CN117822120A - Device and method for growing silicon carbide monocrystal by resistance method with adjustable local heating value - Google Patents
Device and method for growing silicon carbide monocrystal by resistance method with adjustable local heating value Download PDFInfo
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- CN117822120A CN117822120A CN202410232273.2A CN202410232273A CN117822120A CN 117822120 A CN117822120 A CN 117822120A CN 202410232273 A CN202410232273 A CN 202410232273A CN 117822120 A CN117822120 A CN 117822120A
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 182
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 44
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 377
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 377
- 239000010439 graphite Substances 0.000 claims abstract description 377
- 239000013078 crystal Substances 0.000 claims abstract description 139
- 239000002994 raw material Substances 0.000 claims abstract description 36
- 239000002184 metal Substances 0.000 claims description 6
- 230000004308 accommodation Effects 0.000 claims description 2
- 230000020169 heat generation Effects 0.000 claims 1
- 230000000630 rising effect Effects 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 11
- 239000007789 gas Substances 0.000 description 11
- 229910052710 silicon Inorganic materials 0.000 description 11
- 239000010703 silicon Substances 0.000 description 11
- 238000000859 sublimation Methods 0.000 description 6
- 230000008022 sublimation Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000009286 beneficial effect Effects 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
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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Abstract
The invention belongs to the field of silicon carbide crystal growth, and relates to a device and a method for growing silicon carbide single crystals by a resistance method with adjustable local heating value, wherein the device comprises a graphite heating component outside a crucible part, and the heating component comprises: the graphite heating body comprises a plurality of graphite heating parts which are arranged along the axial direction of the crucible part, the graphite heating parts are provided with lower ends which are close to the raw material containing parts and upper ends which are close to the top of the crucible part, the plurality of graphite heating parts are distributed along the periphery of the crucible part, the adjacent graphite heating parts are separated and integrally connected, the integral connection is a first connection or a second connection, the first connection is the integral connection of the upper ends of the adjacent graphite heating parts, the second connection is the integral connection of the lower ends of the adjacent graphite heating parts, and the first connection and the second connection are arranged at intervals; the graphite slide block is arranged on the graphite heating part and is in sliding connection with the heating part, and the graphite slide block slides along the axial direction of the crucible part relative to the graphite heating part, so that the temperature gradient can be regulated in the crystal growth process, and the crystal quality is improved.
Description
Technical Field
The invention belongs to the technical field of silicon carbide crystal growth, and particularly relates to a device and a method for growing silicon carbide single crystals by a resistance method with adjustable local heating value.
Background
Physical Vapor Transport (PVT) is the main method for industrially growing silicon carbide crystals at present, specifically, a silicon carbide 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, a heating body outside the graphite crucible heats to sublimate and decompose the silicon carbide raw material in the graphite crucible, and sublimate and decompose gas grows on the silicon carbide seed crystal to obtain a silicon carbide single crystal.
When the silicon carbide crystal grows, the temperature in the crucible from the silicon carbide raw material to the seed crystal gradually decreases, and a certain temperature gradient is formed. Due to the existence of the temperature gradient, the sublimated and decomposed gas of the silicon carbide raw material grows on the silicon carbide seed crystal to obtain the silicon carbide single crystal. In the growth process, if the temperature field distribution is unreasonable, the growth rate is nonuniform, the morphology and quality of the crystal are affected, in addition, the unreasonable temperature field distribution can also cause stress in the crystal, and adverse effects are caused on the quality and stability of the crystal.
The resistance heating mode adopted in the current industry is generally that a graphite heating body in an integrated mode is arranged outside a graphite crucible to heat the graphite crucible, and the heating value of the graphite heating body is taken as a whole and cannot be locally adjusted, so that great limitation is brought to the accurate adjustment of the temperature field of a growth device.
Disclosure of Invention
The invention aims to overcome the defect that the heating value of a graphite heating element outside a graphite crucible cannot be locally adjusted and the accurate adjustment of a temperature field is limited in the prior art, and provides a device and a method for growing silicon carbide single crystals by a resistance method with adjustable local heating value, which can locally adjust the heating value of a graphite heating element outside the crucible and are beneficial to adjusting the temperature field of a growing device.
In order to achieve the above object, in a first aspect, the present invention provides an apparatus for growing a silicon carbide single crystal by a resistance method with an adjustable local heating value, comprising a crucible portion, a raw material accommodating portion is provided at a lower portion of the crucible portion, a top lower surface of the crucible portion is used for mounting a seed crystal, and further comprising a graphite heating component, the graphite heating component is provided at an outer side of the crucible portion, the graphite heating component comprises:
the graphite heating body comprises a plurality of graphite heating parts which are arranged along the axial direction of the crucible part, wherein each graphite heating part is provided with a lower end close to the raw material containing part and an upper end close to the top of the crucible part, a plurality of graphite heating parts are distributed along the periphery of the crucible part, gaps are reserved between the adjacent graphite heating parts, the adjacent graphite heating parts are integrally connected, the integral connection is a first connection or a second connection, the first connection is the upper end integral connection of the adjacent graphite heating parts, the second connection is the lower end integral connection of the adjacent graphite heating parts, the first connection and the second connection are arranged at intervals, and the plurality of graphite heating parts are sequentially connected through the first connection and the second connection;
and the graphite sliding block is arranged on the graphite heating part and is in sliding connection with the graphite heating part, and slides along the axial direction of the crucible part relative to the graphite heating part.
In some preferred embodiments, the graphite slide is provided with a concave part, the inner contour shape of the concave part is matched with the outer contour shape of the graphite heating part, the graphite heating part is embedded in the concave part, and the graphite slide wraps the edges of the outer wall, the side wall and the inner wall of the graphite heating part.
Preferably, the graphite slide block is formed by splicing a first graphite slide block and a second graphite slide block, the concave part comprises a left half concave part and a right half concave part, the inner contour of the first graphite slide block and the inner contour of the second graphite slide block respectively form the left half concave part and the right half concave part, and the inner contour of the first graphite slide block and the inner contour of the second graphite slide block are spliced to form the concave part.
Preferably, the graphite slide block is provided with a threaded through hole, the threaded through hole is arranged along the axial direction of the crucible part and is formed by splicing a first threaded through hole and a second threaded through hole, and the first threaded through hole and the second threaded through hole are respectively arranged on the first graphite slide block and the second graphite slide block;
the growth device further comprises a connecting shaft which is arranged along the axial direction of the crucible portion, one end of the connecting shaft is fixedly connected with the graphite slide block through the threaded through hole, the other end of the connecting shaft is fixedly connected with the mechanical driving assembly, and the connecting shaft comprises an insulating shaft section.
Preferably, the outer wall of the first graphite slide block and the outer wall of the second graphite slide block are respectively provided with protrusions, and the first threaded through hole and the second threaded through hole are respectively arranged on the protrusions of the first graphite slide block and the protrusions of the second graphite slide block.
Preferably, the connecting shaft comprises a first connecting shaft section, which is a graphite connecting shaft section, and one end of the first connecting shaft section is fixedly connected with the graphite sliding block;
and one end of the second connecting shaft section is fixedly connected with the other end of the first connecting shaft section, the second connecting shaft section comprises a metal connecting shaft section and an insulating shaft section, and the other end of the second connecting shaft section is fixedly connected with the mechanical driving assembly.
In some preferred embodiments, the surface of the graphite slider in sliding contact with the graphite heat-generating part is lined with graphite paper.
In some preferred embodiments, each graphite heat-generating part is provided with a graphite slider, and each graphite slider slides independently relative to the corresponding graphite heat-generating part.
In a second aspect, the present invention provides a method for growing a silicon carbide single crystal using the apparatus according to the first aspect, wherein the growth process includes a temperature increasing stage, a crystal growth stage, and a growth end stage, and in the crystal growth stage, the graphite slider is slid along the axial direction of the crucible portion relative to the graphite heating portion, and the local heating value of the graphite heating component outside the crucible portion is adjusted.
In some preferred embodiments, the crystal growth stage includes a crystal growth stage early stage, a crystal growth stage middle stage and a crystal growth stage late stage, in the crystal growth stage early stage, the graphite slide block is located at a first preset position, a distance between the first preset position and the lower end of the graphite heating part is 0.1-0.4 times of the height of the graphite heating part, in the crystal growth stage middle stage and the crystal growth stage late stage, the graphite slide block is moved up to a second preset position, and a distance between the second preset position and the lower end of the graphite heating part is 0.6-0.8 times of the height of the graphite heating part.
Preferably, in the early stage of the crystal growth stage, the graphite slide blocks on each graphite heating part are located at the first preset position, in the middle stage of the crystal growth stage, part of the graphite slide blocks uniformly distributed along the circumferential direction of the crucible part are moved up to the second preset position at a first preset speed, and in the later stage of the crystal growth stage, the rest of the graphite slide blocks located at the first preset position are moved up to the second preset position at the first preset speed, wherein the first preset speed is 2 mm/h-5 mm/h.
The graphite heating body comprises a plurality of graphite heating parts arranged along the axial direction of a crucible part, the graphite heating parts are provided with lower ends close to a raw material containing part and upper ends close to the top of the crucible part, the graphite heating parts are distributed along the periphery of the crucible part, a gap is reserved between the adjacent graphite heating parts, the adjacent graphite heating parts are integrally connected, the integral connection is a first connection or a second connection, the first connection is the upper ends of the adjacent graphite heating parts and the second connection is the lower ends of the adjacent graphite heating parts and are integrally connected, the first connection and the second connection are arranged at intervals, the graphite heating parts are sequentially connected with the graphite heating parts through the first connection and the second connection, a graphite sliding block which is in sliding connection with the graphite heating parts is arranged on the graphite heating parts, the graphite heating components outside the crucible consist of the graphite heating parts and the graphite sliding blocks which are arranged along the axial direction of the crucible part, the graphite sliding blocks slide along the axial direction of the crucible part relative to the graphite heating parts, the local resistance of the graphite sliding blocks is reduced, the graphite sliding blocks outside the graphite sliding blocks at the position of the graphite sliding blocks can be arranged along the axial direction of the crucible part, the graphite sliding blocks can be realized, the heating blocks at the local silicon crystal heating blocks can be heated, the silicon crystal growth heating effect can be reduced, the silicon crystal growth heating effect can be accurately adjusted, and the silicon carbide crystal growth heating quality can be improved, and the silicon carbide growth temperature can be grown in the growth process can be adjusted.
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 of a graphite heating element according to an embodiment of the present invention.
Fig. 2 is a schematic structural view of one embodiment of a graphite heat-generating component of the present invention.
FIG. 3 is a top cross-sectional view of one embodiment of a graphite heat generating component of the present invention.
Fig. 4 is an enlarged view of a portion of the graphite slider of fig. 3 where it is mated with a graphite heat generating portion.
FIG. 5 is a schematic view of a graphite slider of an embodiment of the present invention.
Description of the reference numerals
1. A graphite heating part; 2. a graphite slide block; 201. a concave portion; 2011. a left half recess; 2012. a right half recess; 202. a first graphite slide; 203. a second graphite slide; 204. a threaded through hole; 2041. a first threaded through hole; 2042. a second threaded through hole; 205. a protrusion; 3. a connecting shaft; 301. a first connecting shaft section; 302. a second connecting shaft section; 4. a mechanical drive assembly.
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, lower, left, right" and "upper" are used generally to refer to the orientation understanding shown in the drawings and in practice, and "inner, outer" are intended to refer to the inner, outer of the outline of the component.
In the description of the present invention, it should be understood that the terms "center," "upper," "lower," "front," "rear," "left," "right," "top," "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 specific orientation, be configured and operated in a specific 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," "secured," and the like are to be construed broadly and include, for example, either fixedly attached, detachably attached, or integrally formed; 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," "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.
The inventor of the present invention researches and discovers that the resistance heating mode adopted in the current industry is generally that an integrated graphite heating body arranged outside a graphite crucible heats the graphite crucible, and the heating value of the graphite heating body is taken as a whole, can not be locally adjusted, and brings great limitation to the accurate adjustment of the temperature field of a growth device.
In a first aspect, the present invention provides an apparatus for growing a silicon carbide single crystal by a resistance method with an adjustable local heating value, comprising: the crucible portion, the lower part of crucible portion is provided with raw materials accommodation portion, the top lower surface of crucible portion is used for installing the seed crystal, still includes graphite heating element, graphite heating element set up in the outside of crucible portion, graphite heating element includes:
the graphite heating body comprises a plurality of graphite heating parts 1 arranged along the axial direction of the crucible part, wherein each graphite heating part 1 is provided with a lower end close to a raw material containing part and an upper end close to the top of the crucible part, the plurality of graphite heating parts 1 are distributed along the periphery of the crucible part, a space is reserved between the adjacent graphite heating parts 1, the adjacent graphite heating parts 1 are integrally connected, the integral connection is a first connection or a second connection, the first connection is the integral connection of the upper ends of the adjacent graphite heating parts 1, the second connection is the integral connection of the lower ends of the adjacent graphite heating parts 1, the first connection and the second connection are arranged at intervals, and the plurality of graphite heating parts 1 are sequentially connected through the first connection and the second connection;
and a graphite slider 2 which is provided on the graphite heat-generating part 1 and is slidably connected to the graphite heat-generating part 1, and which slides in the axial direction of the crucible part with respect to the graphite heat-generating part 1.
The silicon carbide single crystal growth device comprises a crucible part, wherein a raw material containing part and a seed crystal are arranged at the lower part of the crucible part, a graphite heating component is arranged at the outer part of the crucible part, the graphite heating component comprises a graphite heating body and a graphite sliding block, the graphite heating body comprises a plurality of graphite heating parts arranged along the axial direction of the crucible part, the graphite heating parts are provided with lower ends close to the raw material containing part and upper ends close to the top of the crucible part, the graphite heating parts are distributed along the periphery of the crucible part, an interval is reserved between the adjacent graphite heating parts, the adjacent graphite heating parts are integrally connected and are integrally connected into a first connection or a second connection, the first connection is integrally connected with the upper ends of the adjacent graphite heating parts, the second connection is integrally connected with the lower ends of the adjacent graphite heating parts, the first connection and the second connection are arranged at intervals, the graphite sliding block is arranged on the graphite heating parts and is in sliding connection with the graphite heating parts, the graphite sliding block relatively to the graphite heating parts along the axial direction of the crucible part, a pair of electrodes are connected onto the graphite heating parts, the current direction of the graphite heating parts is the graphite heating parts along the axial direction of the graphite heating parts, the graphite heating parts is in the direction of the graphite heating parts, the graphite heating parts can be in the direction of the graphite heating parts, the silicon crystal can be locally grown in the axial direction of the graphite heating parts, and the silicon crystal can be locally in the silicon crystal growth position of the silicon crystal can be accurately adjusted, and the silicon crystal can be locally in the position of the silicon crystal growth device, and the temperature can be adjusted, and the temperature can be locally, and the silicon crystal can be grown, and the silicon crystal can be can easily and the temperature can be easily and has a high.
The first connection and the second connection interval arrangement means a plurality of adjacent graphite heating parts, the upper end of the first graphite heating part is integrally connected with the upper end of the second graphite heating part, the lower end of the second graphite heating part is integrally connected with the lower end of the third graphite heating part, the upper end of the third graphite heating part is integrally connected with the upper end of the fourth graphite heating part, and so on.
The graphite slide block of the present invention is disposed on the graphite heat-generating part and is slidably connected to the graphite heat-generating part, and the manner of slidably connecting the graphite slide block and the graphite heat-generating part is not particularly limited, and the specific structure of the graphite slide block on the graphite heat-generating part is not particularly limited, and for example, the graphite slide block may be sheathed in the circumferential direction of the graphite heat-generating part, and the graphite slide block may be slidably connected to one surface of the graphite heat-generating part, or the like. In some preferred embodiments, referring to fig. 3 and 4, the graphite slider 2 is provided with a recess 201, the inner contour shape of the recess 201 matches the outer contour shape of the graphite heat-generating part 1, the graphite heat-generating part 1 is embedded in the recess 201, and the graphite slider 2 wraps the edges of the outer wall, the side wall and the inner wall of the graphite heat-generating part 1. According to the technical scheme, a concave part is arranged on a graphite sliding block, the inner outline shape of the concave part is matched with the outer outline shape of a graphite heating part, the graphite sliding block wraps the outer wall, the side wall and the edge of the inner wall of the graphite heating part, the graphite heating part is embedded into the concave part, the stability of sliding connection between the graphite sliding block and the graphite heating part is facilitated, the graphite sliding block and the graphite heating part are prevented from being separated, the graphite sliding block slides stably along the axial direction of a crucible part relative to the graphite heating part on the graphite heating part, the outer wall of the graphite heating part refers to one side of the graphite heating part, which is far away from the crucible part, of the graphite sliding block, the inner wall of the graphite heating part refers to one side, close to the crucible part, of the graphite sliding block wraps the inner wall of the graphite heating part, the graphite sliding block does not completely wrap the inner wall of the graphite heating part, and only covers the left side and right sides of the inner wall.
Preferably, referring to fig. 5, the graphite slide 2 is formed by splicing a first graphite slide 202 and a second graphite slide 203, the concave portion includes a left half concave portion 2011 and a right half concave portion 2012, the inner contour of the first graphite slide 202 and the inner contour of the second graphite slide 203 respectively form the left half concave portion 2011 and the right half concave portion 2012, and the inner contour of the first graphite slide 202 and the inner contour of the second graphite slide 203 are spliced to form the concave portion 201. Under this preferred scheme, graphite slider is by first graphite slider and second graphite slider concatenation formation, and the interior profile of first graphite slider and the interior profile of second graphite slider constitute left half concave part and right half concave part respectively, and the interior profile of first graphite slider and the interior profile concatenation of second graphite slider form the concave part, more do benefit to the installation of graphite slider. The invention does not limit the splicing mode of the first graphite slide block 202 and the second graphite slide block 203, and the first graphite slide block 202 and the second graphite slide block 203 are fixedly connected.
Further preferably, referring to fig. 2, 4 and 5, the graphite slide 2 is provided with a threaded through hole 204, which is disposed along the axial direction of the crucible portion and is formed by splicing a first threaded through hole 2041 and a second threaded through hole 2042, and the first threaded through hole 2041 and the second threaded through hole 2042 are respectively disposed on the first graphite slide 202 and the second graphite slide 203;
the growth device further comprises a connecting shaft 3 which is arranged along the axial direction of the crucible portion, one end of the connecting shaft is fixedly connected with the graphite slide block 2 through the threaded through hole 204, the other end of the connecting shaft is fixedly connected with the mechanical driving assembly 4, and the connecting shaft comprises an insulating shaft section.
Under this preferred scheme, set up first screw thread through-hole on the first graphite slider, set up the second screw thread through-hole on the second graphite slider, screw thread through-hole that the axial direction along crucible portion that sets up on first screw thread through-hole and the second screw thread through-hole concatenation formed the graphite slider set up, growing device still includes the connecting axle that sets up along the axial direction of crucible portion, screw thread through-hole and graphite slider fixed connection are passed through to the one end of connecting axle, the other end and the mechanical drive subassembly fixed connection of connecting axle, the connecting axle can play the effect of fixed connection first graphite slider and second graphite slider simultaneously and will set up the mechanical drive subassembly's outside the growth cavity power transmission for the graphite slider, promote the relative graphite portion of generating heat of graphite slider along the gliding effect of the axial direction of crucible portion. The insulating shaft section is arranged on the connecting shaft, and because the insulating shaft section is arranged, the use of a mechanical driving component cannot be influenced by current in the graphite heating component formed by the graphite heating body and the graphite sliding block, the work of the graphite heating component cannot be influenced by the connecting shaft and the mechanical driving component, and the current only flows through the graphite heating body and the graphite sliding block. The mechanical driving component of the invention can be a cylinder, a motor and the like.
The arrangement mode of the threaded through holes is not particularly limited, and specifically, for example, the first threaded through hole and the second threaded through hole may be respectively arranged in the first graphite slide block and the second graphite slide block, which is equivalent to directly punching holes on the first graphite slide block and the second graphite slide block, preferably, the outer wall of the first graphite slide block 202 and the outer wall of the second graphite slide block 203 are respectively provided with a protrusion 205, and the first threaded through hole 2041 and the second threaded through hole 2042 are respectively arranged on the protrusion 205 of the first graphite slide block 202 and the protrusion 205 of the second graphite slide block 203, which is more favorable for the fixed connection of the connecting shaft 3 and the graphite slide block 2.
The invention does not limit the form of the connecting shaft 3, preferably, the connecting shaft 3 comprises a first connecting shaft section 301, which is a graphite connecting shaft section, and one end of the first connecting shaft section is fixedly connected with the graphite sliding block 2; and one end of the second connecting shaft section 302 is fixedly connected with the other end of the first connecting shaft section 301, the second connecting shaft section comprises a metal connecting shaft section and the insulating shaft section, and the other end of the second connecting shaft section is fixedly connected with the mechanical driving assembly 4. Under this preferred scheme, the connecting axle includes the first connecting axle section of graphite connecting axle section form, graphite connecting axle section form first connecting axle section and graphite slider fixed connection, more do benefit to the connection of connecting axle and graphite slider, the connecting axle includes second connecting axle section, the second connecting axle section includes metal connecting axle section and insulating axle section, more do benefit to the connection of connecting axle and mechanical drive subassembly, the insulating axle section of this invention sets up on the second connecting axle section, more do benefit to the selection that prevents high temperature influence insulating axle section material, preferably, the one end of metal connecting axle section and the other end fixed connection of first connecting axle section, the other end of metal connecting axle section and the one end fixed connection of insulating axle section, the other end and the mechanical drive subassembly fixed connection of insulating axle section, more do benefit to the selection that prevents high temperature influence insulating axle section material.
In some preferred embodiments, the surface of the graphite slider 2 in sliding contact with the graphite heat-generating part 1 is lined with graphite paper. Under the preferred scheme, through lining graphite paper, more be favorable to reducing the contact clearance of graphite heating portion and graphite slider and restrain the wearing and tearing of graphite slider and graphite heating portion.
In some preferred embodiments, each graphite heat generating part 1 is provided with the graphite slide 2, and each graphite slide 2 slides independently relative to the corresponding graphite heat generating part 1. Under this preferred scheme, all set up graphite slider on every graphite portion that generates heat, every graphite slider is relative to the graphite portion that generates heat that corresponds independently slides, can the local adjustment be located the arbitrary position of the graphite heating element of the outside of crucible portion generate heat, and the calorific capacity of the graphite heating element of graphite slider place position is low, and the heating capacity of the graphite heating element that does not have graphite slider position is high, more does benefit to the temperature of nimble adjustment carborundum raw materials department and seed crystal department, accurate adjustment carborundum single crystal growth device's temperature field, improves crystal quality.
In some preferred embodiments, the plurality of graphite heating parts 1 have the same structure, and the graphite heating parts 1 are uniformly distributed along the outer circumference of the crucible part, and it is understood that the number of the graphite heating parts is not limited in the present invention, and may be 6, 8, 10, 12, etc.
In a second aspect, the present invention provides a method for growing a silicon carbide single crystal using the apparatus according to the first aspect, wherein the growth process comprises a temperature increasing stage, a crystal growth stage and a growth end stage, and in the crystal growth stage, the graphite slider 2 is slid relative to the graphite heating part 1 along the axial direction of the crucible part, and the local heating value of the graphite heating component outside the crucible part is adjusted. According to the growth method of the silicon carbide single crystal, in the crystal growth stage, the local heating value of the graphite heating component outside the crucible part is adjusted, so that the temperatures of the silicon carbide raw material and the seed crystal can be locally adjusted, the temperature field of the silicon carbide single crystal growth device can be accurately adjusted, and the crystal quality is improved.
In some preferred embodiments, the crystal growth stage includes a crystal growth stage early stage, a crystal growth stage middle stage, and a crystal growth stage late stage, in which the graphite slide 2 is located at a first preset position, a distance between the first preset position and the lower end of the graphite heat-generating part 1 is 0.1 to 0.4 times the height of the graphite heat-generating part 1, and in which the graphite slide 2 is moved up to a second preset position, a distance between the second preset position and the lower end of the graphite heat-generating part 1 is 0.6 to 0.8 times the height of the graphite heat-generating part 1. In the earlier stage of the crystal growth stage, the sublimated raw materials are sufficient, the concentration of sublimated gas in the crucible part is high, under the preferred scheme, in the earlier stage of the crystal growth stage, the graphite slide block is positioned at a first preset position, the distance between the first preset position and the lower end of the graphite heating part is 0.1-0.4 times of the height of the graphite heating part 1, the graphite slide block is close to the silicon carbide raw materials, the heating temperature of the silicon carbide raw materials can be reduced, and the sublimation rate of the raw materials and the growth rate of crystals are controlled. Along with the progress of crystal growth process, the raw materials that can sublimate reduces gradually, the concentration of the sublimation gas in the crucible reduces gradually, under this preferred scheme, crystal growth stage middle stage and crystal growth stage later stage, make the graphite slider move up to the second and predetermine the position, the distance of second predetermine the position and the lower extreme of graphite portion of generating heat is the high 0.6 times ~0.8 times of graphite portion of generating heat, crystal growth stage middle stage and crystal growth stage later stage, graphite slider rises to being close to seed crystal department, can improve the heating temperature of carborundum raw materials, accelerate raw materials sublimation rate, reduce the temperature of seed crystal department, improve the rate that sublimates gas and condense at crystal department, improve crystal growth rate. Under the preferred scheme, the graphite slide block 2 is positioned at a first preset position at the early stage of the crystal growth stage, the graphite slide block 2 is upwards moved to a second preset position at the middle stage of the crystal growth stage and the later stage of the crystal growth stage, the growth rate is aligned more favorably in the whole crystal growth stage, the crystal grows steadily, and the form and quality of the crystal are ensured.
The specific process of moving the graphite slide block 2 up to the second preset position in the middle and later stages of the crystal growth stage is not limited, and the graphite slide block can be moved up to the middle position of the graphite heating part in the middle stage of the crystal growth stage, and the graphite slide block can be further moved up to the second preset position in the later stage of the crystal growth stage. In some preferred embodiments, the graphite slide blocks 2 on each graphite heat generating part 1 are located at the first preset position in the early stage of the crystal growth stage, the graphite slide blocks 2 uniformly distributed along the circumferential direction of the crucible part are moved up to the second preset position at a first preset speed in the middle stage of the crystal growth stage, and the rest of the graphite slide blocks 2 located at the first preset position are moved up to the second preset position at the first preset speed in the later stage of the crystal growth stage, wherein the first preset speed is 2mm/h to 5mm/h. Under this preferred scheme, when all setting up graphite slider on every graphite heating portion, in the long brilliant phase earlier stage, make the graphite slider on every graphite heating portion be located first default position, more do benefit to the heating temperature that reduces the carborundum raw materials, control the sublimation rate of raw materials and the growth rate of crystal. Compared with the earlier stage of the crystal growth stage, the sublimated raw material in the middle stage of the crystal growth stage is reduced, the concentration of sublimated gas is reduced, the part which is uniformly distributed along the circumferential direction of the crucible part is enabled to be upwards moved to a second preset position in the middle stage of the crystal growth stage, the heating temperature of the silicon carbide raw material can be improved, the sublimation rate of the raw material is improved, the temperature of a seed crystal is reduced, the condensation rate of the sublimated gas at a crystal position is improved, the crystal growth rate is improved, the sublimated raw material is gradually reduced in the middle stage of the crystal growth stage, the concentration of the sublimated gas is gradually reduced, the part which is uniformly distributed along the circumferential direction of the crucible part is enabled to be upwards moved to the second preset position in the middle stage of the crystal growth stage at the speed of 2 mm/h-5 mm/h, the heating temperature of the silicon carbide raw material is gradually improved in the middle stage of the crystal growth stage, and the temperature of the seed crystal position is gradually reduced. Compared with the middle stage of the crystal growth stage, the sublimated raw material is further reduced in the later stage of the crystal growth stage, the concentration of sublimated gas is further reduced, the residual graphite slide block 2 positioned at the first preset position is enabled to move upwards to the second preset position in the later stage of the crystal growth stage, the heating temperature of the silicon carbide raw material can be further improved, the sublimation rate of the raw material is improved, the temperature of a seed crystal is further reduced, the condensation rate of the sublimated gas at the crystal position is improved, the crystal growth rate is improved, the sublimated raw material is gradually reduced in the later stage of the crystal growth stage, the concentration of the sublimated gas is gradually reduced, the residual graphite slide block 2 positioned at the first preset position is enabled to move upwards to the second preset position at the speed of 2-5 mm/h in the later stage of the crystal growth stage, the heating temperature of the silicon carbide raw material is more favorably improved gradually in the later stage of the crystal growth stage, and the temperature of the seed crystal is lowered gradually. According to the preferred scheme, at the early stage of the crystal growth stage, the graphite slide blocks on each graphite heating part are located at the first preset position, at the middle stage of the crystal growth stage, part of the graphite slide blocks uniformly distributed along the circumferential direction of the crucible part are moved upwards to the second preset position at the first preset speed, at the later stage of the crystal growth stage, the rest graphite slide blocks located at the first preset position are moved upwards to the second preset position at the first preset speed, the first preset speed is 2-5 mm/h, the crystal growth rate is aligned in the whole crystal growth stage, the crystal grows steadily, and the form and quality of the crystal are guaranteed.
Preferably, in the heating stage, a crucible filled with silicon carbide raw materials and seed crystals is placed in a silicon carbide growing furnace, after vacuumizing, nitrogen and argon are introduced into a furnace shell cavity of the silicon carbide growing furnace, so that the pressure in the furnace shell cavity reaches 10000 Pa-20000 Pa, the power of a graphite heating body is regulated to enable the temperature of the crucible to reach 2100 ℃ to 2300 ℃, the pressure in the furnace shell cavity is controlled to be reduced to 200 Pa-1000 Pa, in the crystal growing stage, the pressure in the furnace shell cavity in the growing furnace is stabilized at 200 Pa-1000 Pa, the temperature of the crucible is stabilized at 2100 ℃ to 2300 ℃, the time in the early stage of the crystal growing stage is 10 h-15 h, the time in the middle stage of the crystal growing stage is 40 h-50 h, the time in the later stage of the crystal growing stage is 30 h-40 h, the pressure in the furnace shell cavity of the silicon carbide growing furnace is increased to 500 Pa-700 Pa, and the temperature of the crucible is reduced to 800 ℃ to 900 ℃ at the end of the crystal growing stage. The control of pressure, temperature and time of each growth stage is more beneficial to the stable growth of crystals and ensures the form and quality of crystals.
Preferably, in the middle of the crystal growth stage, the graphite slide block 2 with the 1/3~3/5 ratio uniformly distributed along the radial direction of the crucible part moves upwards to the second preset position at the first preset speed, which is more beneficial to the alignment of the growth speed and the stable growth of crystals in the whole crystal growth stage, and ensures the form and quality of the crystals.
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 (11)
1. The utility model provides a device of resistance method growth carborundum single crystal of adjustable local calorific capacity, includes crucible portion, the lower part of crucible portion is provided with raw materials accommodation portion, the top lower surface of crucible portion is used for installing the seed crystal, still includes graphite heating element, graphite heating element set up in the outside of crucible portion, its characterized in that, graphite heating element includes:
the graphite heating body comprises a plurality of graphite heating parts (1) which are arranged along the axial direction of the crucible part, wherein each graphite heating part (1) is provided with a lower end close to a raw material containing part and an upper end close to the top of the crucible part, a plurality of graphite heating parts (1) are distributed along the periphery of the crucible part, a space is reserved between every two adjacent graphite heating parts (1), the adjacent graphite heating parts (1) are integrally connected, the integral connection is first connection or second connection, the first connection is the upper end of each adjacent graphite heating part (1) is integrally connected, the second connection is the lower end of each adjacent graphite heating part (1) is integrally connected, the first connection and the second connection are arranged at intervals, and the graphite heating parts (1) are sequentially connected through the first connection and the second connection;
and the graphite sliding block (2) is arranged on the graphite heating part (1) and is in sliding connection with the graphite heating part (1), and slides along the axial direction of the crucible part relative to the graphite heating part (1).
2. The device according to claim 1, characterized in that a recess (201) is provided on the graphite slide (2), the inner contour shape of the recess (201) matches the outer contour shape of the graphite heat-generating part (1), the graphite heat-generating part (1) is embedded in the recess (201), and the graphite slide (2) wraps the edges of the outer wall, the side wall and the inner wall of the graphite heat-generating part (1).
3. The device according to claim 2, characterized in that the graphite slide (2) is formed by a first graphite slide (202) and a second graphite slide (203) being spliced, the recess comprising a left half recess (2011) and a right half recess (2012), the inner contour of the first graphite slide (202) and the inner contour of the second graphite slide (203) constituting the left half recess (2011) and the right half recess (2012), respectively, the inner contour of the first graphite slide (202) and the inner contour of the second graphite slide (203) being spliced to form the recess (201).
4. A device according to claim 3, characterized in that the graphite slide (2) is provided with a threaded through hole (204) arranged in the axial direction of the crucible portion, which is formed by a first threaded through hole (2041) and a second threaded through hole (2042) spliced together, the first threaded through hole (2041) and the second threaded through hole (2042) being arranged on the first graphite slide (202) and the second graphite slide (203), respectively;
the device also comprises a connecting shaft (3) which is arranged along the axial direction of the crucible part, one end of the connecting shaft is fixedly connected with the graphite slide block (2) through the threaded through hole (204), and the other end of the connecting shaft is fixedly connected with the mechanical driving assembly (4) and comprises an insulating shaft section.
5. The device according to claim 4, characterized in that the outer wall of the first graphite slide (202) and the outer wall of the second graphite slide (203) are provided with protrusions (205), respectively, and the first threaded through hole (2041) and the second threaded through hole (2042) are provided on the protrusions (205) of the first graphite slide (202) and on the protrusions (205) of the second graphite slide (203), respectively.
6. The device according to claim 4, characterized in that the connecting shaft (3) comprises a first connecting shaft section (301), which is a graphite connecting shaft section, one end of which is fixedly connected to the graphite slider (2);
and one end of the second connecting shaft section (302) is fixedly connected with the other end of the first connecting shaft section (301), the second connecting shaft section comprises a metal connecting shaft section and an insulating shaft section, and the other end of the second connecting shaft section is fixedly connected with the mechanical driving assembly (4).
7. The device according to claim 1, characterized in that the surface of the graphite slider (2) in sliding contact with the graphite heat-generating part (1) is lined with graphite paper.
8. The device according to claim 1, wherein each graphite heat generating part (1) is provided with the graphite slide block (2), and each graphite slide block (2) slides independently relative to the corresponding graphite heat generating part (1).
9. A method for growing a silicon carbide single crystal using the apparatus according to any one of claims 1 to 8, the growing process comprising a temperature rising stage, a crystal growing stage and a growth ending stage, characterized in that in the crystal growing stage, the graphite slider (2) is slid in the axial direction of the crucible relative to the graphite heat generating part (1), and the local heat generation amount of the graphite heat generating component outside the crucible is adjusted.
10. The growing method according to claim 9, wherein the growing stage includes a crystal growth stage front stage, a crystal growth stage middle stage, and a crystal growth stage rear stage, wherein the graphite slider (2) is positioned at a first preset position at a distance of 0.1 to 0.4 times the height of the graphite heat generating part (1) from the lower end of the graphite heat generating part (1) in the crystal growth stage front stage, and the graphite slider (2) is moved up to a second preset position at a distance of 0.6 to 0.8 times the height of the graphite heat generating part (1) from the lower end of the graphite heat generating part (1) in the crystal growth stage middle stage and the crystal growth stage rear stage.
11. A growth method according to claim 10, characterized in that the graphite slide (2) on each graphite heat-generating part (1) is located at the first preset position in the early stage of the growing stage, that a part of the graphite slide (2) uniformly distributed along the circumferential direction of the crucible part is moved up to the second preset position at a first preset speed in the middle stage of the growing stage, and that the remaining graphite slide (2) located at the first preset position is moved up to the second preset position at a first preset speed in the later stage of the growing stage, the first preset speed being 2mm/h to 5mm/h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202410232273.2A CN117822120B (en) | 2024-03-01 | Device and method for growing silicon carbide monocrystal by resistance method with adjustable local heating value |
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| CN202410232273.2A CN117822120B (en) | 2024-03-01 | Device and method for growing silicon carbide monocrystal by resistance method with adjustable local heating value |
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| CN110923806A (en) * | 2019-12-24 | 2020-03-27 | 西安奕斯伟硅片技术有限公司 | Single crystal furnace and preparation method of single crystal silicon rod |
| CN211497868U (en) * | 2020-03-05 | 2020-09-15 | 福建北电新材料科技有限公司 | Thermal field heating device for improving growth height of silicon carbide crystal |
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