CN115125613B - Growth device for preparing monocrystalline silicon carbide - Google Patents
Growth device for preparing monocrystalline silicon carbide Download PDFInfo
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- CN115125613B CN115125613B CN202210683987.6A CN202210683987A CN115125613B CN 115125613 B CN115125613 B CN 115125613B CN 202210683987 A CN202210683987 A CN 202210683987A CN 115125613 B CN115125613 B CN 115125613B
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- 230000012010 growth Effects 0.000 title claims abstract description 115
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 111
- 230000008859 change Effects 0.000 claims abstract description 17
- 239000007789 gas Substances 0.000 claims description 194
- 239000002994 raw material Substances 0.000 claims description 55
- 238000001816 cooling Methods 0.000 claims description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 26
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 23
- 230000005540 biological transmission Effects 0.000 claims description 23
- 229910052799 carbon Inorganic materials 0.000 claims description 23
- 229910052710 silicon Inorganic materials 0.000 claims description 23
- 239000010703 silicon Substances 0.000 claims description 23
- 238000007664 blowing Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 15
- 239000011261 inert gas Substances 0.000 claims description 14
- 230000007246 mechanism Effects 0.000 claims description 8
- 239000000112 cooling gas Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 description 22
- 238000000859 sublimation Methods 0.000 description 21
- 230000008022 sublimation Effects 0.000 description 21
- 238000000034 method Methods 0.000 description 15
- 230000008569 process Effects 0.000 description 13
- 229910010271 silicon carbide Inorganic materials 0.000 description 13
- 229910002804 graphite Inorganic materials 0.000 description 9
- 239000010439 graphite Substances 0.000 description 9
- 239000012535 impurity Substances 0.000 description 5
- 239000004575 stone Substances 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
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- 238000007906 compression Methods 0.000 description 3
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- 230000000694 effects Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000000712 assembly Effects 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 230000003698 anagen phase Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000011982 device technology Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 230000009643 growth defect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
- C30B23/005—Controlling or regulating flux or flow of depositing species or vapour
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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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
The invention discloses a growth device for preparing monocrystalline silicon carbide, which comprises a growth crucible and an air inlet control assembly, wherein the growth crucible comprises a crucible body and a cover body, silicon carbide powder is contained in the crucible body, and the cover body is arranged on the crucible body; the air inlet control assembly is positioned at the air inlet end of the crucible body and is used for controlling the air entering the crucible body according to the quality change of the silicon carbide powder. The invention can control the gas entering the crucible body according to the mass change of the silicon carbide powder in the crucible body, thereby adjusting the air flow environment in the crucible body and improving the crystal growth speed and the growth quality.
Description
Technical Field
The invention relates to the field of crystal growth, in particular to a growth device for preparing monocrystalline silicon carbide.
Background
Semiconductor silicon carbide single crystal materials have evolved over the last 30 years since commercialization of the 90 s of the last century to become the preferred base materials for power electronics and microwave radio frequency devices. With the continuous development of downstream device technology and continuous improvement of industrialization degree, the quality requirement of silicon carbide single crystal substrates is also becoming severe.
At present, the most mature silicon carbide single crystal preparation technology is a physical vapor transport method (PVT method for short), the basic principle is that a graphite crucible arranged in the center of a coil is heated through medium frequency induction, and after the graphite crucible wall generates heat in an induction way, heat is transmitted to silicon carbide powder in the graphite crucible wall to sublimate the silicon carbide powder. In the growth process, the sublimation of silicon carbide gas and the growth of crystals are mainly promoted by virtue of a temperature gradient and a pressure gradient, but the sublimation speed is slow, and the growth speed of the crystals needs to be improved; and in different periods of crystal growth, the internal atmosphere of the crucible is different, the early stage is rich in silicon and the later stage is rich in carbon, and uneven gas components are easy to cause crystal defects.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides a growth device for preparing monocrystalline silicon carbide, which can control the gas entering the crucible body according to the mass change of silicon carbide powder in the crucible body, thereby adjusting the air flow environment in the crucible body and improving the crystal growth speed and the growth quality.
A growth apparatus for preparing single crystal silicon carbide according to the present invention includes:
The growth crucible comprises a crucible body and a cover body, silicon carbide powder is contained in the crucible body, and the cover body is arranged on the crucible body;
And the air inlet control assembly is positioned at the air inlet end of the crucible body and is used for controlling the air entering the crucible body according to the mass change of the silicon carbide powder.
According to the growth device for preparing the monocrystalline silicon carbide, the sublimation of silicon carbide powder can be promoted by utilizing the airflow formed by introducing the gas, and the sublimated silicon carbide vapor can be driven to move towards the direction of the seed crystal by utilizing the airflow, so that the growth speed of crystals is accelerated. Simultaneously, along with the continuous growth of crystal, the inside air current component of crucible changes gradually, through utilizing the quality change of carborundum powder, automatic control lets in gas to adjust the inside air current environment of crucible body, make the gas composition of letting in can be according to the difference of growth stage and change automatically, ensure that the inside gaseous atmosphere that is in a suitable crystal growth all the time of crucible body, accelerate crystal growth simultaneously, can reduce dislocation and other blemishes etc. that the crystal leads to because the change of the inside composition of crucible body, improved the growth quality of crystal.
In some embodiments of the invention, the intake control assembly includes:
the raw material containing piece is arranged in the crucible body and used for containing the silicon carbide powder;
the elastic piece is connected with the raw material containing piece and is used for driving the raw material containing piece to move along the axial direction of the growth crucible according to the mass change of the silicon carbide powder;
The air flow control valve is positioned at the air inlet end of the crucible body and connected with an air source and is used for controlling air entering the crucible body according to the movement of the raw material containing piece.
In some embodiments of the invention, the raw material containing piece is provided with an air inlet hole and an air outlet hole, the air inlet hole is communicated with the air flow control valve, and the air outlet hole is communicated with the air inlet hole and the interior of the crucible body; the silicon carbide powder is characterized in that a plurality of air outlets are formed, and the air outlets are uniformly formed in the side wall of the raw material containing piece, on which the silicon carbide powder is placed.
In some embodiments of the invention, the air flow control valve is formed with an air port and is provided with a shutter for blocking the air port, the shutter being connected to the raw material container and adapted to block the air port to different extents with movement of the raw material container.
In some embodiments of the present invention, the gas flow control valve is provided with three gas ports, the three gas ports are respectively connected with three different gas sources, the three different gas sources are respectively silicon-rich gas, carbon-rich gas and inert gas, and the shielding member is adapted to change the shielding degree of the three gas ports along with the movement of the raw material containing member, so that the gas introduced into the crucible body meets the requirement of the growth of each stage of the crystal.
In some embodiments of the present invention, the crucible further comprises an air flow mixing bin, the air flow mixing bin is of a hollow structure, an air inlet end and an air outlet end are arranged on the air flow mixing bin, the air flow control valve is arranged at the air inlet end of the air flow mixing bin, and the air outlet end of the air flow mixing bin is used for introducing the air mixed by the air flow mixing bin into the crucible body.
In some embodiments of the invention, the crucible furnace further comprises a transmission assembly for connecting the raw material containing piece and the airflow control valve, wherein the transmission assembly is a flexible transmission mechanism and comprises a guide wheel set arranged outside the crucible body, and the guide wheel set is connected with the raw material containing piece and the airflow control valve through transmission lines.
In some embodiments of the present invention, the apparatus further comprises a transmission assembly connecting the raw material containing member and the air flow control valve, wherein the transmission assembly is a rigid transmission mechanism, and comprises a guiding connecting rod set arranged outside the crucible body, and the guiding connecting rod set is connected with the raw material containing member and the air flow control valve.
In some embodiments of the present invention, a seed crystal fixing part for fixing a seed crystal is provided on an inner wall of the cover body, the seed crystal fixing part is provided with a cooling bin, a cooling component is provided in the cooling bin, the cooling component includes an airflow pipeline and a blowing part, a cooling hole is provided on the blowing part, the airflow pipeline is communicated with the blowing part, and cooling gas flows into the blowing part through the airflow pipeline and enters the cooling bin through the cooling hole.
In some embodiments of the present invention, the inner wall of the crucible body and the seed crystal fixing member together define a diversion cavity, and a first diversion hole which is communicated with the diversion cavity and the outside of the crucible body is arranged on the crucible body; and a second diversion hole which is communicated with the cooling bin and the diversion cavity is formed in the seed crystal fixing piece.
Additional aspects and advantages of the invention 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 invention.
Drawings
FIG. 1 is a schematic diagram of an apparatus for producing single crystal silicon carbide growth in accordance with one embodiment of the present invention;
FIG. 2 is an enlarged schematic view of the inlet control assembly of FIG. 1;
FIG. 3 is a schematic view of an apparatus for producing single crystal silicon carbide growth according to another embodiment of the present invention;
FIG. 4 is an enlarged schematic view of the inlet control assembly of FIG. 3;
FIG. 5 is a schematic view of the construction of the material holding member of the present invention;
FIG. 6 is a top view of FIG. 5;
FIG. 7 is a schematic view of the structure of the cover of the present invention;
FIG. 8 is a bottom view of FIG. 7;
FIG. 9 is a schematic diagram of the configuration of the air flow channels in the air flow heating assembly according to one embodiment of the present invention;
FIG. 10 is a schematic view of the structure of an air flow mixing chamber according to one embodiment of the invention;
FIG. 11 is a schematic view of the structure of a shutter in an airflow control valve according to an embodiment of the invention;
fig. 12 is a schematic view of the connection of the elastic member to other structures according to the present invention.
Reference numerals:
an intake control assembly 100;
a raw material containing member 10; a stone disc 11; a graphite rod 12; an air intake hole 13; an air outlet hole 14; a cavity 15;
An elastic member 20;
an air flow heating assembly 30; a heater body 31; an air flow passage 311;
an air flow mixing bin 40; an air intake end 41; an outlet end 42;
an air flow control valve 50; an air port 51; a shutter 52; an elongated hole 521; a baffle 522; a return spring 53;
A transmission assembly 60; a guide wheel set 61; a drive line 62; a first pulley 611; a second pulley 612; a third pulley 613; a reducing gear set 614; a guide link group 63; a fourth link 631; a third link 632; a sleeve 633; a second link 634; a first link 635;
A cooling assembly 70; an air flow duct 71; a blowing member 72; a cooling hole 721; a gas flow control valve 73;
Growing a crucible 200; a crucible body 201; a cover 202; a seed crystal 203; a seed crystal holder 204; a cooling bin 205; a diversion cavity 206; a first deflector aperture 207; second deflector aperture 208;
a first air port a; a second port b; and a third port c.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
The following disclosure provides many different embodiments, or examples, for implementing different structures of the invention. In order to simplify the present disclosure, components and arrangements of specific examples are described below. They are, of course, merely examples and are not intended to limit the invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples. This repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art will recognize the applicability of other processes and/or the use of other materials.
A growth apparatus for producing single crystal silicon carbide according to an embodiment of the present invention is described below with reference to fig. 1 to 12, including: a growth crucible 200 and an air inlet control assembly 100.
Referring to fig. 1 to 4, a growth crucible 200 includes a crucible body 201 and a cover 202, silicon carbide powder is contained in the crucible body 201, the cover 202 is provided on the crucible body 201, and a seed crystal 203 to be grown is mounted on the cover 202 and is arranged opposite to the silicon carbide powder; the gas inlet control assembly 100 is positioned at the gas inlet end of the crucible body 201 for controlling the gas entering the crucible body 201 according to the mass change of the silicon carbide powder.
After the crucible body 201 heats, heat is transferred to silicon carbide powder in the crucible body and sublimates to the silicon carbide powder, and sublimated silicon carbide vapor moves to a seed crystal 203 to be grown on the cover body 202 and crystal growth is realized on the seed crystal 203. With the introduction of the gas, the sublimation of the silicon carbide powder can be promoted by utilizing the gas flow formed by the introduced gas, and the sublimated silicon carbide vapor can be driven to move towards the direction of the seed crystal by utilizing the gas flow, so that the growth speed of the crystal is accelerated. Because the quality of the silicon carbide powder can change in the growth process, different silicon carbide powder quality represents different growth stages, through the control of the gas introduced, the gas flow environment inside the crucible body 201 can be regulated, so that the gas composition introduced can be flexibly changed according to the different growth stages, the inside of the crucible body 201 is ensured to be always in a gas atmosphere suitable for crystal growth, the crystal growth is accelerated, meanwhile, dislocation, other flaws and the like caused by the change of the components inside the crucible body 201 can be reduced, and the growth quality of the crystal is improved.
Considering that during the crystal growth process, the inside of the crucible body 201 is in a silicon-rich state, and in the later crystal growth period, the inside of the crucible body 201 is in a carbon-rich state due to carbonization of powder, and impurities such as silicon drops and carbon packages are easily generated in the two states, so that crystal defects are caused. Thus, the gas entering the crucible body 201 has a mixture of one or more of a carbon-rich gas, an inert gas, and a silicon-rich gas. For example, when the inside of the crucible body 201 is in a silicon-rich state, the amount and time of introduction of the carbon-rich gas may be controlled, and when the inside of the crucible body 201 is in a carbon-rich state, the amount and time of introduction of the silicon-rich gas may be controlled, and the specific introduction may be determined according to a growth stage, which may be determined according to a mass change of the silicon carbide powder.
In some embodiments of the present invention, referring to FIG. 1, an intake control assembly 100 includes a raw material containing member 10, an elastic member 20, and an airflow control valve 50. The raw material containing piece 10 is movably arranged in the crucible body 201 and is used for containing silicon carbide powder, and one side of the raw material containing piece, which is far away from the cover body 202, penetrates through the side wall of the crucible body 201 and extends to the outside of the crucible body 201; the raw material holding member 10 may be a graphite member so that the raw material holding member 10 has high temperature resistance. The elastic member 20 may be a spring, a leaf spring, or the like, which has an elastic ability to expand and contract and return. The elastic member 20 is connected to the end of the raw material containing member 10 extending out of the crucible body 201, the elastic member 20 is adapted to be stretched or compressed when the mass of the silicon carbide powder changes, and when the mass of the silicon carbide powder changes, the elastic member 20 drives the raw material containing member 10 to move up and down along the axial direction of the growth crucible 200 (i.e., the sublimation direction of the silicon carbide powder or the growth direction of the seed crystal). The gas flow control valve 50 is located at the gas inlet end of the crucible body 201, and is connected to a gas source for controlling the gas entering the crucible body 201 according to the movement of the raw material containing member 10.
It will be appreciated that the mass of silicon carbide powder on the feedstock containing member 10 is the heaviest and the resilient member 20 is in compression during the initial stage of growth. In the growth process, along with continuous sublimation of the silicon carbide powder, the weight of the silicon carbide powder on the raw material containing piece 10 is gradually reduced, the elastic piece 20 continuously stretches upwards and drives the raw material containing piece 10 to move upwards, so that the silicon carbide powder on the raw material containing piece 10 is always kept on a high-temperature line, the stability of the sublimation rate of the silicon carbide powder is ensured, and the growth quality of crystals is improved. Meanwhile, along with the movement condition of the raw material containing member 10, the growth stage of the crystal can be reversely pushed out, the air flow control valve 50 controls the opening and closing of different air valves in combination with different growth stages of the crystal, and the air flow environment inside the crucible body 201 is regulated, so that the inside of the crucible body 201 is always in a gas atmosphere suitable for crystal growth, and the growth quality of the crystal is ensured while the crystal growth is promoted. In addition, the gas flow control valve 50 controls the gas to form gas flow, so that the formed gas flow not only can promote the sublimation of silicon carbide powder, but also can drive the sublimated silicon carbide vapor to move towards the direction of the seed crystal 203, thereby accelerating the growth speed of crystals.
After the growth is completed, the lid 202 may be opened to remove the final crystal. Then, the desired silicon carbide powder is added to the material containing member 10, and the seed crystal 203 is arranged, and the cover 202 is covered to enter the preparation stage for the next seed crystal growth. At this time, the elastic member 20 is restored to the compressed state by the pressure due to the increase of the silicon carbide powder, and the above process is repeated.
In some embodiments of the present invention, referring to fig. 1, 5 and 6, the raw material containing member 10 is provided with an air inlet hole 13 and an air outlet hole 14, the air inlet hole 13 is communicated with the air flow control valve 50, and the air outlet hole 14 is communicated with the air inlet hole 13 and the interior of the crucible body 201; the plurality of air outlets 14 are arranged, and the plurality of air outlets 14 are uniformly arranged on the side wall of the raw material containing piece 10 where the silicon carbide powder is placed. For example, the whole raw material holding member 10 may have a substantially T-shaped structure including a stone mill 11 for holding silicon carbide arranged in the crucible body 201 and a graphite rod 12 provided at the bottom of the stone mill 11 penetrating through the side wall of the crucible body 201, the stone mill 11 having a hollow cavity 15, an air inlet hole 13 arranged through the graphite rod 12, a plurality of air outlet holes 14 provided on the upper wall of the stone mill 11, the air inlet hole 13, the air outlet holes 14 communicating with the cavity 15; the gas passing through the gas flow control valve 50 reaches the bottom of the silicon carbide powder through the gas flow channel formed by the gas inlet hole 13, the cavity 15 and the gas outlet hole 14, and the gas outlet holes 14 are uniformly arranged, so that the uniformity of the gas can be increased to the greatest extent, the gas flow is uniformly increased, the uniform stress of the silicon carbide powder is ensured, the sublimation of the silicon carbide powder is promoted, the movement speed of sublimated silicon carbide vapor to crystals is accelerated, the crystal growth efficiency is improved, the crystal growth defect caused by the non-uniform sublimation of the silicon carbide powder is further reduced, and the crystal growth quality is improved.
In some embodiments of the present invention, referring to fig. 1 and 2, the air flow control valve 50 is formed with an air port 51, and is provided with a shielding member 52 for shielding the air port 51, the shielding member 52 being connected to the raw material container 10, and adapted to shield the air port 51 to varying degrees as the raw material container 10 moves. It will be appreciated that as the silicon carbide powder is continuously reduced during the growth process, under the action of the elastic member 20, the raw material containing member 10 will move upwards along the sublimation direction of the silicon carbide powder, and at the same time, the shielding member 52 connected to the raw material containing member 10 will also move, so as to realize shielding of the gas port 51 to different extents, thereby realizing control of the amount and time of gas flowing through the gas port 51, so that the introduced gas can meet the requirement of the crystal growth stage. The air ports 51 can be provided with one or more air ports 51, and the plurality of air ports 51 can be used for shielding the air ports 51 to different degrees through different gases, namely, shielding one air port to different degrees, and shielding the air ports 51 with different numbers.
In view of this, the gas flow control valve 50 according to the embodiment of the present invention takes carbon-rich gas as an example, and the carbon-rich gas to be introduced may be connected to the gas port 51 in addition to the inert gas being connected to the gas inlet end of the crucible body 201. In this embodiment, the gas flow control valve 50 may be provided with two gas ports 51, one gas port 51 for passing the carbon rich gas and one gas port 51 for passing the inert gas; the gas flow control valve 50 may also be provided with only one gas port 51 for passage of inert gas through the carbon rich gas and into the crucible body 201. For example, in the initial state, the shielding member 52 does not shield the gas port 51, i.e., the gas port 51 is completely exposed, and the carbon-rich gas can be directly introduced into the crucible body 201 through the gas port 51. At the beginning of growth, because the melting point of silicon is low, the inside of the whole crucible body 201 is in a silicon-rich state, and at the moment, the direct introduction of carbon-rich gas can adjust the air flow environment inside the crucible body 201, so that the inside of the crucible body 201 is in a gas atmosphere suitable for crystal growth, and the generation of silicon drops and other impurities is avoided, thereby promoting the crystal growth and ensuring the growth quality of the crystal. As the material containing member 10 rises, the shielding member 52 gradually shields the gas port 51, the amount of carbon-rich gas introduced is gradually reduced, and at the end of the first growth stage, the gas port is just completely shielded by the shielding member 52, and the introduction of the carbon-rich gas into the crucible body 201 is stopped.
Similarly, taking a silicon-rich gas as an example, the silicon-rich gas to be introduced may be connected to the gas port 51. Also, in the present embodiment, the gas flow control valve 50 may be provided with two gas ports 51, one gas port 51 for passing the silicon-rich gas and one gas port 51 for passing the inert gas; the gas flow control valve 50 may also be provided with only one gas port 51 for passage of the silicon-rich gas, and the inert gas may be additionally provided with a passage into the crucible body 201. In the initial state, the shutter 52 completely shields the air port 51. At the beginning of growth, the inside of crucible body 201 is in a silicon-rich state, so that no silicon-rich gas is required to be introduced, and gas port 51 is always blocked. In the later crystal growth stage, the crucible body 201 is in a carbon-rich state due to carbonization of silicon carbide powder, the shielding piece 52 gradually reduces shielding of the air port 51 along with rising of the raw material containing piece 10, and the ventilation amount of the silicon-rich gas is gradually increased, so that the air flow environment in the crucible body 201 is regulated, the inside of the crucible body 201 is in a gas atmosphere suitable for crystal growth, and impurities such as carbon wrapping are avoided, thereby promoting crystal growth and ensuring the growth quality of crystals.
Considering that the functional gases required for different growth stages of the crystal are different, in order to realize synchronous control of all the introduced gases, the gas flow control valve 50 is provided with three gas ports 51, the three gas ports 51 are respectively connected with three different gas sources, the three different gas sources are respectively silicon-rich gas, carbon-rich gas and inert gas, and the shielding piece 52 is suitable for changing the shielding degree of the three gas ports 51 along with the movement of the raw material containing piece so that the gas introduced into the crucible body meets the growth requirement of each stage of the crystal. For example, referring to fig. 2, 4, 10 and 11, the three gas ports 51 are a first gas port a, a second gas port b and a third gas port c, respectively, the carbon-rich gas is connected to the first gas port a, the inert gas is connected to the second gas port b, the silicon-rich gas is connected to the third gas port c, the shielding member 52 may be a baffle plate 522 with an elongated hole 521 formed in the center, the elongated hole 521 on the baffle plate 522 is located above the second gas port b, the shielding member 52 is connected to the raw material containing member 10, and when the raw material containing member 10 moves up and down, the baffle plate 522 can move left and right along the parallel direction of the connecting lines of the three gas ports 51 above the three gas ports 51, so as to ensure that the third gas port c is completely shielded by the baffle plate during the first growth stage of the crystal, and the gas introduced into the crucible body is the carbon-rich gas and the inert gas; in the second growth stage of the crystal, the first gas port a and the third gas port c are both covered, and only inert gas is introduced; in the third growth stage of the crystal, the first gas port a is completely covered by a baffle plate, and the silicon-rich gas and the inert gas are introduced.
It can be understood that in the whole growth process of the crystal, inert gas is directly introduced, and whether the silicon-rich gas and the carbon-rich gas are introduced or not and how much the silicon-rich gas is introduced can be controlled according to the quality change of the silicon carbide powder in different growth stages; for example, during the first growth phase, as the shutter 522 moves slowly, the first port a is gradually blocked, and at this time, the third port c is always completely blocked; in the second growth stage, only the second air port b is exposed, and the first air port a and the third air port c are always in a completely blocked state; in the third growth stage, the third air port c is gradually exposed as the shutter 522 moves further, and the first air port a is always completely blocked.
In other embodiments, the airflow control valve 50 may also be a valve body controlled by software, and the system determines the growth stage after processing and analyzing the change of the quality of the silicon carbide powder, so as to control the opening and closing, the opening degree and the opening time of the airflow control valve 50 to control the gas introduced, and further adjust the airflow environment inside the crucible body 201, so that the inside of the crucible body 201 is always in a gas atmosphere suitable for crystal growth, and the growth quality of the crystal is ensured while promoting the crystal growth.
In some embodiments of the present invention, referring to fig. 1,2 and 10, the air inlet control assembly 100 may further include an air mixing chamber 40, the air mixing chamber 40 has a hollow structure, the air mixing chamber 40 is provided with an air inlet end 41 and an air outlet end 42, the air control valve 50 is provided at the air inlet end 41 of the air mixing chamber 40, and the air outlet end 42 of the air mixing chamber 40 is used for introducing the air mixed by the air mixing chamber 40 into the crucible body 201. The air flow mixing bin 40 is arranged to enable the air to be introduced to be mixed firstly and then enter the crucible body 201 according to the required proportion, so that the uniformity of the air is guaranteed, the inside of the crucible body 201 is more facilitated to be in a gas atmosphere suitable for crystal growth, the growth of crystals is facilitated, and the growth quality of the crystals is guaranteed.
Considering that the temperature of the gas entering the crucible body 201 directly relates to the sublimation condition of the silicon carbide powder, the sublimation condition is affected by the temperature being too low, therefore, in some embodiments of the invention, referring to fig. 1,2 and 9, the gas inlet control assembly 100 may further include a gas flow heating assembly 30 for heating the gas entering the crucible body 201, the gas flow heating assembly 30 includes a heater body 31, and the heater body 31 may be a graphite piece, so that the heater body 31 has high temperature resistance; an air flow channel 311 is formed in the heater body 31, the air flow channel 311 is communicated with the air flow control valve 50 and the air inlet end of the crucible body 201, gas flows into the crucible body 201 through the air flow control valve 50, the air flow channel 311 and the air inlet end of the crucible body 201, the heater body 31 can preheat the gas flowing through the air flow channel 311, and the heated gas can further promote sublimation of silicon carbide powder after entering the crucible body 201, so that sublimation effect is effectively improved, and crystal growth rate is further improved.
It will be appreciated that when the airflow mixing chamber 40 is provided, the airflow heating assembly 30 may be disposed between the airflow mixing chamber 40 and the air inlet end of the crucible body 201, and the mixed gas mixed by the airflow mixing chamber 40 may first enter the airflow heating assembly 30 for heating before entering the crucible body 201, so that the sublimation of the silicon carbide powder may be further promoted by the heated mixed gas. In other words, the combination of the air flow mixing bin 40 and the air flow heating assembly 30 can enable the air flow introduced from the bottom to be fully mixed and heated, and then enter the crucible body 201 after being uniformly mixed and heated, so that difficulty in sublimation of silicon carbide powder caused by direct connection of low-temperature air is avoided, and sublimation effect is effectively improved; moreover, the uniformity of the entering gas can be ensured, and the defect of crystal growth caused by uneven gas introduction can be reduced.
Alternatively, the airflow channel 311 may be a spiral channel or an S-shaped channel, which can increase the contact area and contact duration between the gas and the graphite wall of the heater body 31, compared to a linear channel, so as to ensure the heating effect of the gas.
In other embodiments of the present invention, the gas flow heating assembly 30 may also be a gas flow heating pipe disposed in the sidewall of the crucible body 201, the gas inlet end of the gas flow heating pipe being connected to the gas outlet of the gas flow control valve/gas flow mixing chamber, and the gas outlet end of the gas flow heating pipe being in communication with the interior of the crucible body 201. The air flow heating pipeline is arranged in the inner wall of the crucible body 201, when the crucible body 201 heats, the temperature of the air flow heating pipeline can be increased along with the heating of the air flow heating pipeline, and the air flowing through the air flow heating pipeline can be directly heated, so that the gas entering the crucible body 201 can further promote the sublimation of the silicon carbide powder. Alternatively, the air flow heating pipeline may be a curved pipeline, so that the gas can be fully heated in the side wall of the crucible body 201, the gas entering the crucible body 201 is ensured to be more beneficial to sublimation of silicon carbide powder, and the growth rate of crystals is further improved.
In some embodiments of the present invention, as shown with reference to fig. 2 and 4, a drive assembly 60 connecting the feedstock containing member 10 and the airflow control valve 50 may also be included. The transmission assembly 60 is used for enabling the raw material containing piece 10 to move to drive the airflow control valve 50 to control airflow, and the transmission assembly 60 can be a flexible transmission mechanism or a rigid transmission mechanism. When the airflow control valve 50 includes the shutter 52, the transmission assembly 60 connects the raw material container 10 and the shutter 52.
For example, referring to fig. 2, the transmission assembly 60 is a flexible transmission mechanism, and includes a guide wheel set 61 disposed outside the crucible body, and the guide wheel set 61 is connected to the raw material containing member 10 and the air flow control valve 50 through a transmission line 62. Specifically, the guiding wheel set 61 includes a first pulley 611, a second pulley 612, a third pulley 613 and a reducing gear set 614, where the first pulley 611, the third pulley 613 and the reducing gear set 614 are installed at the bottom of the outer wall of the crucible body 201, the reducing gear set 614 is disposed between the first pulley 611 and the third pulley 613, the second pulley 612 is disposed at one side of the airflow control valve 50 and is located on an extension line of the movement range of the airflow control valve 50, one end of the driving wire 62 is connected with an end portion of the raw material containing member 10 extending out of the crucible body 201, and the other end sequentially passes through the first pulley 611, the reducing gear set 614, the third pulley 613 and the second pulley 612 and is connected with the shielding member 52 of the airflow control valve 50, when the raw material containing member 10 moves upwards under the action of the elastic member 20, one end of the driving wire 62 moves upwards, and the other end drives the shielding member 52 of the airflow control valve 50 to move along the horizontal direction, so as to realize shielding of the air ports 51 to different degrees, thereby adjusting the airflow environment inside the crucible body 201 to be always in a gas atmosphere suitable for crystal growth, thereby promoting crystal growth, and ensuring crystal growth quality. At this time, in order to ensure that the shutter 52 in the air flow control valve 50 can be better reset, a reset spring 53 may be additionally provided, and the reset spring 53 is connected to one end of the shutter 52 away from the driving line 62.
In other embodiments of the present invention, referring to fig. 4, the transmission assembly 60 may be a rigid transmission mechanism, including a guide linkage 63 disposed outside the crucible body 201, and the guide linkage 63 connects the raw material container 10 and the gas flow control valve 50. Specifically, the guide link group 63 includes four links sequentially hinged, namely, a first link 635, a second link 634, a third link 632, and a fourth link 631; the head end of the first connecting rod 635 is connected with the end of the raw material containing piece 10 extending out of the crucible body, and the tail end of the fourth connecting rod 631 is connected with the shielding piece 52 of the airflow control valve 50; the second and fourth connecting rods 634 and 631 are fixed in the axial direction of the respective rods so that the second and fourth connecting rods 634 and 631 can only reciprocate in the axial direction thereof, and the second connecting rod 634 can be fixedly mounted through the sleeve 633 and can move up and down along the sleeve 633; the moving direction of the fourth link 631 coincides with the moving direction of the airflow control valve 50.
It will be appreciated that when the raw material holding member 10 moves upward by the elastic member 20, the second link 634 will move upward in the axial direction thereof by the first link 635, the connection end of the third link 632 and the second link 634 moves upward, and the other end rotates; the fourth connecting rod 631 will drive the shielding piece 52 of the air flow control valve 50 to move, so as to realize shielding of the air port 51 to different degrees, and further adjust the air flow environment inside the crucible body 201, so that the inside of the crucible body 201 is always in a gas atmosphere suitable for crystal growth, and crystal growth is promoted and meanwhile crystal growth quality is ensured.
In some embodiments of the present invention, referring to fig. 1, 7 and 8, a seed crystal fixing member 204 for fixing a seed crystal 203 may be provided on an inner wall of the cover 202, the seed crystal fixing member 204 has a cooling chamber 205, a cooling component 70 is provided in the cooling chamber 205, the cooling component 70 includes an air flow pipe 71 and a blowing member 72, a cooling hole 721 is provided on the blowing member 72, the air flow pipe 71 is communicated with the blowing member 72, and cooling gas flows into the blowing member 72 through the air flow pipe 71 and enters the cooling chamber 205 through the cooling hole 721. After reaching the cooling bin 205, the cooling gas can be used for reducing the temperature of the crystal part and reducing gasification in the crystal growth process; meanwhile, the whole crystal growth surface is increased at the same speed, so that a single surface is generated on the growth surface, the material unavailability caused by uneven crystal shape in the post-treatment process is reduced, and the waste is reduced. Along with the continuous introduction of the cooling gas, the axial temperature gradient formed inside the crucible body 201 can be promoted, the growth of the silicon carbide crystal can be promoted, and the growth efficiency can be improved.
Alternatively, referring to fig. 7, the blowing member 72 is a flow guide member having a gradually increasing diameter. For example, the blowing member 72 is a horn-shaped flow guide member, and the cooling holes 721 are disposed at the outlet of the horn-shaped flow guide member, and the cooling holes 721 may be one or more. When the cooling hole 721 is one, it may be a first through hole having a diameter smaller than the diameter of the outlet and larger than the diameter of the inlet. When there are a plurality of cooling holes 721, there may be a plurality of second through holes provided on the outlet sealing plate, and the aperture of the second through holes is smaller than that of the first through holes.
Optionally, there may be multiple cooling assemblies 70 in the cooling bin 205, where the multiple cooling assemblies 70 may be arranged in the cooling bin 205 according to cooling requirements to cool crystals, and the air flow pipes 71 of each cooling assembly 70 are provided with air flow control valves 73, and the air flow in the corresponding air flow pipe 71 can be controlled by each air flow control valve 73 to adjust the temperature of the corresponding crystal area, so as to control the growth speed of the crystals in different areas, thereby obtaining the required crystal shape, reducing crystal loss caused by irregular shapes due to different growth speeds, and reducing crystal flaws. For example, referring to fig. 7 and 8, there may be four cooling modules 70 uniformly distributed in the cooling chamber 205, and the outlet of the blower 72 in each cooling module 70 is opposite to the side wall of the seed crystal holder 204 on which the seed crystal 203 is mounted.
In some embodiments of the present invention, the inner wall of the crucible body 201 and the seed crystal fixing member 204 together define a diversion cavity 206, and a first diversion hole 207 is formed on the crucible body 201 and is communicated with the diversion cavity 206 and the outside of the crucible body 201; the seed crystal fixing piece 204 is provided with a second diversion hole 208 which is communicated with the cooling bin 205 and the diversion cavity 206. Specifically, an annular groove is disposed on the inner wall of the crucible body 201 opposite to the seed crystal fixing member 204, and the flow guiding cavity 206 is defined by the groove and the seed crystal fixing member 204. In the growth process, since the gas is continuously introduced into the crucible body 201, the sublimation of the silicon carbide powder into the gas is promoted to flow upwards, and meanwhile, the pressure in the crucible body 201 is increased, so that the air flow flowing into the crucible body 201 from the air inlet end of the crucible body 201 flows into the crucible body along the crystal surface after the crystal growth is finished, the internal pressure of the crucible body 201 is reduced, and impurities such as carbon packages generated in the growth process are taken away by the air flow continuously.
It will be appreciated that when the waste gas (the reacted gas in the crucible body 201) enters the flow guiding cavity 206, the waste gas flows out of the crucible body 201 from the first flow guiding hole 207, so that the pressure of the inner growth part in the crucible body 201 is reduced, and a pressure gradient is formed by ventilation and matching with the lower part, so that the pressure in the crucible body 201 is always kept high at the lower part and low at the upper part. Meanwhile, the impurities of the silicon carbide vapor are taken away by utilizing the continuous flow of the gas, so that the purity of the crystal is improved. In addition, the gas used in the cooling bin 205 flows out through the second diversion hole 208, is converged into the diversion cavity 206, and flows out together with the gas in the diversion cavity 206.
Alternatively, there may be a plurality of first diversion holes 207, and the plurality of first diversion holes 207 are uniformly formed around the diversion cavity 206 on the crucible body 201. It can be appreciated that the first uniformly opened diversion holes 207 can better convey the gas in the diversion cavity 206 to the outside of the crucible body 201, and uniform release is also more beneficial to ensuring that the pressure at the upper part of the crucible body 201 is in a stable condition, so as to avoid excessive accumulation of the gas at a certain position of the diversion cavity 206.
Optionally, there may be a plurality of second diversion holes 208, where the plurality of second diversion holes 208 are uniformly formed around the cooling bin 205. It can be appreciated that the second diversion holes 208 which are uniformly formed are also more beneficial to uniformly and outwardly discharging the cooling gas after being used in the cooling bin 205, so as to ensure that the cooling bin 205 is in a stable environment.
In some embodiments of the present invention, referring to fig. 1 and 3, the elastic member 20 may have a gas inlet and a gas outlet that are communicated with each other while having compression and expansion functions, and the gas entering the crucible body 201 passes through the elastic member 20 before entering, so that the compression and expansion of the elastic member 20 do not affect the gas transmission therein. Specifically, it may be directly connected between the air inlet hole 13 of the raw material holding member 10 and the outlet of the air flow passage 311 in the air flow heating assembly 30. Of course, referring to fig. 12, the elastic member 20 may not have an air inlet and an air outlet, and accordingly, the air inlet hole 13 of the raw material container 10 is directly connected to the outlet of the air flow channel 311 in the air flow heating assembly 30.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; the device can be mechanically connected, electrically connected and communicated; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that: many changes, modifications, substitutions and variations may be made to the embodiments without departing from the spirit and principles of the invention, the scope of which is defined by the claims and their equivalents.
Claims (8)
1. A growth apparatus for producing single crystal silicon carbide, comprising:
The growth crucible comprises a crucible body and a cover body, silicon carbide powder is contained in the crucible body, and the cover body is arranged on the crucible body;
the air inlet control component is positioned at the air inlet end of the crucible body and is used for controlling the air entering the crucible body according to the mass change of the silicon carbide powder;
The intake air control assembly includes:
the raw material containing piece is arranged in the crucible body and used for containing the silicon carbide powder;
the elastic piece is connected with the raw material containing piece and is used for driving the raw material containing piece to move along the axial direction of the growth crucible according to the mass change of the silicon carbide powder;
The air flow control valve is positioned at the air inlet end of the crucible body and connected with an air source, and is used for controlling air entering the crucible body according to the movement of the raw material containing piece;
The air flow control valve is provided with an air port, and is provided with a shielding piece for shielding the air port, and the shielding piece is connected with the raw material containing piece and is suitable for shielding the air port to different degrees along with the movement of the raw material containing piece.
2. The growth device for preparing single crystal silicon carbide according to claim 1, wherein the raw material holding member is provided with an air inlet hole and an air outlet hole, the air inlet hole is communicated with the air flow control valve, and the air outlet hole is communicated with the air inlet hole and the interior of the crucible body; the silicon carbide powder is characterized in that a plurality of air outlets are formed, and the air outlets are uniformly formed in the side wall of the raw material containing piece, on which the silicon carbide powder is placed.
3. A growth apparatus for producing single crystal silicon carbide according to claim 1 wherein said gas flow control valve is provided with three said gas ports, said three gas ports being respectively connected to three different gas sources, said three different gas sources being respectively a silicon-rich gas, a carbon-rich gas and an inert gas, said shielding member being adapted to vary the degree of shielding of said three gas ports in response to movement of said source material holding member so that the gas introduced into said crucible body meets the requirements for growth of the respective phases of the crystal.
4. The growth apparatus for producing single crystal silicon carbide according to claim 1, further comprising a gas flow mixing chamber, wherein the gas flow mixing chamber has a hollow structure, the gas flow mixing chamber is provided with a gas inlet end and a gas outlet end, the gas flow control valve is provided at the gas inlet end of the gas flow mixing chamber, and the gas outlet end of the gas flow mixing chamber is used for introducing the gas mixed by the gas flow mixing chamber into the crucible body.
5. The apparatus of claim 1, further comprising a transmission assembly connecting the source material holding member and the gas flow control valve, wherein the transmission assembly is a flexible transmission mechanism comprising a guide wheel set disposed outside the crucible body, and wherein the guide wheel set is connected to the source material holding member and the gas flow control valve by a transmission line.
6. The apparatus of claim 1, further comprising a drive assembly connecting the source material holder and the gas flow control valve, wherein the drive assembly is a rigid drive mechanism comprising a guide linkage disposed outside the crucible body, the guide linkage connecting the source material holder and the gas flow control valve.
7. A growth apparatus for producing single crystal silicon carbide according to any of claims 1 to 6 wherein a seed crystal fixing member for fixing a seed crystal is provided on an inner wall of the cover body, the seed crystal fixing member has a cooling chamber, a cooling component is provided in the cooling chamber, the cooling component includes an air flow pipe and a blowing member, a cooling hole is provided in the blowing member, the air flow pipe is communicated with the blowing member, and a cooling gas flows into the blowing member through the air flow pipe and enters the cooling chamber through the cooling hole.
8. A growth apparatus for producing single crystal silicon carbide as claimed in claim 7 wherein the inner wall of the crucible body and the seed crystal fixing member together define a flow guiding chamber, the crucible body being provided with a first flow guiding hole communicating the flow guiding chamber with the outside of the crucible body; and a second diversion hole which is communicated with the cooling bin and the diversion cavity is formed in the seed crystal fixing piece.
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