CN117646278A - Growth device and growth method of silicon carbide single crystal with bottom supplied and discharged - Google Patents
Growth device and growth method of silicon carbide single crystal with bottom supplied and discharged Download PDFInfo
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- CN117646278A CN117646278A CN202410122723.2A CN202410122723A CN117646278A CN 117646278 A CN117646278 A CN 117646278A CN 202410122723 A CN202410122723 A CN 202410122723A CN 117646278 A CN117646278 A CN 117646278A
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- 239000013078 crystal Substances 0.000 title claims abstract description 71
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 61
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 186
- 230000007246 mechanism Effects 0.000 claims abstract description 76
- 239000000463 material Substances 0.000 claims abstract description 61
- 238000003756 stirring Methods 0.000 claims abstract description 55
- 238000010438 heat treatment Methods 0.000 claims abstract description 36
- 238000007599 discharging Methods 0.000 claims abstract description 12
- 238000005452 bending Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 13
- 230000008901 benefit Effects 0.000 description 11
- 239000007789 gas Substances 0.000 description 11
- 230000008022 sublimation Effects 0.000 description 10
- 238000000859 sublimation Methods 0.000 description 10
- 238000003763 carbonization Methods 0.000 description 8
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000000428 dust Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 230000001737 promoting effect Effects 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 230000003685 thermal hair damage Effects 0.000 description 4
- 230000002035 prolonged effect Effects 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000013589 supplement Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000561734 Celosia cristata Species 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 210000001520 comb Anatomy 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001629 suppression Effects 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
- 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
-
- 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
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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 belongs to the technical field of silicon carbide crystal growth, and particularly relates to a growth device and a growth method of silicon carbide single crystals with bottom feeding and discharging. The growth device comprises a crucible part, the lower part of which is a raw material accommodating part and comprises a crucible bottom, and a feed inlet and a residual material outlet are arranged on the crucible bottom; the spiral feeding mechanism is vertically arranged and enters the raw material accommodating part through the feeding hole; the stirring structure is positioned on the spiral feeding mechanism in the raw material accommodating part and used for stirring residual raw materials after growth in the raw material accommodating part to the residual material outlet; and a heating portion provided outside the crucible portion and provided along a circumferential direction of the raw material accommodating portion. During crystal growth, raw materials can be supplemented into the crucible part, and large-size silicon carbide single crystals can be grown.
Description
Technical Field
The invention belongs to the technical field of silicon carbide crystal growth, and particularly relates to a growth device and a growth method of silicon carbide single crystals with bottom feeding and discharging.
Background
Physical Vapor Transport (PVT) is the main method for industrially growing silicon carbide crystals at present, specifically, a silicon carbide polycrystalline raw material is filled in a closed cavity formed by a graphite crucible and a crucible cover, a silicon carbide seed crystal sheet is adhered to the inner wall of the crucible cover, and a heating body outside the graphite crucible is heated in an inert atmosphere environment to sublimate the silicon carbide polycrystalline raw material at the lower part of the graphite crucible, and sublimate gas is used for growing and crystallizing on the silicon carbide seed crystal to obtain silicon carbide single crystals.
The size of the graphite crucible is limited due to the influence of factors such as uniform heating and temperature gradient, and the amount of the silicon carbide polycrystalline raw material filled in the graphite crucible is limited, so that the size of the grown silicon carbide crystal is limited to a certain extent, and the large-size crystal is difficult to grow.
Disclosure of Invention
The invention aims to overcome the defect that when a silicon carbide single crystal grows in the prior art, the quantity of silicon carbide polycrystalline raw materials filled in a graphite crucible is limited, and a large-size silicon carbide single crystal is difficult to grow.
In order to achieve the above object, in a first aspect, the present invention provides a growth apparatus for a bottom-feed silicon carbide single crystal, comprising:
the lower part of the crucible part is a raw material accommodating part and comprises a crucible bottom, and a feed inlet and a residual material outlet are arranged on the crucible bottom;
the spiral feeding mechanism is vertically arranged and enters the raw material accommodating part through the feeding hole;
the stirring structure is positioned on the spiral feeding mechanism in the raw material accommodating part and used for stirring residual raw materials after growth in the raw material accommodating part to the residual material outlet;
and a heating portion provided outside the crucible portion and provided along a circumferential direction of the raw material accommodating portion.
In some preferred embodiments, the feed port is located in the center of the crucible bottom.
Preferably, the lower end of the heating part is lower than the crucible bottom.
Preferably, the material stirring structure is an arc material stirring plate arranged along the circumferential direction of the spiral feeding mechanism, the bending direction of each arc material stirring plate is the same, the lower surface of each arc material stirring plate is provided with a saw-tooth structure, and the arc material stirring plate is positioned at the top end of the spiral feeding mechanism.
Preferably, a blade is provided on the screw feeder in the raw material accommodating portion along a circumferential direction of the screw feeder, the blade is in a linear shape, and the blade is provided at a lower end of the screw feeder in the raw material accommodating portion.
Preferably, the outer end of at least one of said blades is in sliding engagement with the crucible wall of said crucible portion.
Preferably, the outer end portion extends in an axial direction of the crucible wall, the extended extension surface of the outer end portion being in sliding engagement with the crucible wall.
In some preferred embodiments, the growth device further comprises:
the raw material bin is arranged below the crucible part and is provided with an air inlet;
the feeding pipe is vertically arranged, the upper end of the feeding pipe is connected with the feeding hole, the lower end of the feeding pipe is connected with the upper part of the raw material bin, the feeding pipe is communicated with the raw material accommodating part and the raw material bin, and the spiral feeding mechanism enters the raw material accommodating part from the raw material bin through the feeding pipe;
the surplus bin is arranged below the crucible part and is provided with an air outlet;
and the upper end of the residual discharging pipe is connected with the residual outlet, the lower end of the residual discharging pipe is connected with the upper part of the residual bin, and the residual discharging pipe is communicated with the raw material accommodating part and the residual bin.
In some preferred embodiments, the crucible portion comprises a crucible wall and a crucible cover, wherein the lower part of the crucible cover is used for installing seed crystals, the crucible cover covers the upper part of the crucible wall, and the crucible cover is in sealed sliding connection with the crucible wall.
In a second aspect, the present invention provides a method for growing a silicon carbide single crystal in the apparatus for growing a silicon carbide single crystal according to the first aspect, the method comprising: the vertical screw feeding mechanism that sets up carries silicon carbide polycrystalline raw materials to raw materials holding portion from the feed inlet at the bottom of the crucible, is located the stirring structure on the screw feeding mechanism in the raw materials holding portion will the residual raw materials after growing in the raw materials holding portion is allocated to be located the surplus material export at the bottom of the crucible.
According to the silicon carbide single crystal growth device, the feeding hole is formed in the bottom of the crucible, the vertically arranged spiral feeding mechanism enters the raw material accommodating part through the feeding hole, unreacted raw materials can be continuously provided into the crucible through the spiral feeding mechanism, and the size of the grown silicon carbide single crystal is remarkably improved. According to the invention, the residual material outlet is arranged on the bottom of the crucible, the stirring structure is arranged on the spiral feeding mechanism positioned in the raw material accommodating part, the spiral feeding mechanism drives the stirring structure to rotate, so that residual raw materials after growth in the raw material accommodating part can be conveyed into the residual material outlet, and discharged from the raw material accommodating part of the crucible part.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural view showing an embodiment of a silicon carbide single crystal growth apparatus according to the present invention.
FIG. 2 is a cross-sectional view taken at section A-A of one embodiment of a silicon carbide single crystal growth apparatus of the present invention.
Description of the reference numerals
1. A crucible portion; 101. a feed inlet; 102. a residue outlet; 103. a crucible wall; 104. a crucible cover; 2. a spiral feeding mechanism; 3. a material stirring structure; 4. a heating section; 5. a blade; 6. a raw material bin; 601. an air inlet; 7. a feed pipe; 8. a residual bin; 801. an air outlet; 9. a residual material outlet pipe; 10. a seal ring; 11. and a lifting mechanism.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In this document, unless otherwise indicated, terms of orientation such as "upper" and "lower" are used generally to refer to the orientation shown in the drawings and in the practice, and "inner" and "outer" are intended to refer to the interior and exterior of the outline of the component.
In the description of the present invention, it should be understood that the terms "center," "length," "upper," "lower," "vertical," "horizontal," "top," "bottom," "inner," "outer," "axial," "radial," "circumferential," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the present invention and simplify description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be configured and operated in a particular orientation, and thus should not be construed as limiting the present invention.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and the like are to be construed broadly, and may be fixedly attached, detachably attached, or integrally formed, for example; can be mechanically or electrically connected; 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" a second feature may be that the first feature is directly above or obliquely above the second feature, or simply indicates that the first feature is higher in level than the second feature. The first feature being "under" the second feature may be the first feature being directly under or obliquely under the second feature, or simply indicating that the first feature is level less than the second feature.
The inventors of the present invention have studied and found that, when a silicon carbide single crystal is grown by a physical transportation method, the amount of a silicon carbide polycrystalline material charged in a graphite crucible is constant, and it is difficult to grow a large-sized silicon carbide single crystal.
In this regard, referring to fig. 1, the present invention provides a growth apparatus for silicon carbide single crystals with bottom feed and discharge, comprising a crucible portion 1, the lower portion of which is a raw material accommodating portion, comprising a crucible bottom, on which a feed inlet 101 and a remainder outlet 102 are provided;
a screw feeding mechanism 2 vertically arranged to enter the raw material accommodating portion through the feed port 101;
a stirring structure 3, which is located on the spiral feeding mechanism 2 in the raw material accommodating portion and is used for stirring the residual raw material after growth in the raw material accommodating portion to the residual material outlet 102;
and a heating section 4 provided outside the crucible section 1 and provided along the circumferential direction of the raw material accommodating section.
According to the growth device for the silicon carbide single crystal, the feeding hole is formed in the bottom of the crucible, the vertically arranged spiral feeding mechanism enters the raw material accommodating part through the feeding hole, unreacted raw materials can be continuously provided into the crucible through the spiral feeding mechanism, and the size of the grown silicon carbide single crystal is remarkably improved.
When a silicon carbide single crystal is grown by a physical gas phase transport method, silicon elements and silicon-rich atomic groups preferentially escape from raw materials, the raw materials are gradually carbonized (the content of C in the raw materials is higher than that of Si), the raw materials with serious carbonization generate carbon dust, and the carbon dust is deposited on a crystal growth interface along with gas flow, so that the crystal quality is affected. According to the invention, the residual material outlet is arranged on the bottom of the crucible, the spiral feeding mechanism is vertically arranged, the stirring structure is arranged on the spiral feeding mechanism positioned in the raw material accommodating part, the spiral feeding structure drives the stirring structure to rotate, so that residual raw materials which participate in growth in the raw material accommodating part can be transferred into the residual material outlet, and are discharged from the raw material accommodating part of the crucible part.
The main structure for realizing continuous growth is a raw material bin, a growth bin and a recovery bin which are horizontally arranged and communicated with each other, a feeding mechanism feeds silicon carbide polycrystalline raw materials in the raw material bin into the growth bin and feeds residues in the growth bin into the recovery bin, the feeding direction of the feeding mechanism extends along the horizontal direction, the silicon carbide polycrystalline raw materials are heated and sublimated when being conveyed from one end entering the growth bin to one end leaving the growth bin on the feeding mechanism, the raw materials enter the growth bin from the raw material bin through the communicating pipe and enter the recovery bin through the communicating pipe, the raw materials are in the whole process of being horizontally arranged on the feeding mechanism, a heating body cannot directly heat the raw materials entering the growth bin, the heating body is far away from powder materials needing to be heated and sublimated, the heating temperature of the heating body needs to be adjusted to be relatively higher, the silicon carbide raw materials far away from the heating body reach the sublimation temperature, equipment directly heated by the heating body is easy to be subjected to thermal damage, the equipment life is influenced, the raw materials are heated to the sublimation temperature on the feeding mechanism, and the feeding mechanism can cause relatively large thermal damage.
According to the invention, the feeding port and the excess material outlet are positioned on the bottom of the crucible, the heating part is arranged in the circumferential direction of the raw material accommodating part, the raw material to be sublimated in the raw material accommodating part is directly heated by the heating part, so that the heat efficiency of the heating part can be improved, the heat waste is reduced, when the heating body is used for indirectly heating the silicon carbide raw material, the heating body needs to have higher heating temperature to enable the raw material to reach the sublimation temperature, and the directly heated equipment is thermally damaged, so that the service life of the equipment is prolonged.
In some preferred embodiments, the feed port 101 is located in the center of the crucible bottom. In the preferred scheme, the feeding hole 101 is positioned in the center of the bottom of the crucible and is used for feeding from the middle of the bottom of the crucible, so that the silicon carbide raw material is more beneficial to promoting the uniform sublimation, inhibiting the carbonization of the raw material and improving the utilization rate of the silicon carbide raw material, and in the second aspect, the heating part is circumferentially arranged along the outer side of the crucible part, the spiral feeding mechanism 2 is positioned at the center axis position of the crucible part 1, the heating of the spiral feeding mechanism 2 by the heating part can be reduced, the spiral feeding mechanism 2 is more beneficial to avoiding the thermal damage of the spiral feeding mechanism 2, and the service life of the spiral feeding mechanism 2 is prolonged; in the third aspect, the middle part of the feed inlet is fed, so that the replacement of new and old materials from the center to the two sides is facilitated, and the influence of the reacted materials on the crystal growth is reduced.
Preferably, the lower end of the heating part 4 is lower than the crucible bottom. Under this preferred scheme, the lower extreme of heating portion 4 is less than the crucible bottom, and feed inlet 101 is located the central authorities of crucible bottom more do benefit to under the prerequisite that avoids screw feeding mechanism 2 to receive the thermal damage, preheat the raw materials that will get into crucible portion through the feed inlet, promote the raw materials sublimation, improve carborundum raw materials utilization ratio. Optionally, the lower end of the heating part 4 extends to be flush with the inner surface of the crucible wall along the radial direction of the crucible part 1, which is more beneficial to improving the preheating effect of the raw materials.
Preferably, referring to fig. 2, the material stirring structure 3 is an arc material stirring plate arranged along the circumferential direction of the spiral feeding mechanism 2, the bending direction of each arc material stirring plate is the same, the lower surface of each arc material stirring plate is provided with a saw-tooth structure, and the arc material stirring plate is located at the top end of the spiral feeding mechanism 2. The arc-shaped material stirring plates are arranged along the circumferential direction of the spiral feeding mechanism 2, the bending direction of each arc-shaped material stirring plate is clockwise or anticlockwise, and the bending direction of each arc-shaped material stirring plate is the same. Under this preferred scheme, supplementary raw materials gets into from crucible bottom, and arc dials the flitch and is located spiral feeding mechanism 2's top for the raw materials that gets into the crucible carries out sublimation reaction more fully, more does benefit to the improvement carborundum raw materials utilization ratio, dials the flitch for the same arc of crooked direction that sets up along spiral feeding mechanism 2's circumference of material structure 3, more does benefit to and dials the residual raw materials after growing smoothly to clout export 102, and the lower surface that the flitch was dialled to the arc is provided with the cockscomb structure, more does benefit to and dials residual raw materials to clout export 102. Preferably, the ratio of the radial length of the arc stirring plate to the radius of the crucible wall of the crucible portion is 0.9 to 0.95, the residue outlet 102 is arranged at the edge of the bottom of the crucible, the radial length of the arc stirring plate refers to the distance between the end of the arc stirring plate and the central axis of the crucible portion, the raw materials entering the crucible portion are more favorable for fully performing sublimation reaction, and the utilization rate of silicon carbide raw materials is improved. Preferably, the arc-shaped material stirring plates are uniformly arranged along the circumferential direction of the spiral feeding mechanism 2, and the number of the arc-shaped material stirring plates is 2 to 6.
Preferably, referring to fig. 2, on the screw feeding mechanism 2 in the raw material accommodating portion, a blade 5 is provided along a circumferential direction of the screw feeding mechanism 2, the blade 5 is in a straight line shape, and the blade 5 is provided at a lower end of the screw feeding mechanism 2 in the raw material accommodating portion. Under this preferred scheme, in the raw materials holds the lower extreme of screw feeding mechanism 2 in the portion sets up blade 5 along circumference, and when screw feeding mechanism 2 rotatory pay-off, it is rotatory to drive blade 5, can the even raw materials of new replenishment of misce bene and part are through the material of reaction, and the raw materials of new replenishment evenly distributed in the raw materials holds the portion, more does benefit to promoting the abundant reaction sublimation of raw materials, and the heating portion 4 sets up along the outside circumference of crucible portion 1, and blade 5's setting also can even raw materials, more does benefit to the suppression raw materials carbonization, prevents that the carbon dust from following the air current deposit on crystal growth interface to improve crystal quality. The shape of the blades 5 is a straight line shape, which means that each blade 5 is arranged along the radial direction of the raw material containing part, each blade 5 is not bent anticlockwise or clockwise, and the blades 5 are more beneficial to inhibiting the blades 5 from distributing unreacted and sufficient raw materials entering the raw material containing part to the residue outlet 102, so that the raw materials are fully sublimated, and the utilization rate of the silicon carbide raw materials is improved. Preferably, the blades 5 are uniformly arranged along the circumferential direction of the screw feeding mechanism 2, and the number of the blades 5 is 2 to 6.
The blade 5 of the invention is arranged at the lower end of the spiral feeding mechanism 2 in the raw material accommodating part, and when the spiral feeding mechanism 2 rotates for feeding, the blade 5 is driven to rotate, the raw material supplement and the raw material mixing are simultaneously carried out by the power of the spiral feeding mechanism 2, the raw material supplement and the raw material mixing are synchronously carried out without arranging an independent raw material mixing structure, an additional system is not required to control the raw material mixing process, the even distribution of the newly-supplemented raw materials in the raw material accommodating part is facilitated, and the full reaction utilization of the raw materials is promoted. The stirring structure 3 is located on the spiral feeding mechanism 2 in the raw material accommodating portion, when the spiral feeding mechanism 2 rotates, the stirring structure 3 is driven to rotate, raw material supplement, raw material uniform mixing and residual raw material discharge after growth are performed through the power of the spiral feeding mechanism 2, and it can be understood that the rotating speed of the stirring structure 3 can be adjusted through a differential structure, for example, the rotating speed of the stirring structure 3 is enabled to be smaller, the discharge speed of the raw material after growth is reduced, the full sublimation reaction of the silicon carbide raw material is facilitated, and the silicon carbide raw material utilization rate is improved.
According to the invention, the stirring structure 3 is arranged on the spiral feeding mechanism 2 in the raw material accommodating part, the spiral feeding mechanism 2 drives the stirring structure 3 to rotate, residual raw materials after growth in the raw material accommodating part enter the residual material outlet, and the residual raw materials are discharged from the raw material accommodating part in the crucible, so that carbon dust deposition on a crystal growth interface can be inhibited, the crystal quality is influenced, the heating part 4 is circumferentially arranged along the outer side of the crucible part 1, the blades 5 are arranged on the spiral feeding mechanism 2 in the raw material accommodating part, the spiral feeding mechanism 2 drives the blades 5 to rotate, raw materials can be uniformly mixed, carbonization of the raw materials can be more favorably inhibited, and the blades 5 are driven to rotate and the stirring structure 3 is driven to rotate by the spiral feeding mechanism 2, so that the influence of carbonization of the raw materials can be fully reduced, and the crystal quality is improved.
Preferably, the outer end of at least one of said blades 5 is in sliding engagement with the crucible wall of said crucible portion 1. The crucible wall 103 is close to the heating part, a small amount of sediment is easy to adhere to the inner wall of the crucible, the sediment is not easy to remove and discharge, the heating temperature of raw materials close to the inner wall of the crucible is higher than that of raw materials in the middle part, silicon elements and atomic groups rich in silicon are easier to sublimate, a small amount of carbonized raw materials are easy to adhere to the inner wall of the crucible, and a carbonization zone is easy to generate near the inner wall of the crucible. Under this preferred scheme, the outer tip of at least one blade 5 and the crucible wall sliding fit of crucible, when screw feeding mechanism 2 drove blade 5 rotatory, the outer tip of blade 5 slides on the crucible inner wall, can get rid of a small amount of deposit that adheres to on the crucible inner wall, and the carbonization raw materials near the reduction crucible inner wall gets into the surplus material export through stirring structure 3 transfer raw materials after going on growing in the raw materials holding part, can get rid of a small amount of deposit and carbonization raw materials in the crucible portion, more does benefit to improvement crystal quality. The outer end of the blade 5 refers to the end of the blade 5 remote from the screw feed mechanism 2, the free end of the blade 5.
Further preferably, referring to fig. 1, the outer end extends in the axial direction of the crucible wall 103, the extended extension of the outer end being a sliding fit with the crucible wall. The outer end part extends along the axial direction of the crucible wall 103, and the outer end part can extend downwards or upwards or simultaneously extend upwards and downwards.
In some preferred embodiments, the growth device further comprises: a raw material bin 6, which is arranged below the crucible part 1 and is provided with an air inlet 601;
a feeding pipe 7 vertically arranged, the upper end of which is connected to the feeding port 101, the lower end of which is connected to the upper part of the raw material bin 6, and which communicates the raw material accommodating part and the raw material bin 6, and the screw feeding mechanism 2 passes through the feeding pipe 7 from the raw material bin 6 to enter the raw material accommodating part;
a residual bin 8 which is arranged below the crucible part 1 and is provided with an air outlet 801;
and the upper end of the residual material outlet pipe 9 is connected with the residual material outlet 102, the lower end of the residual material outlet pipe is connected with the upper part of the residual material bin 8, and the residual material outlet pipe is communicated with the raw material accommodating part and the residual material bin 8.
Under this preferred scheme, set up the former feed bin 6 that has air inlet 601 in the below of crucible portion 1, through feed tube 7 intercommunication raw materials holding part and former feed bin 6, screw feeding mechanism gets into the raw materials holding part from the former feed bin through the feed tube, the below of crucible portion 1 sets up the surplus storehouse 8 that has gas outlet 801, go out surplus feed tube 9 intercommunication raw materials holding part and surplus storehouse, when the carborundum single crystal grows, let in process gas in the carborundum single crystal growth device through air inlet 601, process gas passes through former feed bin 6, feed tube 7, crucible portion 1, go out surplus feed tube 9, surplus storehouse 8, flow out from the gas outlet 801 on the surplus storehouse 8, more do benefit to the raw materials in promoting crucible portion 1 keeps lasting fluffy state, do benefit to abundant sublimating of raw materials, improve the raw materials utilization ratio, process gas's filling is also more do benefit to promoting raw materials to carry smoothly and get into in the crucible portion 1. The process gas may be nitrogen, argon, or the like.
In some preferred embodiments, the crucible portion 1 includes a crucible wall 103 and a crucible cover 104, wherein a lower portion of the crucible cover 104 is used for mounting seed crystal, the crucible cover 104 covers over the crucible wall 103, and the crucible cover 104 is in a sealed sliding connection with the crucible wall 103. Avoid along with the growth of crystal, the crystal face is close to the raw materials gradually, under this preferred scheme, through crucible cover 104 and crucible wall 103 sealing sliding connection, at the in-process that silicon carbide single crystal grows, can drive the crystal promotion on it through promoting crucible cover 104, along with the promotion of crystal, more do benefit to and avoid the crystal face to be close to the raw materials gradually after, the crystal receives the heating influence of the outside heating portion of crucible portion, the temperature gradient of crystal growth can not satisfy, unable crystallization on the crystal face after the sublimation gas rises, avoid the distance of crystal face and raw materials face too near, lead to the carbon dust to get into the crystal, thereby defect such as inclusion in the silicon carbide crystal is significantly reduced. The crucible cover 104 and the crucible wall 103 can be connected in a sealing and sliding manner by means of the sealing ring 10. A lifting mechanism 11 can be arranged at the center of the top of the crucible cover 104, and the lifting mechanism 11 drives the crucible cover and the crystal to lift. Preferably, the crucible cover 103 is rotatable relative to the crucible wall 104 to facilitate uniform crystal growth of the sublimated gases on the crystal.
When the growth device of the silicon carbide single crystal is used, the crucible part 1, the spiral feeding structure 2 and the stirring structure 3 can be assembled together, the heating part 4 is arranged on the outer circumference of the raw material containing part, a certain amount of raw materials are conveyed into the crucible part 1 through the spiral feeding structure 2, the temperature is increased for growth of the silicon carbide crystal, the spiral feeding structure 2 rotates to drive the stirring structure 3 to rotate during crystal growth, the stirring structure 3 transfers residual raw materials after growth in the raw material containing part, the residual raw materials enter the residual material outlet 102, residual raw materials are discharged from the raw material containing part of the crucible part 1, the spiral feeding structure 2, the stirring structure 3 and the blades 4 can be assembled together, during crystal growth, the spiral feeding structure 2 rotates to drive the stirring structure 3 and the blades 4 to transfer residual raw materials after growth in the raw material containing part, the blades 4 are uniformly mixed, the crucible part 1, the spiral feeding structure 2, the stirring structure 3, the blades 4, the raw material bin 6, the material bin 7, the material bin 8, the residual material 9 and the residual material lifting structure 3 can be assembled together, the crucible part 11 can be lifted up and the residual material lifting structure 3, and the residual material lifting structure 11 can be rotated during crystal growth, and the residual material lifting structure 11 can be assembled together, and the residual material can be lifted and the material in the crucible part 11.
In a second aspect, the present invention provides a method for growing a silicon carbide single crystal performed in the apparatus for growing a silicon carbide single crystal according to the first aspect, the method comprising: the vertical screw feeding mechanism 2 conveys silicon carbide polycrystalline raw materials to the raw material accommodating part from the feeding port 101 at the bottom of the crucible, and the stirring structure 3 on the screw feeding mechanism 2 in the raw material accommodating part distributes the residual raw materials after growth in the raw material accommodating part to the residual material outlet 102 at the bottom of the crucible. In the growth method of the invention, unreacted silicon carbide polycrystalline raw material is continuously supplied into the crucible part 1 through the screw feeding mechanism 2, the size of the grown silicon carbide single crystal can be increased, residual raw material after growth in the raw material accommodating part is discharged through the stirring structure 3, carbon dust deposition on a crystal growth interface can be inhibited, the thermal efficiency of the heating part can be improved, the heat waste is reduced, the service lives of the crucible and the feeding mechanism are prolonged, the reaction of the raw material is more uniform, and the growth efficiency of the silicon carbide single crystal is improved through feeding from the bottom of the crucible and discharging the residual material from the bottom of the crucible.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
1. A growth apparatus for a bottom-feed silicon carbide single crystal, comprising:
the crucible part (1) is provided with a raw material accommodating part at the lower part and comprises a crucible bottom, wherein a feed inlet (101) and a residue outlet (102) are arranged on the crucible bottom;
a screw feeding mechanism (2) which is vertically arranged and enters the raw material accommodating part through the feeding port (101);
a stirring structure (3) which is positioned on the spiral feeding mechanism (2) in the raw material accommodating part and used for stirring the residual raw materials after growth in the raw material accommodating part to the residual material outlet (102);
and a heating unit (4) provided outside the crucible unit (1) and provided in the circumferential direction of the raw material accommodating unit.
2. A growth device according to claim 1, characterized in that the feed opening (101) is located in the centre of the crucible bottom.
3. A growing device according to claim 2, characterized in that the lower end of the heating part (4) is lower than the crucible bottom.
4. The growth device according to claim 2, wherein the material stirring structure (3) is an arc-shaped material stirring plate arranged along the circumferential direction of the spiral feeding mechanism (2), the bending direction of each arc-shaped material stirring plate is the same, the lower surface of each arc-shaped material stirring plate is provided with a saw-tooth-shaped structure, and the arc-shaped material stirring plates are positioned at the top end of the spiral feeding mechanism (2).
5. The growing apparatus according to claim 2 or 4, wherein a blade (5) is provided on the screw feeding mechanism (2) in the raw material accommodating portion in the circumferential direction of the screw feeding mechanism (2), the blade (5) is in a straight line shape, and the blade (5) is provided at the lower end of the screw feeding mechanism (2) in the raw material accommodating portion.
6. A growing device according to claim 5, characterized in that the outer end of at least one of the blades (5) is in sliding engagement with the crucible wall of the crucible portion (1).
7. A growth device as claimed in claim 6, wherein the outer end portion extends in an axial direction of the crucible wall, the extended extension of the outer end portion being a sliding fit with the crucible wall.
8. The growth device of claim 1, further comprising:
a raw material bin (6) which is arranged below the crucible part (1) and is provided with an air inlet (601);
the feeding pipe (7) is vertically arranged, the upper end of the feeding pipe is connected with the feeding hole (101), the lower end of the feeding pipe is connected with the upper part of the raw material bin (6) and is communicated with the raw material accommodating part and the raw material bin (6), and the spiral feeding mechanism (2) enters the raw material accommodating part from the raw material bin (6) through the feeding pipe (7);
the surplus bin (8) is arranged below the crucible part (1) and is provided with an air outlet (801);
and the upper end of the residual discharging pipe (9) is connected with the residual discharging outlet (102), the lower end of the residual discharging pipe is connected with the upper part of the residual discharging bin (8), and the residual discharging pipe is communicated with the raw material containing part and the residual discharging bin (8).
9. The growth device according to claim 1, wherein the crucible portion (1) comprises a crucible wall (103) and a crucible cover (104), the lower part of the crucible cover (104) is used for installing seed crystals, the crucible cover (104) covers the upper part of the crucible wall (103), and the crucible cover (104) is in sealing sliding connection with the crucible wall (103).
10. A growth method of a silicon carbide single crystal, characterized in that it is performed in the growth apparatus of a silicon carbide single crystal according to any one of claims 1 to 9, the growth method comprising: the vertical screw feeding mechanism (2) is used for conveying silicon carbide polycrystalline raw materials to the raw material accommodating part from a feed inlet (101) at the bottom of the crucible, and the stirring structure (3) on the screw feeding mechanism (2) in the raw material accommodating part is used for stirring residual raw materials after growth in the raw material accommodating part to a residual material outlet (102) at the bottom of the crucible.
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