CN104514034A - High-temperature device and method for silicon carbide growth - Google Patents
High-temperature device and method for silicon carbide growth Download PDFInfo
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- CN104514034A CN104514034A CN201510008972.XA CN201510008972A CN104514034A CN 104514034 A CN104514034 A CN 104514034A CN 201510008972 A CN201510008972 A CN 201510008972A CN 104514034 A CN104514034 A CN 104514034A
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- silicon carbide
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 46
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000009413 insulation Methods 0.000 claims abstract description 9
- 239000000779 smoke Substances 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 35
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 17
- 239000001301 oxygen Substances 0.000 claims description 17
- 229910052760 oxygen Inorganic materials 0.000 claims description 17
- 239000000567 combustion gas Substances 0.000 claims description 15
- 239000012159 carrier gas Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000002485 combustion reaction Methods 0.000 claims description 6
- 238000010276 construction Methods 0.000 claims description 6
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 6
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 claims description 6
- 229910003468 tantalcarbide Inorganic materials 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 5
- 239000004215 Carbon black (E152) Substances 0.000 claims description 4
- 239000007770 graphite material Substances 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000005611 electricity Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
Abstract
The invention relates to a high-temperature device and method for silicon carbide growth. The device comprises a housing, a growth chamber, a gas outlet pipe, a temperature detector, a growth source gas inlet pipe, a rotatable loading disc, a gas distribution disc, a heater, a thermal insulation layer and a smoke exhaust pipe, wherein the housing adopts a cylindrical structure; the growth chamber adopts a cylindrical structure and is located in the middle of the housing; the gas outlet pipe and the temperature detector are fixed at the top of the growth chamber; the growth source gas inlet pipe is located on the side wall in the growth chamber and extends to the bottom of the growth chamber; the rotatable loading disc is connected to the middle of the growth chamber through a shaft rod from top to bottom; the gas distribution disc is fixed at the bottom of the growth chamber; the heater is located below the growth chamber and in the housing, and a burning chamber is formed between the heater and the growth chamber; the thermal insulation layer surrounds the growth chamber; one end of the smoke exhaust pipe is fixed on the thermal insulation layer and communicated with the burning chamber, and the other end of the smoke exhaust pipe extends out of a room via the housing. The device and the method provided by the invention can avoid high electricity consumption, increase the production efficiency and lower the energy consumption.
Description
Technical field
The present invention relates to technical field of semiconductors, particularly relate to a kind of high temperature service and method of growth of silicon carbide, can be used for the growth of bulk single crystal silicon carbide and the quick growth of silicon carbide homogeneity thick film epitaxial material.
Background technology
Silicon carbide (SiC) is third generation semiconductor material, due to its band gap length, 3.2eV can be reached, it is 3 times of Si, therefore, it has high critical breakdown electric field (10 times of Si), the features such as high carrier saturation concentration (2 times of Si), in addition, it also has the feature of high heat conductance (3 times of Si), therefore, it is at military and high temperature that is space industry, high frequency, high-power electric and electronic, photoelectric device aspect has superior using value, and be expected to progressively replace existing silica-based high power device, become the base mateiral of power electronic semiconductor of future generation.
Silicon carbide single crystal material generally adopts the method for physical vapor transport (PVT) to be prepared.As shown in Figure 1, its core is employing one high temperature service, and scheme adopts several groups of radio-frequency heaters 103, induction heating carried out in growth of graphite room 105, makes raw material district 112 be in a high-temperature field (about 2100 degrees Celsius), sic raw material is distilled; Between raw material district 112 and seed crystal 111, set up a negative temperature gradient, make silicon carbide crystalline growth on seed crystal 111.PVT method growth velocity is generally 200-300 micron per hour, affects by this, and growing a thick crystal of 20 centimetres needs 3-5 days time, and institute's power consumption is huge.Power consumption is the one of the main reasons that current PVT method carborundum crystals cost remains high.If improve growth velocity, then need higher growth temperature and better thermograde.
In addition, the occasion such as rheotaxy (LPE), chemical vapour deposition (CVD) of silicon carbide generally needs the growing environment of 17002000 degrees Celsius, also needs to adopt high temperature service.The type of heating mainly electrically heated of current employing, as resistive heating or radio-frequency induction heating, by type of heating, efficiency and the impact of holding time, can cause a large amount of power consumption, raise the cost of manufacturing silicon carbide semiconductor.
Summary of the invention
In order to solve the problem, the invention provides a kind of high temperature service for growth of silicon carbide and method, employing flame heats, efficient, the high energy of gas flame is utilized to produce and maintain growth room's high temperature, required hot environment can be provided for PVT, LPE, CVD preparation of silicon carbide, compared with electrically heated, both can avoid huge power consumption, and can enhance productivity again, reduce energy consumption etc.
The invention provides a kind of high temperature service for growth of silicon carbide, comprising:
One shell is tubular construction;
One growth room, be tubular construction, it is positioned at the centre of shell;
One escape pipe, it is fixed on the top of growth room;
One hygrosensor, it is fixed on the top of growth room;
One growth source inlet pipe, it is positioned at the sidewall of growth room, and leads to the bottom of growth room;
One rotatable load plate, it is connected to the middle part of growth room from top to bottom by an axostylus axostyle;
One even gas dish, it is fixed on the bottom of growth room;
One well heater, it is positioned at below growth room, in the enclosure, forms a combustion chamber between this well heater and growth room;
One thermal insulation layer, it is centered around the outside of growth room;
One smoke exhaust pipe, its one end is fixed on thermal insulation layer and is communicated with combustion chamber, and the other end leads to outdoor through shell.
The present invention also provides a kind of growth of silicon carbide method, and it adopts high temperature service as claimed in claim 1, comprises the steps:
Step 1: silicon carbide seed is fixed on rotatable load plate, raw material powder is placed in even gas dish, vacuumizes;
Step 2: pass into reductibility carrier gas in growth room;
Step 3: the inlet pipe opening well heater, passes into combustion gas and oxygen, controls to be warming up to growth temperature;
Step 4: in temperature-rise period, passes into silicon source gas, when arriving growth temperature, passes into carbon-source gas;
Step 5: close silicon source gas, pass into rare gas element;
Step 6: close carbon-source gas, closes reductibility carrier gas, completes the growth of silicon carbide;
Step 7: the flow reducing combustion gas and oxygen, closes oxygen and combustion gas subsequently, closes well heater 30, cooling.
Well heater of the present invention is made up of flame spray dish, admission passage, smoke-exhaust pipeline, the temperature regulator that form feedback system with hygrosensor, and reliably, easy and simple to handle, security is high, can reach the object of continuous firing for its structure.
Accompanying drawing explanation
For further illustrating technology contents of the present invention, be described in detail as follows below in conjunction with embodiment and accompanying drawing, wherein:
Fig. 1 is high temperature service schematic diagram in prior art;
Fig. 2 is the schematic diagram of the high temperature service embodiment for growth of silicon carbide provided by the invention;
Fig. 3 is method flow diagram of the present invention;
Fig. 4 is the schematic diagram of an embodiment of growth of silicon carbide method provided by the invention;
Fig. 5 is the schematic diagram of another embodiment of growth of silicon carbide method provided by the invention.
Embodiment
Below in conjunction with accompanying drawing, exemplary embodiments of the present invention are described.For clarity and brevity, actual embodiment is not limited to these technical characteristics described in specification sheets.It should be understood, however, that in the process improving practical embodiments described in any one, the decision of multiple specific embodiment must be the specific objective that can realize improvement personnel, such as, defer to industry and to be correlated with the restriction relevant with business, described restriction changes along with the difference of embodiment.And even it should be understood that the effect of aforementioned improved is very complicated and consuming time, but this remains routine techniques means for the those skilled in the art knowing benefit of the present invention.
Refer to shown in Fig. 2, the invention provides a kind of high temperature service for growth of silicon carbide, comprising:
One shell 21 is tubular construction;
One growth room 24, be tubular construction, it is positioned at the centre of shell 21, and its material is high purity graphite material or high-purity zirconia pottery, and inwall scribbles tantalum carbide coating;
One escape pipe 25, it is fixed on the top of growth room 24;
One hygrosensor 26, it is fixed on the top of growth room 24;
One growth source inlet pipe 27, it is positioned at the sidewall of growth room 24, and leads to the bottom of growth room 24;
One rotatable load plate 28, it is connected to the middle part of growth room 24 from top to bottom by an axostylus axostyle, its material is high-purity, high strength, high-density graphite material, and surface covers through silicon carbide or tantalum carbide coating;
One even gas dish 29, it is fixed on the bottom of growth room 24, with raw material tank, is high purity graphite material or high-purity zirconia pottery, with tantalum carbide coating;
One well heater 30, it is positioned at below growth room 24, in shell 21, forms a combustion chamber between this well heater 30 and growth room 24, described well heater 30 is made up of a flame spray dish 301, support bar 302 and inlet pipe 303, and described flame spray dish 301 is quartzy material or metal material;
One thermal insulation layer 22, it is centered around the outside of growth room 24, and its material is silica aerogel paper;
One smoke exhaust pipe 23, its one end is fixed on thermal insulation layer 22 and is communicated with combustion chamber, and the other end leads to outdoor through shell 21.
Refer to shown in Fig. 3, and Fig. 2 is consulted in combination, the invention provides a kind of growth of silicon carbide method, comprises the steps:
Step 1: silicon carbide seed be fixed on rotatable load plate 28, raw material powder is placed in even gas dish 29, vacuumizes;
Step 2: pass into reductibility carrier gas in growth room 24, described in pass into growth room 24 carrier gas be the mixed gas of H2 or H2 and rare gas element Ar;
Step 3: the inlet pipe 303 opening well heater 30, pass into combustion gas and oxygen, control is warming up to growth temperature, it is two growth temperature sections that described control is warming up to growth temperature, first temperature section is 1300-1500 degree Celsius, and the second temperature section is 1700-2300 degree Celsius, described in pass into inlet pipe 303 combustion gas be hydrocarbon polymer, preferably, this hydrocarbon polymer is acetylene;
Step 4: in temperature-rise period, passes into silicon source gas, when arriving growth temperature, passes into carbon-source gas;
Step 5: close silicon source gas, pass into rare gas element;
Step 6: close carbon-source gas, closes reductibility carrier gas, completes the growth of silicon carbide;
Step 7: the flow reducing combustion gas and oxygen, closes oxygen and combustion gas subsequently, closes well heater 30, cooling.
Refer to shown in Fig. 4, the invention provides a kind of growth of silicon carbide method, preferably, comprise the steps:
Step 1: 1 inclined 4 end 4H-SiC (0001) substrate slice of 4 inches of N-shapeds is fixed on rotatable load plate 28,500 grams of high-purity silicon carbide raw material powders is placed in the raw material tank on even gas dish 29, is evacuated to 1E-3 handkerchief,
After step 2:1 hour, in growth room 24, pass into reductibility carrier gas H
2, flow is 10slm, and to arrange growth room's air pressure be 5000 handkerchiefs.
Step 3: after stablizing for about 5 minutes, open the inlet pipe 303 of well heater 30, first pass into acetylene (C
2h
2), light, then pass into oxygen (O
2), regulating gas/oxygen proportion is 2/1, and acetylene flow is adjusted to 1.5slm gradually, makes torch height reach 10 centimetres.
Step 4: in temperature-rise period, when temperature is higher than 1600 degrees Celsius, passes into the silicon source gas SiH of 80sccm
4.When arriving growth temperature 2100 degrees Celsius, pass into the carbon-source gas C of 80sccm
2h
4.
Step 5: be incubated after 10 minutes, closes SiH
4, reduce H2 flow to 2slm, pass into rare gas element Ar simultaneously, in this process, keep H
2flow and Ar flow sum are 10slm.
C is closed after step 6:10 minute
2h
4, close H
2, keep logical Ar, and make Ar flow be 10slm.Now carry out silicon carbide PVT growth, grow the growth completing silicon carbide after 2 hours;
Step 7: reduce combustion gas C2H2 and oxygen O
2flow, close oxygen and combustion gas subsequently, close well heater flame, growth room's Temperature fall.
Shown in Fig. 5, the invention provides a kind of growth of silicon carbide method, preferably, comprise the steps:
Step 1: 1 inclined 4 end 4H-SiC (0001) substrate slice of 4 inches of p-types is fixed on rotatable load plate 28, is evacuated to 1E-3 handkerchief,
After step 2:1 hour, in growth room 24, pass into reductibility pass into carrier gas H2, flow is 10slm, and to arrange growth room's air pressure be 5000 handkerchiefs.
Step 3: after stablizing for about 5 minutes, open the inlet pipe 303 of well heater 30, first pass into acetylene (C2H
2), light, then pass into oxygen (O
2), regulating gas/oxygen proportion is 1/1, and acetylene flow is adjusted to 1slm gradually, makes torch height reach 8 centimetres.
Step 4: when temperature reaches 1400 degrees Celsius, keeps 1 hour, makes H2 carry out etched clean to substrate slice surface.After this continue to heat up, in temperature-rise period, pass into the silicon source gas SiH of 20sccm
4.When temperature arrives 1600 degrees Celsius, pass into the carbon-source gas C of 10sccm
2h
4.When temperature arrives 2000 degrees Celsius, increase SiH
4and C
2h
4flow, make it to reach 120sccm and 100sccm respectively, now carry out silicon carbide HTCVD growth.
Step 5: be incubated after 100 minutes, closes SiH
4;
C is closed after step 6:5 minute
2h
4, complete the growth of silicon carbide, keep logical H
2, and make H
2flow is 10slm.
Step 7: reduce combustion gas C
2h
2with oxygen O
2flow, close oxygen and combustion gas subsequently, close well heater flame, make growth room's Temperature fall.
Although based on some preferred embodiments, invention has been described, and those skilled in the art should know, and scope of the present invention is not limited to those embodiments.Without departing from the spirit and substance in the present invention, those of ordinary skill in the art can carry out variations and modifications to embodiment on understanding basis of the present invention, and therefore falls into the protection domain of claims of the present invention restriction.
Claims (10)
1., for a high temperature service for growth of silicon carbide, comprising:
One shell is tubular construction;
One growth room, be tubular construction, it is positioned at the centre of shell;
One escape pipe, it is fixed on the top of growth room;
One hygrosensor, it is fixed on the top of growth room;
One growth source inlet pipe, it is positioned at the sidewall of growth room, and leads to the bottom of growth room;
One rotatable load plate, it is connected to the middle part of growth room from top to bottom by an axostylus axostyle;
One even gas dish, it is fixed on the bottom of growth room;
One well heater, it is positioned at below growth room, in the enclosure, forms a combustion chamber between this well heater and growth room;
One thermal insulation layer, it is centered around the outside of growth room;
One smoke exhaust pipe, its one end is fixed on thermal insulation layer and is communicated with combustion chamber, and the other end leads to outdoor through shell.
2. the high temperature service for growth of silicon carbide according to claim 1, the inwall of wherein said growth room scribbles tantalum carbide coating.
3. the high temperature service for growth of silicon carbide according to claim 1, the surface of wherein said rotatable load plate covers through silicon carbide or tantalum carbide coating.
4. the high temperature service for growth of silicon carbide according to claim 1, wherein said even gas dribbling has raw material tank, is high purity graphite material or high-purity zirconia pottery, with tantalum carbide coating.
5. the high temperature service for growth of silicon carbide according to claim 1, wherein said well heater is made up of a flame spray dish, support bar and inlet pipe.
6. a growth of silicon carbide method, it adopts high temperature service as claimed in claim 1, comprises the steps:
Step 1: silicon carbide seed is fixed on rotatable load plate, raw material powder is placed in even gas dish, vacuumizes;
Step 2: pass into reductibility carrier gas in growth room;
Step 3: the inlet pipe opening well heater, passes into combustion gas and oxygen, controls to be warming up to growth temperature;
Step 4: in temperature-rise period, passes into silicon source gas, when arriving growth temperature, passes into carbon-source gas;
Step 5: close silicon source gas, pass into rare gas element;
Step 6: close carbon-source gas, closes reductibility carrier gas, completes the growth of silicon carbide;
Step 7: the flow reducing combustion gas and oxygen, closes oxygen and combustion gas subsequently, closes well heater 30, cooling.
7. growth of silicon carbide method according to claim 6, it is two growth temperature sections that wherein said control is warming up to growth temperature, and the first temperature section is 1300-1500 degree Celsius, and the second temperature section is 1700-2300 degree Celsius.
8. growth of silicon carbide method according to claim 6, the wherein said carrier gas passing into growth room 24 is H
2or H
2with the mixed gas of rare gas element Ar.
9. growth of silicon carbide method according to claim 6, the combustion gas wherein passing into described inlet pipe is hydrocarbon polymer.
10. growth of silicon carbide method according to claim 9, the hydrocarbon polymer wherein passing into described inlet pipe is acetylene.
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Cited By (4)
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---|---|---|---|---|
CN106048729A (en) * | 2016-06-28 | 2016-10-26 | 山东天岳先进材料科技有限公司 | Device for growing large-diameter silicon carbide crystal by PVT method |
CN108298543A (en) * | 2018-04-27 | 2018-07-20 | 王金波 | It is a kind of using flame as the preparation method of the high-purity silicon carbide powder of heat source |
CN113026106A (en) * | 2021-05-19 | 2021-06-25 | 浙江大学杭州国际科创中心 | Growth process of silicon carbide crystal |
CN114975097A (en) * | 2022-04-11 | 2022-08-30 | 江苏超芯星半导体有限公司 | Silicon carbide crystal and preparation method and application thereof |
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CN106048729A (en) * | 2016-06-28 | 2016-10-26 | 山东天岳先进材料科技有限公司 | Device for growing large-diameter silicon carbide crystal by PVT method |
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CN114975097A (en) * | 2022-04-11 | 2022-08-30 | 江苏超芯星半导体有限公司 | Silicon carbide crystal and preparation method and application thereof |
CN114975097B (en) * | 2022-04-11 | 2024-02-23 | 江苏超芯星半导体有限公司 | Silicon carbide crystal and preparation method and application thereof |
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