CN112225575A - High-performance carbon/carbon combined hot pressing die - Google Patents
High-performance carbon/carbon combined hot pressing die Download PDFInfo
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- CN112225575A CN112225575A CN202011045673.0A CN202011045673A CN112225575A CN 112225575 A CN112225575 A CN 112225575A CN 202011045673 A CN202011045673 A CN 202011045673A CN 112225575 A CN112225575 A CN 112225575A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/1208—Containers or coating used therefor
- B22F3/1216—Container composition
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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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
- C04B2235/02—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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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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
- C04B2235/02—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
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/3873—Silicon nitrides, e.g. silicon carbonitride, silicon oxynitride
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- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
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Abstract
The invention discloses a high-performance carbon/carbon combined hot pressing die. The key point is that the cylindrical carbon/carbon hot pressing die is provided with an inner ring wall (1) and an outer ring wall (2), the inner ring wall (1) is formed by overlapping a plurality of annular carbon/carbon material monomers (3), an ultrahigh-temperature adhesive layer (4) is arranged between the surfaces of the monomers (3), the outer ring wall (2) is formed by winding a plurality of layers of carbon fibers impregnated with impregnation liquid, and the carbon/carbon hot pressing die is heated, pressurized and cured, is densified by CVD and is fired at high temperature to form an integral structure. The inner ring wall of the invention is formed by superposing a plurality of annular monomers, the monomers can achieve uniform density and reach higher density, and the monomers are constrained by the surrounding structure of the outer ring wall to form a combined structure, so that the thickness of the integral hot-pressing die reaches a certain scale, and the uniform density and higher density of the integral die can be ensured.
Description
The technical field is as follows:
the invention relates to the field of high-temperature manufacturing such as powder metallurgy or ceramic material preparation, in particular to a high-performance mold prepared from a carbon/carbon material.
Background art:
the preparation process of the ceramic material comprises an important blank sintering process, wherein multi-component powder is prepared to form a blank, the blank is placed into a cylindrical mold to be fired at high temperature, and pressure is applied through two ends or one open end of the mold, so that the blank is sintered at high temperature and high pressure to obtain the ceramic material with the required advanced performance. The graphite mold is prepared from a graphite material, and the graphite mold can meet high temperature conditions, such as a high temperature of more than 2000 ℃, but the tensile strength of the graphite material is not high enough, and the pressure applied in the high-temperature pressurizing preparation process of the ceramic material is usually more than 50Mpa, for example, in the preparation of materials such as boron carbide, silicon nitride, alumina and the like, and larger pressure can be applied to increase the compactness of the ceramic material. The graphite mold is easily subjected to brittle fracture in the pressurizing process due to certain brittleness of the graphite material, which can cause serious production accidents. At present, a mold of a carbon/carbon material is also provided, which is a mold of an integrated structure prepared by a conventional carbon/carbon material preparation process including steps of carbon cloth net tire needling, preform preparation, CVD vapor deposition and the like, and has improved tensile strength compared with a graphite mold. Therefore, the service life of the existing carbon/carbon material mold is far from the required 300-furnace service life requirement, so that the problem of improving the service life of the mold is still a urgent need to be solved.
The invention content is as follows:
the invention aims to disclose a carbon/carbon material combined hot pressing die with high performance and long service life.
The technical scheme for realizing the invention is as follows: the cylindrical carbon/carbon hot pressing mold is provided with an inner annular wall and an outer annular wall, wherein the inner annular wall is formed by overlapping a plurality of annular carbon/carbon material monomers, an ultrahigh-temperature adhesive layer is arranged between the surfaces of the monomers, the outer annular wall is formed by winding a plurality of layers of carbon fibers impregnated with impregnating solution, and the carbon/carbon hot pressing mold is of an integral structure through heating, pressurizing, curing, CVD densification and high-temperature firing.
The monomer is prepared by superposing a plurality of layers of carbon fiber cloth impregnated with impregnating solution, and carrying out high-temperature heating curing, CVD densification and high-temperature treatment, the thickness of the monomer is 12-20 mm, and the content of carbon fibers in the monomer is 70-90%.
The monomer is prepared by winding carbon fiber bundles soaked with impregnation liquid into a flat ring shape through high-pressure heating curing and high-temperature treatment, the thickness of the monomer is 15-20 mm, and the content of carbon fibers in the monomer is 70-90%.
One surface of the single body is provided with a convex part, and the other surface is provided with a concave part.
The ultra-high temperature adhesive layer before curing is composed of, by weight, 25-35% of phenolic resin, 10-25% of silica sol, 10-15% of nano-scale carbon black, 8-15% of silicon powder with the particle size of 30-50 microns, 4-6% of silicon nitride with the particle size of 30-50 microns and 10-17% of chopped carbon fibers with the length of 2-5 mm.
The outer annular wall of the surface of the inner annular wall is formed by winding 8-12 layers of integral carbon fiber cloth soaked with the impregnation liquid.
The outer ring wall on the surface of the inner ring wall is formed by spirally winding carbon fiber cloth strips soaked with impregnation liquid and the axial direction of the cylindrical inner ring wall at an included angle, the number of layers is 8-12, the number of even layers is the same, and the winding directions of adjacent layers are opposite.
The included angle between the wound carbon fiber cloth strip with the impregnation liquid and the axial direction of the cylindrical inner annular wall is 54-55 degrees.
The impregnating solution comprises, by weight, 60-70% of phenolic resin, 10-15% of nano-carbon black, 2-5% of short carbon fibers with the length of 2-5 mm and 8-15% of silicon powder with the particle size of 30-50 mu m.
In the technical scheme disclosed by the invention, the inner ring wall is formed by overlapping a plurality of annular monomers, the monomers can be uniform in density and reach higher density, and are constrained by the surrounding structure of the outer ring wall to form a combined structure, so that the thickness of the whole hot-pressing die reaches a certain scale, the uniform density and higher density of the whole hot-pressing die can be ensured, the strength and thermal performance of the hot-pressing die reach higher levels, the tensile strength and radial force resistance of the cylindrical hot-pressing die are greatly improved by the unique structure of the inner ring wall and the outer ring wall of the hot-pressing die, the whole preparation process time is reduced, the performance and service life of the cylindrical hot-pressing die are greatly improved, and the preparation cost is reduced.
Description of the drawings:
fig. 1 is an overall state diagram of a cylindrical hot press die according to the present invention.
Fig. 2 is a schematic sectional structure view of fig. 1.
FIG. 3 is a schematic cross-sectional view of the single body of the present invention.
FIG. 4 is a schematic cross-sectional view of another structure of the monomer of the present invention.
The specific implementation mode is as follows:
detailed description of the embodiments of the present invention will be given in conjunction with the accompanying drawings, and it should be noted that the detailed description of the embodiments of the present invention is made for the purpose of facilitating understanding of the technical spirit of the entire invention, and should not be construed as limiting the scope of the claims of the present invention.
Referring to fig. 1 to 4, a technical solution of an embodiment of the present invention is: the cylindrical carbon/carbon hot pressing mold is provided with an inner annular wall 1 and an outer annular wall 2, wherein the inner annular wall 1 is formed by overlapping a plurality of annular carbon/carbon material monomers 3, an ultrahigh-temperature adhesive layer 4 is arranged between the surfaces of the monomers 3, the outer annular wall 2 is formed by winding a plurality of layers of carbon fibers impregnated with impregnating liquid, and the carbon/carbon hot pressing mold is of an integral structure through heating, pressurizing, curing, CVD (chemical vapor deposition) densification and high-temperature firing. The annular monomers 3 of the inner annular wall 1 are flat annular carbon/carbon materials, similar to common annular gaskets, and can be heated, pressurized and cured to 1.5g/cm due to the specific shape of the monomers 33The density of the monomer 3 can still reach 1.5g/cm after high-temperature sintering and CVD vapor deposition3Above, what is more critical is that the density of the monomer 3 is basically uniform due to the smaller thickness, so that the whole inner annular wall 1 with larger volume or size has basically uniform density, the unevenness of thermal stress in a high-temperature environment in the using process and the unevenness of internal stress when the external force is applied are reduced, the tensile and compression resistance of the inner annular wall 1 are improved, and the tensile and compression resistance of the whole inner annular wall 1 is also improved due to the uniformity of the carbon fiber trend or distribution of the monomer 3; and the outer annular wall 2The radial expansion of the inner annular wall 1 is applied with a strong constraint force, and the strong constraint force is obtained from the winding structure of the multilayer carbon fiber cloth and the tensile resistance of the carbon fiber; the combined structural characteristics of the inner and outer annular walls (1, 2) enable the cylindrical carbon/carbon hot-pressing die to have excellent axial tensile and compressive resistance and excellent radial deformation resistance, and due to the high density and uniform density of the inner annular wall 1 and the outer annular wall 2, the cylindrical carbon/carbon hot-pressing die has excellent thermodynamic performance and greatly prolongs the service life.
The monomer 3 is prepared by superposing a plurality of layers of carbon fiber cloth impregnated with impregnation liquid and carrying out high-temperature heating curing, CVD densification and high-temperature treatment; the structure ensures that the monomer 3 has good distribution uniformity of carbon fibers, does not have weak links for resisting radial force, is particularly beneficial to the curing process when pressure is applied, the thickness of the monomer 3 is 12-20 mm, and the thickness range can effectively control the uniformity of unit density and the unit density to reach 1.5g/cm3The content of the carbon fiber in the monomer 3 is 70-90%, and the balance is components or structures after the impregnation liquid is subjected to high-temperature treatment and pyrolytic carbon generated by CVD vapor deposition.
The monomer 3 is formed by winding a carbon fiber bundle impregnated with an impregnating solution into a flat ring shape, curing the carbon fiber bundle into a ring monomer 3 with a required size through heating and pressurizing, and obtaining the monomer 3 of the carbon/carbon material through high-temperature treatment and CVD vapor deposition, wherein the thickness of the monomer 3 is 15-20 mm, and the density is 1.5g/cm3The content of carbon fiber in the monomer 3 is 70-90%, and the balance is components or structures after the impregnation liquid is subjected to high-temperature treatment and pyrolytic carbon generated by CVD vapor deposition; the single body 3 is tightly wound in a flat mold under a certain tension, so that the single body 3 has excellent radial acting force resistance, the tensile resistance of the existing carbon fiber bundle is reflected in an optimal mode, and the service life of the hot-pressing mold is prolonged.
One surface of the monomer 3 is provided with a convex part 5, the other surface is provided with a concave part 6, the convex part 5 and the concave part 6 are mutually embedded when two adjacent monomers 3 are superposed, the integral structure strength of the inner ring wall 1 can be further improved, the erosion resistance of the inner ring wall 1 is improved, the convex part 5 and the concave part 6 can be arranged at the inner circle edge or the outer circle edge of the circular monomer 3 or the middle position of the circular surface, and the heating, pressurizing and curing processes of the monomers 3 can be realized.
The ultra-high temperature adhesive layer 4 before curing is composed of, by weight, 25-35% of phenolic resin, 10-25% of silica sol, 10-15% of nano-scale carbon black, 8-15% of silicon powder with the particle size of 30-50 microns, 4-6% of silicon nitride with the particle size of 30-50 microns and 10-17% of chopped carbon fibers with the length of 2-5 mm. In the process of heating, pressurizing and curing the adhesive, part of the adhesive can penetrate into the surface layer of the monomer 3, a plurality of annular monomers 3 are sintered into a cylindrical inner annular wall 1 in a high-temperature treatment stage, and the components of the adhesive contain ceramic components, so that the ultrahigh-temperature adhesive layer 4 has high strength and good oxidation resistance, and the overall strength performance of the inner annular wall 1 is further improved.
The outer annular wall 2 on the surface of the inner annular wall 1 is formed by winding 8-12 layers of integral carbon fiber cloth soaked with the impregnation liquid; the winding tension of the carbon fiber cloth is 50-60 kg during winding so as to improve the compactness of the wound carbon fiber cloth layer, the integral carbon fiber cloth can enable the integrity of the outer ring wall 2 to be good, and the tensile resistance of the outer ring wall 2 to be balanced. The outer ring wall 2 on the surface of the inner ring wall 1 is formed by spirally winding carbon fiber cloth strips soaked with impregnation liquid and the axial direction of the cylindrical inner ring wall 1 at an included angle, the number of layers is 8-12, the winding directions of adjacent layers are opposite, the winding tension of the carbon fiber cloth strips is 40-50 kg during winding, the winding structure not only ensures that the compactness of the multilayer carbon fiber cloth layer is good, but also the stress of the carbon fiber bundles inside can be mutually offset, and has excellent tensile resistance, and through repeated tests and detection, the included angle between the wound carbon fiber cloth strip with the impregnating solution and the axial direction of the cylindrical inner annular wall 1 is 54-55 degrees, when the outer annular wall 2 is subjected to external force, the tensile resistance of the carbon fiber bundle is fully exerted, and the filaments are obliquely and integrally extruded, so that the deformation resistance is greatly improved, and the strength of the outer annular wall 2 is greatly improved; and the outer annular wall 2 of the carbon/carbon material is obtained by pressurization directional solidification, high-temperature treatment and CVD vapor deposition, the content of carbon fibers in the outer annular wall 2 is 70-90%, and the balance is components or structures after the impregnation liquid is subjected to high-temperature treatment and pyrolytic carbon generated by CVD vapor deposition.
The impregnating solution comprises, by weight, 60-70% of phenolic resin, 10-15% of nano-scale carbon black, 2-5% of short cut carbon fibers with the length of 2-5 mm and 8-15% of silicon powder with the particle size of 30-50 mu m; the impregnation liquid has good rheological property and dispersibility, and can be uniformly dispersed among carbon fiber filaments of carbon fiber cloth or carbon fiber bundles, and the specific granularity required by the carbon black and the silicon powder is to ensure uniform distribution in the carbon fiber cloth or the carbon fiber bundles on one hand, and to improve the reaction in the high-temperature treatment process and obtain a structure in the high-temperature treatment process on the other hand, so as to increase the structural strength of the carbon/carbon material.
Claims (9)
1. A high-performance carbon/carbon combined hot pressing die is characterized in that a cylindrical carbon/carbon hot pressing die is provided with an inner annular wall (1) and an outer annular wall (2), the inner annular wall (1) is formed by overlapping a plurality of annular carbon/carbon material monomers (3), an ultrahigh-temperature adhesive layer (4) is arranged between the surfaces of the monomers (3), the outer annular wall (2) is formed by winding a plurality of layers of carbon fibers impregnated with impregnating liquid, and the carbon/carbon combined hot pressing die is of an integrated structure through heating, pressurizing, curing, CVD densification and high-temperature firing.
2. The high-performance carbon/carbon combined hot press mold as claimed in claim 1, wherein the single body (3) is prepared by stacking a plurality of layers of carbon fiber cloth impregnated with impregnation liquid, and performing high-temperature heating curing, CVD densification and high-temperature treatment, the thickness of the single body (3) is 12-20 mm, and the content of carbon fiber in the single body (3) is 70-90%.
3. The high-performance carbon/carbon combined hot press mold as claimed in claim 1, wherein the single body (3) is prepared by winding carbon fiber bundles impregnated with the impregnation liquid into a flat ring shape, and performing high-pressure heating curing and high-temperature treatment, the thickness of the single body (3) is 15-20 mm, and the carbon fiber content in the single body (3) is 70-90%.
4. The high performance carbon/carbon combined hot press mold as claimed in claim 1, 2 or 3, wherein the single body (3) has a convex portion (5) on one surface and a concave portion (6) on the other surface.
5. The high-performance carbon/carbon combined hot press mold as claimed in claim 4, wherein the ultra-high temperature adhesive layer (4) comprises, by weight, 25-35% of phenolic resin, 10-25% of silica sol, 10-15% of nano-scale carbon black, 8-15% of silica powder with a particle size of 30-50 μm, 4-6% of 30-50 μm of silicon nitride and 10-17% of chopped carbon fibers with a length of 2-5 mm before curing.
6. The high-performance carbon/carbon combined hot press mold as claimed in claim 5, wherein the outer annular wall (2) of the surface of the inner annular wall (1) is formed by winding 8-12 layers of integral carbon fiber cloth impregnated with impregnation liquid.
7. The high-performance carbon/carbon combined hot press mold according to claim 5, wherein the outer annular wall (2) on the surface of the inner annular wall (1) is formed by spirally winding carbon fiber cloth strips impregnated with impregnating solution and the axial direction of the cylindrical inner annular wall (1) at an included angle, the number of layers is an even number of layers of 8-12, and the winding directions of adjacent layers are opposite.
8. The high performance carbon/carbon combined hot press mold as claimed in claim 7, wherein the included angle between the wound carbon fiber cloth strip with impregnation liquid and the axial direction of the cylindrical inner annular wall (1) is 54 ° to 55 °.
9. The high-performance carbon/carbon combined hot press mold according to claim 6, 7 or 8, wherein the impregnating solution comprises, by weight, 60 to 70% of phenolic resin, 10 to 15% of nano-carbon black, 2 to 5% of short carbon fibers having a length of 2 to 5mm, and 8 to 15% of silicon powder having a particle size of 30 to 50 μm.
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| CN113416087A (en) * | 2021-07-20 | 2021-09-21 | 西安美兰德新材料有限责任公司 | Preparation method of high-strength combined carbon/carbon hot-pressing mold |
| CN113927714A (en) * | 2021-10-15 | 2022-01-14 | 西安美兰德新材料有限责任公司 | Carbon-carbon combined hot-pressing mold and preparation method thereof |
| 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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| 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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| CN112225575B (en) | 2022-06-03 |
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