CN114059154A - Silicon carbide single crystal growth device and method - Google Patents
Silicon carbide single crystal growth device and method Download PDFInfo
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- CN114059154A CN114059154A CN202111362867.8A CN202111362867A CN114059154A CN 114059154 A CN114059154 A CN 114059154A CN 202111362867 A CN202111362867 A CN 202111362867A CN 114059154 A CN114059154 A CN 114059154A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 117
- 239000013078 crystal Substances 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 199
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 149
- 239000010439 graphite Substances 0.000 claims abstract description 149
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 43
- 239000002245 particle Substances 0.000 claims abstract description 42
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 22
- 239000010703 silicon Substances 0.000 claims abstract description 22
- 238000000859 sublimation Methods 0.000 claims abstract description 13
- 230000008022 sublimation Effects 0.000 claims abstract description 13
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 10
- 238000002109 crystal growth method Methods 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims description 16
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000005260 corrosion Methods 0.000 claims description 14
- 230000007797 corrosion Effects 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 10
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 10
- 241001330002 Bambuseae Species 0.000 claims description 10
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 10
- 239000011425 bamboo Substances 0.000 claims description 10
- 150000002736 metal compounds Chemical class 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000011863 silicon-based powder Substances 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
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- 230000003628 erosive effect Effects 0.000 description 1
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- 238000001704 evaporation Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
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- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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- 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
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a silicon carbide single crystal growth device which comprises a first graphite crucible capable of containing silicon carbide powder, wherein at least two layers of graphite baffle discs are arranged in the first graphite crucible, and the graphite baffle discs divide a channel between silicon carbide seed crystals and the silicon carbide powder into a plurality of communicating channels connected with S-shaped channels. When the silicon carbide single crystal growth apparatus of the present invention is operated, Si containing fine carbon particlesmCnWhen the atmosphere flows in the communicating channel, the resistance of the tiny carbon particles is larger than that of gas at the turning part of the flowing channel, and the tiny carbon particles are deposited at the turning part, so that the purpose of reducing the inclusion in the silicon carbide single crystal is achieved, and the influence of the inclusion on the quality of the silicon carbide single crystal and the growth speed of the crystal is avoided. The invention also provides a silicon carbide single crystal growth method, which can generate carbon particles in the decomposition and sublimation stages of silicon carbide powder, the carbon particles move along the communicating channel and deposit in the communicating channel, silicon vapor reacts with the carbon particles, and the silicon carbide single crystal is grown in the carbon particlesAnd growing the silicon seed crystal surface.
Description
Technical Field
The invention relates to the technical field of silicon carbide single crystal materials, in particular to a silicon carbide single crystal growth device and a silicon carbide single crystal growth method.
Background
Silicon carbide single crystal materials are representative of third-generation wide band gap semiconductor materials, have properties such as a wide bandgap, high thermal conductivity, high electron saturation mobility, and high breakdown electric field, are significantly superior to first-generation semiconductor materials such as silicon and second-generation semiconductor materials such as GaAs, and are considered to be ideal semiconductor materials for manufacturing optoelectronic devices, high-frequency high-power devices, high-temperature electronic devices, and the like. The LED light source has wide application in the aspects of white light illumination, light storage, screen display, aerospace, high-temperature radiation environment, oil exploration, automation, radar and communication, electric vehicles, power electronics and the like.
The growth of silicon carbide single crystal materials is difficult, and a physical vapor deposition method (also called PVT or modified Lely method) is generally adopted at present, wherein the silicon carbide powder is taken as a general raw material, the silicon carbide powder is heated to a certain temperature and is obviously sublimated, and decomposed silicon carbide gas is transported along a temperature gradient and is condensed at a silicon carbide seed crystal. The PVT method for growing SiC single crystal mainly comprises three processes, namely decomposition and sublimation of raw materials, mass transmission and crystallization on seed crystal.
(1) The decomposition and sublimation stages of the raw materials mainly generate the following reactions:
SiC(s)＝Si(g)+C(s) (1-1)
2SiC(s)＝Si(g)+SiC2(g) (1-2)
2SiC(s)＝C(s)+Si2C(g) (1-3)
(2) during the mass transfer stage, the Si vapor further reacts with the side wall of the graphite crucible to form Si2C and SiC2
2C(s)+Si(g)＝SiC2(g) (1-4)
C(s)+2Si(g)＝Si2C(g) (1-5)
(3) On the surface of the seed crystal, three gas phases are grown by the following reactions:
SiC2(g)+Si2C(g)＝3SiC(s) (1-6)
Si(g)+SiC2(g)＝2SiC(s) (1-7)
from the above reaction formula, it is seen that fine carbon particles are generated in the decomposition and sublimation stages of the raw material, and the fine carbon particles are also transported along the temperature gradient and finally form inclusions in the silicon carbide single crystal, thereby affecting the quality of the silicon carbide single crystal. In the mass transfer stage, the Si vapor reacts with the side wall of the graphite crucible to erode the surface of the graphite, and in the erosion process, tiny carbon particles are generated and can be transported along with the gas to form a wrappage in the silicon carbide single crystal.
In the prior art, the Chinese patent with the publication number of CN204570093U discloses a wrapping-free silicon carbide single crystal growth chamber, a graphite filter screen is arranged between a silicon carbide raw material and seed crystals on the inner wall of the growth chamber, the upper surface and the lower surface of the filter screen are coated with high-temperature-resistant metal compound coatings, the coatings can filter the tiny carbon particles in the decomposition and sublimation stages of the raw material, but the tiny carbon particles in the mass transmission stage can not be processed, the aperture of the graphite filter screen is less than 10 micrometers, the filter screen is difficult to process, and the filter screen is used for processing SimCnAtmosphere (with gas phase component Si)mCnCollectively represent a gaseous product of formula (1-1) -formula (1-7), which is gaseous Si when m is 1 and n is 0; when m is equal to n is equal to 1, the SiC is in a gaseous state; when m is 2 and n is 1, it is gaseous Si2C; when m is 1 and n is 2, the SiC is gaseous SiC2(ii) a Where reference is made to "SimCnAtmosphere "the same as here") is large, which easily causes insufficient evaporation amount, thereby affecting the crystal growth rate.
Therefore, how to change the current situation that in the prior art, tiny carbon particles are easy to form inclusions in the growth process of the silicon carbide single crystal material, and the quality and the crystal growth speed of the silicon carbide single crystal are affected, becomes a problem to be solved by the technical staff in the field.
Disclosure of Invention
The invention aims to provide a silicon carbide single crystal growth device and a silicon carbide single crystal growth method, which are used for solving the problems in the prior art, reducing inclusions formed by tiny carbon particles and avoiding the inclusions from influencing the quality and the crystal growth speed of a silicon carbide single crystal.
In order to achieve the purpose, the invention provides the following scheme: the invention provides a silicon carbide single crystal growth device which comprises a first graphite crucible capable of containing silicon carbide powder, wherein a silicon carbide seed crystal is arranged in the first graphite crucible, a gap is formed between the silicon carbide seed crystal and the silicon carbide powder, at least two layers of graphite baffle discs are arranged in the first graphite crucible, the outer surface of each graphite baffle disc is provided with a corrosion-resistant coating, each corrosion-resistant coating is made of a metal compound, the melting point of the metal compound is higher than the sublimation temperature of the silicon carbide, the graphite baffle discs are connected with the inner wall of the first graphite crucible, and the graphite baffle discs are arranged between the silicon carbide seed crystal and the silicon carbide powder;
the graphite baffle plate divides a channel between the silicon carbide seed crystal and the silicon carbide powder into a plurality of communicating channels connected with each other in an S-shaped channel, and the cavity where the silicon carbide powder is located is communicated with the cavity where the silicon carbide seed crystal is located by the communicating channels.
Preferably, a second crucible is further arranged in the first graphite crucible, and one of the following substances is arranged in the second crucible: silicon powder, silicon dioxide powder, a mixture of silicon dioxide powder and carbon powder and a mixture of silicon powder.
Preferably, the second crucible is arranged in the silicon carbide powder, the first graphite crucible and the second crucible are coaxially arranged, and the distance between the bottom of the second crucible and the bottom wall of the first graphite crucible is 10-90 mm.
Preferably, the graphite baffle disc has a groove facing the silicon carbide powder.
Preferably, the graphite baffle discs are perpendicular to the axis of the first graphite crucible, the graphite baffle discs are arranged in a staggered mode, and gaps are reserved between the adjacent graphite baffle discs.
Preferably, a graphite sliding block is arranged on the inner wall of the first graphite crucible, and the graphite baffle disc is arranged on the graphite sliding block.
Preferably, first graphite crucible is split type structure, first graphite crucible includes graphite crucible bucket, the short section of thick bamboo of graphite and graphite crucible lid, can hold in the graphite crucible bucket the carborundum powder, the short section of thick bamboo of graphite set up in the graphite crucible bucket with between the graphite crucible lid, the graphite crucible bucket and the graphite crucible lid respectively with the short section of thick bamboo of graphite can be dismantled and be connected, the carborundum seed crystal with the graphite crucible lid links to each other.
Preferably, the graphite crucible barrel and the graphite crucible cover are respectively in threaded connection with the short graphite barrel.
Preferably, the second crucible comprises a second crucible body and a second crucible cover, the second crucible body can contain silicon-containing materials, and the second crucible cover is detachably connected with the second crucible body.
The invention also provides a silicon carbide single crystal growth method, which is characterized in that by using the silicon carbide single crystal growth device, carbon particles can be generated in the decomposition and sublimation stages of the silicon carbide powder, the carbon particles move along the communicating channel and are deposited in the communicating channel, silicon vapor reacts with the carbon particles, and the silicon carbide single crystal grows on the surface of the silicon carbide seed crystal.
Compared with the prior art, the invention has the following technical effects: the silicon carbide single crystal growth device comprises a first graphite crucible capable of containing silicon carbide powder, wherein a silicon carbide seed crystal is arranged in the first graphite crucible, a gap is formed between the silicon carbide seed crystal and the silicon carbide powder, at least two layers of graphite baffle discs are also arranged in the first graphite crucible, the outer surface of each graphite baffle disc is provided with a corrosion-resistant coating, each corrosion-resistant coating is made of a metal compound, the melting point of the metal compound is higher than the sublimation temperature of the silicon carbide, the graphite baffle discs are connected with the inner wall of the first graphite crucible, and the graphite baffle discs are arranged between the silicon carbide seed crystal and the silicon carbide powder; the graphite baffle plate divides a channel between the silicon carbide seed crystal and the silicon carbide powder into a plurality of communicating channels connected with each other through S-shaped channels, and the cavity where the silicon carbide powder is located is communicated with the cavity where the silicon carbide seed crystal is located through the communicating channels.
According to the silicon carbide single crystal growth device, at least two layers of graphite baffle discs are arranged between the silicon carbide seed crystal and the silicon carbide powder, so that the silicon carbide powder and the silicon carbide seed crystal are communicated by the communicating channel, the communicating channel comprises a plurality of connected S-shaped channels, and when the device works, Si containing tiny carbon particlesmCnWhen the atmosphere flows in the communicating channel, the resistance of the tiny carbon particles is larger than that of gas at the turning part of the flowing channel, and the tiny carbon particles are deposited at the turning part, so that the purpose of reducing the inclusion in the silicon carbide single crystal is achieved, and the influence of the inclusion on the quality of the silicon carbide single crystal and the growth speed of the crystal is avoided. It should be noted that the outer surface of the graphite baffle plate is provided with the corrosion-resistant coating, the melting point of the material of the corrosion-resistant coating is higher than the biochemical temperature of the silicon carbide, and the graphite baffle plate and the Si are prevented from contactingmCnAtmosphere reaction, connected passage also prolongs SimCnThe distance of the atmosphere from the silicon carbide seed crystal is such that SimCnSiC required for growing crystal by reaction of silicon vapor in atmosphere and tiny carbon particles2(g)And Si2C(g)。
The invention also provides a silicon carbide single crystal growth method, which utilizes the silicon carbide single crystal growth device to generate carbon particles in the decomposition and sublimation stages of silicon carbide powder, the carbon particles move along the communicating channel and deposit in the communicating channel, silicon vapor reacts with the carbon particles, and the silicon carbide single crystal grows on the surface of the silicon carbide seed crystal. By adopting the method for growing the silicon carbide single crystal, the tiny carbon particles are deposited in the communicating pipe channel, the inclusions in the silicon carbide single crystal are reduced, gas flows in the communicating pipe channel, the time of the atmosphere reaching the silicon carbide seed crystal is prolonged, the tiny carbon particles in the atmosphere have sufficient time to react with silicon steam, the tiny carbon particles in the atmosphere are reduced, and the growth speed of the crystal is ensured.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic sectional view showing the structure of an apparatus for growing a silicon carbide single crystal according to the present invention;
FIG. 2 is a schematic structural view of a graphite shutter disk of the silicon carbide single crystal growth apparatus of the present invention;
wherein, 1 is first graphite crucible, 101 is the graphite crucible bucket, 102 is the short section of thick bamboo of graphite, 103 is the graphite crucible lid, 2 is the carborundum seed crystal, 3 is the graphite fender dish, 301 is the recess, 4 is the second crucible, 401 is the second crucible body, 402 is the second crucible lid, 5 is the graphite slider.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a silicon carbide single crystal growth device and a silicon carbide single crystal growth method, which are used for solving the problems in the prior art, reducing inclusions formed by tiny carbon particles and avoiding the inclusions from influencing the quality and the crystal growth speed of a silicon carbide single crystal.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Referring to fig. 1-2, fig. 1 is a schematic sectional view of an apparatus for growing a silicon carbide single crystal according to the present invention, and fig. 2 is a schematic structural view of a graphite baffle plate of the apparatus for growing a silicon carbide single crystal according to the present invention.
The invention provides a silicon carbide single crystal growth device, which comprises a first graphite crucible 1 capable of containing silicon carbide powder, wherein a silicon carbide seed crystal 2 is arranged in the first graphite crucible 1, a gap is formed between the silicon carbide seed crystal 2 and the silicon carbide powder, at least two layers of graphite baffle discs 3 are also arranged in the first graphite crucible 1, the outer surface of each graphite baffle disc 3 is provided with a corrosion-resistant coating, the corrosion-resistant coating is made of a metal compound, the melting point of the metal compound is higher than the sublimation temperature of the silicon carbide, the graphite baffle discs 3 are connected with the inner wall of the first graphite crucible 1, and the graphite baffle discs 3 are arranged between the silicon carbide seed crystal 2 and the silicon carbide powder; the graphite baffle disc 3 divides a channel between the silicon carbide seed crystal 2 and the silicon carbide powder into a plurality of communicating channels connected with the S-shaped channels, and the cavity where the silicon carbide powder is located is communicated with the cavity where the silicon carbide seed crystal 2 is located by the communicating channels.
According to the silicon carbide single crystal growth device, at least two layers of graphite baffle discs 3 are arranged between the silicon carbide seed crystal 2 and the silicon carbide powder, so that the silicon carbide powder and the silicon carbide seed crystal 2 are communicated by utilizing the communicating channel which comprises a plurality of connected S-shaped channels, and when the device works, Si containing tiny carbon particlesmCnWhen the atmosphere flows in the communicating channel, the resistance of the tiny carbon particles is larger than that of gas at the turning part of the flowing channel, and the tiny carbon particles are deposited at the turning part, so that the purpose of reducing the inclusion in the silicon carbide single crystal is achieved, and the influence of the inclusion on the quality of the silicon carbide single crystal and the growth speed of the crystal is avoided. It should be noted that the outer surface of the graphite baffle plate 3 is provided with the corrosion-resistant coating, and the melting point of the material of the corrosion-resistant coating is higher than the biochemical temperature of the silicon carbide, so that the graphite baffle plate 3 and the Si are prevented from being contactedmCnAtmosphere reaction, connected passage also prolongs SimCnThe distance of the atmosphere from the silicon carbide seed crystal 2 is such that Si is presentmCnSiC required for growing crystal by reaction of silicon vapor in atmosphere and tiny carbon particles2(g)And Si2C(g)。
In addition, a second crucible 4 is provided in the first graphite crucible 1, and one of the following substances is provided in the second crucible 4: silicon powder, silicon dioxide powder, a mixture of silicon dioxide powder and carbon powder (the molar ratio of silicon dioxide to carbon powder is more than 0.5), a mixture of silicon dioxide powder and carbon powder and a mixture of silicon powder (the molar ratio of silicon dioxide to carbon powder is more than 0.5). The silicon powder in the second crucible 4 slowly volatilizes at high temperature, or the silicon dioxide powder reacts with the carbon powder at high temperature to generate silicon which volatilizes at high temperature, so that the silicon concentration in the atmosphere can be supplemented, and in the flowing process of the atmosphere, the silicon reacts with the tiny carbon particles mixed in the atmosphere to generate SiC2(g)And Si2C(g)。
In the present embodiment, the second crucible 4 is disposed in the silicon carbide powder, the first graphite crucible 1 is disposed coaxially with the second crucible 4, and the distance between the bottom of the second crucible 4 and the bottom wall of the first graphite crucible 1 is 10 to 90 mm. So that the silicon in the second crucible 4 can be uniformly heated and volatilized to supplement the silicon concentration in the atmosphere.
Specifically, the graphite baffle disc 3 is provided with a groove 301 facing silicon carbide powder, and the arrangement of the groove 301 further enables tiny carbon particles to be deposited smoothly, so that the inclusions in the silicon carbide single crystal are reduced.
In other embodiments of the present invention, the graphite baffles 3 may be arranged perpendicular to the axis of the first graphite crucible 1, the graphite baffles 3 are arranged in a staggered manner, and a gap is formed between adjacent graphite baffles 3 to form an S-shaped channel, and the specific number of the graphite baffles 3 may be set according to production requirements in practical applications.
More specifically, a graphite sliding block 5 is arranged on the inner wall of the first graphite crucible 1, and the graphite baffle disc 3 is arranged on the graphite sliding block 5, so that convenience is provided for the installation and fixation of the graphite baffle disc 3. It is also noted here that the corrosion-resistant coating on the outer surface of the graphite baffle disk 3 may be made of carbide, nitride or other mixtures of rare metals, including tantalum, hafnium, niobium, titanium, tungsten, vanadium.
In order to improve the operation convenience, first graphite crucible 1 is split type structure, first graphite crucible 1 includes graphite crucible bucket 101, short section of thick bamboo 102 of graphite and graphite crucible lid 103, can hold carborundum powder in the graphite crucible bucket 101, short section of thick bamboo 102 of graphite sets up between graphite crucible bucket 101 and graphite crucible lid 103, graphite crucible bucket 101 and graphite crucible lid 103 can dismantle with short section of thick bamboo 102 of graphite respectively and be connected, the convenience of raw materials setting and spare part installation has been improved, carborundum seed crystal 2 links to each other with graphite crucible lid 103. In actual operation, the graphite crucible barrel 101 and the graphite crucible cover 103 can be selected to be respectively in threaded connection with the short graphite barrel 102, and the connection and the fastening are realized, so that the disassembly and the assembly are convenient.
Correspondingly, the second crucible 4 comprises a second crucible body 401 and a second crucible cover 402, the second crucible body 401 can contain silicon-containing materials, the second crucible cover 402 is detachably connected with the second crucible body 401 so as to be convenient for placing the materials into the second crucible 4, and the second crucible 4 is placed in the first graphite crucible 1 to supplement the silicon concentration in the atmosphere.
Further, the invention also provides a silicon carbide single crystal growth method, by utilizing the silicon carbide single crystal growth device, carbon particles can be generated in the decomposition and sublimation stages of silicon carbide powder, the carbon particles move along the communicating channel and are deposited in the communicating channel, silicon vapor reacts with the carbon particles, and the silicon carbide single crystal grows on the surface of the silicon carbide seed crystal 2.
Decomposition of silicon carbide raw material at high temperature, SimCnWhen gas passes through a communication channel formed by the graphite baffle disc 3, tiny carbon particles are blocked and deposited, the surface of the graphite baffle disc 3 is coated with a corrosion-resistant coating, so the outer surface of the graphite baffle disc 3 cannot be corroded, no tiny carbon particles are generated, the second crucible 4 is used for supplementing silicon concentration, the silicon concentration in the atmosphere is higher, and the silicon has enough time to react with the tiny carbon particles in the atmosphere, so that the inclusions in the silicon carbide single crystal are reduced.
The principle and the implementation mode of the invention are explained by applying a specific example, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A silicon carbide single crystal growth device is characterized by comprising a first graphite crucible capable of containing silicon carbide powder, wherein a silicon carbide seed crystal is arranged in the first graphite crucible, a gap is formed between the silicon carbide seed crystal and the silicon carbide powder, at least two layers of graphite baffle discs are arranged in the first graphite crucible, the outer surface of each graphite baffle disc is provided with a corrosion-resistant coating, each corrosion-resistant coating is made of a metal compound, the melting point of the metal compound is higher than the sublimation temperature of the silicon carbide, the graphite baffle discs are connected with the inner wall of the first graphite crucible, and the graphite baffle discs are arranged between the silicon carbide seed crystal and the silicon carbide powder;
the graphite baffle plate divides a channel between the silicon carbide seed crystal and the silicon carbide powder into a plurality of communicating channels connected with each other in an S-shaped channel, and the cavity where the silicon carbide powder is located is communicated with the cavity where the silicon carbide seed crystal is located by the communicating channels.
2. A silicon carbide single crystal growth apparatus according to claim 1, wherein: a second crucible is further arranged in the first graphite crucible, and one of the following substances is arranged in the second crucible: silicon powder, silicon dioxide powder, a mixture of silicon dioxide powder and carbon powder and a mixture of silicon powder.
3. A silicon carbide single crystal growth apparatus according to claim 2, wherein: the second crucible is arranged in the silicon carbide powder, the first graphite crucible and the second crucible are coaxially arranged, and the distance between the bottom of the second crucible and the bottom wall of the first graphite crucible is 10-90 mm.
4. A silicon carbide single crystal growth apparatus according to claim 1, wherein: the graphite baffle disc is provided with a groove facing the silicon carbide powder.
5. A silicon carbide single crystal growth apparatus according to claim 1, wherein: the graphite baffle discs are perpendicular to the axis of the first graphite crucible and are arranged in a staggered mode, and gaps are reserved between the adjacent graphite baffle discs.
6. A silicon carbide single crystal growth apparatus according to claim 1, wherein: the inner wall of the first graphite crucible is provided with a graphite sliding block, and the graphite baffle disc is arranged on the graphite sliding block.
7. A silicon carbide single crystal growth apparatus according to claim 1, wherein: first graphite crucible is split type structure, first graphite crucible includes graphite crucible bucket, short section of thick bamboo of graphite and graphite crucible lid, can hold in the graphite crucible bucket carborundum powder, short section of thick bamboo of graphite set up in graphite crucible bucket with between the graphite crucible lid, graphite crucible bucket and graphite crucible lid respectively with the short section of thick bamboo of graphite can be dismantled and be connected, the carborundum seed crystal with the graphite crucible lid links to each other.
8. A silicon carbide single crystal growth apparatus according to claim 2, wherein: the graphite crucible barrel and the graphite crucible cover are respectively in threaded connection with the short graphite barrel.
9. A silicon carbide single crystal growth apparatus according to claim 2, wherein: the second crucible comprises a second crucible body and a second crucible cover, the second crucible body can contain silicon-containing materials, and the second crucible cover is detachably connected with the second crucible body.
10. A silicon carbide single crystal growth method using the silicon carbide single crystal growth apparatus according to any one of claims 1 to 9, characterized in that: carbon particles are generated in the decomposition and sublimation stages of the silicon carbide powder, the carbon particles move along the communicating channel and deposit in the communicating channel, silicon vapor reacts with the carbon particles, and a silicon carbide single crystal grows on the surface of the silicon carbide seed crystal.
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| CN115838963A (en) * | 2022-12-30 | 2023-03-24 | 浙江晶越半导体有限公司 | Be applied to crucible device of sublimation method growth carborundum single crystal |
| CN116497438A (en) * | 2023-06-27 | 2023-07-28 | 北京青禾晶元半导体科技有限责任公司 | Silicon carbide single crystal growth device and growth method |
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