CN115786871A - Silicon carbide coating graphite base and preparation method thereof - Google Patents
Silicon carbide coating graphite base and preparation method thereof Download PDFInfo
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- CN115786871A CN115786871A CN202211650737.9A CN202211650737A CN115786871A CN 115786871 A CN115786871 A CN 115786871A CN 202211650737 A CN202211650737 A CN 202211650737A CN 115786871 A CN115786871 A CN 115786871A
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Abstract
The application discloses a silicon carbide coating graphite base and a preparation method thereof, wherein the preparation method comprises the steps of firstly forming a SiC base layer on the surface of the graphite base by adopting a CVR (chemical vapor deposition) technology, then forming a SiC intermediate layer on the SiC base layer by adopting an HPCVD (high pressure chemical vapor deposition) technology, and finally forming a SiC outer layer on the SiC intermediate layer by adopting an LPCVD technology, wherein the SiC base layer is tightly combined with the graphite base, no obvious interface exists between the SiC intermediate layer and the SiC base layer, the density of the whole coating and the bonding strength of the coating and the graphite base are effectively improved, the deposition speed of the SiC intermediate layer is accelerated under the action of high pressure, and the manufacturing cost is effectively reduced; when the thickness of the coating reaches 100 mu m, only the total deposition time less than or equal to 10h is needed, so that the production cost is saved, and the industrialization is facilitated; the SiC outer layer is smooth and compact, and the surface roughness is effectively reduced.
Description
Technical Field
The application relates to the technical field of graphite bases of semiconductors, in particular to a silicon carbide coating graphite base and a preparation method thereof.
Background
Because of its superior properties such as large forbidden band width, high breakdown electric field, large thermal conductivity, high electron saturation drift rate, and strong radiation resistance, the third-generation semiconductor material represented by gallium nitride (GaN) is widely used in the fields of solid-state light sources, cores of power electronics and microwave radio-frequency devices, semiconductor lighting, and the like. Particularly, because the GaN material has the characteristics of high efficiency, low loss and high frequency, the GaN material has great application potential in the fields of semiconductor illumination (LED) and display.
Currently, gaN single crystal epitaxial growth technology is the most commonly used method for preparing single crystal GaN, wherein a silicon carbide (SiC) coated graphite susceptor is a key consumable in production, and the performance and quality of the susceptor play a crucial role in the quality of the wafer epitaxial layer. The silicon carbide coated graphite susceptor has unique advantages: high purity, compactness, uniformity and excellent thermal shock resistance and oxidation resistance, and improves the product quality and the process efficiency, thereby realizing the reduction of the whole operation cost. The preparation method of the silicon carbide coating graphite base is widely applied to Chemical Vapor Deposition (CVD) and Chemical Vapor Reaction (CVR). Wherein, CVD mainly comprises: low-pressure Chemical Vapor Deposition (Low-pressure Chemical Vapor Deposition, abbreviated to LP CVD) and High-pressure Chemical Vapor Deposition (High-pressure Chemical Vapor Deposition, abbreviated to HP CVD).
Although the SiC coating prepared by the common chemical vapor deposition method and the chemical reaction method has high purity and good density, the deposition speed is slow, the coating thickness of 100 mu m needs to be deposited for 20 hours or more, and the production cost is very high.
Disclosure of Invention
The invention provides a silicon carbide coating graphite base and a preparation method thereof, and aims to solve the technical problems of long time consumption and high cost in preparation of the silicon carbide coating graphite base in the prior art.
The technical scheme provided by the invention is as follows:
in a first aspect of the invention, a preparation method of a graphite base coated with silicon carbide is provided, which comprises the following steps:
s1, pretreating a graphite base and then placing the pretreated graphite base in a vacuum furnace; mixing Si powder with SiO 2 Mixing the powder and placing the powder in the vacuum furnace; vacuumizing the vacuum furnace, introducing argon to protect the vacuum furnace, heating to 1850-2050 ℃, preserving the temperature, and forming a SiC base layer on the surface of the graphite base;
s2, reducing the temperature in the vacuum furnace to 1050-1200 ℃, setting the pressure to 1-150 KPa, conveying trichloromethyl silane into the vacuum furnace through carrier gas, introducing diluent gas, and preserving heat to form a SiC intermediate layer on the SiC base layer;
s3, adjusting the pressure in the vacuum furnace to 0.4 KPa-1 KPa, conveying trichloromethylsilane into the vacuum furnace through carrier gas, introducing diluent gas, preserving heat, and forming an SiC outer layer on the SiC intermediate layer.
Further, in the step S1, the Si powder and the SiO 2 The mol ratio of the powder is 1.05-1.10: 1.
Further, in step S2, the SiC intermediate layer is formed for 2h.
Further, in step S3, the SiC outer layer is formed for 4 hours.
In step S2 and step S3, the carrier gas is hydrogen, and the diluent gas is argon or hydrogen.
Further, in the step S2 and the step S3, the flow rate of the carrier gas hydrogen is 2L/min, the flow rate of the argon gas is 6L/min, and the flow rate of the diluent hydrogen is 5L/min.
Further, in the step S2 and the step S3, the flow ratio of the carrier gas hydrogen to the trichloromethylsilane is 10: 1.
Further, a total thickness of the SiC base layer formed in the step S2 and the SiC intermediate layer formed in the step S1 is greater than or equal to 100 μm.
In a second aspect of the present invention, a silicon carbide coated graphite susceptor is provided, which is prepared by the above-mentioned preparation method of the silicon carbide coated graphite susceptor.
Further, the SiC intermediate layer is filled in the pores of the SiC base layer.
According to the preparation method of the silicon carbide coating graphite base, firstly, a SiC base layer is formed on the surface of the graphite base by adopting a CVR technology, then a SiC intermediate layer is formed on the SiC base layer by adopting an HPCVD technology, and finally a SiC outer layer is formed on the SiC intermediate layer by adopting an LPCVD technology, wherein the SiC base layer is tightly combined with the graphite base, no obvious interface exists between the SiC intermediate layer and the SiC base layer, the density of the whole coating and the bonding strength of the coating and the graphite base are effectively improved, the deposition speed of the SiC intermediate layer is accelerated under the action of high pressure, and the manufacturing cost is effectively reduced; the SiC outer layer is smooth and compact, and the surface roughness is effectively reduced. According to the preparation method of the silicon carbide coating graphite base, the HPCVD technology, the LPCVD technology and the CVR technology are combined, the performance of the SiC coating is guaranteed, the deposition time of the coating is greatly shortened, when the thickness of the coating reaches 100 micrometers, only the total deposition time less than or equal to 10 hours is needed, the production cost is saved, and the industrialization is facilitated.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a flow chart of a method for preparing a silicon carbide coated graphite susceptor in an embodiment of the present invention;
FIG. 2 is a schematic representation of the surface micro-topography of the coating on the silicon carbide coated graphite susceptor prepared in example 1 of the present invention;
FIG. 3 is a schematic illustration of the thickness of a coating on a silicon carbide coated graphite susceptor prepared in example 1 of the present invention;
FIG. 4 is a schematic representation of the coating cross-sectional micro-topography on the silicon carbide coated graphite susceptor prepared in example 1 of the present invention;
FIG. 5 is a microscope photograph of an epitaxially grown GaN single crystal on a silicon carbide-coated graphite susceptor prepared in example 1 of the present invention;
FIG. 6 is a plan view of a high-temperature furnace test specimen after GaN single crystals are epitaxially grown on a graphite susceptor coated with silicon carbide prepared in example 1 of the present invention;
fig. 7 is a bottom view of a high-temperature furnace test performed on a silicon carbide-coated graphite susceptor obtained in example 1 of the present invention after GaN single crystals were epitaxially grown thereon.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all 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 application.
It should be understood that the structures, ratios, sizes, etc. shown in the drawings are only used for matching the disclosure of the present disclosure to be understood and read by those skilled in the art, and are not used to limit the practical limitations of the present disclosure, so that the modifications of the structures, the changes of the ratio relationships, or the adjustments of the sizes, should not be within the scope of the disclosure of the present disclosure without affecting the efficacy and the achievable purpose of the present disclosure.
As shown in fig. 1, an embodiment of the present application provides a method for preparing a graphite susceptor coated with silicon carbide, including the following steps:
s1, pretreating a graphite base and then placing the pretreated graphite base in a vacuum furnace; mixing Si powder with SiO 2 Mixing the powders and placing the mixture in a vacuum furnace; vacuumizing the vacuum furnace, introducing argon to protect the vacuum furnace, heating to 1850-2050 ℃, preserving the temperature, and forming a SiC base layer on the surface of the graphite base;
s2, reducing the temperature in the vacuum furnace to 1050-1200 ℃, setting the pressure to 1-150 KPa, conveying trichloromethylsilane into the vacuum furnace through carrier gas, introducing diluent gas, preserving heat, and forming a SiC intermediate layer on the SiC base layer;
s3, adjusting the pressure in the vacuum furnace to 0.4 KPa-1 KPa, conveying trichloromethylsilane into the vacuum furnace through carrier gas, introducing diluent gas, preserving heat, and forming an SiC outer layer on the SiC intermediate layer.
The Chemical Vapor Reaction (CVR) is carried out by mixing Si powder with SiO 2 Mixing the powder in a graphite crucible according to a certain proportion, placing a graphite base above the crucible, and obtaining SiO at 1850-2050 ℃ in a high-temperature furnace 2 The SiC coating prepared by the method is tightly combined with the matrix, the thickness of the coating can reach more than 100 mu m, but the porosity of the material can still be reserved.
The Chemical Vapor Deposition (CVD) method mainly adopts trichloromethylsilane (CH) at a certain deposition temperature 3 SiCl 3 Abbreviated as MTS) as precursor, typically H 2 Ar is diluent gas and MTS is in gas form through oil temperature heating, and then carrier gas H is utilized through bubbling 2 And carrying the graphite substrate into a deposition furnace, and forming a SiC coating through a series of chemical reaction changes to deposit on the surface of the graphite substrate. The deposition temperature is 1050-1200 ℃, and the deposition pressure is 0.2-150 KPa. The research finds that the LPCVD technology is most widely applied, and the surface of the generated coating is smooth and compact; however, in the LPCVD process, the deposition rate of SiC on the surface of a substrate is low due to the short retention time of active products decomposed by a gas source in the furnace, and the utilization rate of raw materials is low, so that the preparation cost is increased sharply, and the industrialization process is limited seriously. To overcome the above problems, HPCVD is an effective way. Compared with LPCVD, HPCVD has high deposition pressure, long retention time of active substances after gas source decomposition and full reaction, and finally can realize rapid deposition of SiC. The SiC coating prepared by combining the two methods has high purity, is smooth and compact, and can quickly deposit a coating with the thickness of more than or equal to 100 mu m. But the resulting SiC coated substrate was found to have poor bond strength.
In the embodiment of the application, the SiC base layer is deposited on the graphite base by the CVR technology, the SiC base layer is tightly combined with the graphite base, and the bonding strength of the coating and the graphite base is improved; then forming a SiC intermediate layer on the SiC base layer by an HPCVD technology, and finding that no obvious interface exists between the SiC intermediate layer and the SiC base layer through characterization, which shows that the SiC intermediate layer fills the pores of the SiC base layer, thereby effectively improving the density of the coating and the bonding strength between the coating and the graphite base; in addition, the combination of CVR technology and HPCVD technology can rapidly carry out deposition, so that the thickness of the coating is greater than or equal to 100 μm, and the deposition is only required to be less than 10h, thereby effectively reducing the cost. And finally, forming a SiC outer layer on the SiC middle layer by an LPCVD technology, wherein the SiC outer layer is smooth and compact, and the roughness of the surface of the coating is effectively reduced. According to the SiC coating prepared on the surface of the graphite base, the coating is tightly combined, the overall performance is greatly improved, the surface is smooth, and the defects of air holes, air bubbles and the like are almost eliminated, so that the technical problems that the preparation of the silicon carbide coating graphite base is long in time consumption, high in cost, porous in coating and weak in interlayer bonding strength are solved.
Further, in step S1, si powder and SiO 2 The mol ratio of the powder is 1.05-1.10: 1. During the actual preparation of the coating, the amount of Si powder to be added is greater than SiO 2 In an amount of SiO 2 And (4) completely reacting.
In a second aspect of the embodiments of the present application, there is also provided a silicon carbide coated graphite susceptor, which is prepared by the above preparation method.
Si powder and SiO powder used in the following examples 2 Powders of high purity Si powder and high purity SiO powder, respectively 2 The purity of the powder is over 99.99 percent.
Example 1
A process for preparing graphite base with silicon carbide coating includes such steps as preparing high-purity Si powder and high-purity SiO 2 The powders were mixed and placed at the bottom of a graphite crucible, which was then placed in a vacuum furnace. To prevent SiO 2 Powder residue, si powder amount more than SiO 2 And (3) powder. In this example, the mass of Si powder is 117g 2 The mass of the powder was 251g. The graphite base is pretreated and then placed above a graphite gas distribution plate, a vacuum furnace is vacuumized and heated in an argon atmosphere, the temperature is raised to 1850 ℃ at the speed of 10 ℃/min, and then the temperature is kept in the furnace for 2 hours, and a SiC base layer is formed on the surface of the graphite base. And then, reducing the temperature in the vacuum furnace to 1100 ℃, setting the deposition pressure to be 100KPa, conveying trichloromethylsilane into the vacuum furnace through carrier gas hydrogen, introducing argon and diluting hydrogen, setting the flow of the carrier gas hydrogen to be 2L/min, setting the flow of the diluting hydrogen to be 5L/min, setting the flow of the argon to be 6L/min, keeping the temperature for 2h, and generating a SiC intermediate layer on the surface of the SiC base layer of the graphite base. And finally, reducing the deposition pressure in the vacuum furnace to 500Pa, conveying trichloromethylsilane into the vacuum furnace through carrier gas hydrogen, introducing argon and diluted hydrogen, wherein the flow of the carrier gas hydrogen is 2L/min, the flow of the diluted hydrogen is 5L/min, the flow of the argon is 6L/min, and keeping the temperature for 4h to form an SiC outer layer on the SiC intermediate layer. The total deposition time for the three coatings in this example was 8 hours.
SEM analysis and detection of the coating surface and cross-section of the silicon carbide coated graphite susceptor prepared in this example showed the results of analysis in fig. 2 to 4, in which the dark portion was the graphite susceptor and the light portion was the SiC coating. Referring to fig. 2, the SiC coating prepared in this example has a smooth and dense surface. Referring to fig. 3, the thickness of the SiC coating prepared in this example is greater than 100 μm. Referring to fig. 4, the SiC coating formed on the surface of the graphite base by the preparation method of this embodiment has high purity of the coating structure and good compactness, and the SiC base layer, the SiC intermediate layer and the SiC outer layer are not layered and are well bonded with the graphite base.
The SiC coating prepared in this example was subjected to a performance test. The SiC coating graphite base is an important consumable material for GaN single crystal epitaxial growth, so that the growth condition of a GaN single crystal wafer is an important index for embodying the performance of the SiC coating graphite base. As shown in fig. 5, which is a microscopic characterization image of a GaN wafer, it can be seen that a crack-free GaN thin film was epitaxially grown on the SiC-coated substrate. In addition, the SiC coated graphite base is subjected to a high-temperature furnace burning test, and the test conditions are as follows: and (3) keeping the temperature at 1400 ℃, introducing nitrogen and 5% hydrogen as gas, and keeping the temperature for 3h to obtain a top view of the real object shown in figure 6 and a bottom view of the real object shown in figure 7, wherein the coating does not crack or fall off, so that the SiC coating has excellent thermal shock resistance.
Example 2
A process for preparing graphite base with silicon carbide coating includes such steps as preparing high-purity Si powder and high-purity SiO 2 The powders were mixed and placed at the bottom of a graphite crucible, which was then placed in a vacuum furnace. To prevent SiO 2 Powder residue, si powder amount more than SiO 2 And (3) powder. In this example, the mass of Si powder is 117g 2 The mass of the powder was 251g. After pretreatment, a graphite base is placed above a graphite gas distribution plate, a vacuum furnace is vacuumized and heated in an argon atmosphere, the temperature is raised to 1950 ℃ at the speed of 15 ℃/min, and then the temperature is kept in the furnace for 2h, so that a SiC base layer is formed on the surface of the graphite base. And then, reducing the temperature in the vacuum furnace to 1150 ℃, setting the deposition pressure to be 60KPa, conveying trichloromethyl silane into the vacuum furnace through carrier gas hydrogen, introducing argon and diluting hydrogen, setting the flow of the carrier gas hydrogen to be 2L/min, setting the flow of the diluting hydrogen to be 5L/min, setting the flow of the argon to be 6L/min, keeping the temperature for 3h, and generating a SiC intermediate layer on the surface of the SiC base layer of the graphite base. And finally, reducing the deposition pressure in the vacuum furnace to 600Pa, conveying trichloromethylsilane into the vacuum furnace through carrier gas hydrogen, introducing argon and diluted hydrogen, wherein the flow of the carrier gas hydrogen is 2L/min, the flow of the diluted hydrogen is 5L/min, the flow of the argon is 6L/min, and keeping the temperature for 4h to form an SiC outer layer on the SiC intermediate layer. The total deposition time for the three coatings in this example was 9h.
Example 3
Graphite base with silicon carbide coatingThe preparation method comprises the steps of firstly, mixing high-purity Si powder and high-purity SiO 2 The powders were mixed and placed at the bottom of a graphite crucible, which was then placed in a vacuum furnace. For preventing SiO 2 Powder residue, si powder amount more than SiO 2 And (3) powder. In this example, the mass of Si powder is 117g 2 The mass of the powder was 251g. The method comprises the steps of pretreating a graphite base, placing the pretreated graphite base above a graphite gas distribution plate, vacuumizing a vacuum furnace, heating in an argon atmosphere, heating to 2050 ℃ at the speed of 12 ℃/min, preserving heat in the furnace for 2 hours, and forming a SiC base layer on the surface of the graphite base. And then, reducing the temperature in the vacuum furnace to 1200 ℃, setting the deposition pressure to be 20KPa, conveying trichloromethyl silane into the vacuum furnace through carrier gas hydrogen, introducing argon and diluting hydrogen, setting the flow of the carrier gas hydrogen to be 2L/min, setting the flow of the diluting hydrogen to be 5L/min, setting the flow of the argon to be 6L/min, keeping the temperature for 4h, and generating a SiC intermediate layer on the surface of the SiC base layer of the graphite base. And finally, reducing the deposition pressure in the vacuum furnace to 800Pa, conveying trichloromethylsilane into the vacuum furnace through carrier gas hydrogen, introducing argon and diluted hydrogen, wherein the flow of the carrier gas hydrogen is 2L/min, the flow of the diluted hydrogen is 5L/min, the flow of the argon is 6L/min, and keeping the temperature for 4h to form an SiC outer layer on the SiC intermediate layer. The total deposition time for the three coatings in this example was 10h.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A preparation method of a graphite base with a silicon carbide coating is characterized by comprising the following steps:
s1, pretreating a graphite base and then placing the pretreated graphite base in a vacuum furnace; mixing Si powder with SiO 2 Mixing the powder and placing the powder in the vacuum furnace; vacuumizing the vacuum furnace, introducing argon to protect the vacuum furnace, heating to 1850-2050 ℃, and preserving heat to form a SiC base layer on the surface of the graphite base;
s2, reducing the temperature in the vacuum furnace to 1050-1200 ℃, setting the pressure to 1-150 KPa, conveying trichloromethylsilane into the vacuum furnace through carrier gas, introducing diluent gas, and preserving heat to form a SiC intermediate layer on the SiC base layer;
s3, adjusting the pressure in the vacuum furnace to 0.4 KPa-1 KPa, conveying trichloromethylsilane into the vacuum furnace through carrier gas, introducing diluent gas, preserving heat, and forming an SiC outer layer on the SiC intermediate layer.
2. The method of preparing the silicon carbide coated graphite susceptor as claimed in claim 1, wherein the Si powder and the SiO powder are mixed in step S1 2 The mol ratio of the powder is 1.05-1.10: 1.
3. The method of preparing a silicon carbide coated graphite susceptor as set forth in claim 1, wherein in the step S2, the SiC intermediate layer is formed for a time of 2 to 4 hours.
4. The method of preparing a silicon carbide coated graphite susceptor as set forth in claim 1, wherein in said step S3, the SiC outer layer is formed for 4 hours.
5. The method of any one of claims 1 to 4, wherein the carrier gas is hydrogen and the diluent gas is argon or hydrogen in the steps S2 and S3.
6. The method of preparing a silicon carbide coated graphite susceptor as claimed in claim 5, wherein in the steps S2 and S3, the flow rate of hydrogen as a carrier gas is 2L/min, the flow rate of argon is 6L/min, and the flow rate of diluted hydrogen is 5L/min.
7. The method of claim 5, wherein the flow ratio of hydrogen as a carrier gas to trichloromethylsilane in the steps S2 and S3 is 10: 1.
8. The method of producing the silicon carbide coated graphite susceptor according to any one of claims 1 to 4, wherein the total thickness of the SiC base layer formed in the step S2 and the SiC intermediate layer formed in the step S1 is 100 μm or more.
9. A silicon carbide coated graphite susceptor produced by the method of producing a silicon carbide coated graphite susceptor as claimed in any one of claims 1 to 8.
10. The silicon carbide coated graphite susceptor of claim 9, wherein the SiC intermediate layer fills pores of the SiC base layer.
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