描述本申请和简化描述,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本申请的限制。In the description of the present application, it should be understood that the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "Back","Left","Right","Vertical","Horizontal","Top","Bottom","Inner","Outer","Clockwise","Counterclockwise","Axial" , "circumferential" and so on The orientations or positional relationships shown are based on the orientations or positional relationships shown in the drawings, and are only for the convenience of describing the application and simplifying the description, rather than indicating or implying that the referred device or element must have a specific orientation, use a specific orientation construction and operation, therefore should not be construed as limiting the application.

此外,限定有“第一”、“第二”的特征可以明示或者隐含地包括一个或者更多个该特征,用于区别描述特征,无顺序之分,无轻重之分。在本申请的描述中,除非另有说明,“多个”的含义是两个或两个以上。In addition, the features defined as "first" and "second" may explicitly or implicitly include one or more of these features, which are used to describe the features differently, without order or importance. In the description of the present application, unless otherwise specified, "plurality" means two or more.

在本申请的描述中,需要说明的是,除非另有明确的规定和限定,术语“安装”、“相连”、“连接”应做广义理解,例如,可以是固定连接,也可以是可拆卸连接,或一体地连接;可以是机械连接,也可以是电连接;可以是直接相连,也可以通过中间媒介间接相连,可以是两个元件内部的连通。对于本领域的普通技术人员而言,可以具体情况理解上述术语在本申请中的具体含义。In the description of this application, it should be noted that unless otherwise specified and limited, the terms "installation", "connection", and "connection" should be understood in a broad sense, for example, it can be a fixed connection or a detachable connection. Connected, or integrally connected; it can be mechanically connected or electrically connected; it can be directly connected or indirectly connected through an intermediary, and it can be the internal communication of two components. Those of ordinary skill in the art can understand the specific meanings of the above terms in this application in specific situations.

下面参考图1-图3描述本申请实施例的制造碳化硅晶体的装置的结构。The structure of the device for manufacturing silicon carbide crystals according to the embodiment of the present application will be described below with reference to FIGS. 1-3 .

本申请实施例公开了一种制造碳化硅晶体的装置,如图1所示,该制造碳化硅晶体的装置包括壳体1、坩埚组件2、籽晶组件3和石墨件5,壳体1限定出容纳腔11,坩埚组件2包括石墨坩埚21和设在石墨坩埚21内的非石墨坩埚22,非石墨坩埚22用于承载助溶剂溶液,籽晶组件3可升降配合在壳体1内,且籽晶组件3的一端伸入坩埚组件2内,籽晶组件3用于承载碳化硅晶体,加热件4设在容纳腔11内且环绕坩埚组件2设置,石墨件5可升降地配合在壳体1内,石墨件5的一端浸入助溶剂溶液内。The embodiment of the present application discloses a device for manufacturing silicon carbide crystals. As shown in FIG. Out of the housing chamber 11, the crucible assembly 2 includes a graphite crucible 21 and a non-graphite crucible 22 disposed in the graphite crucible 21, the non-graphite crucible 22 is used to carry the cosolvent solution, the seed crystal assembly 3 can be lifted and fitted in the housing 1, and One end of the seed crystal assembly 3 extends into the crucible assembly 2, the seed crystal assembly 3 is used to carry the silicon carbide crystal, the heating element 4 is arranged in the accommodation chamber 11 and is arranged around the crucible assembly 2, and the graphite element 5 can be raised and lowered to fit in the housing 1, one end of the graphite piece 5 is immersed in the co-solvent solution.

可以理解的是,在实际工作过程中,在加热件4将坩埚组件2内的助溶剂溶液加热到指定温度后,将籽晶组件3和石墨件5下降至与助溶剂溶液接触的位置,石墨件5中的碳溶解至助溶剂溶液中,由于籽晶组件3处过冷,碳在籽晶组件3的下表面析出,并和助溶剂溶液中的硅结合形成碳化硅晶体。由于本实施例的坩埚组件2包括石墨坩埚21和设在石墨坩埚21内的非石墨坩埚22,在整个反应过程中,石墨坩埚21不会出现溶解腐蚀的现象,并且由于非石墨坩埚22的阻隔,石墨坩埚21内不会出现冷热冲击的现象,降低了石墨坩埚21产生裂纹的几率,延长石墨坩埚21的使用寿命,从而延长了石墨坩埚21的更换周期,降低了碳化硅晶体的制造成本。It can be understood that, in the actual working process, after the heating element 4 heats the co-solvent solution in the crucible assembly 2 to a specified temperature, the seed crystal assembly 3 and the graphite component 5 are lowered to a position in contact with the co-solvent solution. The carbon in piece 5 dissolves into the co-solvent solution, and due to the supercooling of the seed crystal component 3, the carbon precipitates on the lower surface of the seed crystal component 3, and combines with the silicon in the co-solvent solution to form silicon carbide crystals. Since the crucible assembly 2 of the present embodiment includes a graphite crucible 21 and a non-graphite crucible 22 disposed in the graphite crucible 21, during the entire reaction process, the graphite crucible 21 will not undergo dissolution and corrosion, and due to the barrier of the non-graphite crucible 22 , there will be no cold and heat shock in the graphite crucible 21, which reduces the probability of cracks in the graphite crucible 21, prolongs the service life of the graphite crucible 21, thereby prolonging the replacement cycle of the graphite crucible 21 and reducing the manufacturing cost of silicon carbide crystals .

与此同时,非石墨坩埚22的熔点略高于助溶剂溶液的温度,随着晶体生长时间的增加,非石墨坩埚22可能会发生软化变形。因此,将非石墨坩埚22置于石墨坩埚21中,石墨坩埚21在高温下形状稳定,可以有效地维持非石墨坩埚22的形状,从而避免非石墨坩埚22变形严重导致不能顺利产生碳化硅晶体 的现象发生。At the same time, the melting point of the non-graphite crucible 22 is slightly higher than the temperature of the co-solvent solution, and as the crystal growth time increases, the non-graphite crucible 22 may soften and deform. Therefore, if the non-graphite crucible 22 is placed in the graphite crucible 21, the shape of the graphite crucible 21 is stable at a high temperature, and the shape of the non-graphite crucible 22 can be effectively maintained, thereby avoiding the serious deformation of the non-graphite crucible 22 that cannot produce silicon carbide crystals smoothly. phenomenon occurs.

需要补充说明的是,本实施例的非石墨坩埚22是指除高纯石墨之外的、造价更为低廉的坩埚,例如,当助溶剂的温度约1400℃,采用了石英坩埚,石英熔点约1750℃,略高于助溶剂的温度。又例如,助溶剂的温度约1800℃,采用了刚玉坩埚,刚玉熔点约2000℃,略高于助溶剂的温度。本实施的非石墨坩埚22还可以采用钨、钼等不和助溶剂发生化学反应的高熔点金属材料制造。It should be added that the non-graphite crucible 22 in this embodiment refers to a crucible with a lower cost than high-purity graphite. For example, when the temperature of the co-solvent is about 1400 ° C, a quartz crucible is used, and the melting point of quartz is about 1750°C, slightly higher than the temperature of the co-solvent. For another example, the temperature of the co-solvent is about 1800°C, and a corundum crucible is used, and the melting point of corundum is about 2000°C, which is slightly higher than the temperature of the co-solvent. The non-graphite crucible 22 in this embodiment can also be made of high-melting-point metal materials such as tungsten and molybdenum that do not chemically react with the co-solvent.

在一些可选的实施例中,容纳腔11具有至少一个抽气口且和真空获得装置连接,可将容纳腔11内气压降低至预期值。容纳腔11具有至少一个充气口,可以充入氮气、氩气、氦气或其他惰性气体。In some optional embodiments, the accommodating chamber 11 has at least one air suction port and is connected to a vacuum obtaining device, which can reduce the air pressure in the accommodating chamber 11 to a desired value. The containing chamber 11 has at least one gas filling port, which can be filled with nitrogen, argon, helium or other inert gases.

在一些可选的实施例中,容纳腔11和至少一个真空计连接。由此,实验人员可以直观的观察容纳腔11内的真空度。In some optional embodiments, the containing chamber 11 is connected to at least one vacuum gauge. Thus, the experimenter can intuitively observe the vacuum degree in the accommodation chamber 11 .

在一些可选的实施例中,助溶剂溶液除了包括Si元素之外,还可以包括Ti、Cr、Sc、Ni、Al、Co、Mn、Mg、Ge、As、P、N、O、B、Dy、Y、Nb、Nd、Fe中的一种或多种元素,可以根据实际需要选择。In some optional embodiments, the co-solvent solution may also include Ti, Cr, Sc, Ni, Al, Co, Mn, Mg, Ge, As, P, N, O, B, One or more elements of Dy, Y, Nb, Nd, and Fe can be selected according to actual needs.

在一些实施例中,如图1所示,制碳化硅晶体的装置还包括支撑杆6,支撑杆6穿设在壳体1上,支撑杆6的一端伸入壳体1且与石墨件5相连,另一端伸出壳体1且与外部驱动机构相连。可以理解的是,由于在整个生长过程中容纳腔11内部始终处于较高温度的状态,如果将驱动石墨件5的驱动件设在容纳腔11内,容易造成驱动件损坏。在本实施例中,通过设置支撑杆6将驱动支撑杆6运动的驱动件设置为设在壳体1外侧的外部驱动机构,在保证能够稳定地结晶的前提下,不会使得驱动石墨件5的驱动件处于高温的工作环境,从而延长其使用寿命。In some embodiments, as shown in FIG. 1 , the device for making silicon carbide crystals further includes a support rod 6 , the support rod 6 is passed through the housing 1 , and one end of the support rod 6 extends into the housing 1 and connects with the graphite piece 5 connected, and the other end protrudes from the casing 1 and is connected with the external drive mechanism. It can be understood that, since the inside of the containing cavity 11 is always at a relatively high temperature during the whole growth process, if the driving element for driving the graphite element 5 is arranged in the containing cavity 11 , it is easy to cause damage to the driving element. In this embodiment, by setting the support rod 6, the driving member that drives the support rod 6 is set as an external drive mechanism located outside the housing 1, so that the graphite member 5 will not be driven under the premise of ensuring stable crystallization. The driving parts are in a high temperature working environment, thus prolonging their service life.

图2中示意出了部分的石墨件5的截面。FIG. 2 schematically shows a section of a part of the graphite member 5 .

在一些实施例中,如图2-图3所示,石墨件5为环状,石墨件5的内壁或外壁设有孔槽结构51。可以理解的是,石墨件5为环状且内部和/或外壁设有孔槽结构51,这样能够提升石墨件5与助溶剂溶液的接触面积,提升石墨件5的溶解效率,从而提升碳化硅的制造效率。In some embodiments, as shown in FIGS. 2-3 , the graphite piece 5 is ring-shaped, and the inner or outer wall of the graphite piece 5 is provided with a hole structure 51 . It can be understood that the graphite part 5 is ring-shaped and the inner and/or outer walls are provided with a hole structure 51, which can increase the contact area between the graphite part 5 and the cosolvent solution, improve the dissolution efficiency of the graphite part 5, and thereby improve the silicon carbide. manufacturing efficiency.

在一些实施例中,如图2-图3所示,孔槽结构51包括多个凹槽,多个凹槽沿石墨件5的轴向和/或周向间隔设置,每个凹槽沿石墨件5的周向或者轴向延伸设置。由此,孔槽结构51能够较为方便的加工,降低了石墨件5的加工难度。这里需要补充说明的是,在本申请的其他实施例中,石墨件5也可以形成为多孔的结构或者具有其他镂空结构的形状,并不限于本实施例的环状。 In some embodiments, as shown in FIGS. 2-3 , the hole structure 51 includes a plurality of grooves, the plurality of grooves are arranged at intervals along the axial and/or circumferential directions of the graphite member 5, and each groove is arranged along the graphite The circumferential or axial extension of the member 5 is set. Thus, the hole structure 51 can be processed more conveniently, which reduces the processing difficulty of the graphite piece 5 . What needs to be added here is that in other embodiments of the present application, the graphite member 5 may also be formed in a porous structure or in a shape with other hollow structures, and is not limited to the ring shape in this embodiment.

在一些实施例中,籽晶组件3包括籽晶杆31和籽晶托32,籽晶杆31穿设在壳体1上,籽晶杆31的一端伸出壳体1且与外部驱动机构相连,另一端伸入坩埚组件2,籽晶托32设在籽晶杆31伸入坩埚组件2的一端,籽晶托32用于承载生长的碳化硅晶体。可以理解的是,由于在整个生长过程中容纳腔11内部始终处于较高温度的状态,如果将驱动籽晶组件3的驱动件设在容纳腔11内,容易造成驱动件损坏。在本实施例中,通过设置籽晶杆31,将用于驱动籽晶组件3的驱动件设在容纳腔11外部以成为外部驱动结构,在保证能够稳定地结晶的前提下,不会使得驱动籽晶组件3的驱动件处于高温的工作环境,从而延长驱动件的使用寿命。In some embodiments, the seed assembly 3 includes a seed rod 31 and a seed holder 32, the seed rod 31 is passed through the housing 1, and one end of the seed rod 31 protrudes from the housing 1 and is connected to an external drive mechanism , the other end extends into the crucible assembly 2, and the seed crystal support 32 is provided at one end of the seed rod 31 protruding into the crucible assembly 2, and the seed crystal support 32 is used to carry the growing silicon carbide crystal. It can be understood that since the interior of the chamber 11 is always at a relatively high temperature during the entire growth process, if the driver for driving the seed crystal assembly 3 is placed in the chamber 11 , the driver may be easily damaged. In this embodiment, by setting the seed crystal rod 31, the driving member for driving the seed crystal assembly 3 is set outside the housing cavity 11 to form an external driving structure. On the premise of ensuring stable crystallization, the drive will not The driving part of the seed crystal assembly 3 is in a high-temperature working environment, thereby prolonging the service life of the driving part.

在一些实施例中,在本实施例的籽晶托32可以采用石墨托也可以采用其他耐高温的金属托,可以根据实际需要选择。In some embodiments, the seed crystal holder 32 in this embodiment may be a graphite holder or other high-temperature-resistant metal holders, which may be selected according to actual needs.

外部驱动机构在驱动籽晶杆31升降时还可以驱动籽晶杆31转动,这样坩埚组件2内的液体就会被搅动,从而更好地提升结晶效果。与此同时,外部驱动机构可以根据实际需要选择电机带动滚珠丝杠、气缸或者电动推杆等任何能够实现直线驱动和转动驱动的结构,在此不对外部驱动机构进行限定。The external drive mechanism can also drive the seed rod 31 to rotate when driving the seed rod 31 up and down, so that the liquid in the crucible assembly 2 will be stirred, thereby better improving the crystallization effect. At the same time, the external drive mechanism can choose any structure that can realize linear drive and rotational drive, such as a motor driving a ball screw, a cylinder, or an electric push rod, according to actual needs, and the external drive mechanism is not limited here.

在一些实施例中,籽晶组件3还包括设在籽晶托32上的籽晶片33,籽晶片33用于承载生长的碳化硅晶体。可以理解的是,籽晶托32上设置籽晶片33能够使生成的碳化硅晶体的晶型和籽晶片一致,同时更为方便地将生成的碳化硅晶体从籽晶组件3上剥离。In some embodiments, the seed crystal assembly 3 further includes a seed wafer 33 disposed on the seed crystal support 32 , and the seed wafer 33 is used to support the growing silicon carbide crystal. It can be understood that setting the seed wafer 33 on the seed crystal support 32 can make the crystal form of the generated silicon carbide crystal consistent with the seed wafer, and at the same time, it is more convenient to peel the generated silicon carbide crystal from the seed crystal assembly 3 .

在一些实施例中,制造碳化硅晶体的装置还包括坩埚托7,坩埚托7穿设在壳体1上,坩埚托7的一端伸出壳体1且与外部驱动机构相连,另一端与石墨坩埚21相连。可以理解的是,由于在整个生长过程中容纳腔11内部始终处于较高温度的状态,如果将驱动坩埚组件2的驱动件设在容纳腔11内,容易造成驱动件损坏。在本实施例中,通过设置坩埚托7,将用于坩埚组件2的驱动件设在容纳腔11外侧,在保证能够稳定地结晶的前提下,不会使得驱动件处于高温的工作环境,从而延长坩埚组件2的驱动件的使用寿命。In some embodiments, the device for manufacturing silicon carbide crystals further includes a crucible holder 7, the crucible holder 7 is pierced on the housing 1, one end of the crucible holder 7 protrudes from the housing 1 and is connected to an external drive mechanism, and the other end is connected to the graphite The crucibles 21 are connected. It can be understood that, since the inside of the containing chamber 11 is always at a relatively high temperature during the whole growth process, if the driving part for driving the crucible assembly 2 is arranged in the containing chamber 11, the driving part may be easily damaged. In this embodiment, by setting the crucible holder 7, the driving part used for the crucible assembly 2 is arranged outside the containing chamber 11, under the premise of ensuring stable crystallization, the driving part will not be placed in a high-temperature working environment, thereby The service life of the drives of the crucible assembly 2 is extended.

外部驱动机构在驱动石墨坩埚21升降时还可以驱动石墨坩埚21转动,这样石墨坩埚21内的液体就会被搅动,从而更好地提升结晶效果。与此同时,外部驱动机构可以根据实际需要选择电机带动滚珠丝杠、气缸或者电动推杆等任何能够实现直线驱动和转动驱动的结构,在此不对外部驱动机构进行限定。The external drive mechanism can also drive the graphite crucible 21 to rotate when driving the graphite crucible 21 up and down, so that the liquid in the graphite crucible 21 will be stirred, thereby better improving the crystallization effect. At the same time, the external drive mechanism can choose any structure that can realize linear drive and rotational drive, such as a motor driving a ball screw, a cylinder, or an electric push rod, according to actual needs, and the external drive mechanism is not limited here.

在一些实施例中,加热件4包括形成为螺旋状的感应加热线圈。可以理解对,采用感应加热线圈进行加热,在工作过程中,感应加热线圈通过交变电流, 产生交变磁场,从而在石墨坩埚21中产生感应电流,实现对石墨坩埚21的加热,然后热量从石墨坩埚21传导至非石墨坩埚22,使得非石墨坩埚22中的助溶剂熔化并升温至所需要的温度。相比于热传导的加热结构,本实施例中,采用感应加热线圈进行加热,加热温度更高,电能的利用率更高,且可以对石墨坩埚2中的液体起到电磁搅拌的效果。In some embodiments, the heating element 4 comprises an induction heating coil formed in a helical shape. It can be understood that the induction heating coil is used for heating. During the working process, the induction heating coil passes an alternating current, An alternating magnetic field is generated, thereby generating an induced current in the graphite crucible 21 to realize heating of the graphite crucible 21, and then the heat is conducted from the graphite crucible 21 to the non-graphite crucible 22, so that the cosolvent in the non-graphite crucible 22 melts and heats up to the required temperature. Compared with the heating structure of heat conduction, in this embodiment, the induction heating coil is used for heating, the heating temperature is higher, the utilization rate of electric energy is higher, and the liquid in the graphite crucible 2 can be electromagnetically stirred.

在一些实施例中,感应加热线圈为等螺距螺旋管,即相邻两匝之间的间距为固定值。这样能够提升感应加热线圈的加热均匀度。感应加热线圈的匝数可以根据实际需要选择10-20匝,当然也可以是其他匝数。In some embodiments, the induction heating coil is a helical tube with equal pitch, that is, the distance between two adjacent turns is a fixed value. This can improve the heating uniformity of the induction heating coil. The number of turns of the induction heating coil can be selected as 10-20 turns according to actual needs, and of course other turns can also be used.

在一些实施例中,感应加热线圈的纵截面为圆环或矩形环,即感应加热线圈为中空结构,从而使得感应加热线圈可通水冷却,避免感应加热线圈过热的现象发生。在一些实施例中,感应加热线圈通过柔性的电路和水路和设置在壳体1上的真空馈通件,真空馈通件再和腔室外部的电源和循环水源连接。真空馈通件可以根据实际需要设置为插头结构,方便安装以及拆卸。In some embodiments, the longitudinal section of the induction heating coil is a circular ring or a rectangular ring, that is, the induction heating coil is a hollow structure, so that the induction heating coil can be cooled by water to avoid overheating of the induction heating coil. In some embodiments, the induction heating coil passes through a flexible circuit and a water circuit, and a vacuum feedthrough provided on the housing 1 , and the vacuum feedthrough is then connected to a power source and a circulating water source outside the chamber. The vacuum feedthrough can be set as a plug structure according to actual needs, which is convenient for installation and disassembly.

在一些实施例中,感应加热线圈的电流频率1-100kHz。In some embodiments, the current frequency of the induction heating coil is 1-100 kHz.

在一些实施例中,制造碳化硅晶体的装置还包括隔热层8,隔热层8设在加热件4与石墨坩埚21之间,且环绕石墨坩埚21设置。隔热层8的设置能避免石墨坩埚21的热量流失。In some embodiments, the device for manufacturing silicon carbide crystals further includes a heat insulating layer 8 , and the heat insulating layer 8 is disposed between the heating element 4 and the graphite crucible 21 and is disposed around the graphite crucible 21 . The setting of the heat insulating layer 8 can avoid the heat loss of the graphite crucible 21 .

例如,隔热层材料为具有较低热导率的石墨毡。For example, the insulating layer material is graphite felt with low thermal conductivity.

实施例:Example:

下面参考图1描述本申请一个实施例的制造碳化硅晶体装置。An apparatus for manufacturing a silicon carbide crystal according to an embodiment of the present application will be described below with reference to FIG. 1 .

如图1所示,该制造碳化硅晶体的装置包括壳体1、坩埚组件2、籽晶组件3、石墨件5、支撑杆6、坩埚托7和隔热层8,壳体1限定出容纳腔11,坩埚组件2包括石墨坩埚21和设在石墨坩埚21内的非石墨坩埚22,非石墨坩埚22用于承载助溶剂溶液,支撑杆6穿设在壳体1上,支撑杆6的一端伸入壳体1且与石墨件5相连,另一端伸出壳体1且与外部驱动机构相连。如图2-图3所示,石墨件5为环状结构,石墨件5的外周或者内周壁上设有多个凹槽,多个凹槽沿石墨件5的轴向和/或周向间隔设置,每个凹槽沿石墨件5的周向或者轴向延伸设置。籽晶组件3包括籽晶杆31和籽晶托32,籽晶杆31穿设在壳体1上,籽晶杆31的一端伸出壳体1且与外部驱动机构相连,且能够在外部驱动机构的驱动下升降以及旋转,籽晶杆31的另一端伸入坩埚组件2,籽晶托32设在籽晶杆31伸入坩埚组件2的一端,籽晶片33设在籽晶托32伸入坩埚组件2的一端,籽晶片33用于承载生长的碳化硅晶体。加热件4设在容纳腔11内且包 括形成为螺旋状的感应加热线圈。坩埚托7穿设在壳体1上,坩埚托7的一端伸出壳体1且与外部驱动机构相连,另一端与石墨坩埚21相连。隔热层8设在加热件4与石墨坩埚21之间,且环绕石墨坩埚21设置。As shown in Figure 1, the device for manufacturing silicon carbide crystals includes a housing 1, a crucible assembly 2, a seed crystal assembly 3, a graphite piece 5, a support rod 6, a crucible holder 7 and a thermal insulation layer 8, and the housing 1 defines a housing The cavity 11, the crucible assembly 2 includes a graphite crucible 21 and a non-graphite crucible 22 arranged in the graphite crucible 21, the non-graphite crucible 22 is used to carry a cosolvent solution, the support rod 6 is installed on the shell 1, and one end of the support rod 6 It extends into the casing 1 and connects with the graphite piece 5, and the other end extends out of the casing 1 and connects with the external drive mechanism. As shown in Figures 2-3, the graphite part 5 is a ring structure, and the outer or inner peripheral wall of the graphite part 5 is provided with a plurality of grooves, and the plurality of grooves are spaced along the axial and/or circumferential direction of the graphite part 5 Each groove is set along the circumferential or axial extension of the graphite member 5 . The seed crystal assembly 3 includes a seed crystal rod 31 and a seed crystal holder 32, the seed crystal rod 31 is penetrated on the housing 1, and one end of the seed crystal rod 31 protrudes from the housing 1 and is connected with an external drive mechanism, and can be driven externally Driven by the mechanism to lift and rotate, the other end of the seed rod 31 extends into the crucible assembly 2, the seed holder 32 is set at the end where the seed rod 31 extends into the crucible assembly 2, and the seed wafer 33 is located at the end of the seed holder 32. At one end of the crucible assembly 2, the seed wafer 33 is used to support the growing silicon carbide crystal. The heating element 4 is arranged in the accommodating chamber 11 and includes Included is an induction heating coil formed in a helical shape. The crucible holder 7 is mounted on the casing 1 , one end of the crucible holder 7 protrudes from the casing 1 and is connected with an external driving mechanism, and the other end is connected with a graphite crucible 21 . The heat insulation layer 8 is arranged between the heating element 4 and the graphite crucible 21 and is arranged around the graphite crucible 21 .

下面参考图4描述本申请实施例的制造碳化硅晶体的方法的流程。The flow of the method for manufacturing a silicon carbide crystal according to the embodiment of the present application will be described below with reference to FIG. 4 .

本申请还公开了一种制造碳化硅晶体的方法,制造碳化硅晶体的方法采用前文的制造碳化硅晶体的装置进行,制造碳化硅晶体的方法包括:The present application also discloses a method for manufacturing silicon carbide crystals. The method for manufacturing silicon carbide crystals is carried out by using the aforementioned device for manufacturing silicon carbide crystals. The method for manufacturing silicon carbide crystals includes:

S1:利用真空装置对容纳腔11进行抽气并且注入惰性气体;S1: using a vacuum device to evacuate the chamber 11 and inject an inert gas;

例如,首先采用真空装置对容纳腔11进行抽气,使得容纳腔11内的压力下降至所设定的值,随后向容纳腔11中充入氮气、氩气、氦气或其他惰性气体,使得压力上升至所设定的值。抽气到达的压力以及充气到达的压力值均可以根据实际需要选择,在此不对设定的压力值做出限定。For example, first use a vacuum device to evacuate the chamber 11, so that the pressure in the chamber 11 drops to a set value, and then fill the chamber 11 with nitrogen, argon, helium or other inert gases, so that The pressure rises to the set value. Both the suction pressure and the inflation pressure can be selected according to actual needs, and the set pressure values are not limited here.

S2:启动加热件4使得助溶剂熔化并且使得助溶剂溶液到达指定温度;S2: Start the heating element 4 to melt the co-solvent and make the co-solvent solution reach a specified temperature;

例如,可以采用非接触的加热件4(例如感应加热线圈),向感应加热线圈中通过交变电流加热石墨坩埚21,石墨坩埚21的热量可以传递到非石墨坩埚22上,使非石墨坩埚22内的助溶剂溶液到达指定温度。这里需要额外说明的是,在本实施例中,助溶剂溶液的温度可以采用现有的检测装置进行检测,在此无需对如何检测以及控制做出限定;For example, a non-contact heating element 4 (such as an induction heating coil) can be used to heat the graphite crucible 21 by an alternating current in the induction heating coil, and the heat of the graphite crucible 21 can be transferred to the non-graphite crucible 22 to make the non-graphite crucible 22 The co-solvent solution in it reaches the specified temperature. What needs to be additionally explained here is that in this embodiment, the temperature of the co-solvent solution can be detected by using an existing detection device, and there is no need to limit how to detect and control it here;

S3:降低籽晶组件3使得籽晶组件3的下表面接触助溶剂溶液;S3: lowering the seed crystal assembly 3 so that the lower surface of the seed crystal assembly 3 contacts the co-solvent solution;

例如,籽晶组件3的下表面可以正好接触到助溶剂溶液的液面,也可以浸入液面一定的深度,这样能够较好地实现过冷有助于碳析出,从而与助溶剂溶液中的硅结合形成碳化硅晶体。For example, the lower surface of the seed crystal assembly 3 can just touch the liquid level of the co-solvent solution, and can also be immersed in a certain depth of the liquid level, so that supercooling can be better realized and carbon is precipitated, thereby being compatible with the co-solvent solution. The silicon combines to form silicon carbide crystals.

S4:降低石墨件5使得石墨件5浸入助溶剂溶液;S4: lowering the graphite piece 5 so that the graphite piece 5 is immersed in the co-solvent solution;

例如,石墨件5进入助溶剂溶液后,石墨件5内的碳会溶解到助溶剂中。For example, after the graphite piece 5 enters the co-solvent solution, the carbon in the graphite piece 5 will dissolve into the co-solvent.

S5:提拉籽晶组件3实现碳化硅晶体生长。S5: Pulling the seed crystal component 3 to realize silicon carbide crystal growth.

例如,提升籽晶组件3的过程中,碳化硅晶体就能够不断生长在籽晶组件3的下表面上。For example, during the process of lifting the seed crystal assembly 3 , silicon carbide crystals can continuously grow on the lower surface of the seed crystal assembly 3 .

这里需要说明的是,当碳化硅晶体生长结束后,需要提升石墨件5并且使得石墨件5脱离助溶剂溶液以避免石墨件5的浪费。并且同时关闭加热件4,等助溶剂冷却至设定的安全温度。It should be noted here that after the silicon carbide crystal growth is completed, the graphite piece 5 needs to be lifted and separated from the co-solvent solution to avoid waste of the graphite piece 5 . And at the same time turn off the heating element 4, and wait for the auxiliary solvent to cool down to the set safe temperature.

在一些实施例中,在步骤S3中,降低籽晶组件3还可以提拉籽晶组件3使得籽晶组件3的下表面位于助溶剂溶液的液面上方,以使籽晶组件3提拉出部分助溶剂溶液。可以理解的是,这样能够使得籽晶组件3的下表面位于助溶剂 的液面的上方,由于表面张力的作用提拉起一部分溶液,形成弯月面,这样有助于碳化硅晶体的生成。In some embodiments, in step S3, lowering the seed crystal assembly 3 can also lift the seed crystal assembly 3 so that the lower surface of the seed crystal assembly 3 is above the liquid level of the co-solvent solution, so that the seed crystal assembly 3 can be pulled out Partial co-solvent solution. It can be understood that, in this way, the lower surface of the seed crystal assembly 3 can be located Above the liquid level, due to the effect of surface tension, a part of the solution is lifted to form a meniscus, which helps the formation of silicon carbide crystals.

在一些实施例中,籽晶组件3的下表面与助溶剂的液面的距离为0.1mm-3mm。In some embodiments, the distance between the lower surface of the seed crystal assembly 3 and the liquid surface of the co-solvent is 0.1 mm-3 mm.

在一些实施例中,提拉籽晶组件3时可以同时驱动籽晶组件3转动并且驱动坩埚组件2转动。由此,能够使得助溶剂溶液发生摇晃,从而有助于碳化硅晶体的生成。In some embodiments, when the seed crystal assembly 3 is pulled, the seed crystal assembly 3 can be driven to rotate and the crucible assembly 2 can be driven to rotate at the same time. As a result, the co-solvent solution can be shaken, thereby contributing to the formation of silicon carbide crystals.

在一些实施例中,提拉籽晶组件3时同时驱动石墨件5下降以维持助溶剂溶液的液面高度不变,增加石墨件5浸入助溶剂溶液中的深度,使得助溶剂溶液的液面高度在晶体生长的全过程中基本保持不变,从而保证碳化硅晶体的生成的稳定性和一致性。In some embodiments, when the seed crystal assembly 3 is pulled, the graphite part 5 is driven down to maintain the liquid level of the cosolvent solution constant, and the depth at which the graphite part 5 is immersed in the cosolvent solution is increased, so that the liquid level of the cosolvent solution The height remains basically unchanged during the whole process of crystal growth, thereby ensuring the stability and consistency of the formation of silicon carbide crystals.

本申请实施例中的制造碳化硅晶体的方法,由于在整个制造方法中,采用石墨件作为外部碳源,石墨坩埚不会出现溶解腐蚀的现象,降低了石墨坩埚产生裂纹的几率,延长石墨坩埚的使用寿命,从而延长了石墨坩埚的更换周期,降低了碳化硅晶体的制造成本。In the method for manufacturing silicon carbide crystals in the embodiment of the present application, since graphite parts are used as an external carbon source in the entire manufacturing method, the phenomenon of dissolution and corrosion will not occur in the graphite crucible, which reduces the probability of cracks in the graphite crucible and extends the graphite crucible. The service life of the graphite crucible is extended, and the cost of silicon carbide crystal manufacturing is reduced.

在本说明书的描述中,参考术语“有些实施例”、“其他实施例”、等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本申请的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。 In the description of this specification, descriptions with reference to the terms "some embodiments", "other embodiments", etc. mean that specific features, structures, materials or characteristics described in connection with the embodiments or examples are included in at least one implementation of the present application. example or examples. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

Claims (10)

一种制造碳化硅晶体的装置,包括:A device for manufacturing silicon carbide crystals, comprising: 壳体(1),所述壳体(1)限定出容纳腔(11);A housing (1), the housing (1) defining an accommodating chamber (11); 坩埚组件(2),所述坩埚组件(2)包括石墨坩埚(21)和设在所述石墨坩埚(21)内的非石墨坩埚(22),所述非石墨坩埚(22)用于承载助溶剂溶液;Crucible assembly (2), described crucible assembly (2) comprises graphite crucible (21) and the non-graphite crucible (22) that is arranged in described graphite crucible (21), and described non-graphite crucible (22) is used for carrying auxiliary solvent solution; 籽晶组件(3),所述籽晶组件(3)可升降配合在所述壳体(1)内,且所述籽晶组件(3)的一端伸入所述坩埚组件(2)内,所述籽晶组件(3)用于承载碳化硅晶体;a seed crystal assembly (3), the seed crystal assembly (3) can be lifted and fitted in the housing (1), and one end of the seed crystal assembly (3) extends into the crucible assembly (2), The seed crystal assembly (3) is used to carry silicon carbide crystals; 加热件(4),所述加热件(4)设在所述容纳腔(11)内且环绕所述坩埚组件(2)设置;a heating element (4), the heating element (4) is arranged in the accommodating cavity (11) and arranged around the crucible assembly (2); 石墨件(5),所述石墨件(5)可升降地配合在所述壳体(1)内,所述石墨件(5)的一端浸入所述助溶剂溶液内。A graphite piece (5), the graphite piece (5) is fitted in the casing (1) in a liftable manner, and one end of the graphite piece (5) is immersed in the co-solvent solution. 根据权利要求1所述的制造碳化硅晶体的装置,还包括支撑杆(6),所述支撑杆(6)穿设在所述壳体(1)上,所述支撑杆(6)的一端伸入所述壳体(1)且与所述石墨件(5)相连,所述支撑杆(6)的另一端伸出所述壳体(1)且与外部驱动机构相连。The device for manufacturing silicon carbide crystals according to claim 1, further comprising a support rod (6), the support rod (6) passing through the housing (1), one end of the support rod (6) The other end of the support rod (6) extends out of the casing (1) and is connected with the external driving mechanism. 根据权利要求1所述的制造碳化硅晶体的装置,其中,所述石墨件(5)为环状,所述石墨件(5)的内壁或外壁中的至少一个设有孔槽结构(51)。The device for manufacturing silicon carbide crystals according to claim 1, wherein the graphite piece (5) is annular, and at least one of the inner wall or the outer wall of the graphite piece (5) is provided with a hole structure (51) . 根据权利要求3所述的制造碳化硅晶体的装置,其中,所述孔槽结构(51)包括多个凹槽,多个所述凹槽沿所述石墨件(5)的轴向或周向间隔设置,每个所述凹槽沿所述石墨件(5)的周向或者轴向延伸设置。The device for manufacturing silicon carbide crystals according to claim 3, wherein the hole structure (51) includes a plurality of grooves, and the plurality of grooves are along the axial or circumferential direction of the graphite piece (5) Arranged at intervals, each of the grooves is arranged along the circumferential or axial extension of the graphite member (5). 根据权利要求1所述的制造碳化硅晶体的装置,其中,所述籽晶组件(3)包括:The device for manufacturing silicon carbide crystals according to claim 1, wherein the seed crystal assembly (3) comprises: 籽晶杆(31),所述籽晶杆(31)穿设在所述壳体(1)上,所述籽晶杆(31)的一端伸出所述壳体(1)且与外部驱动机构相连,所述籽晶杆(31)的另一端伸入所述坩埚组件(2);A seed rod (31), the seed rod (31) is passed through the casing (1), and one end of the seed rod (31) protrudes from the casing (1) and is connected with an external drive The mechanism is connected, and the other end of the seed rod (31) extends into the crucible assembly (2); 籽晶托(32),所述籽晶托(32)设在所述籽晶杆(31)伸入所述坩埚组件(2)的一端;A seed crystal holder (32), the seed crystal holder (32) is arranged at the end where the seed crystal rod (31) extends into the crucible assembly (2); 籽晶片(33),所述籽晶片(33)设在所述籽晶托(32)伸入所述坩埚组件(2)的一端,所述籽晶片(33)用于承载生长的碳化硅晶体。A seed wafer (33), the seed wafer (33) is arranged at one end of the seed crystal holder (32) extending into the crucible assembly (2), and the seed wafer (33) is used to carry the grown silicon carbide crystal . 根据权利要求1所述的制造碳化硅晶体的装置,还包括坩埚托(7),所述坩埚托(7)穿设在所述壳体(1)上,所述坩埚托(7)的一端伸出所述壳体(1)且与外部驱动机构相连,所述坩埚托(7)的另一端与所述石墨坩埚(21)相连。The device for manufacturing silicon carbide crystals according to claim 1, further comprising a crucible holder (7), the crucible holder (7) is installed on the housing (1), and one end of the crucible holder (7) It protrudes from the casing (1) and is connected with an external drive mechanism, and the other end of the crucible holder (7) is connected with the graphite crucible (21). 根据权利要求1所述的制造碳化硅晶体的装置,还包括隔热层(8),所述隔热层(8)设在所述加热件(4)与所述石墨坩埚(21)之间,且环绕所述石墨坩埚(21) 设置。The device for manufacturing silicon carbide crystals according to claim 1, further comprising a thermal insulation layer (8), and the thermal insulation layer (8) is arranged between the heating element (4) and the graphite crucible (21) , and surround the graphite crucible (21) set up. 一种制造碳化硅晶体的方法,所述制造碳化硅晶体的方法采用如权利要求1-7中任一项所述的制造碳化硅晶体的装置进行,所述制造碳化硅晶体的方法包括:A method for manufacturing silicon carbide crystals, the method for manufacturing silicon carbide crystals is performed using the device for manufacturing silicon carbide crystals according to any one of claims 1-7, the method for manufacturing silicon carbide crystals includes: 利用真空装置对容纳腔(11)进行抽气并且注入惰性气体;Using a vacuum device to evacuate the chamber (11) and inject an inert gas; 启动加热件(4)使得助溶剂熔化并且使得助溶剂溶液到达指定温度;Start the heating element (4) to melt the co-solvent and make the co-solvent solution reach a specified temperature; 降低籽晶组件(3)使得所述籽晶组件(3)的下表面接触所述助溶剂溶液;lowering the seed crystal assembly (3) so that the lower surface of the seed crystal assembly (3) contacts the co-solvent solution; 降低石墨件(5)使得所述石墨件(5)浸入所述助溶剂溶液;Lowering the graphite part (5) so that the graphite part (5) is immersed in the co-solvent solution; 提拉所述籽晶组件(3)实现碳化硅晶体生长。The seed crystal assembly (3) is pulled to realize silicon carbide crystal growth. 根据权利要求8所述的制造碳化硅晶体的方法,在降低籽晶组件(3)使得所述籽晶组件(3)的下表面接触所述助溶剂溶液之后还包括:The method for manufacturing silicon carbide crystals according to claim 8, after lowering the seed crystal assembly (3) such that the lower surface of the seed crystal assembly (3) contacts the co-solvent solution, further comprising: 提拉所述籽晶组件(3)使得所述籽晶组件(3)的下表面位于所述助溶剂溶液的液面上方,以使所述籽晶组件(3)提拉出部分所述助溶剂溶液。Pulling the seed crystal assembly (3) makes the lower surface of the seed crystal assembly (3) above the liquid level of the co-solvent solution, so that the seed crystal assembly (3) pulls out part of the co-solvent solution. solvent solution. 根据权利要求8所述的制造碳化硅晶体的方法,还包括:The method for manufacturing silicon carbide crystals according to claim 8, further comprising: 提拉所述籽晶组件(3)时同时驱动所述石墨件(5)下降以维持所述助溶剂溶液的液面高度不变。 When the seed crystal assembly (3) is pulled, the graphite member (5) is driven down at the same time to maintain the liquid level of the co-solvent solution constant.
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