CN111217617A - Ultrahigh-temperature large-scale complex carbon/carbon material component - Google Patents
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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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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/95—Products characterised by their size, e.g. microceramics
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Abstract
The invention discloses an ultrahigh-temperature large complex carbon/carbon material component. The key point is that the composite material comprises at least two carbon/carbon material component prefabricated bodies prepared from carbon fiber cloth and impregnation liquid, wherein the carbon/carbon material component prefabricated bodies are provided with connecting surfaces which are matched and contacted with each other, an adhesive layer is arranged between the connecting surfaces of the carbon/carbon material component prefabricated bodies, and the ultrahigh-temperature large-scale complex carbon/carbon material component is prepared by high-temperature sintering. The size of the large complex carbon/carbon material component with the ultra-high temperature (more than 2000 ℃) can reach about two meters, and the large complex carbon/carbon material component has the performances of high strength and high temperature resistance (more than 2000 ℃).
Description
The technical field is as follows:
the invention relates to a carbon/carbon composite material, in particular to a large-scale carbon/carbon component with a complex structure and an ultrahigh temperature (more than 2000 ℃).
Background art:
the C/C composite material is the most advanced high-temperature structure/function composite material in the present generation, has excellent high-temperature mechanical properties and thermophysical properties such as light specific gravity, heat resistance, high strength, ablation resistance and the like, is widely applied to the field of aerospace, but is only limited to small components with medium and high temperature and simple shapes.
With the development of engineering technology, the civil fields of metallurgy, machinery, photovoltaics, chemical industry and the like have urgent needs for C/C composite materials. And the requirements of various complicated shapes and structures need to be met, and particularly the requirement on large complicated special-shaped components is more urgent. In recent years, with the rapid development of the photovoltaic industry, the demand of single crystal silicon and polycrystalline silicon production for large and complex components is particularly urgent, for example, a large gas limiting cylinder (1200mm by 1650mm by 5-8mm) is required for an ultra-large vapor deposition furnace in the single crystal silicon field, and a large thin-wall flat plate is required for a large deposition furnace in the polycrystalline silicon field. However, the manufacturing of such large C/C complex profiled components is difficult to realize due to the limitations of both equipment and the existing production process (preform-CVD method). Therefore, how to prepare the complex special-shaped component of the large-scale C/C material still remains to be solved urgently.
The invention content is as follows:
the invention aims to disclose a large-size carbon/carbon composite material component which is high-temperature resistant and has a special-shaped structure.
The technical solution for realizing the invention is as follows: the composite material comprises at least two carbon/carbon material component prefabricated bodies prepared from carbon fiber cloth and impregnation liquid, wherein the carbon/carbon material component prefabricated bodies are connected with each other in a matched and contacted manner, an adhesive layer is arranged between the connection surfaces of the carbon/carbon material component prefabricated bodies, and the ultrahigh-temperature large-scale complex carbon/carbon material component is prepared by high-temperature sintering.
The carbon/carbon material component prefabricated body is formed by laminating at least more than two layers of carbon fiber cloth soaked with the impregnation liquid and then heating; the connection surface of the prefabricated body of the carbon/carbon material component is step-shaped, tenon-and-groove-shaped, curved surface-shaped or plane-shaped.
The carbon/carbon material component prefabricated body is in a cylindrical shape, or a curved plate shape, a flat plate shape or a special-shaped structure.
The impregnating solution comprises the following components in percentage by weight: adding 40-55% of phenolic resin powder into 40-60% of ethanol, uniformly stirring, then adding 8-12% of graphite powder and 3-5% of zirconia powder, uniformly stirring, and standing for 20-40 hours to obtain an impregnation liquid.
The carbon/carbon material component is prefabricated into a cylinder shape, and the preparation steps are as follows:
a. soaking the carbon fiber cloth in the soaking solution, taking out, putting into a vacuum furnace, heating to 950 ℃, and preserving heat for 1-2 hours to obtain pre-soaked carbon fiber cloth;
b. winding the pre-impregnated carbon fiber cloth on a cylindrical mold, wherein the winding rolling pressure is 0.3-0.6 Mpa, the tension is 200-300 kg, the winding temperature is 90-110 ℃, and the winding speed is 2-4 r/min, so as to obtain a cylindrical carbon/carbon material member blank;
c. and (3) putting the primary blank into a pressurizing directional curing furnace, sealing, vacuumizing to-0.1 Mpa at a speed of 100-200 Pa/h, heating the interior of the cylindrical primary blank, keeping the temperature of the exterior of the cylindrical primary blank at normal temperature or cooling to keep the normal temperature, heating the interior of the cylindrical primary blank to 100 ℃, keeping the temperature for 30 minutes, continuously heating, pressurizing to 0.2-0.5 Mpa, heating to 180-200 ℃, keeping the temperature and maintaining the pressure for 2 hours, and thus obtaining the preform.
The carbon/carbon material component prefabricated body is of a curved plate shape, a flat plate shape or a special-shaped structure, and is prepared by laminating and hot-pressing at least two layers of carbon fiber cloth soaked with impregnation liquid, wherein the forming pressure is 5-10 Mpa, and the forming temperature is 100-180 ℃; and (4) placing the mixture into a high-temperature furnace, and heating to 900-1000 ℃ to obtain a preform.
The adhesive of the adhesive layer comprises the following components in percentage by weight:
the preparation steps of the adhesive are as follows: and sequentially adding the coupling agent, the auxiliary agent, the graphite powder, the silicon powder, the carbon felt powder and the short carbon fibers into liquid phenolic resin, adding the next component after adding one component and stirring uniformly, finally adding the short carbon fibers, stirring for 10-25 minutes, then putting into a ball mill, milling for 30-45 minutes, putting into a closed container, and standing for 20-36 hours to obtain the adhesive.
The high-temperature preparation steps of the carbon/carbon material component are as follows:
firstly, after the adhesive is coated on the connecting surface of a carbon/carbon material component prefabricated body, pressurizing and gluing, wherein the gluing pressure is 5-10 Mpa, and the gluing temperature is 100-200 ℃;
②, placing the mixture into a high-temperature furnace, keeping the temperature for 2-3 hours, wherein the firing temperature is 1700-2000 ℃;
thirdly, under the condition of 1040-1100 ℃, the obtained product is subjected to carbon material density increase according to a conventional CVD process, and the deposition time is 50-200 hours, so that the ultrahigh-temperature large complex carbon/carbon material component is obtained.
The size of the large complex carbon/carbon material component with ultrahigh temperature (more than 2000 ℃) formed by the technical scheme can reach about two meters, the wall thickness of the component is 5-15 mm, the component has high strength and high temperature (more than 2000 ℃) resistance under the size, more importantly, the component has a complex special-shaped structure, and the connecting part of the special-shaped structure has excellent mechanical property, which cannot be achieved by the prior art.
The specific implementation mode is as follows:
the following detailed description of the present invention is given in detail, and it should be noted that the description of the embodiments of the present invention is made for the purpose of facilitating a comprehensive understanding of the technical contents of the present invention, and should not be construed as limiting the scope of the claims of the present invention.
The technical solution of the specific embodiment of the invention is as follows: the method comprises at least two carbon/carbon material component prefabricated bodies prepared from carbon fiber cloth and impregnation liquid, wherein connecting surfaces which are matched and contacted with each other are arranged between the carbon/carbon material component prefabricated bodies, two or more carbon/carbon material component prefabricated bodies can be matched to form a special-shaped component prefabricated body with a larger size through the connecting surfaces, an adhesive layer is arranged between the connecting surfaces of the carbon/carbon material component prefabricated bodies, and the ultrahigh-temperature large-scale complex carbon/carbon material component is prepared by high-temperature sintering. The carbon/carbon material component prefabricated body can be a large-size thin-wall structure, and also has high-temperature resistance, high density and good structural strength, the adhesive layer has excellent high-temperature resistance after being fired at high temperature, the general working temperature is 1700-2000 ℃, and also has very good mechanical properties, the interlayer shear strength is higher than or equal to 12Mpa, the elastic modulus is higher than or equal to 20Gpa, the compression strength is higher than or equal to 150Mpa, the tensile strength is higher than or equal to 60Mpa, and more importantly, the coefficient of thermal expansion and contraction of the adhesive layer is very close to the coefficient of thermal expansion and contraction of the carbon/carbon material component, so that the carbon/carbon material component prefabricated body can be ensured not to have micro cracks caused by thermal stress in the long-term use process, and the service life, the strength and the air tightness are.
The carbon/carbon material component prefabricated body is formed by laminating at least more than two layers of carbon fiber cloth soaked with the impregnation liquid and then heating; the connection surface of the prefabricated body of the carbon/carbon material component is step-shaped, tenon-and-groove-shaped, curved surface-shaped or plane-shaped. The prefabricated part comprises at least two layers of carbon fiber cloth impregnated with impregnation liquid, wherein the carbon fiber cloth is prepared by laminating, but not limited to two layers, and 5-10 layers can be selected according to the thickness of the carbon fiber cloth layer and the technical requirements of carbon/carbon material components; the various forms of the joint faces of the carbon/carbon material member preforms described above are options for facilitating joint structures between different shapes of carbon/carbon material member preforms for joining at different locations between the various preforms. The prefabricated body of the carbon/carbon material component has a cylindrical, or bent plate-shaped, or flat-plate-shaped or special-shaped structure, and the prefabricated bodies in various shapes can form large-sized and complex-shaped components with various technical requirements through the adhesive so as to meet the requirements of different use states.
The carbon/carbon material component preform is prepared from carbon fiber cloth and impregnation liquid, wherein the impregnation liquid comprises the following components in percentage by weight: adding 40-55% of phenolic resin powder into 40-60% of ethanol, uniformly stirring, then adding 8-12% of graphite powder and 3-5% of zirconia powder, uniformly stirring, and standing for 20-40 hours to obtain an impregnation liquid; the trade name of the phenolic resin powder is PF-4012, the granularity of graphite powder is 10000 meshes, the zirconia powder is industrial pure, ethanol is industrial pure and can be purchased in the market, the standing of the impregnating solution enables the components to be fully fused, the selection of the granularity of the specific components enables the components and the carbon fiber cloth to be mutually permeated, and more importantly, the granularity of the specific components enables the components of the impregnating solution and the fibers of the carbon fiber cloth to form a high-strength micro-crystalline structure in the high-temperature treatment process, so that the carbon/carbon material member has good oxidation resistance while having high strength.
The carbon/carbon material component prefabricated body is described to be cylindrical, and the preparation steps are as follows: a. soaking the carbon fiber cloth in the soaking solution, taking out, putting into a vacuum furnace, heating to 950 ℃, and preserving heat for 1-2 hours to obtain pre-soaked carbon fiber cloth; b. winding the pre-impregnated carbon fiber cloth on a cylindrical mold, wherein the winding rolling pressure is 0.3-0.6 Mpa, the tension is 200-300 kg, the winding temperature is 90-110 ℃, and the winding speed is 2-4 r/min, so as to obtain a cylindrical carbon/carbon material member blank; c. and (3) putting the primary blank into a pressurizing directional curing furnace, sealing, vacuumizing to-0.1 Mpa at a speed of 100-200 Pa/h, heating the interior of the cylindrical primary blank, keeping the temperature of the exterior of the cylindrical primary blank at normal temperature or cooling to be at normal temperature, heating the interior of the cylindrical primary blank to 100 ℃, keeping the temperature for 30 minutes, continuously heating, pressurizing to 0.2-0.5 Mpa, heating to 180-200 ℃, keeping the temperature and maintaining the pressure for 2 hours, and thus obtaining the preform.
In the step a, the carbon fiber cloth and the impregnation liquid are subjected to preliminary reaction to release volatile components, meanwhile, the carbon fiber cloth is subjected to heat treatment to eliminate the self-elasticity, so that the carbon fiber cloth is in a stable state, and the step c is used for further treating the cylindrical blank, so that the stress generated in the step b is eliminated, and meanwhile, the cylindrical blank is further solidified into a whole.
The carbon/carbon material component prefabricated body is in a curved plate shape, a flat plate shape or a special-shaped structure, and is prepared by laminating and hot-pressing at least two layers of carbon fiber cloth soaked with impregnation liquid, wherein the forming pressure is 5-10 Mpa, and the forming temperature is 100-180 ℃; placing the mixture into a high-temperature furnace, and heating to 900-1000 ℃ to obtain a prefabricated body; the density of the prefabricated body is increased by pressurizing, meanwhile, part of volatile components are released by heating, and the prefabricated body is preliminarily carbonized and solidified and molded in a high-temperature state.
The carbon/carbon material component prefabricated body is formed by bonding an adhesive on a connecting surface to form a larger prefabricated body with a complex structure, wherein the adhesive comprises the following components in percentage by weight: 35-50% of liquid phenolic resin with the trade name of PF-9300; 3-5% of coupling agent with the trade name of KH-550; 3-5% of an auxiliary agent with the trade name of OBSH; 10-15% of graphite powder with the granularity of 2000 meshes; 6-10% of silicon powder with the granularity of 1000 meshes; 8-15% of carbon felt powder with the granularity of 100 meshes; 3-10% of short carbon fiber, and the length is 5-10 mm. The components can be directly purchased from the market.
The adhesive forms a matrix of the carbon/carbon material after high-temperature treatment, and simultaneously forms a small amount of more complex micro-crystalline structure, so that the adhesive layer has good strength, the density of the adhesive and the prefabricated part of the bonded carbon/carbon material component is also close in the high-temperature treatment process, the coefficient of expansion with heat and contraction with cold is also quite close, the finally prepared carbon/carbon material component has excellent integral mechanical property, and the service life is greatly prolonged.
The preparation steps of the adhesive are as follows: sequentially adding the coupling agent, the auxiliary agent, the graphite powder, the silicon powder, the carbon felt powder and the short carbon fibers into liquid phenolic resin, adding the next component after adding one component and stirring uniformly, finally adding the short carbon fibers, stirring for 10-25 minutes, then putting into a ball mill, milling for 30-45 minutes, putting into a closed container, and standing for 20-36 hours to obtain the adhesive; through the preparation steps, the components of the adhesive are fully fused with each other, the excellent mutual mixing degree and the excellent space embedding degree among the component particles are obtained, and an adhesive layer with excellent mechanical property can be obtained in the subsequent high-temperature firing.
the high-temperature preparation steps of the carbon/carbon material component comprise the steps of coating the adhesive on the connecting surface of the carbon/carbon material component preform to form a large-scale complex-structure preform, applying pressure to bond the preform at the bonding pressure of 5-10 Mpa and the bonding temperature of 100-200 ℃, placing the preform into a high-temperature furnace at the firing temperature of 1700-2000 ℃, and preserving heat for 2-3 hours, and performing carbon material density increasing on the preform by using a conventional CVD process at the temperature of 1000-1100 ℃ for 50-200 hours to obtain the ultrahigh-temperature large-scale complex carbon/carbon material component.
Claims (9)
1. The large-scale complicated charcoal/carbon material component of a kind of ultra-high temperature, characterized by that to include at least two charcoal/carbon material component prefabricates prepared from carbon fiber cloth and impregnating solution, there are the joint faces that match each other and contact between the charcoal/carbon material component prefabricates, there are adhesive layers between the joint faces of the charcoal/carbon material component prefabricates, burn and make said large-scale complicated charcoal/carbon material component of ultra-high temperature through the high temperature.
2. The ultrahigh-temperature large complex carbon/carbon material member as claimed in claim 1, wherein the carbon/carbon material member preform is formed by laminating at least two or more layers of carbon fiber cloth impregnated with an impregnation solution and heating the laminated cloth; the connection surface of the prefabricated body of the carbon/carbon material component is step-shaped, tenon-and-groove-shaped, curved surface-shaped or plane-shaped.
3. The ultrahigh-temperature large complex carbon/carbon material member as claimed in claim 1 or 2, wherein the preform of the carbon/carbon material member is in the shape of a cylinder, or a curved plate, a flat plate, or a special-shaped structure.
4. The ultrahigh-temperature large complex carbon/carbon material member as claimed in claim 3, wherein the impregnation solution comprises the following components in percentage by weight: adding 40-55% of phenolic resin powder into 40-60% of ethanol, uniformly stirring, then adding 8-12% of graphite powder and 3-5% of zirconia powder, uniformly stirring, and standing for 20-40 hours to obtain an impregnation liquid.
5. The ultrahigh-temperature large complex carbon/carbon material member as claimed in claim 4, wherein the carbon/carbon material member is prefabricated in a cylindrical shape and is prepared by the following steps:
a. soaking the carbon fiber cloth in the soaking solution, taking out, putting into a vacuum furnace, heating to 950 ℃, and preserving heat for 1-2 hours to obtain pre-soaked carbon fiber cloth;
b. winding the pre-impregnated carbon fiber cloth on a cylindrical mold, wherein the winding rolling pressure is 0.3-0.6 Mpa, the tension is 200-300 kg, the winding temperature is 90-110 ℃, and the winding speed is 2-4 r/min, so as to obtain a cylindrical carbon/carbon material member blank;
c. and (3) putting the primary blank into a pressurizing directional curing furnace, sealing, vacuumizing to-0.1 Mpa at a speed of 100-200 Pa/h, heating the interior of the cylindrical primary blank, keeping the temperature of the exterior of the cylindrical primary blank at normal temperature or cooling to keep the normal temperature, heating the interior of the cylindrical primary blank to 100 ℃, keeping the temperature for 30 minutes, continuously heating, pressurizing to 0.2-0.5 Mpa, heating to 180-200 ℃, keeping the temperature and maintaining the pressure for 2 hours, and thus obtaining the preform.
6. The ultrahigh-temperature large-scale complex carbon/carbon material member as claimed in claim 4, wherein the carbon/carbon material member preform is in a curved plate shape, a flat plate shape or a special-shaped structure, and is prepared by hot-pressing at least two layers of carbon fiber cloth layers impregnated with impregnation liquid, wherein the molding pressure is 5-10 MPa, and the molding temperature is 100-180 ℃; and (4) placing the mixture into a high-temperature furnace, and heating to 900-1000 ℃ to obtain a preform.
7. The ultrahigh-temperature large complex carbon/carbon material member as claimed in claim 5 or 6, wherein the adhesive of the adhesive layer comprises the following components in percentage by weight:
8. the ultrahigh-temperature large complex carbon/carbon material member as claimed in claim 7, wherein the adhesive is prepared by the steps of: and sequentially adding the coupling agent, the auxiliary agent, the graphite powder, the silicon powder, the carbon felt powder and the short carbon fibers into liquid phenolic resin, adding the next component after adding one component and stirring uniformly, finally adding the short carbon fibers, stirring for 10-25 minutes, then putting into a ball mill, milling for 30-45 minutes, putting into a closed container, and standing for 20-36 hours to obtain the adhesive.
9. The ultrahigh-temperature large complex carbon/carbon material member as claimed in claim 8, wherein the high-temperature preparation step of the carbon/carbon material member is as follows:
firstly, after the adhesive is coated on the connecting surface of a carbon/carbon material component prefabricated body, pressurizing and gluing, wherein the gluing pressure is 5-10 Mpa, and the gluing temperature is 100-200 ℃;
②, placing the mixture into a high-temperature furnace, wherein the firing temperature is 1700-2200 ℃, and preserving heat for 2-3 hours;
thirdly, under the condition of 1040-1100 ℃, the obtained product is subjected to carbon material density increase according to a conventional CVD process, and the deposition time is 50-200 hours, so that the ultrahigh-temperature large complex carbon/carbon material component is obtained.
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| CN112225575A (en) * | 2020-09-28 | 2021-01-15 | 烟台凯泊复合材料科技有限公司 | High-performance carbon/carbon combined hot pressing die |
| CN112225574A (en) * | 2020-09-28 | 2021-01-15 | 烟台凯泊复合材料科技有限公司 | Manufacturing method of high-performance carbon/carbon combined hot-pressing mold |
| CN114409422A (en) * | 2022-01-25 | 2022-04-29 | 烟台凯泊复合材料科技有限公司 | Preparation method of high-temperature-resistant light ceramic heat shield |
| CN114621031A (en) * | 2022-01-25 | 2022-06-14 | 烟台凯泊复合材料科技有限公司 | Method for strengthening surface layer of C/C structural member of thermal field of single crystal furnace |
| CN115353406A (en) * | 2022-07-05 | 2022-11-18 | 烟台凯泊复合材料科技有限公司 | Airplane carbon material brake disc formed by waste carbon material discs and preparation method thereof |
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