CN115536418A - Preparation method of C-SiC double-coating carbon/carbon composite material crucible - Google Patents
Preparation method of C-SiC double-coating carbon/carbon composite material crucible Download PDFInfo
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- CN115536418A CN115536418A CN202211245656.0A CN202211245656A CN115536418A CN 115536418 A CN115536418 A CN 115536418A CN 202211245656 A CN202211245656 A CN 202211245656A CN 115536418 A CN115536418 A CN 115536418A
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 140
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 239000011248 coating agent Substances 0.000 title claims abstract description 69
- 238000000576 coating method Methods 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 238000005475 siliconizing Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002296 pyrolytic carbon Substances 0.000 claims abstract description 19
- 239000006255 coating slurry Substances 0.000 claims abstract description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 20
- 238000000151 deposition Methods 0.000 claims description 14
- 230000008021 deposition Effects 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 12
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000004917 carbon fiber Substances 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- WIEXMPDBTYDSQF-UHFFFAOYSA-N 1,3-bis(furan-2-yl)propan-2-one Chemical compound C=1C=COC=1CC(=O)CC1=CC=CO1 WIEXMPDBTYDSQF-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000007849 furan resin Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000003345 natural gas Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000005011 phenolic resin Substances 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000009941 weaving Methods 0.000 claims description 5
- 150000001721 carbon Chemical class 0.000 claims description 4
- 238000000280 densification Methods 0.000 claims description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 11
- 239000010703 silicon Substances 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 230000003628 erosive effect Effects 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 3
- 238000007581 slurry coating method Methods 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 26
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 229920001568 phenolic resin Polymers 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
- C04B41/5059—Silicon carbide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention relates to a preparation method of a C-SiC double-coating carbon/carbon composite material crucible. The method comprises the following steps: s1, preparing a pyrolytic carbon coating; s2, preparing coating slurry; s3, coating slurry on the coating; and S4, gas-phase siliconizing to prepare the SiC coating. According to the invention, a pyrolytic carbon coating is prepared on the surface of the carbon/carbon composite material crucible by CVD, a uniform carbon layer is prepared on the surface of the crucible by adopting a slurry coating mode, and the carbon layer coated on the surface is reacted to generate a SiC layer by combining with gas-phase siliconizing. The preparation of the first pyrolytic carbon coating closes all open pores on the surface of the crucible, so that the erosion influence of gas-phase silicon on a base material during gas-phase siliconizing can be effectively prevented, the preparation of the second coating carbon layer provides a reaction raw material for generating SiC for the gas-phase silicon, and a compact SiC coating can be generated on the surface. The invention ensures that a compact SiC coating is generated on the surface of the crucible, prolongs the service life of the material, and prevents the corrosion influence of Si steam on the matrix material in the reaction process of Si and C.
Description
Technical Field
The invention relates to the technical field of preparation of carbon/carbon composite material crucibles, in particular to a preparation method of a C-SiC double-coating carbon/carbon composite material crucible.
Background
The carbon/carbon composite material crucible is an important thermal field material for producing the silicon single crystal rod, with the rapid development of the photovoltaic semiconductor industry, the single crystal solar panel gradually occupies the leading position of the market, and the consumption demand of the carbon/carbon composite material crucible is increased day by day.
The prior production method of monocrystalline silicon mainly adopts a czochralski method, and a quartz crucible filled with polycrystalline silicon materials is placed in a carbon/carbon composite material crucible. Since the pulling temperature of the single crystal silicon rod is as high as about 1550 ℃, high-temperature silicon vapor, silicon-containing gas and silicon dioxide (main components of the quartz crucible) can react in the carbon/carbon composite material crucible to corrode the carbon/carbon composite material crucible, thereby seriously affecting the service life of the crucible.
The carbon/carbon composite material crucible is used as a key bearing thermal field component of the quartz crucible, so that the problem of erosion failure of the carbon/carbon composite material crucible under the condition of a single crystal silicon rod drawing working condition is effectively solved, the service life of the carbon/carbon composite material crucible is prolonged, and the problem to be solved is to further reduce the cost of the single crystal silicon solar cell. The erosion-resistant coating is prepared on the surface of the carbon/carbon composite material crucible, so that the erosion resistance of the carbon/carbon composite material crucible can be effectively improved, and the service life of a product is prolonged.
At present, a chemical reaction method is adopted, silicon dioxide and metal silicon are used as raw materials, a uniform silicon carbide coating is generated on the surface of a carbon/carbon composite material crucible under a certain temperature condition, or a chemical vapor deposition process is adopted to generate a silicon carbide coating and a silicon nitride coating in situ reaction on the surface of the carbon/carbon composite material crucible, or a plasma method is utilized to prepare the silicon carbide coating on the surface of the crucible, and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a C-SiC double-coating carbon/carbon composite material crucible, which ensures that a compact SiC coating is generated on the surface of the crucible to prolong the service life of the material, prevents Si steam from corroding a base material in the reaction process of Si and C, is simple and convenient in process and is suitable for industrial production.
In order to solve the technical problems, the technical scheme of the invention is as follows: a preparation method of a C-SiC double-coating carbon/carbon composite material crucible comprises the following steps:
step S1: preparation of pyrolytic carbon coating
Weaving a carbon fiber preform of a carbon/carbon composite material crucible in a three-dimensional needling manner, and putting the woven carbon fiber preform into a chemical vapor deposition furnace for carbon depositionDensifying to reach density of 1.2-1.6g/cm 3 Preparing a pyrolytic carbon coating on the surface of the carbon/carbon composite material crucible by CVD;
step S2: preparation of coating slurries
Mixing liquid resin, ethanol and C powder in proportion, taking TMAH as a dispersing agent with the mass ratio of 0.2-0.8wt%, and mixing for 24-48h by a roller ball mill to obtain uniformly dispersed coating slurry;
and step S3: application of coating slurries
Coating the obtained coating slurry on the surface of the carbon/carbon composite material crucible, drying, and repeating for 2-4 times to obtain a coating with the thickness of 40-80 μm on the surface of the carbon/carbon composite material crucible;
and step S4: siC coating prepared by gas phase siliconizing
And (3) carrying out gas-phase siliconizing treatment on the carbon/carbon composite material crucible with the surface coated with the slurry in a siliconizing furnace to obtain the carbon/carbon composite material crucible with the surface provided with the C-SiC double coating.
Preferably, in the step S1, when the pyrolytic carbon coating is prepared, natural gas is used as a gaseous precursor, the deposition temperature is 1000-1200 ℃, the gas flow is 100-500SLM, the deposition time is 10-30h, and the thickness is 1-3 μm.
Preferably, in the step S2, the resin is one of a phenol resin, a furan resin or a furfuryl ketone resin.
Preferably, in the step S2, the particle size of the C powder is 1 to 10 μm.
Preferably, in the step S2, the ratio is a mass ratio of 2 to 3.
Preferably, in the step S4, the temperature when the gas phase siliconizing treatment is performed in the siliconizing furnace is 1550-1800 ℃, the vacuum degree is less than 50pa, and the reaction time is 0.5-4h.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, a pyrolytic carbon coating is prepared on the surface of the carbon/carbon composite material crucible by CVD, then a uniform carbon layer is prepared on the surface of the crucible by adopting a slurry coating mode, and the carbon layer coated on the surface is reacted by combining with gas-phase siliconizing to generate a SiC layer. The preparation of the first pyrolytic carbon coating closes all open pores on the surface of the crucible, so that the corrosion influence of gas-phase silicon on a base material during gas-phase siliconizing can be effectively prevented, the preparation of the second coating carbon layer provides a reaction raw material for generating SiC for the gas-phase silicon, and a compact SiC coating can be generated on the surface. The preparation method not only ensures that the compact SiC coating is generated on the surface of the crucible to prolong the service life of the material, but also prevents the Si steam from corroding the base material in the reaction process of Si and C, and the process method is simple, convenient and fast and is suitable for industrial production.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, and is not intended to limit the present invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
A preparation method of a C-SiC double-coating carbon/carbon composite material crucible comprises the following steps:
step S1: preparation of pyrolytic carbon coating
Weaving a carbon fiber preform of a carbon/carbon composite material crucible in a three-dimensional needling manner, and putting the woven carbon fiber preform into a chemical vapor deposition furnace for carbon deposition densification to reach the density of 1.2g/cm 3 The pyrolytic carbon coating is prepared on the surface of a carbon/carbon composite material crucible by CVD (CVD is short for Chemical Vapor Deposition and refers to gas phase reaction at high temperature), natural gas is used as a gaseous precursor, the Deposition temperature is 1000 ℃, the gas flow is 100SLM, the Deposition time is 30h, and the thickness is about 1 μm.
And 2, step: preparation of coating slurries
Mixing liquid phenolic resin, furan resin or furfuryl ketone resin and ethanol with C powder with the particle size of 1-10 μm, wherein the mass ratio is 2.
And step 3: application of coating pastes
And (3) coating the obtained coating slurry on the surface of the carbon/carbon composite material crucible, drying, and repeating for 2 times to obtain a coating with the thickness of 40 mu m on the surface of the carbon/carbon composite material.
And 4, step 4: preparation of SiC coating by gas phase siliconizing
And (3) carrying out gas-phase siliconizing treatment on the carbon/carbon composite material crucible with the surface coated with the slurry in a siliconizing furnace, wherein the process temperature is 1550-DEG C, the vacuum degree is less than 50pa, and the reaction time is 0.5h, so that the carbon/carbon composite material crucible with the C-SiC double coating on the surface is obtained.
Example 2
A preparation method of a C-SiC double-coating carbon/carbon composite material crucible comprises the following steps:
step S1: preparation of pyrolytic carbon coating
Weaving a carbon fiber preform of a carbon/carbon composite material crucible in a three-dimensional needling manner, and putting the woven carbon fiber preform into a chemical vapor deposition furnace for carbon deposition densification to reach the density of 1.3g/cm 3 The pyrolytic carbon coating is prepared on the surface of a carbon/carbon composite material crucible by CVD, natural gas is used as a gaseous precursor, the deposition temperature is 1100 ℃, the gas flow is 300SLM, the deposition time is 20h, and the thickness is about 2 mu m.
Step S2: preparation of coating slurries
Mixing liquid phenolic resin, furan resin or furfuryl ketone resin and ethanol with C powder with the particle size of 5 mu m, wherein the mass ratio is 2.5.
And step S3: application of coating pastes
And (3) coating the obtained coating slurry on the surface of the carbon/carbon composite material crucible, drying, and repeating for 3 times to obtain a coating with the thickness of 60 mu m on the surface of the carbon/carbon composite material.
And step S4: preparation of SiC coating by gas phase siliconizing
And (3) carrying out gas-phase siliconizing treatment on the carbon/carbon composite material crucible with the surface coated with the slurry in a siliconizing furnace, wherein the process temperature is 1650 ℃, the vacuum degree is less than 50pa, and the reaction time is 2h, so that the carbon/carbon composite material crucible with the C-SiC double coating on the surface is obtained.
Example 3
A preparation method of a C-SiC double-coating carbon/carbon composite material crucible comprises the following steps:
step S1: preparation of pyrolytic carbon coating
Weaving a carbon fiber preform of the carbon/carbon composite material crucible in a three-dimensional needling manner, and putting the woven carbon fiber preform into a chemical vapor deposition furnace for carbon deposition densification to reach the density of 1.6g/cm 3 The pyrolytic carbon coating is prepared on the surface of a carbon/carbon composite material crucible by CVD, natural gas is used as a gaseous precursor, the deposition temperature is 1200 ℃, the gas flow is 500SLM, the deposition time is 10h, and the thickness is about 3 mu m.
Step 2: preparation of coating slurries
Mixing liquid phenolic resin, furan resin or furfuryl ketone resin and ethanol with C powder with the particle size of 1-10 mu m, wherein the mass ratio is 3.
And 3, step 3: application of coating slurries
And (3) coating the obtained coating slurry on the surface of the carbon/carbon composite material crucible, drying, and repeating for 4 times to obtain a coating with the thickness of 80 microns on the surface of the carbon/carbon composite material.
And 4, step 4: preparation of SiC coating by gas phase siliconizing
And (3) carrying out gas-phase siliconizing treatment on the carbon/carbon composite material crucible with the surface coated with the slurry in a siliconizing furnace, wherein the process temperature is 1800 ℃, the vacuum degree is less than 50pa, and the reaction time is 4 hours, so that the carbon/carbon composite material crucible with the C-SiC double coating on the surface is obtained.
According to the invention, a pyrolytic carbon coating is prepared on the surface of the carbon/carbon composite material crucible by CVD, then a uniform carbon layer is prepared on the surface of the crucible by adopting a slurry coating mode, and the carbon layer coated on the surface is reacted by combining with gas-phase siliconizing to generate a SiC layer. The preparation of the first pyrolytic carbon coating closes all open pores on the surface of the crucible, so that the erosion influence of gas-phase silicon on a base material during gas-phase siliconizing can be effectively prevented, the preparation of the second coating carbon layer provides a reaction raw material for generating SiC for the gas-phase silicon, and a compact SiC coating can be generated on the surface. The preparation method not only ensures that a compact SiC coating is generated on the surface of the crucible to prolong the service life of the material, but also prevents the Si steam from corroding the base material in the reaction process of Si and C, and meanwhile, the process method is simple and convenient and is suitable for industrial production.
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (6)
1. A preparation method of a C-SiC double-coating carbon/carbon composite material crucible is characterized by comprising the following steps:
step S1: preparation of pyrolytic carbon coating
Weaving a carbon fiber preform of a carbon/carbon composite material crucible in a three-dimensional needling manner, and putting the woven carbon fiber preform into a chemical vapor deposition furnace for carbon deposition densification to reach the density of 1.2-1.6g/cm 3 Preparing a pyrolytic carbon coating on the surface of the carbon/carbon composite material crucible by CVD;
step S2: preparation of coating slurries
Mixing liquid resin, ethanol and C powder in proportion, taking TMAH as a dispersing agent with the mass ratio of 0.2-0.8wt%, and mixing for 24-48h by a roller ball mill to obtain uniformly dispersed coating slurry;
and step S3: application of coating pastes
Coating the obtained coating slurry on the surface of the carbon/carbon composite material crucible, drying, and repeating for 2-4 times to obtain a coating with the thickness of 40-80 μm on the surface of the carbon/carbon composite material crucible;
and step S4: siC coating prepared by gas phase siliconizing
And carrying out gas-phase siliconizing treatment on the carbon/carbon composite material crucible with the surface coated with the slurry in a siliconizing furnace to obtain the carbon/carbon composite material crucible with the C-SiC double coating on the surface.
2. The method for preparing the C-SiC double-coated carbon/carbon composite crucible as claimed in claim 1, wherein the method comprises the following steps: in the step S1, when the pyrolytic carbon coating is prepared, natural gas is used as a gaseous precursor, the deposition temperature is 1000-1200 ℃, the gas flow is 100-500SLM, the deposition time is 10-30h, and the thickness is 1-3 μm.
3. The method of making a carbon/carbon composite crucible of claim 1, wherein: in the step S2, the resin is one of a phenol resin, a furan resin or a furfuryl ketone resin.
4. The method for preparing the C-SiC double-coated carbon/carbon composite crucible as claimed in claim 1, wherein the method comprises the following steps: in the step S2, the particle size of the C powder is 1 to 10 μm.
5. The method for preparing the C-SiC double-coated carbon/carbon composite crucible as claimed in claim 1, wherein the method comprises the following steps: in the step S2, the ratio is a mass ratio of 2 to 3.
6. The method of making a carbon/carbon composite crucible of claim 1, wherein: in the step S4, the temperature is 1550-1800 ℃, the vacuum degree is less than 50pa and the reaction time is 0.5-4h when the gas-phase siliconizing treatment is carried out in the siliconizing furnace.
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| CN109354506A (en) * | 2018-10-22 | 2019-02-19 | 湖南国科碳陶新材料科技有限公司 | A kind of high-temperature oxidation resistant carbon ceramic composite material and preparation method thereof |
| CN112759423A (en) * | 2020-12-28 | 2021-05-07 | 湖南世鑫新材料有限公司 | Coating carbon-carbon composite material crucible and preparation method thereof |
| CN113277867A (en) * | 2021-05-11 | 2021-08-20 | 广州三的投资管理企业（有限合伙） | Preparation method of carbon/silicon carbide composite material crucible |
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Application publication date: 20221230 |