CN113293356A - Device for preparing carbon-carbon composite material - Google Patents

Device for preparing carbon-carbon composite material Download PDF

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Publication number
CN113293356A
CN113293356A CN202110385195.6A CN202110385195A CN113293356A CN 113293356 A CN113293356 A CN 113293356A CN 202110385195 A CN202110385195 A CN 202110385195A CN 113293356 A CN113293356 A CN 113293356A
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tool
carbon
prefabricated part
frock
preparing
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郭李梁
朱振业
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26Deposition of carbon only
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83Carbon fibres in a carbon matrix
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45559Diffusion of reactive gas to substrate

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Composite Materials (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

A device for preparing carbon-carbon composite material relates to the technical field of new material preparation, wherein a prefabricated body is arranged in a tool, a heater is arranged outside the tool, an air inlet pipe (12) is arranged at the lower part of the tool, an air exhaust pipe (1) is arranged at the upper part of the tool, air is conveyed from inside to outside, deposition of pyrolytic carbon is propelled from high temperature to low temperature to finish densification, so that the deposition rate is improved, the uniformity of density is ensured, the surface of the prefabricated body is effectively prevented from crusting, one-step forming of the prefabricated body can be realized, and the like.

Description

Device for preparing carbon-carbon composite material
Technical Field
The invention relates to the technical field of new material preparation, in particular to a device for preparing a carbon-carbon composite material.
Background
Carbon/carbon composites (c-c composite or carbon-carbon composite materials) are known as carbon matrix composites reinforced with carbon fibers and their fabrics. Has a low density of<2.0g/cm3) High strength, high specific modulus, high thermal conductivity, low expansion coefficient, good friction performance, good thermal shock resistance and sizeThe high-temperature-resistant material has the advantages of high stability, is a few of alternative materials applied above 1650 ℃ nowadays, has the highest theoretical temperature higher than 2600 ℃, and is considered to be one of the most promising high-temperature materials.
Due to its unique properties, carbon/carbon composites have been widely used in the fields of intraocular lens preparation, aerospace, automotive industry, medicine, etc., such as rocket engine nozzles and throat liners thereof, thermal protection systems for end caps and wing leading edges of space shuttles, aircraft brake discs, etc.
The existing carbon/carbon composite material is usually prepared by a chemical vapor deposition method (CVD) and a traditional chemical liquid deposition method (CLD), wherein the traditional chemical liquid deposition method (CLD) is specifically realized by a chemical liquid deposition furnace, the heating time of a preform in the production of the equipment is 1/50-1/100 hours of the chemical vapor deposition method (CVD), and the skeleton density of the preform can be controlled from 0.3-0.8 g/cm3Is increased to 1.3 g/cm3However, the condensing device of the equipment adopts a blade type condenser, the recovery rate of the precursor is low, the environmental pollution is large, the method is not easy to control the product density, the production cost is greatly increased, the size of the prefabricated part is strictly limited, if the prefabricated part is large, the equipment power is extremely high, and the traditional Chemical Liquid Deposition (CLD) can not be popularized and applied in a large range by combining the factors. Wherein the specific device for realizing the Chemical Vapor Deposition (CVD) method is a chemical vapor deposition furnace, the device heats the whole preform in the production process, the process time lasts about 500-2000 hours, and the skeleton density of the preform is from 0.3-0.8 g/cm3Is increased to 1.3 g/cm3The above. The existing chemical vapor deposition device is in the middle of the deposition process, the surface of a prefabricated body is easy to crust, the gas path is closed, continuous deposition cannot be carried out, when continuous deposition cannot be carried out, the prefabricated body needs to be taken out for graphitization treatment, the crust part on the surface of the prefabricated body is machined and removed after graphitization treatment, a gas path channel is opened, then the gas path channel is placed into the deposition device again for deposition, in the deposition process, if the crust phenomenon occurs again, graphitization and machining are repeated, and subsequent deposition can be carried outAnd the process is complicated until the deposition of the prefabricated body is finished and the design requirement is met, the production period is long, and finally the cost is high. It is important to provide a device for preparing carbon-carbon composite material.
Disclosure of Invention
In order to overcome the defects in the background technology, the invention provides a device for preparing a carbon-carbon composite material, which can force gas to be conveyed from inside to outside, and the deposition of pyrolytic carbon is advanced from high temperature to low temperature to finish densification, thereby improving the deposition rate, ensuring the uniformity of density, effectively avoiding the surface incrustation of a preform, realizing the one-step molding of the preform and the like.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the utility model provides a device for preparing carbon-carbon composite, includes heater, preform apron, frock, exhaust tube, intake pipe and furnace body be equipped with at least one inclosed frock in the furnace body be equipped with at least one preform in the frock, be equipped with the preform apron at the open end of preform, be equipped with the exhaust tube that link up to below the tool apron in the frock above the tool apron, the upper end of exhaust tube passes the outside mechanism of bleeding of furnace body coupling, is equipped with the intake pipe that extends to the furnace body outside in the frock above the tool bottom plate, intake-tube connection gas mixer is equipped with the heater in the outside of frock, the heater connection heating source form device for preparing carbon-carbon composite.
In the device for preparing the carbon-carbon composite material, the heater is an induction heater or a resistance heater.
The device for preparing the carbon-carbon composite material comprises a tool, wherein the tool comprises a tool cover plate, a tool main body and a tool bottom plate, the tool main body is arranged on the tool bottom plate, the tool cover plate is arranged on the tool main body to enable the tool to form a cavity, and an air inlet pipe is arranged in the middle of the tool bottom plate.
When the prefabricated bodies are arranged in a plurality, the plurality of prefabricated bodies are arranged in a sleeved mode.
The device for preparing the carbon-carbon composite material is characterized in that when the number of the prefabricated bodies is three, the three prefabricated bodies are arranged to be a prefabricated body C, a prefabricated body B and a prefabricated body A, a prefabricated body cover plate C is arranged at the opening end of the prefabricated body C, the prefabricated body B is sleeved outside the prefabricated body C, a prefabricated body cover plate B is arranged at the opening end of the prefabricated body B, the prefabricated body A is sleeved outside the prefabricated body B, and a prefabricated body cover plate A is arranged at the opening end of the prefabricated body A.
According to the device for preparing the carbon-carbon composite material, when the tools are arranged in a plurality of ways, the tools are arranged in an up-and-down overlapping mode.
The device for preparing the carbon-carbon composite material comprises three tools, wherein the three tools are arranged in a vertically overlapped mode, an exhaust pipe is arranged on a tool cover plate in the upper tool, a tool bottom plate in the upper tool is arranged on a tool main body in the middle tool, the tool bottom plate in the middle tool is arranged on the tool main body in the lower tool, air inlets are respectively arranged on the tool bottom plate in the upper tool and the tool bottom plate in the middle tool, the upper tool, the middle tool and the lower tool are communicated through the air inlets to form an air exhaust passage, and an air inlet pipe is arranged on the tool bottom plate in the lower tool.
In the device for preparing the carbon-carbon composite material, the inner wall of the furnace body is provided with the heat-insulating layer.
In the device for preparing the carbon-carbon composite material, the gas mixer is respectively connected with a gas source and a carrier gas.
The device for preparing the carbon-carbon composite material is characterized in that the air exhaust mechanism comprises a vacuum pump and an air pipe, one end of the air pipe is connected with an air exhaust pipe, and the other end of the air pipe is connected with the vacuum pump.
By adopting the technical scheme, the invention has the following advantages:
the prefabricated body is arranged in the tool, the heater is arranged outside the tool, the air inlet pipe is arranged at the lower part of the tool, the exhaust pipe is arranged at the upper part of the tool, gas is conveyed from inside to outside, deposition of pyrolytic carbon is advanced from high temperature to low temperature to complete densification, so that the deposition rate is improved, the uniformity of density is ensured, the surface crusting of the prefabricated body is effectively avoided, one-step forming of the prefabricated body can be realized, and the like.
Drawings
FIG. 1 is a schematic view of a first structure of the present invention;
FIG. 2 is a second schematic structural view of the present invention;
FIG. 3 is a schematic view of a third structure of the present invention;
FIG. 4 is a schematic gas flow diagram of the present invention;
in the figure: 1. an air exhaust pipe; 2. a tooling cover plate; 3. a prefabricated cover plate A; 4. a prefabricated cover plate B; 5. a prefabricated cover plate C; 6. a preform C; 7. a preform B; 8. a preform A; 9. a tool main body; 10. a tooling bottom plate; 11. an induction heater; 12. an air inlet pipe; 13. a furnace body; 14. an air inlet; 15. a resistance heater.
Detailed Description
The present invention will be explained in more detail by the following examples, which are not intended to limit the invention;
it should be noted that the directions or positional relationships indicated by "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", etc., used in describing the structure of the present invention are based on the directions or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and thus, should not be construed as limiting the present invention.
The device for preparing the carbon-carbon composite material comprises a heater, a prefabricated body cover plate, a tool, an exhaust tube 1, an air inlet tube 12 and a furnace body 13, wherein in the implementation, a heat insulation layer is arranged on the inner wall of the furnace body 13, at least one closed tool is arranged in the furnace body 13, at least one prefabricated body is arranged in the tool, the prefabricated body cover plate is arranged at the opening end of the prefabricated body, the exhaust tube 1 penetrating below the tool cover plate 2 is arranged on the tool cover plate 2 in the tool, the upper end of the exhaust tube 1 penetrates through the furnace body 13 to be connected with an external exhaust mechanism, the exhaust mechanism can enable air in the tool to realize forced flow, so that the inner shell of the prefabricated body is prevented from forming and blocking an air channel, in the implementation, the exhaust mechanism comprises a vacuum pump and an air tube, one end of the air tube is connected with the exhaust tube 1, and the other end of the air tube is connected with the vacuum pump, the air exhaust mechanism can also be arranged as other devices with air exhaust function, an air inlet pipe 12 extending out of the furnace body 13 is arranged on the upper surface of the tool bottom plate 10 in the tool, the air inlet pipe 12 is connected with an air mixer, the air mixer is respectively connected with an air source and carrier gas, and the air of the air source is carbon-containing gas (mainly hydrocarbon gas), such as methane, natural gas, propane, butane and the like. The carrier gas is nitrogen, argon, hydrogen, helium and the like; the device is characterized in that a heater is arranged outside the tool, the heater is an induction heater 11 or a resistance heater 15, and the heater is connected with a heating source to form the device for preparing the carbon-carbon composite material.
Further, as shown in fig. 1, the tool comprises a tool cover plate 2, a tool main body 9 and a tool bottom plate 10, the tool main body 9 is arranged on the tool bottom plate 10, the tool cover plate 2 is arranged on the tool main body 9 to enable the tool to form a cavity, an air inlet pipe 12 is arranged in the middle of the tool bottom plate 10, and an air exhaust pipe 1 is arranged on the tool cover plate 2.
Further, as shown in fig. 1, 2 and 3, when a plurality of preforms are provided, the plurality of preforms are sleeved. When the number of the prefabricated bodies is three, the three prefabricated bodies are arranged into a prefabricated body C6, a prefabricated body B7 and a prefabricated body A8, a prefabricated body cover plate C5 is arranged at the opening end of the prefabricated body C6, a prefabricated body B7 is sleeved outside the prefabricated body C6, a prefabricated body cover plate B4 is arranged at the opening end of the prefabricated body B7, a prefabricated body A8 is sleeved outside the prefabricated body B7, and a prefabricated body cover plate A3 is arranged at the opening end of the prefabricated body A8.
Further, as shown in fig. 1, 2, and 3, when the plurality of tools are provided, the plurality of tools are stacked up and down. When the frock sets up to three, three frock superposes from top to bottom and sets up, set up exhaust tube 1 on frock apron 2 in the frock of upper strata, frock bottom plate 10 in the frock of upper strata sets up in the frock main part 9 of middle level in the frock of middle level, frock bottom plate 10 in the frock of middle level sets up in the frock main part 9 of lower floor, set up air inlet 14 respectively on frock bottom plate 10 in the frock of upper strata and the frock of middle level, upper strata frock, middle level frock and lower floor's frock pass through air inlet 14 intercommunication and form the route of bleeding, set up intake pipe 12 in the frock bottom plate 10 of lower floor.
In the specific implementation of the invention, the flow direction of the gas is as shown in fig. 4, the mixed gas enters the lower layer of the tool through the gas inlet pipe 12 at the lower end, then sequentially passes through the preform C6, the preform B7 and the preform A8, enters the middle layer of the tool through the gas inlet 14, sequentially passes through the preform C6, the preform B7 and the preform A8, enters the upper layer of the tool through the gas inlet 14, sequentially passes through the preform C6, the preform B7 and the preform A8, enters the gas extraction pipe 1 through the gas inlet 14, and the gas is extracted by the gas extraction mechanism, during the implementation, the heater heats the tool main body 9 in the tool, the tool main body 9 uniformly transfers the heat to the preform A8, the preform B7 and the preform C6, at this time, because the temperature of the preform A8 close to the tool main body 9 is the highest, the temperature of the preform B7 is slightly lower than that of the preform A8, the temperature of the preform C6 is the lowest, and when the mixed gas flows out of the gas diffusion pipe 12 and then enters the preform C6, In the preform B7, the preform A8, the carbon-containing gas in the mixed gas is adsorbed on the surface of the fiber, then the carbon is formed by pyrolysis, the gas-phase by-product molecules are desorbed and diffused to be discharged out of the preform A8, the preform B7 and the preform C6, the final by-product is discharged out of the tool through the exhaust tube 1, the carbon-containing gas is conveyed from inside to outside, the deposition of the pyrolytic carbon is propelled from high temperature to low temperature to complete densification, so that the deposition rate is improved, the uniformity of the density is ensured, the surface crusting of the preform is effectively avoided, and the one-step forming of the preform and the like can be realized.
In the implementation of the invention, the main parameters for preparing the carbon-carbon composite material are as follows:
heating temperature/. degree.C Pressure/pa Flow rate Deposition time/hour Incrustation Uniformity of Formation of carbon Black Final density g/cm3 Further deposit
1150 5000 1 230 Whether or not Is that Whether or not 1.63 Whether or not
1200 500 0.5 360 Whether or not Is that Whether or not 1.52 Whether or not
1250 8000 1.15 200 Whether or not Is that Whether or not 1.4 Whether or not
The present invention is not described in detail in the prior art.
The embodiments selected for the purpose of disclosing the invention, are presently considered to be suitable, it being understood, however, that the invention is intended to cover all variations and modifications of the embodiments which fall within the spirit and scope of the invention.

Claims (10)

1. The utility model provides a preparation carbon-carbon composite's device, includes heater, preform apron, frock, exhaust tube (1), intake pipe (12) and furnace body (13), characterized by: be equipped with at least one inclosed frock in furnace body (13) be equipped with at least one preform in the frock, be equipped with the preform apron at the open end of preform, be equipped with on the frock apron (2) in the frock and link up exhaust tube (1) below frock apron (2), the upper end of exhaust tube (1) is passed furnace body (13) and is connected outside air exhaust mechanism, is equipped with above frock bottom plate (10) in the frock and extends to outside intake pipe (12) of furnace body (13), gas mixer is connected in intake pipe (12), is equipped with the heater in the outside of frock, heater connection heating source forms preparation carbon-carbon composite's device.
2. The apparatus for preparing a carbon-carbon composite material according to claim 1, wherein: the heater is an induction heater (11) or a resistance heater (15).
3. The apparatus for preparing a carbon-carbon composite material according to claim 1, wherein: the tool comprises a tool cover plate (2), a tool main body (9) and a tool bottom plate (10), wherein the tool main body (9) is arranged on the tool bottom plate (10), the tool cover plate (2) is arranged on the tool main body (9) to enable the tool to form a cavity, an air inlet pipe (12) is arranged in the middle of the tool bottom plate (10), and an exhaust pipe (1) is arranged on the tool cover plate (2).
4. The apparatus for preparing a carbon-carbon composite material according to claim 1, wherein: when the prefabricated part sets up to a plurality of, a plurality of prefabricated parts are for cup jointing the setting.
5. The apparatus for preparing a carbon-carbon composite material according to any one of claims 1 or 4, wherein: when the prefabricated part sets up to three, three prefabricated part sets up to prefabricated part C (6), prefabricated part B (7) and prefabricated part A (8) the open end of prefabricated part C (6) is equipped with prefabricated part apron C (5), cup joints prefabricated part B (7) in the outside of prefabricated part C (6) the open end of prefabricated part B (7) is equipped with prefabricated part apron B (4), cup joints prefabricated part A (8) in the outside of prefabricated part B (7) the open end of prefabricated part A (8) is equipped with prefabricated part apron A (3).
6. The apparatus for preparing a carbon-carbon composite material according to claim 1, wherein: when the frock sets up to a plurality ofly, stack setting about a plurality of frocks.
7. The apparatus for preparing a carbon-carbon composite material according to any one of claims 1, 3 or 6, wherein: the tool is arranged to be three, the three tools are arranged in an up-and-down overlapping mode, the exhaust pipe (1) is arranged on the tool cover plate (2) in the upper tool, the tool bottom plate (10) in the upper tool is arranged on the tool main body (9) in the middle tool, the tool bottom plate (10) in the middle tool is arranged on the tool main body (9) in the lower tool, the air inlets (14) are respectively arranged on the upper tool and the lower tool, the upper tool, the middle tool and the lower tool are communicated through the air inlets (14) to form an exhaust passage, and the air inlet pipe (12) is arranged on the tool bottom plate (10) in the lower tool.
8. The apparatus for preparing a carbon-carbon composite material according to claim 1, wherein: and the inner wall of the furnace body (13) is provided with a heat-insulating layer.
9. The apparatus for preparing a carbon-carbon composite material according to claim 1, wherein: the gas mixer is respectively connected with a gas source and a carrier gas.
10. The apparatus for preparing a carbon-carbon composite material according to claim 1, wherein: the air exhaust mechanism comprises a vacuum pump and an air pipe, one end of the air pipe is connected with the air exhaust pipe (1), and the other end of the air pipe is connected with the vacuum pump.
CN202110385195.6A 2021-04-09 2021-04-09 Device for preparing carbon-carbon composite material Pending CN113293356A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110699667A (en) * 2019-11-25 2020-01-17 美尔森银河新材料(烟台)有限公司 Charcoal carbon crucible apparatus for producing
CN114411115A (en) * 2021-12-09 2022-04-29 安徽绿能技术研究院有限公司 Double-loop double-carbon-source rapid directional vapor deposition method
CN115369357A (en) * 2022-08-15 2022-11-22 湖南晶碳新材料有限公司 Carbon-carbon composite material production device

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110699667A (en) * 2019-11-25 2020-01-17 美尔森银河新材料(烟台)有限公司 Charcoal carbon crucible apparatus for producing
CN114411115A (en) * 2021-12-09 2022-04-29 安徽绿能技术研究院有限公司 Double-loop double-carbon-source rapid directional vapor deposition method
CN115369357A (en) * 2022-08-15 2022-11-22 湖南晶碳新材料有限公司 Carbon-carbon composite material production device
CN115369357B (en) * 2022-08-15 2023-10-20 湖南晶碳新材料有限公司 Carbon-carbon composite material production device

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