CN117164390A - Silicon carbide coating on graphite substrate and preparation method thereof - Google Patents
Silicon carbide coating on graphite substrate and preparation method thereof Download PDFInfo
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- CN117164390A CN117164390A CN202311213255.1A CN202311213255A CN117164390A CN 117164390 A CN117164390 A CN 117164390A CN 202311213255 A CN202311213255 A CN 202311213255A CN 117164390 A CN117164390 A CN 117164390A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 97
- 238000000576 coating method Methods 0.000 title claims abstract description 65
- 239000011248 coating agent Substances 0.000 title claims abstract description 61
- 239000000758 substrate Substances 0.000 title claims abstract description 60
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 49
- 239000010439 graphite Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 68
- 238000000034 method Methods 0.000 claims abstract description 37
- 239000011159 matrix material Substances 0.000 claims abstract description 20
- 238000000151 deposition Methods 0.000 claims description 29
- 230000008021 deposition Effects 0.000 claims description 29
- 238000005229 chemical vapour deposition Methods 0.000 claims description 23
- 238000005498 polishing Methods 0.000 claims description 20
- 238000004381 surface treatment Methods 0.000 claims description 20
- 238000007740 vapor deposition Methods 0.000 claims description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 239000007791 liquid phase Substances 0.000 claims description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 239000000853 adhesive Substances 0.000 claims description 8
- 230000001070 adhesive effect Effects 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000000462 isostatic pressing Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 6
- 238000005524 ceramic coating Methods 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 230000001680 brushing effect Effects 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims 1
- 239000005052 trichlorosilane Substances 0.000 claims 1
- 238000005299 abrasion Methods 0.000 abstract description 7
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 238000005137 deposition process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 8
- 238000005530 etching Methods 0.000 description 6
- 244000137852 Petrea volubilis Species 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000001020 plasma etching Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a silicon carbide coating on a graphite substrate and a preparation method thereof, belonging to the technical field of silicon carbide ceramic materials. The method can realize the preparation of the silicon carbide coating with high quality and uniform thickness by optimizing the sintering process and the deposition process parameters, provides a method for improving the abrasion resistance and the high temperature resistance of the graphite matrix, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of silicon carbide ceramic materials, in particular to a preparation method of a high-purity silicon carbide etching consumable material for the semiconductor industry.
Background
With the development of semiconductor technology, plasma etching is becoming a widely used technology in semiconductor manufacturing processes. The plasma generated by the plasma etching has strong corrosiveness and can cause serious corrosion to the process cavity and elements in the cavity in the process of etching the wafer. Therefore, components in contact with plasma in semiconductor processing equipment are required to have better plasma etch resistance.
SiC is widely used for semiconductor processing equipment parts due to its excellent properties. For example, silicon carbide has excellent high temperature resistance and is widely used as a core component of various deposition apparatuses. Silicon carbide has excellent thermal conductivity and electrical conductivity, is matched with a Si wafer and is used as a focusing ring material, and SiC has more excellent plasma etching resistance, so that the silicon carbide is an excellent candidate material.
The SiC etching ring is a key consumable of semiconductor materials in a plasma etching link, and is an indispensable important material in the semiconductor chip industry chain. The SiC etching ring has extremely high purity requirement, and the SiC thick-layer block is grown by adopting a CVD process in the conventional process at present and is manufactured by precision machining, and is mainly used for the preparation link of the semiconductor etching process.
Various methods for producing SiC ceramics are available, such as a reactive sintering method, a pressureless sintering method, a hot pressing method, a hot isostatic pressing method, a chemical vapor deposition method (CVD), a chemical vapor infiltration method (CVI), and the like. Among them, the CVD method is the preferred method for producing high-performance silicon carbide. This is mainly due to the following characteristics of CVD: (1) The purity of the silicon carbide material prepared by the CVD method is high and can reach more than 99.9%, and the silicon carbide material is a single-phase material; (2) The silicon carbide material prepared by the CVD method has high density and basically can reach theoretical density; (3) the temperature of the CVD process is relatively low. The biggest disadvantage of CVD processes is that the manufacturing process is time consuming. In the above-mentioned various sintering methods, only the reaction sintering method and the CVD method are combined, namely, the CVD film layer is prepared on the sample prepared by the reaction sintering method, so that the defect of non-uniformity of phases of the reaction sintering method and the time consumption of the CVD process can be overcome, and the preparation method is a better choice for preparing silicon carbide etching rings.
Disclosure of Invention
The technical problems to be solved are as follows: the invention aims to overcome the defects and provide a silicon carbide coating on a graphite substrate and a preparation method thereof. According to the invention, a silicon carbide substrate is prepared by sintering, and then a silicon carbide coating can be prepared by vapor deposition. In addition, the preparation of the silicon carbide coating with high quality and uniform thickness can be realized by optimizing the sintering process and the deposition process parameters, and the method is used for improving the abrasion resistance and the high temperature resistance of the graphite matrix, and has wide application prospect.
The technical scheme is as follows: a preparation method of a silicon carbide coating on a graphite substrate comprises the following steps:
s1: preparation of graphite matrix: selecting an isostatic pressing graphite matrix and carrying out surface treatment to improve the adhesive force;
s2: preparation of sintering agent: uniformly mixing a silane coupling agent, silicon carbide powder and a liquid phase sintering aid in a certain mass ratio, and then uniformly spraying or brushing on the surface of a graphite substrate;
s3: sintering to prepare a silicon carbide substrate: placing the graphite substrate sprayed or coated with the sintering agent in a high-temperature furnace for sintering treatment, so that the surface of the graphite substrate is sintered to prepare a layer of silicon carbide substrate;
s4: vapor deposition preparation of silicon carbide coating: placing the sintered silicon carbide substrate in a vapor deposition device, performing silicon carbide deposition, and performing multiple depositions according to the requirement to obtain the required thickness and performance of the coating;
s5: surface treatment: and carrying out surface treatment on the silicon carbide coating obtained through deposition to obtain the silicon carbide coating.
Preferably, the surface treatment in the step S1 specifically includes: polishing with 400# abrasive paper, polishing, ultrasonic cleaning with absolute ethyl alcohol, and drying.
Preferably, in the step S2, the mass ratio of the silane coupling agent, the silicon carbide powder and the liquid phase sintering aid is (4-10): 1-2.5): 0.1-0.22.
Further, the liquid phase sintering aid comprises Al 2 O 3 、AlN、Y 2 O 3 、Y 2 O 3 -Al 2 O 3 、Sc 2 O 3 Re and Re-Al. Preferably, in the step S3, the sintering temperature is 1620-1850 ℃, the sintering time is 1-2 h, the sintering pressure is 3-50 MPa, and the sintering atmosphere is argon.
Preferably, the silicon carbide substrate in the step S3 has a thickness of 5 to 30 μm.
Preferably, the vapor deposition in step S4 is chemical vapor deposition.
Preferably, the vapor deposition conditions in the step S4 are as follows: MTS-H 2 Ar system, deposition temperature is 1100-1250 deg.c and deposition pressure is 10-30 kPa.
Further, the MTS-H 2 In the Ar systemThe molar ratio of the trichloromethylsilane to the hydrogen to the argon is 1:5:2.
Preferably, the surface treatment method in step S5 includes sanding, polishing and applying a ceramic coating.
The beneficial effects are that:
1. the silicon carbide matrix is prepared by sintering, so that a uniform and compact matrix structure can be provided, and the adhesive force and mechanical property of the coating are improved.
2. Chemical vapor deposition can achieve uniform deposition of silicon carbide coatings, and thickness and performance of the coatings can be controlled by adjusting deposition parameters.
3. The silicon carbide coating prepared by the invention has excellent high temperature resistance and abrasion resistance, and is suitable for high temperature process and friction and abrasion environment.
Drawings
FIG. 1 is a scanning electron microscope image of the silicon carbide coating prepared in example 1;
FIG. 2 is a scanning electron microscope image of the silicon carbide coating prepared in comparative example 1.
Detailed Description
The invention will be further described with reference to the following specific examples and drawings, which are illustrative of the invention and the invention is not limited to the following examples:
example 1
S1: preparation of graphite matrix: selecting an isostatic pressing graphite substrate, performing surface treatment to improve adhesive force, firstly polishing by using 400# sand paper, then polishing, finally ultrasonically cleaning by using absolute ethyl alcohol, and drying;
s2: preparation of sintering agent: silane coupling agent, silicon carbide powder and liquid phase sintering aid Al 2 O 3 Uniformly mixing the materials according to the mass ratio of 4:1:0.12, and uniformly coating the materials on the surface of a graphite matrix;
s3: sintering to prepare a silicon carbide substrate: placing the graphite substrate coated with the sintering agent in a high-temperature furnace, and sintering for 1h in argon at the sintering temperature of 1820 ℃ and the sintering pressure of 45MPa to prepare a silicon carbide substrate with the thickness of more than ten micrometers on the surface;
s4: vapor deposition preparation of silicon carbide coating: carbonizing the sintered productThe silicon substrate is placed in a vapor deposition device and is subjected to a chemical vapor deposition method in MTS-H 2 Silicon carbide deposition is carried out in an Ar system at a temperature of 1100 ℃ and a pressure of 30kPa, with multiple depositions being carried out as required to obtain the desired coating thickness and properties;
s5: surface treatment: the silicon carbide coating obtained by deposition is subjected to surface polishing treatment to improve the optical and mechanical properties of the coating.
Example 2
S1: preparation of graphite matrix: selecting an isostatic pressing graphite substrate, performing surface treatment to improve adhesive force, firstly polishing by using 400# sand paper, then polishing, finally ultrasonically cleaning by using absolute ethyl alcohol, and drying;
s2: preparation of sintering agent: silane coupling agent, silicon carbide powder and liquid phase sintering aid Y 2 O 3 Uniformly mixing in a mass ratio of 5:1.5:0.1, and uniformly coating on the surface of a graphite matrix;
s3: sintering to prepare a silicon carbide substrate: placing the graphite substrate coated with the sintering agent in a high-temperature furnace, and sintering for 2 hours in argon at a sintering temperature of 1680 ℃ and a sintering pressure of 25MPa to prepare a silicon carbide substrate with a thickness of more than ten micrometers on the surface;
s4: vapor deposition preparation of silicon carbide coating: placing the sintered silicon carbide substrate in a vapor deposition device, and performing chemical vapor deposition on MTS-H 2 Silicon carbide deposition is carried out in an Ar system at a temperature of 1180 ℃ and a pressure of 20kPa, with multiple depositions being carried out as required to obtain the desired coating thickness and properties;
s5: surface treatment: the silicon carbide coating obtained by deposition is subjected to surface polishing treatment to improve the optical and mechanical properties of the coating.
Example 3
S1: preparation of graphite matrix: selecting an isostatic pressing graphite substrate, performing surface treatment to improve adhesive force, firstly polishing by using 400# sand paper, then polishing, finally ultrasonically cleaning by using absolute ethyl alcohol, and drying;
s2: preparation of sintering agent: silane coupling agent, silicon carbide powder and liquid phase sintering aid Y 2 O 3 -Al 2 O 3 Uniformly mixing the materials according to the mass ratio of 6:1:0.15, and uniformly coating the materials on the surface of a graphite matrix;
s3: sintering to prepare a silicon carbide substrate: placing the graphite substrate coated with the sintering agent in a high-temperature furnace, and sintering for 1.5 hours in argon at a sintering temperature of 1800 ℃ and a sintering pressure of 35MPa to prepare a silicon carbide substrate with a thickness of more than ten micrometers on the surface;
s4: vapor deposition preparation of silicon carbide coating: placing the sintered silicon carbide substrate in a vapor deposition device, and performing chemical vapor deposition on MTS-H 2 Silicon carbide deposition at 1180 ℃ and 25kPa pressure under Ar system, multiple depositions as needed to obtain the desired coating thickness and properties;
s5: surface treatment: the silicon carbide coating obtained by deposition is subjected to surface polishing treatment to improve the optical and mechanical properties of the coating.
Example 4
S1: preparation of graphite matrix: selecting an isostatic pressing graphite substrate, performing surface treatment to improve adhesive force, firstly polishing by using 400# sand paper, then polishing, finally ultrasonically cleaning by using absolute ethyl alcohol, and drying;
s2: preparation of sintering agent: uniformly mixing a silane coupling agent, silicon carbide powder and a liquid phase sintering aid AlN in a mass ratio of 4:1:0.12, and uniformly coating on the surface of a graphite matrix;
s3: sintering to prepare a silicon carbide substrate: placing the graphite substrate coated with the sintering agent in a high-temperature furnace, and sintering for 2 hours in argon at a sintering temperature of 1780 ℃ and a sintering pressure of 45MPa to prepare a silicon carbide substrate with a thickness of more than ten micrometers on the surface;
s4: vapor deposition preparation of silicon carbide coating: placing the sintered silicon carbide substrate in a vapor deposition device, and performing chemical vapor deposition on MTS-H 2 Silicon carbide deposition is carried out in an Ar system at a temperature of 1250 ℃ and a pressure of 30kPa, with multiple depositions being carried out as required to obtain the desired coating thickness and properties;
s5: surface treatment: the silicon carbide coating obtained by deposition is subjected to surface polishing treatment to improve the optical and mechanical properties of the coating.
Example 5
S1: preparation of graphite matrix: selecting an isostatic pressing graphite substrate, performing surface treatment to improve adhesive force, firstly polishing by using 400# sand paper, then polishing, finally ultrasonically cleaning by using absolute ethyl alcohol, and drying;
s2: preparation of sintering agent: uniformly mixing a silane coupling agent, silicon carbide powder and a liquid phase sintering aid Re according to the mass ratio of 9:1.2:0.2, and uniformly coating on the surface of a graphite substrate;
s3: sintering to prepare a silicon carbide substrate: placing the graphite substrate coated with the sintering agent in a high-temperature furnace, and sintering for 1.2 hours in argon at a sintering temperature of 1790 ℃ and a sintering pressure of 50MPa to prepare a silicon carbide substrate with a thickness of more than ten micrometers on the surface;
s4: vapor deposition preparation of silicon carbide coating: placing the sintered silicon carbide substrate in a vapor deposition device, and performing chemical vapor deposition on MTS-H 2 Silicon carbide deposition is carried out in an Ar system at a temperature of 1250 ℃ and a pressure of 30kPa, with multiple depositions being carried out as required to obtain the desired coating thickness and properties;
s5: surface treatment: the silicon carbide coating obtained through deposition is subjected to surface subsequent ceramic coating treatment so as to improve the optical and mechanical properties of the coating.
Comparative example 1
This comparative example differs from example 1 in that the sintering to prepare silicon carbide substrate operation described in step S3 is not performed.
Comparative example 2
This comparative example differs from example 1 in that the chemical vapor deposition process for preparing a silicon carbide coating layer described in step S4 is not performed.
Performance test 1
The measurements of the indexes such as the thickness of the silicon carbide substrate sintered, the thickness of the vapor deposited silicon carbide coating, the compactibility, the adhesion to the graphite substrate, the abrasion resistance, the uniformity and the high temperature resistance of the samples in the above examples and comparative examples are shown in Table 1.
TABLE 1 sample index measurement results
As can be seen from table 1, the silicon carbide coatings prepared in examples 1 to 5 all have excellent compactness, abrasion resistance, uniformity and strong adhesion on the graphite substrate, and the thickness and performance of the coatings can be controlled by adjusting the chemical vapor deposition parameters.
As can be seen from a comparison of example 1 (fig. 1) and comparative example 1 (fig. 2), the preparation of the silicon carbide matrix by sintering first in example 1 provides a uniform, dense matrix structure, improving the adhesion and mechanical properties of the coating. The silicon carbide substrate sintered in example 1 had a thickness of 16.4 μm and the silicon carbide coating vapor deposited had a thickness of 67.8 μm, as identified by dimensions 1 and 2 in fig. 1, resulting in a silicon carbide coating having excellent high temperature resistance and abrasion resistance.
As can be seen from a comparison of example 1 and comparative example 2 in table 1, the silicon carbide coating prepared in example 1 has excellent uniformity, while the uniformity in comparative example 2 is poor, indicating that chemical vapor deposition can achieve uniform deposition of the silicon carbide coating.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (10)
1. The preparation method of the silicon carbide coating on the graphite substrate is characterized by comprising the following steps of:
s1: preparation of graphite matrix: selecting an isostatic pressing graphite matrix and carrying out surface treatment to improve the adhesive force;
s2: preparation of sintering agent: uniformly mixing a silane coupling agent, silicon carbide powder and a liquid phase sintering aid in a certain mass ratio, and then uniformly spraying or brushing on the surface of a graphite substrate;
s3: sintering to prepare a silicon carbide substrate: placing the graphite substrate sprayed or coated with the sintering agent in a high-temperature furnace for sintering treatment, so that the surface of the graphite substrate is sintered to prepare a layer of silicon carbide substrate;
s4: vapor deposition preparation of silicon carbide coating: placing the sintered silicon carbide substrate in a vapor deposition device, performing silicon carbide deposition, and performing multiple depositions according to the requirement to obtain the required thickness and performance of the coating;
s5: surface treatment: and carrying out surface treatment on the silicon carbide coating obtained through deposition to obtain the silicon carbide coating.
2. A method of preparing a silicon carbide coating on a graphite substrate as claimed in claim 1, wherein: the surface treatment in the step S1 specifically comprises the following steps: polishing with 400# abrasive paper, polishing, ultrasonic cleaning with absolute ethyl alcohol, and drying.
3. A method of preparing a silicon carbide coating on a graphite substrate as claimed in claim 1, wherein: in the step S2, the mass ratio of the silane coupling agent, the silicon carbide powder and the liquid phase sintering aid is (4-10): 1-2.5): 0.1-0.22.
4. A method of preparing a silicon carbide coating on a graphite substrate as claimed in claim 1 or claim 3, wherein: the liquid phase sintering aid comprises Al 2 O 3 、AlN、Y 2 O 3 、Y 2 O 3 -Al 2 O 3 、Sc 2 O 3 Re and Re-Al.
5. A method of preparing a silicon carbide coating on a graphite substrate as claimed in claim 1, wherein: in the step S3, the sintering temperature is 1620-1850 ℃, the sintering time is 1-2 h, the sintering pressure is 3-50 MPa, and the sintering atmosphere is argon.
6. A method of preparing a silicon carbide coating on a graphite substrate as claimed in claim 1, wherein: the thickness of the silicon carbide matrix in the step S3 is 5-30 mu m.
7. A method of preparing a silicon carbide coating on a graphite substrate as claimed in claim 1, wherein: the vapor deposition in step S4 is chemical vapor deposition.
8. A method of preparing a silicon carbide coating on a graphite substrate as claimed in claim 1, wherein: the vapor deposition conditions in the step S4 are as follows: MTS-H 2 Ar system, deposition temperature is 1100-1250 deg.c and deposition pressure is 10-30 kPa.
9. A method of preparing a silicon carbide coating on a graphite substrate as claimed in claim 8, wherein: the MTS-H 2 The molar ratio of trichlorosilane, hydrogen and argon in the Ar system is 1:5:2.
10. A method of preparing a silicon carbide coating on a graphite substrate as claimed in claim 1, wherein: the surface treatment method in step S5 includes sanding, polishing and applying a ceramic coating.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311213255.1A CN117164390A (en) | 2023-09-20 | 2023-09-20 | Silicon carbide coating on graphite substrate and preparation method thereof |
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| CN202311213255.1A CN117164390A (en) | 2023-09-20 | 2023-09-20 | Silicon carbide coating on graphite substrate and preparation method thereof |
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