CN116623284B - Silicon carbide and growth device and growth method thereof - Google Patents
Silicon carbide and growth device and growth method thereof Download PDFInfo
- Publication number
- CN116623284B CN116623284B CN202310623791.2A CN202310623791A CN116623284B CN 116623284 B CN116623284 B CN 116623284B CN 202310623791 A CN202310623791 A CN 202310623791A CN 116623284 B CN116623284 B CN 116623284B
- Authority
- CN
- China
- Prior art keywords
- crucible
- silicon carbide
- diameter
- heat preservation
- growth
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 55
- 238000010438 heat treatment Methods 0.000 claims abstract description 54
- 238000004321 preservation Methods 0.000 claims abstract description 43
- 239000000463 material Substances 0.000 claims abstract description 25
- 230000006698 induction Effects 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- 238000003786 synthesis reaction Methods 0.000 claims description 17
- 239000012535 impurity Substances 0.000 claims description 16
- 230000001681 protective effect Effects 0.000 claims description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 239000004020 conductor Substances 0.000 claims description 4
- 239000011810 insulating material Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052751 metal Inorganic materials 0.000 abstract description 11
- 239000002184 metal Substances 0.000 abstract description 11
- 239000002253 acid Substances 0.000 abstract description 7
- 238000005406 washing Methods 0.000 abstract description 7
- 239000007789 gas Substances 0.000 description 33
- 238000009413 insulation Methods 0.000 description 12
- 239000000843 powder Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 238000011049 filling Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000003763 carbonization Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 239000011863 silicon-based powder Substances 0.000 description 5
- 229920000297 Rayon Polymers 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 4
- 229910021384 soft carbon Inorganic materials 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
-
- 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
Abstract
The invention provides silicon carbide, a growth device and a growth method thereof, wherein the growth device comprises: a container body; the heat preservation layer is arranged in the container body, an opening is formed in the top of the heat preservation layer, and the opening can accommodate the temperature measuring device; the crucible is arranged in the heat preservation layer, a cavity protruding into the crucible is formed in the bottom of the crucible, the crucible comprises a crucible cover, the crucible cover is positioned at the top of the crucible, and a through hole is formed in the crucible cover; the heating body comprises a column body and a disc body, the column body is embedded into the cavity, and the disc body is arranged in the heat preservation layer; and the induction coil is arranged around the container body. The silicon carbide synthesized by the device does not need acid washing subsequently, the material blocks are loose, a conventional crushing process is not needed, the problem of metal pollution can be effectively avoided, and after crushing, the silicon carbide can be washed by only a small amount of pure water, so that the consumption of the pure water is effectively reduced, and the cost is reduced.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to silicon carbide, a growth device and a growth method thereof.
Background
Silicon carbide (SiC) is a third-generation semiconductor material with wide forbidden band, high critical electric field and high saturation mobility, has great advantages in the field of power devices, and is widely applied to the fields of new energy automobiles, photovoltaic power generation, railway traffic, power systems and the like.
However, siC crystal growth is extremely difficult due to the physical and chemical properties of SiC that are stable. The single crystal substrate for manufacturing the SiC device is mainly prepared by a Physical Vapor Transport (PVT) method, the raw material is SiC powder, and parameters such as purity, particle size, crystal form and the like of the powder have certain influence on the quality of SiC single crystal grown by the PVT method and the quality of the device manufactured later. The cost of the substrate sheet accounts for about 50% of the whole industrial chain, and the quality and cost of the powder directly affect the production cost of the substrate. At present, an improved self-propagating method is generally adopted for synthesizing SiC in industrialized production, for example CN113739562A discloses a self-propagating method high-temperature high-pressure silicon nitride powder preparation device, wherein the silicon nitride powder preparation device comprises a furnace body, a skip car, a feeding system, a self-propagating reaction ignition system, a vacuum system, a gas circuit system, a cooling system and an automatic control system, wherein a reaction space is arranged in the furnace body; can provide the self-propagating method preparation of large-scale silicon nitride with controllable batch production, and obtain the silicon nitride with higher purity. CN109336114B discloses a method for improving the synthesis efficiency of high-purity silicon carbide powder, which comprises the following steps of S1, uniformly mixing high-purity carbon powder and high-purity silicon powder to obtain raw materials; s2, placing the raw materials into a cavity of a crucible, and synthesizing high-purity silicon carbide powder by a high-temperature self-propagating method. However, due to the problems of insufficient impurity removal and caking of the material blocks in the synthesis process, the subsequent crushing processing is needed, the metal pollution risk exists in the conventional processing process, so that the surface metal of the powder is higher, the complicated pickling and water washing processes are needed, the pure water consumption and pollution discharge burden are increased, the risks of acid removal and incomplete surface metal removal exist, and the crystal growth is affected to a certain extent.
Therefore, how to avoid acid washing, reduce the pure water consumption, and improve the quality of silicon carbide at the same time is a current urgent problem to be solved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide silicon carbide and a growth device and a growth method thereof. The invention provides an improved silicon carbide growing device, the silicon carbide synthesized by the device does not need acid washing treatment subsequently, the material blocks are loose, the conventional crushing process is not needed, the metal pollution problem in the crushing process is avoided, the crushed silicon carbide can be washed by only a small amount of pure water, the consumption of the pure water is effectively reduced, and the cost is reduced.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a silicon carbide growth apparatus comprising:
a container body;
the heat preservation layer is arranged in the container body, an opening is formed in the top of the heat preservation layer, and the opening can accommodate the temperature measuring device;
the crucible is arranged in the heat preservation layer, a cavity protruding into the crucible is formed in the bottom of the crucible, the crucible comprises a crucible cover, the crucible cover is positioned at the top of the crucible, and a through hole is formed in the crucible cover;
the heating body comprises a column body and a disc body, the column body is embedded into the cavity, and the disc body is arranged in the heat preservation layer;
and the induction coil is arranged around the container body.
The invention provides an improved silicon carbide growing device, the silicon carbide synthesized by the device does not need acid washing treatment subsequently, the material blocks are loose, the conventional crushing process is not needed, the metal pollution problem in the crushing process is avoided, the crushed silicon carbide can be washed by only a small amount of pure water, the consumption of the pure water is effectively reduced, and the cost is reduced.
According to the invention, the top of the crucible is provided with the through holes, so that on one hand, a large axial temperature gradient can be formed, the crystallinity and granularity of the silicon carbide powder are improved, and on the other hand, the growth device is matched to further optimize the impurity discharge effect, so that the synthesized silicon carbide powder does not need a subsequent pickling process.
As a preferable technical scheme of the invention, the ratio of the diameter of the cavity to the diameter of the crucible is 1 (3-30), for example, the ratio can be 1:3, 1:5, 1:7, 1:9, 1:11, 1:13, 1:15, 1:17, 1:19, 1:21, 1:23, 1:25, 1:27, 1:29 or 1:30, etc.
In the invention, if the ratio of the diameter of the cavity to the diameter of the crucible is too small, namely the diameter of the cavity is too small, the size of the central columnar heating element is limited, the central radial heat compensation is insufficient, the effect of uniform temperature cannot be achieved, the phenomenon of solid agglomeration still exists at the middle and lower parts of the material block, and the impurity emission is insufficient; if the ratio of the diameter of the cavity to the diameter of the crucible is too large, namely the diameter of the cavity is too large, the crucible material containing area is reduced, the single synthesis weight is limited, and on the other hand, the central compensation temperature and the compensation area are too large, so that large-area carbonization of synthesized powder in the crucible is easily caused, and the yield and the quality are affected.
Preferably, the ratio of the height of the chamber to the height of the crucible is 1 (1.5-5), which may be, for example, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5, 1:5, etc.
In the invention, the ratio of the height of the cavity to the height of the crucible is too small, namely the height of the cavity is too small, the size of the central columnar heating element is limited, the axial temperature compensation area is insufficient, the top and bottom temperature cannot achieve a uniform effect, and the phenomenon of relatively solid agglomeration still exists at the lower part of the material block; if the ratio of the height of the cavity to the height of the crucible is too large, namely the height of the cavity is too large, the crucible material containing area is reduced, the single synthesis weight is limited, and on the other hand, the central compensation temperature and the compensation area are too large, so that large-area carbonization of synthesized powder in the crucible is easily caused, and the yield and the quality are affected.
As a preferable technical scheme of the invention, the heating element is made of conductive material.
Preferably, the conductive material comprises graphite.
The resistivity of the graphite material was in the range of 8 to 13. Mu. Ω. M.
The resistivity of the heating element is preferably 10 to 13. Mu. OMEGA.m, for example, 10. Mu. OMEGA.m, 11. Mu. OMEGA.m, 12.2. Mu. OMEGA.m, 12.4. Mu. OMEGA.m, 12.6. Mu. OMEGA.m, 12.8. Mu. OMEGA.m, 13. Mu. OMEGA.m, or the like, which is larger than the crucible.
In the invention, the resistivity of the heating element is larger than that of the crucible, and is preferably 10-13 mu omega m, so as to enhance the heating value and solve the problems of insufficient impurity removal, insufficient synthesis, tight agglomeration, auxiliary crushing, cleaning and the like caused by low temperature of the center of the silicon carbide powder.
As a preferable technical scheme of the invention, the ratio of the diameter of the column body to the diameter of the cavity is (0.4-0.9): 1, for example, 0.4:1, 0.5:1, 0.6:1, 0.7:10.8:1, 0.9:1 or the like can be adopted.
Preferably, the ratio of the height of the column to the height of the chamber is (0.2-0.9): 1, which may be, for example, 0.2:1, 0.4:1, 0.6:1, 0.8:1, or 0.9:1, etc.
Preferably, the ratio of the diameter of the tray body to the diameter of the crucible is (0.6-1.2): 1, for example, 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1:1, 1.1:1 or 1.2:1, etc.
In the invention, if the diameter of the tray body is too small, on one hand, the heating value at the bottom of the crucible is not sufficiently supplemented, and on the other hand, the vertical stability of the column body is affected to a certain extent; if the diameter is too large, the suitability of the existing heat preservation size is affected.
Preferably, the thickness of the tray body is 10-50mm, for example, 10mm, 15mm, 20mm, 25mm, 30mm, 35mm, 40mm, 45mm or 50mm, etc.
In the invention, if the thickness of the tray body is too small, the mechanical stability is affected to a certain extent; if the thickness of the tray body is too large, the size of the lower heat preservation layer needs to be thickened on one hand, the utilization rate of the cavity is reduced, the risk of overflowing the coil heating area exists on the other hand, and the heating value of the tray body is reduced.
As a preferable technical scheme of the invention, the crucible is made of graphite.
Preferably, the porosity of the crucible is 15-18%, for example, 15%, 15.5%, 16%, 16.5%, 17%, 17.5%, 18%, etc.
In the invention, the porosity of the crucible is 15-18%, so that the discharge of impurity gases (such as S, cl and impurity elements such as metals) is facilitated.
Preferably, the diameter of the circumference of the through hole is 50-300mm, for example, 50mm, 100mm, 150mm, 200mm, 250mm or 300mm, etc.
The circumference of the through hole can be a circumference with the center point of the crucible cover as the center and the diameter of 50-300 mm.
Preferably, the average diameter of the holes is 3-15mm, and may be, for example, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm, 10mm, 11mm, 12mm, 13mm, 14mm or 15mm, etc.
In the invention, if the average diameter of the holes is too small, the impurity removal is insufficient, the efficacy on the temperature gradient is weakened, and the center caking and bottom carbonization are easy to cause; if the average diameter of the holes is too large, the upper heat insulation layer is deteriorated, caking and firm phenomenon is easy to occur at the top of the material block, the material block is difficult to break, and a large amount of silicon gas is dissipated into a thermal field, so that a graphite piece and a heat insulation structure are damaged.
Preferably, the number of the holes is 3-20, for example, 3, 5, 7, 9, 11, 13, 15, 17 or 20 holes, etc.
As a preferred embodiment of the present invention, the crucible or the induction coil is movable up and down.
In the invention, the purpose of the crucible or the induction coil capable of moving up and down is to change the relative position of the crucible in the coil by matching with the growth process of silicon carbide, so that the upper part and the lower part are heated and synthesized uniformly, and the firmness of a silicon carbide block is further reduced.
Preferably, the movement speed of the crucible or the induction coil is independently 0-20mm/h, and may be, for example, 0mm/h, 1mm/h, 3mm/h, 5mm/h, 7mm/h, 10mm/h, 13mm/h, 15mm/h, 17mm/h, 20mm/h, or the like.
In the present invention, "independently" means that the movement speeds of both the crucible and the induction coil are selected so as not to interfere with each other, and may be the same or different. The same applies to the "independent" case.
Preferably, the movement distance of the crucible or the induction coil is independently 10-100mm, for example, 10mm, 20mm, 30mm, 40mm, 50mm, 60mm, 70mm, 80mm, 90mm or 100mm, etc.
As a preferable technical scheme of the invention, the heat insulation layer comprises an upper heat insulation layer, a lower heat insulation layer and a side heat insulation layer, wherein the upper heat insulation layer is provided with an opening, and the lower heat insulation layer is internally provided with the heating body.
Preferably, the heat insulation layer is a heat insulation material.
The heat insulating material is not particularly limited, and may be, for example, any one or a combination of at least two of a soft carbon felt, a hard carbon felt, or a carbon-carbon composite material, wherein the carbon felt may be a viscose-based or pitch-based material, etc.
In a second aspect, the present invention provides a method of growing silicon carbide using the silicon carbide growing apparatus of the first aspect, the method comprising the steps of:
(1) Placing a silicon source and a carbon source into a crucible for pretreatment to remove impurity gas;
(2) Heating a heating body through an induction coil, so that the crucible is subjected to primary heating at a temperature T1;
(3) And (3) carrying out a synthesis reaction at a temperature T2 to obtain the silicon carbide.
The invention is not limited to the kind of the silicon source, and can be exemplified by silicon powder; the kind of the carbon source is not limited, and may be exemplified by carbon powder.
In a preferred embodiment of the present invention, the particle diameter D50 of the silicon source is less than 2mm, and may be, for example, 1mm or 1.5 mm.
Preferably, the particle diameter D50 of the carbon source in step (1) is less than 100. Mu.m, for example, 90. Mu.m, 70. Mu.m, 50. Mu.m, 30. Mu.m, 10. Mu.m, etc.
Preferably, the molar ratio of the silicon source to the carbon source in step (1) is (1-1.1): 1, which may be, for example, 1:1, 1.02:1, 1.04:1, 1.06:1, 1.08:1, 1.1:1, or the like.
As a preferred technical solution of the present invention, the step of preprocessing in step (1) specifically includes:
(a) Vacuumizing and heating under the first power;
(b) Charging protective gas, and vacuumizing;
(c) To a second power and then to preheat.
The pretreatment is carried out for the purpose of removing impurity gases.
The number of times that the steps (a) and (b) are alternately repeated is not particularly limited in the present invention, and is exemplified, for example, by repeating 1 to 10 times, including 1, 3, 5, 7, 10 times, etc.
Preferably, the first power is 1-10% of the set power value, for example, may be 1%, 3%, 5%, 7%, 9% or 10% of the set power value.
Preferably, the second power is 3-25% of the set power value, for example, may be 3%, 5%, 7%, 9%, 11%, 13%, 15%, 17%, 19%, 21%, 23% or 25% of the set power value.
Preferably, the preheating temperature is 900-1200 ℃, and can be 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃ or the like.
The invention is not limited to the kind of the protective gas, and can be exemplified by pure Ar gas, ar/H 2 Mixture gas or He/H 2 Mixture of gases, where H 2 The ratio of (2) may be 0-40%.
Preferably, the T1 in the step (2) is 1300-1700 ℃, and for example, 1300 ℃, 1400 ℃, 1500 ℃, 1600 ℃, 1700 ℃ or the like can be adopted.
In the present invention, the purpose of heating at 1300-1700 ℃ is to synthesize beta phase silicon carbide.
Preferably, the primary heating time in step (2) is 1-30h, for example, 1h, 5h, 10h, 15h, 20h, 25h or 30h, etc.
Preferably, the synthesis reaction of step (3) is carried out in a protective atmosphere.
Preferably, the gas in the protective atmosphere comprises pure Ar gas, ar/H 2 Mixture gas or He/H 2 Any one of the mixed gases.
The flow rate of the gas in the protective atmosphere is not limited, and may be selected within a range of not more than 2000sccm, for example, 100sccm, 500sccm, 1000sccm, 1500sccm, 2000sccm, or the like.
Preferably, the pressure in the synthesis reaction in the step (3) is 1-30KPa, for example, 1KPa, 5KPa, 10KPa, 15KPa, 20KPa, 25KPa or 30KPa, etc.
Preferably, the T2 in the step (3) is 2000-2300 ℃, and may be 2000 ℃, 2050 ℃, 2100 ℃, 2150 ℃, 2200 ℃, 2250 ℃, 2300 ℃ or the like.
Preferably, the synthesis reaction time in step (3) is 1-80h, for example, 1h, 5h, 10h, 15h, 20h, 25h, 30h, 35h, 40h, 45h, 50h, 55h, 60h, 65h, 70h, 75h or 80h, etc.
Preferably, after the synthesis reaction is finished, stopping heating, introducing protective gas to 30-80Kpa, cooling to room temperature, and taking out the synthesized silicon carbide powder.
The room temperature is not particularly limited in the present invention, and may be exemplified by 25.+ -. 5 ℃, such as 20 ℃, 25 ℃ or 30 ℃ or the like.
In a third aspect, the present invention provides silicon carbide grown using a silicon carbide growth apparatus as described in the first aspect or obtained using a silicon carbide growth method as described in the second aspect.
In the invention, the silicon carbide is alpha phase.
It should be noted that the silicon carbide blocks synthesized by the method are loose, and the conventional jaw, hammer or roller type crushing method is not needed, but the crushing is completed in a hydraulic mode. The hydraulic pressure that this hydraulic pressure mode adopted sets up to design equipment by oneself, and upper and lower clamp plate cladding tantalum sheet, auxiliary parts such as scraper blade, baffle, screen cloth are non-metal material such as polypropylene, polytetrafluoroethylene or nylon, can avoid the introduction of metal. And the crushed silicon carbide is washed by a small amount of pure water, so that carbonaceous dust can be cleaned, and powder materials with impurity ash content meeting the requirement of conductive crystal growth can be obtained after drying.
The numerical ranges recited herein include not only the recited point values, but also any point values between the recited numerical ranges that are not recited, and are limited to, and for the sake of brevity, the invention is not intended to be exhaustive of the specific point values that the recited range includes.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides an improved silicon carbide growing device, the silicon carbide synthesized by the device does not need acid washing treatment subsequently, the material blocks are loose, the conventional crushing process is not needed, the metal pollution problem in the crushing process is avoided, the crushed silicon carbide can be washed by only a small amount of pure water, the consumption of the pure water is effectively reduced, and the cost is reduced.
Drawings
Fig. 1 is a schematic view of a silicon carbide growth apparatus according to an embodiment of the present invention.
Wherein, 1-an insulating layer; 11-an upper heat preservation layer; 12-a side heat preservation layer; 13-a lower heat preservation layer; 2-a crucible; 21-a crucible cover; 3-chamber; 4-a heating element; 41-a column; 42-tray body.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The present embodiment provides a silicon carbide growing device, as shown in fig. 1, including:
a container body;
the heat preservation layer 1 is made of a viscose-based soft carbon felt and is arranged in the container body, the heat preservation layer 1 comprises an upper heat preservation layer 11, a lower heat preservation layer 13 and a side heat preservation layer 12, the upper heat preservation layer 11 is provided with an opening, the opening can accommodate a temperature measuring device, and a heating body 4 is arranged in the lower heat preservation layer 13;
the crucible 2 is made of graphite and is arranged in the heat insulation layer 1, a cavity 3 protruding into the crucible 2 is arranged at the bottom of the crucible 2, the crucible 2 comprises a crucible cover 21 and is positioned at the top of the crucible 2, and a through hole is formed in the crucible cover 21;
the heating element 4 is made of graphite, the heating element 4 comprises a column 41 and a disc 42, the column 41 is embedded into the cavity 3, and the disc 42 is arranged in the heat preservation layer 1;
and the induction coil is arranged around the container body.
Wherein, the ratio of the diameter of the cavity 3 to the diameter of the crucible 2 is 1:5, the ratio of the height of the cavity 3 to the height of the crucible 2 is 1:1.7, the resistivity of the heating element 4 is 12.5 mu Ω·m, the ratio of the diameter of the column 41 to the diameter of the cavity 3 is 0.8:1, the ratio of the height of the column 41 to the height of the cavity 3 is 0.9:1, the ratio of the diameter of the tray 42 to the diameter of the crucible 2 is 0.7:1, the thickness of the tray 42 is 30mm, the porosity of the crucible 2 is 17%, the circumferential diameter of the through holes is 260mm, the average diameter of the holes is 10mm, and the number of the holes is 3.
Example 2
The present embodiment provides a silicon carbide growing device, as shown in fig. 1, including:
a container body;
the heat preservation layer 1 is made of a viscose-based soft carbon felt and is arranged in the container body, the heat preservation layer 1 comprises an upper heat preservation layer 11, a lower heat preservation layer 13 and a side heat preservation layer 12, the upper heat preservation layer 11 is provided with an opening, the opening can accommodate a temperature measuring device, and a heating body 4 is arranged in the lower heat preservation layer 13;
the crucible 2 is made of graphite and is arranged in the heat insulation layer 1, a cavity 3 protruding into the crucible 2 is arranged at the bottom of the crucible 2, the crucible 2 comprises a crucible cover 21 and is positioned at the top of the crucible 2, and a through hole is formed in the crucible cover 21;
the heating element 4 is made of graphite, the heating element 4 comprises a column 41 and a disc 42, the column 41 is embedded into the cavity 3, and the disc 42 is arranged in the heat preservation layer 1;
and the induction coil is arranged around the container body.
Wherein, the ratio of the diameter of the cavity 3 to the diameter of the crucible 2 is 1:6, the ratio of the height of the cavity 3 to the height of the crucible 2 is 1:2.5, the resistivity of the heating element 4 is 12 mu Ω·m, the ratio of the diameter of the column 41 to the diameter of the cavity 3 is 0.9:1, the ratio of the height of the column 41 to the height of the cavity 3 is 0.8:1, the ratio of the diameter of the tray 42 to the diameter of the crucible 2 is 0.6:1, the thickness of the tray 42 is 20mm, the porosity of the crucible 2 is 15%, the diameter of the circumference where the through holes are located is 200mm, the average diameter of the holes is 8mm, and the number of the holes is 6.
Example 3
The present embodiment provides a silicon carbide growing device, as shown in fig. 1, including:
a container body;
the heat preservation layer 1 is made of a viscose-based soft carbon felt and is arranged in the container body, the heat preservation layer 1 comprises an upper heat preservation layer 11, a lower heat preservation layer 13 and a side heat preservation layer 12, the upper heat preservation layer 11 is provided with an opening, the opening can accommodate a temperature measuring device, and a heating body 4 is arranged in the lower heat preservation layer 13;
the crucible 2 is made of graphite and is arranged in the heat insulation layer 1, a cavity 3 protruding into the crucible 2 is arranged at the bottom of the crucible 2, the crucible 2 comprises a crucible cover 21 and is positioned at the top of the crucible 2, and a through hole is formed in the crucible cover 21;
the heating element 4 is made of graphite, the heating element 4 comprises a column 41 and a disc 42, the column 41 is embedded into the cavity 3, and the disc 42 is arranged in the heat preservation layer 1;
and the induction coil is arranged around the container body.
Wherein, the ratio of the diameter of the cavity 3 to the diameter of the crucible 2 is 1:8, the ratio of the height of the cavity 3 to the height of the crucible 2 is 1:1.54, the resistivity of the heating element 4 is 13 mu Ω·m, the ratio of the diameter of the column 41 to the diameter of the cavity 3 is 0.8:1, the ratio of the height of the column 41 to the height of the cavity 3 is 0.9:1, the ratio of the diameter of the tray 42 to the diameter of the crucible 2 is 0.8:1, the thickness of the tray 42 is 50mm, the porosity of the crucible 2 is 18%, the diameter of the circumference where the through holes are located is 300mm, the average diameter of the holes is 15mm, and the number of the holes is 12.
Example 4
This example differs from example 1 in that the ratio of the diameter of the chamber 3 to the diameter of the crucible 2 is 1:2.
The remaining structure and parameters remain the same as in example 1.
Example 5
This example differs from example 1 in that the ratio of the diameter of the chamber 3 to the diameter of the crucible 2 is 1:35.
The remaining structure and parameters remain the same as in example 1.
Example 6
This embodiment differs from embodiment 1 in that the ratio of the height of the chamber 3 to the height of the crucible 2 is 1:1.
The remaining structure and parameters remain the same as in example 1.
Example 7
This embodiment differs from embodiment 1 in that the ratio of the height of the chamber 3 to the height of the crucible 2 is 1:10.
The remaining structure and parameters remain the same as in example 1.
Example 8
This example differs from example 1 in that the average diameter of the holes is 1mm.
The remaining structure and parameters remain the same as in example 1.
Example 9
This example differs from example 1 in that the average diameter of the holes is 20mm.
The remaining structure and parameters remain the same as in example 1.
Comparative example 1
The comparative example is different from example 1 in that the crucible cover 21 is not provided with a through hole.
The remaining structure and parameters remain the same as in example 1.
Comparative example 2
This comparative example is different from example 1 in that the bottom of the crucible 2 is not provided with a chamber 3 protruding inside the crucible 2, and the heat generating body 4 includes only a plate 42.
The remaining structure and parameters remain the same as in example 1.
Application example 1
The application example provides a growth method of silicon carbide, wherein the growth method adopts the growth device described in the embodiment 1, and the growth method comprises the following steps:
(1) Fully and uniformly mixing silicon powder with the particle size D50 of 1mm and carbon powder with the particle size D50 of 50 mu m according to the molar ratio of 1:1, and filling the mixture into a crucible 2;
(2) Placing the silicon carbide growing device into a furnace, and vacuumizing to be less than 10 -3 Pa, maintaining the vacuum degree for 3h;
(3) Heating by adopting power control, wherein the first power is output according to 10% of a set value of 30 kW;
(4) Charging protective gas to 30KPa and maintaining for 1 hr, and vacuumizing to 10 -1 Pa；
Wherein, the steps (2) - (4) are repeated for 5 times, and the protective gas is pure Ar gas;
(5) Raising to a second power, wherein the second power is output according to 15% of a set value of 30kW, and the control pressure is smaller than 1000Pa;
(6) Changing to temperature control, preheating at 1000 ℃ for 5 hours, and maintaining the pressure to be less than 2000Pa;
(7) Heating to 1500deg.C for 5h while maintaining pressure less than 10000Pa;
(8) Filling 1000sccm of pure Ar gas, raising the pressure to 15KPa for 1h, then raising the temperature to 2200 ℃ for 4h, and carrying out synthesis reaction for 40 h;
(9) Stopping heating, filling pure Ar gas to 50KPa, cooling to 25 ℃, and taking out the synthesized silicon carbide;
wherein, steps (2) - (8) can cooperate crucible 2 to reciprocate, and the velocity of movement is 2mm/h, and the travel distance is 40mm, and the purpose is that the upper and lower part is heated and synthesized evenly, further reduces the material piece degree of setting.
Application example 2
The application example provides a growth method of silicon carbide, wherein the growth method adopts the growth device described in the embodiment 2, and the growth method comprises the following steps:
(1) Fully and uniformly mixing silicon powder with the particle diameter D50 of 1mm and carbon powder with the particle diameter D50 of 50 mu m according to the mol ratio of 1.05:1, and filling the mixture into a crucible 2;
(2) Placing the silicon carbide growing device into a furnace, and vacuumizing to be less than 10 -3 Pa, maintaining the vacuum degree for 3h;
(3) Heating by adopting power control, wherein the first power is output according to 5% of a set value of 30 kW;
(4) Charging protective gas to 1KPa and maintaining for 10 hr, and vacuumizing to 10 -1 Pa；
Wherein the protective gas is Ar/H 2 Mixture gas, H 2 The ratio of (2) is 20%;
(5) Raising to a second power, wherein the second power is output according to 25% of a set value of 30kW, and the control pressure is smaller than 1000Pa;
(6) Changing to temperature control, preheating at 900 ℃ for 10 hours, and maintaining the pressure to be less than 2000Pa;
(7) Heating to 1300 ℃ for 1h, and maintaining the pressure to be less than 10000Pa;
(8) Filling 1000sccm of Ar/H 2 Mixed gas (H) 2 The ratio of (2) is 20%), the pressure is increased to 5KPa for 0.5h, then the temperature is increased to 2200 ℃ for 4h, and the synthesis reaction is carried out for 80 h;
(9) Stopping heating and filling Ar/H 2 Mixed gas (H) 2 The ratio of the silicon carbide to the silicon carbide is 20 percent to 30KPa, and after cooling to room temperature, the synthesized silicon carbide is taken out;
wherein, step (2) - (8) can cooperate the upper and lower removal of induction coil, and the velocity of movement is 5mm/h, and the travel distance is 10mm, and the purpose is so that upper and lower part is heated and synthetic even, further reduces the material piece degree of setting.
Application example 3
The application example provides a growth method of silicon carbide, wherein the growth method adopts the growth device described in the embodiment 3, and the growth method comprises the following steps:
(1) Fully and uniformly mixing silicon powder with the particle diameter D50 of 1mm and carbon powder with the particle diameter D50 of 50 mu m according to the molar ratio of 1.1:1, and filling the mixture into a crucible 2;
(2) Placing the silicon carbide growing device into a furnace, and vacuumizing to be less than 10 -3 Pa, maintaining the vacuum degree for 3h;
(3) Heating by adopting power control, wherein the first power is output according to 10% of a set value of 30 kW;
(4) Charging protective gas to 60KPa for 0.5h, and vacuumizing to 10 -1 Pa；
Wherein steps (2) - (4) are repeated 10 times, and the protective gas is He/H 2 Mixture gas, H 2 The ratio of (2) is 20%;
(5) Raising to a second power, wherein the second power is output according to 25% of a set value of 30kW, and the control pressure is smaller than 1000Pa;
(6) Changing to temperature control, preheating at 1200 ℃ for 1h, and maintaining the pressure to be less than 2000Pa;
(7) Heating to 1700 deg.c for 1 hr while maintaining pressure less than 10000Pa;
(8) Filling 1000sccm of He/H 2 Mixed gas (H) 2 The ratio of (2%) is 20%), the pressure is increased to 30KPa for 2 hours, then the temperature is increased to 2300 ℃ for 4 hours, and the synthesis reaction is carried out for 10 hours;
(9) Stopping heating and filling He/H 2 Mixed gas (H) 2 The ratio of the silicon carbide to the silicon carbide is 20 percent to 80KPa, and after cooling to 25 ℃, the synthesized silicon carbide is taken out;
wherein, steps (2) - (8) can cooperate crucible 2 to reciprocate, and the velocity of movement is 20mm/h, and the travel distance is 100mm, and the purpose is that the upper and lower part is heated and synthetic even, further reduces the material piece degree of setting.
Application examples 4 to 9
Application examples 4 to 9 respectively provide a growth method of silicon carbide, which employs the growth apparatuses described in examples 4 to 9 respectively, and which are consistent with application example 1.
Comparative examples 1 to 2 were used
The use of comparative examples 1-2 provides a growth method of silicon carbide, respectively, using the growth apparatus described in comparative examples 1-2, respectively, which all remain the same as in application example 1.
Performance testing
The silicon carbide powders prepared in the above application examples 1 to 9 and comparative examples 1 to 2 were subjected to the appearance of lump, the firmness and the Glow Discharge Mass Spectrum (GDMS) ash test.
Test conditions: and (3) observing the appearance of the material block on site, wherein the firmness is tested by adopting a press, and the contents of Al, fe and Cu in the silicon carbide are tested by GDMS ash.
The test results are shown in Table 1.
TABLE 1
/>
Analysis:
from the table, the invention provides an improved silicon carbide growth device, the silicon carbide synthesized by the device does not need acid washing treatment subsequently, the material blocks are loose, the conventional crushing process is not needed, the metal pollution problem in the crushing process is avoided, the crushed silicon carbide can be washed by only a small amount of pure water, the consumption of the pure water is effectively reduced, and the cost is reduced.
As can be seen from the data of application examples 1 and 4-5, the ratio of the diameter of the chamber to the diameter of the crucible is too small, i.e. the diameter of the chamber is too small, so that the size of the central columnar heating element is limited, the central radial heat compensation is insufficient, the effect of uniform temperature cannot be achieved, the material block still has the condition of solid agglomeration, and the impurity removal is insufficient; if the ratio of the diameter of the chamber to the diameter of the crucible is too large, i.e. the diameter of the chamber is too large, the central compensation temperature and the compensation area are too large, so that the synthesized powder is carbonized in a large area, and the yield and the quality are affected.
As can be seen from the data of application examples 1 and 6-7, the ratio of the height of the chamber to the height of the crucible is too small, i.e. the height of the chamber is too small, which can cause the limitation of the size of the central columnar heating element, the insufficiency of the axial temperature compensation area, the uneven effect of the top and bottom temperature, and the phenomenon of more solid agglomeration at the lower part of the material block; if the ratio of the height of the cavity to the height of the crucible is too large, namely the height of the cavity is too large, the crucible containing area becomes small, the single synthesis weight is limited, and on the other hand, the central compensation temperature and the compensation area are too large, so that large-area carbonization of synthesized powder in the crucible is easily caused, and the yield and the quality are affected.
As can be seen from the data of application examples 1 and 8 to 9, if the average diameter of the holes is too small, the impurity removal is insufficient, the efficacy on the temperature gradient is weakened, and the center caking and bottom carbonization are easily caused; if the average diameter of the holes is too large, the upper heat preservation is poor, caking and firmness are easy to occur at the top of the material block, the material block is difficult to break, and a large amount of silicon gas is dissipated into a thermal field, so that a graphite piece and a heat preservation structure are damaged.
As is clear from the data of application example 1 and application comparative example 1, if no through hole is formed in the crucible cover, carbonization of the bottom of the block is relatively increased, and the impurity removing effect is deteriorated.
As is clear from the data of application example 1 and application comparative example 2, if the bottom of the crucible is not provided with a cavity protruding from the inside of the crucible, and the heating element only includes a plate body, the temperature gradient increases, the lower part of the block shows signs of blackening in a large area, dense crystallization occurs at the top due to the large temperature gradient, the crushing is difficult under a press, and the probability of recrystallization of the generated impurity gas in the material under the large temperature gradient increases, and the detected metal impurities also relatively increase.
The applicant states that the process of the invention is illustrated by the above examples, but the invention is not limited to, i.e. does not mean that the invention must be carried out in dependence on the above process steps. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of selected raw materials, addition of auxiliary components, selection of specific modes, etc. fall within the scope of the present invention and the scope of disclosure.
Claims (25)
1. A silicon carbide growing device, comprising:
a container body;
the heat preservation layer is arranged in the container body, an opening is formed in the top of the heat preservation layer, and the opening can accommodate the temperature measuring device;
the crucible is arranged in the heat preservation layer, a cavity protruding into the crucible is formed in the bottom of the crucible, the crucible comprises a crucible cover, the crucible cover is positioned at the top of the crucible, and a through hole is formed in the crucible cover;
the diameter of the circumference of the through hole is 200-300mm;
the average diameter of the holes is 3-10mm;
the number of the holes is 3-6;
the heating body comprises a column body and a disc body, the column body is embedded into the cavity, and the disc body is arranged in the heat preservation layer;
the ratio of the diameter of the cavity to the diameter of the crucible is 1 (3-6);
the ratio of the height of the cavity to the height of the crucible is 1 (1.5-2.5);
and the induction coil is arranged around the container body.
2. The silicon carbide growing device according to claim 1, wherein the heating element is a conductive material.
3. The silicon carbide growing device of claim 2, wherein the conductive material comprises graphite.
4. The silicon carbide growing device according to claim 1, wherein the resistivity of the heating element is greater than that of the crucible.
5. The silicon carbide growing device according to claim 1, wherein the electric resistivity of the heat-generating body is 10 to 13 μΩ ∙ m.
6. The silicon carbide growth device as claimed in claim 1, wherein the ratio of the diameter of the cylinder to the diameter of the chamber is (0.4-0.9): 1.
7. The silicon carbide growing device according to claim 1, wherein the ratio of the diameter of the disk to the diameter of the crucible is (0.6-1.2): 1.
8. The silicon carbide growing device of claim 1, wherein the thickness of the tray is 10-50mm.
9. The silicon carbide growing device of claim 1, wherein the crucible material comprises graphite.
10. The silicon carbide growing device according to claim 1, wherein the porosity of the crucible is 15-18%.
11. A silicon carbide growing device according to claim 1 wherein the crucible or induction coil is movable up and down.
12. A silicon carbide growth apparatus according to claim 1 wherein the speed of movement of the crucible or the induction coil is independently 0-20mm/h.
13. A silicon carbide growth apparatus according to claim 1 wherein the distance of movement of the crucible or the induction coil is independently 10-100mm.
14. The silicon carbide growing device according to claim 1, wherein the heat-insulating layer comprises an upper heat-insulating layer, a lower heat-insulating layer, and a side heat-insulating layer, the upper heat-insulating layer being provided with an opening, the lower heat-insulating layer being provided with the heating element.
15. The silicon carbide growing device of claim 1, wherein the insulating layer is a thermal insulating material.
16. A method of growing silicon carbide, wherein the method employs the silicon carbide growing apparatus according to any one of claims 1 to 15, the method comprising the steps of:
(1) Placing a silicon source and a carbon source into a crucible for pretreatment to remove impurity gas;
(2) Heating a heating body through an induction coil, so that the crucible is subjected to primary heating at a temperature T1;
(3) And (3) carrying out a synthesis reaction at a temperature T2 to obtain the silicon carbide.
17. The growth method according to claim 16, wherein the step of pre-treating of step (1) comprises:
(a) Vacuumizing and heating under the first power;
(b) Charging protective gas, and vacuumizing;
(c) To a second power and then to preheat.
18. A method of growing according to claim 17 wherein the first power is 1-10% of the set power value.
19. A method of growing according to claim 17 wherein the second power is 3-25% of the set power value.
20. A method of growing according to claim 17 wherein the pre-heating is at a temperature of 900-1200 ℃.
21. The growth method according to claim 16, wherein T1 in step (2) is 1300-1700 ℃.
22. The growth method according to claim 16, wherein the primary heating in step (2) is performed for a period of 1 to 30 hours.
23. The growth method according to claim 16, wherein the synthesis reaction of step (3) is performed in a protective atmosphere.
24. The growth method according to claim 16, wherein T2 in step (3) is 2000-2300 ℃.
25. The growth method according to claim 16, wherein the synthesis reaction in step (3) takes 1 to 80 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310623791.2A CN116623284B (en) | 2023-05-30 | 2023-05-30 | Silicon carbide and growth device and growth method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310623791.2A CN116623284B (en) | 2023-05-30 | 2023-05-30 | Silicon carbide and growth device and growth method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116623284A CN116623284A (en) | 2023-08-22 |
| CN116623284B true CN116623284B (en) | 2024-02-23 |
Family
ID=87613070
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310623791.2A Active CN116623284B (en) | 2023-05-30 | 2023-05-30 | Silicon carbide and growth device and growth method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116623284B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010105863A (en) * | 2008-10-30 | 2010-05-13 | Bridgestone Corp | Apparatus and method for manufacturing silicon carbide single crystal |
| CN112919473A (en) * | 2021-04-22 | 2021-06-08 | 山西烁科晶体有限公司 | Method for synthesizing low-nitrogen high-purity silicon carbide powder |
| CN113120909A (en) * | 2021-03-09 | 2021-07-16 | 浙江晶越半导体有限公司 | Preparation method of high-purity semi-insulating silicon carbide powder |
| CN218166979U (en) * | 2022-08-29 | 2022-12-30 | 宁波合盛新材料有限公司 | Device for synthesizing high-purity silicon carbide raw material |
| CN115676833A (en) * | 2021-07-28 | 2023-02-03 | 北京北方华创微电子装备有限公司 | Method for improving synthesis efficiency of silicon carbide powder |
-
2023
- 2023-05-30 CN CN202310623791.2A patent/CN116623284B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010105863A (en) * | 2008-10-30 | 2010-05-13 | Bridgestone Corp | Apparatus and method for manufacturing silicon carbide single crystal |
| CN113120909A (en) * | 2021-03-09 | 2021-07-16 | 浙江晶越半导体有限公司 | Preparation method of high-purity semi-insulating silicon carbide powder |
| CN112919473A (en) * | 2021-04-22 | 2021-06-08 | 山西烁科晶体有限公司 | Method for synthesizing low-nitrogen high-purity silicon carbide powder |
| CN115676833A (en) * | 2021-07-28 | 2023-02-03 | 北京北方华创微电子装备有限公司 | Method for improving synthesis efficiency of silicon carbide powder |
| CN218166979U (en) * | 2022-08-29 | 2022-12-30 | 宁波合盛新材料有限公司 | Device for synthesizing high-purity silicon carbide raw material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116623284A (en) | 2023-08-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100523315C (en) | Split type tantalum crucible and manufacturing method thereof | |
| KR101413653B1 (en) | A method for manufacturing SiC powders with high purity | |
| TWI248916B (en) | Flexible high purity expanded graphite sheet, and carbon crucible lining using said sheet | |
| CN109502589A (en) | A method of preparing high-purity silicon carbide powder | |
| CN110396717B (en) | High-quality high-purity semi-insulating silicon carbide single crystal, substrate and preparation method thereof | |
| KR101976594B1 (en) | Silicon carbide powder, method for manufacturing the same and method for fabricating single crystal | |
| CN102296362A (en) | Single-crystal diamond growth base material and method for manufacturing single-crystal diamond substrate | |
| CN110016718A (en) | A kind of processing method for growing silicon carbide crystal with high quality feedstock purification | |
| WO2015061160A1 (en) | Process for making chemically activated carbon | |
| CN114182357A (en) | Method for regrowing silicon carbide single crystal by using broken crystal grains of silicon carbide crystal | |
| JP2011162414A (en) | Method for producing silicon carbide crystal and silicon carbide crystal | |
| CN111424320B (en) | Crucible, growth method and growth device for silicon carbide single crystal growth | |
| JP2018016498A (en) | Method for manufacturing silicon carbide single crystal ingot | |
| JP2011219286A (en) | Method and system for manufacturing silicon and silicon carbide | |
| JP2019112241A (en) | Silicon carbide growth apparatus with specific shape | |
| CN110565167A (en) | Charging device and charging method for growing SiC single crystal by PVT method | |
| CN102021653A (en) | Method for growing silicon carbide single crystal by using high-density material block | |
| CN116623284B (en) | Silicon carbide and growth device and growth method thereof | |
| US20040250764A1 (en) | Method and apparatus for production of high purity silicon | |
| KR20150123806A (en) | Method for producing silicon carbide and silicon carbide | |
| KR20200044596A (en) | Recycling method of SiC by-product from the deposition process into the source of single crystal | |
| JP2009184897A (en) | Method for manufacturing silicon carbide single crystal | |
| CN111575801B (en) | Preparation method and wafer growth raw material | |
| CN116119670A (en) | Preparation method of ultralow N, B content silicon carbide raw material | |
| US8282904B2 (en) | Cylindrical vessel made of carbon and process for making silicon |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |