CN114133262A - Wet needling process for preparing carbon/carbon composite material - Google Patents
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- 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
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- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C04B2235/5216—Inorganic
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Abstract
The invention discloses a wet needling process for preparing a carbon/carbon composite material, and relates to the technical field of preparation of carbon/carbon composite materials. The process comprises the following steps: dipping the carbon fiber net tire into the slurry to obtain a carbon fiber net tire prefabricated body; laminating the carbon fiber mesh tire prefabricated body and the carbon fiber cloth to obtain a slurry-containing carbon fiber fabric; carrying out needling on the carbon fiber fabric containing the sizing agent to obtain the needled fabric containing the sizing agent; sequentially heating, curing and carbonizing the slurry-containing needled fabric to obtain a low-density carbon/carbon composite material blank; repeatedly carrying out the processes of dipping, heating, curing and carbonizing on the low-density carbon/carbon composite material green body to obtain a high-density carbon/carbon composite material green body; carrying out high-temperature heat treatment on the high-density carbon/carbon composite material blank to obtain a carbon/carbon composite material; the slurry is an ethanol suspension of asphalt and graphite powder. The process method shortens the preparation period of the carbon/carbon composite material prepared by the needle punching method.
Description
Technical Field
The invention relates to the technical field of carbon/carbon composite material preparation, in particular to a wet needling process for preparing a carbon/carbon composite material.
Background
The needling forming process is to laminate sheet-shaped two-dimensional materials, then carry out needling in the longitudinal direction of the laminated fibers by using felting needles with barbs, so that the fibers in a two-dimensional plane can be pulled to the direction vertical to the two-dimensional plane, the two adjacent layers are both needled, and finally a large number of longitudinal fibers are connected to form the three-dimensional fabric. Compared with a fiber cloth laying forming mode, the process increases longitudinal fiber constraint and increases interlayer binding force; compared with a weaving process, the needling process is simpler and more convenient, and the forming speed is high.
The designability of the carbon/carbon composite properties is shown by the variation of the preformed reinforcement structure and densification process to meet different application requirements. Where a prefabricated reinforcement (preform) is the basis of a C/C composite, its structural form and properties have a large influence on the final properties of the composite. The principle of the needling preform is that after laid layers of non-woven cloth and a carbon fiber net tire, a special functional felting needle with a barb on an edge is adopted for needling, fibers in a net tire layer are carried to a Z direction (the direction vertical to the net tire) by means of reverse direction barbed piercing, so that vertical fiber clusters are generated, the non-woven cloth and the net tire are mutually entangled and mutually constrained, and a quasi three-dimensional net structure preform with certain strength on a plane and between layers is formed. The needling preform overcomes the defect of lack of connection between 2D carbon cloth laminated material layers, and has the advantages of unlimited product shape and thickness, excellent product performance and the like.
At present, the method for preparing the carbon/carbon composite material by using the needling forming process is mainly a dry needling method, and has the defects of long impregnation time (1-2 months for each impregnation) and more impregnation times (7-8 times for impregnation).
Therefore, the wet needling process for preparing the carbon/carbon composite material, which can shorten the preparation period of the carbon/carbon composite material, is provided, and has important significance for the technical field of carbon/carbon composite material preparation.
Disclosure of Invention
The invention aims to provide a wet needling process for preparing a carbon/carbon composite material, which aims to solve the problems in the prior art and shorten the preparation period of preparing the carbon/carbon composite material by a needling method.
In order to achieve the purpose, the invention provides the following scheme:
one of the technical schemes of the invention is a wet needling process for preparing a carbon/carbon composite material, which comprises the following steps:
step 1, dipping a carbon fiber net tire into slurry to obtain a carbon fiber net tire prefabricated body;
step 2, laminating the carbon fiber mesh prefabricated body and carbon fiber cloth to obtain a slurry-containing carbon fiber fabric; carrying out needling on the carbon fiber fabric containing the sizing agent to obtain the needled fabric containing the sizing agent; sequentially heating, curing and carbonizing the slurry-containing needled fabric to obtain a low-density carbon/carbon composite material blank;
step 3, repeatedly carrying out the processes of dipping, heating, curing and carbonizing on the low-density carbon/carbon composite material green body to obtain a high-density carbon/carbon composite material green body; carrying out high-temperature heat treatment on the high-density carbon/carbon composite material blank to obtain the carbon/carbon composite material;
in the step 1, the slurry is an ethanol suspension of asphalt and graphite powder.
Further, in the step 1, the mass ratio of the asphalt to the graphite powder in the slurry is 0.5-1.25: 1; the mass ratio of the total mass of the asphalt and the graphite powder to the mass of the ethanol is 2.5-3.5: 7.
Further, in the step 1, the carbon fiber net tire accounts for 12-25% of the mass of the slurry.
Further, in the step 2, the heating temperature is 80-90 ℃ and the time is 8-12 h; the curing temperature is 400-600 ℃, and the curing time is 24-48 h; the carbonization temperature is 800-900 ℃, and the carbonization time is 2-4 h.
Further, the slurry for impregnation in the step 3 is an ethanol suspension of asphalt and graphite powder, or an ethanol suspension of carbon black and phenolic resin;
the mass ratio of the asphalt to the graphite powder in the ethanol suspension of the asphalt and the graphite powder is 1:1, and the mass ratio of the total mass of the asphalt and the graphite powder to the ethanol is 3: 7;
the mass ratio of the carbon black to the ethanol to the phenolic resin in the ethanol suspension of the carbon black and the phenolic resin is 15:70: 15.
Further, the pressure of the impregnation in the step 3 is 1-5 Mpa, and the time is 4-6 h.
And (3) filling the graphite powder and the asphalt or the graphite powder and the phenolic resin in the slurry into the low-density carbon/carbon composite material by pressure impregnation.
Further, in the step 3, the heating temperature is 80-90 ℃ and the time is 8-12 h; the curing temperature is 400-600 ℃, and the curing time is 24-48 h; the carbonization temperature is 800-900 ℃, and the carbonization time is 2-4 h.
Further, in the step 3, the number of times of repetition is 3-5 times.
Further, in the step 3, the temperature of the high-temperature heat treatment is 1500-1800 ℃ and the time is 2 hours.
According to the second technical scheme, the carbon/carbon composite material is prepared by the preparation process.
The technical idea of the invention is as follows:
the slurry for impregnation is a mixture consisting of asphalt, graphite and ethanol, the carbon content in the carbon fiber net tire can be adjusted by controlling the ratio of the asphalt to the graphite in the mixture, and the carbon fiber net tire is impregnated in the slurry before needling, so that the solid content of the needled fabric is increased, and the carbon/carbon composite material prepared by the conventional preparation method (the carbon/carbon composite material is impregnated in the slurry for a long time for many times after needling) can have the effect of similar mechanical property with the carbon/carbon composite material prepared by the conventional preparation method under the condition of reducing the subsequent impregnation steps.
The invention discloses the following technical effects:
according to the invention, the carbon fiber cloth and the carbon fiber net tire impregnated with the slurry are laminated and then needled, so that the fiber damage can be reduced in the needling process, and the subsequent impregnation times can be reduced.
The invention greatly improves the densification efficiency by introducing the slurry doped with the asphalt and the graphite into the carbon fiber mesh, and shortens the period of preparing the high-density carbon/carbon composite material by over 80 percent.
According to the invention, the carbon fibers are pre-impregnated, so that the sufficient filling and interface bonding of the carbon fibers can be ensured, and the reduction of the carbon fibers caused by rapid preparation is avoided.
Compared with the traditional high-pressure densification process for preparing the high-densification material, the method disclosed by the invention has the advantages that the low-pressure impregnation and carbonization are realized, the use of high-pressure and ultrahigh-pressure densification equipment is avoided, the preparation period of the high-density carbon/carbon composite material is prolonged, and the process safety is greatly improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a flow diagram of a process for preparing a carbon/carbon composite according to the present invention;
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The "parts" in the present invention are all parts by mass unless otherwise specified.
The raw materials used in the examples of the present invention were commercially available unless otherwise specified.
The slurry for impregnation is an ethanol suspension with the weight ratio of asphalt to natural flake graphite powder being 1:1, wherein the mass ratio of the total mass of the asphalt and the natural flake graphite powder to the ethanol is 3: 7.
The phenolic resin used in the embodiment of the invention is specifically phenolic resin PF-7215 which is purchased from Jinan Shengquan group GmbH.
The process flow for preparing the carbon/carbon composite material according to the embodiment of the invention is shown in fig. 1.
Example 1
Step 1, a chopped carbon fiber net tire (a chopped fiber net tire prepared from Dongli T700-12K carbon fibers and having a net tread density of 80 g/m) with a thickness of 1mm is used2) And (3) putting the carbon fiber net blank into the slurry for dipping to obtain a carbon fiber net blank preform, wherein the mass of the carbon fiber net blank accounts for 20 +/-3% of the mass of the slurry.
And 2, laminating the carbon fiber plain cloth and the carbon fiber mesh blank prefabricated body prepared in the step 1 by using a graphite flat plate with sieve pores as a tool to obtain a slurry-containing carbon fiber fabric, and needling the slurry-containing carbon fiber fabric on a needling machineNeedling to obtain a needled fabric containing the pulp, heating (drying) to remove an ethanol solvent in the needled fabric containing the pulp, wherein the heating temperature is 80 ℃ (80-90 ℃ and 80 ℃ equivalent effect), the time is 12h, then curing for 32h (24-48 h and 32h equivalent effect) at 500 ℃ (400-600 ℃ and 500 ℃ equivalent effect in sequence, carbonizing for 2h at 900 ℃ to obtain a low-density carbon/carbon composite material blank (redundant pulp in the process can be filtered from a sieve mesh of a graphite plate and can be continuously recycled as pulp for impregnation), and the density is about 0.92g/cm3。
Step 3, immersing the low-density carbon/carbon composite material blank into the slurry, pressurizing to 1MPa for pressurized liquid-phase impregnation, wherein the impregnation time is 6h, removing the redundant slurry on the surface after taking out, heating to remove the ethanol solvent, wherein the heating temperature is 80 ℃, the time is 12h, then sequentially curing for 32h (the effect of 24-48 h is equivalent to that of 32 h) at 500 ℃ (400-600 ℃) and carbonizing for 2h at 900 ℃;
sequentially placing the mixture into slurry, carrying out pressure impregnation under the condition of 3MPa for 6 hours, heating to remove an ethanol solvent at 80 ℃ for 12 hours, curing for 32 hours (the effect is equivalent to that of 32 hours) at 500 ℃ (400-600 ℃ and 500 ℃), and carbonizing for 2 hours at 900 ℃; repeating the above process for 2 times (i.e. 3 times for all of the steps of pressure impregnation under 3MPa, heating, curing and carbonization) to obtain a high-density carbon/carbon composite material blank. Carrying out high-temperature heat treatment on the high-density carbon/carbon composite material blank at 1500 ℃ for 2h to obtain the high-density carbon/carbon composite material blank with the density of 1.85g/cm3The carbon/carbon composite of (1).
As a result: the preparation cycle of the high-density carbon/carbon composite material prepared by the embodiment is 6 days, and specifically, the ball milling and mixing time in the process of preparing the impregnating slurry is 12 hours; the carbon fiber net tire is soaked in the soaking slurry and then is laminated and cured to obtain the slurry-containing needled fabric, which needs 24 hours (the needling process time is short); the carbonization process of the carbon/carbon composite material blank needs 2 hours; the carbon/carbon composite material with high density is obtained by carrying out dipping-curing-carbonization for 3 times, and finally, the carbon/carbon composite material is sintered at high temperature, and 48 hours is needed by combining with subsequent cooling; the whole preparation cycle took 6 days.
Example 2
Step 1, a carbon fiber net tire (a chopped fiber net tire prepared from Dongli T700-12K carbon fibers and having a net tread density of 80 g/m) with a thickness of 1mm is used2) Putting the carbon fiber net blank into the slurry, and uniformly dipping to obtain a prefabricated body containing the carbon fiber net blank, wherein the weight of the carbon fiber net blank is 15 +/-3% of that of the dipping slurry.
And 2, laminating carbon fiber plain cloth and the carbon fiber mesh blank prefabricated body prepared in the step 1 by using a graphite flat plate with sieve pores as a tool to obtain a slurry-containing carbon fiber fabric, needling the slurry-containing carbon fiber fabric on a needling machine to obtain the slurry-containing needled fabric, sequentially drying for 12 hours at 85 ℃ (80-90 ℃ and 85 ℃ equivalent in effect), curing for 32 hours (24-48 hours and 32 hours equivalent in effect) at 500 ℃ (400-600 ℃ and 500 ℃ equivalent in effect), and carbonizing for 2 hours at 900 ℃ to obtain the low-density carbon/carbon composite material (the density is about 1.1 g/cm)3). (the excessive slurry will be filtered from the screen holes of the graphite plate in the process, and can be recycled as the slurry for impregnation).
And 3, taking carbon black as filling carbon particles, fully dispersing the carbon black into a phenolic resin solution diluted by ethanol to form a suspension A (the mass ratio of the carbon black to the ethanol to the phenolic resin is 15:70:15), immersing the low-density carbon/carbon composite material prepared in the step 2 into the suspension, carrying out pressure impregnation under the condition of 5MPa pressure for 6h (in the process, the carbon black and the phenolic resin are filled into the low-density carbon/carbon composite material), then heating (volatilizing the ethanol solvent and curing the resin) for 12h at the heating temperature of 85 ℃, curing for 32h (the effects of 24-48 h and 32 h) at 500 ℃ (400-600 ℃ are equivalent to the effects of 500 ℃), and then carbonizing for 2h at 900 ℃. This filling process was repeated 2 times;
and then sequentially placing the mixture into the suspension A, carrying out pressure impregnation under the condition of 3MPa for 6 hours, then heating (volatilizing an ethanol solvent and curing resin) at the temperature of 80-90 ℃ for 12 hours, curing for 32 hours (24-48 hours and 32 hours with equivalent effects) at 500 ℃ (400-600 ℃ and 500 ℃), and then carbonizing for 2 hours at 900 ℃. Cooling, sequentially placing in the suspension A, soaking for 6h under 4MPa, heating (volatilizing ethanol solvent and curing resin) at 80-90 deg.C for 12 deg.Ch, curing for 32h (the effect is equivalent to that of 32h in 24-48 h) at 500 ℃ (400-600 ℃ and 500 ℃), and then carbonizing for 2h at 900 ℃. And after cooling, sequentially placing the mixture into the suspension A, soaking the mixture for 6 hours under the pressure of 5MPa, heating (volatilizing an ethanol solvent and curing resin) at the temperature of 80-90 ℃ for 12 hours, curing the mixture for 32 hours (with the effect equivalent to that of 32 hours) at the temperature of 500 ℃ (400-600 ℃ and 500 ℃), and then carbonizing the mixture for 2 hours at the temperature of 900 ℃ to obtain the high-density carbon/carbon composite material. Heat treating the high-density carbon/carbon composite material at 1500 deg.C for 2h to obtain the product with density of 1.8g/cm3The carbon/carbon composite of (1).
As a result: the preparation cycle of the high-density carbon/carbon composite material prepared by the embodiment is 7.5 days, and specifically, the ball milling and mixing time in the process of preparing the impregnating slurry is 12 hours; the carbon fiber net tire is soaked in the soaking slurry and solidified to obtain the shaped carbon fiber, which takes 24 hours (the time of the needling process is short); the whole carbonization process of the carbon/carbon composite material blank needs 24 hours; the carbon/carbon composite material with high density is obtained by carrying out dipping-curing-carbonization for 4 times, and finally, the carbon/carbon composite material is sintered at high temperature, and 48 hours is needed by combining with subsequent cooling; the whole preparation cycle required 7.5 days.
Comparative example 1
The same as example 1, except that step 4 was replaced by using medium temperature coal pitch as impregnant, and high pressure densification and high temperature heat treatment were performed by conventional method, and the density was about 1.85g/cm after repeating the above steps three times3A carbon/carbon composite. The method comprises the following specific steps:
step 1: and (3) alternately laminating the carbon fiber cloth and the carbon fiber net tire, and needling to obtain the carbon fiber fabric.
Step 2: high-temperature asphalt is adopted as an impregnation raw material, cyclic impregnation and carbonization are carried out for 7 times, nitrogen is respectively used for pressurizing to the pressure of 50, 65 and 80MPa, the set temperature is 190 ℃, impregnation is carried out for 3 hours, then the product is taken out, redundant asphalt is removed, and the product is taken out after carbonization is carried out for 2 hours at 850 ℃.
And step 3: and (3) carrying out high-temperature graphitization treatment, wherein the high-temperature treatment temperature is 2000 ℃, and the treatment is carried out for 2-3 h under the protection of argon gas to obtain the final carbon/carbon composite material.
As a result: the preparation period for the high-density carbon/carbon composite material prepared by this comparative example was 49 days (each impregnation period was about 7 days). The production cycle of example 1 was reduced by 80% or more compared with example 1.
Comparative example 2
The same as in example 1, except that the step of dipping the carbon fiber web in the slurry in step 1 was omitted.
As a result: the preparation period for preparing the high-density carbon/carbon composite material according to this comparative example was 49 days.
The properties of the carbon/carbon composite materials prepared in examples 1 to 2 and comparative examples 1 to 2 were verified, and the flexural strength of the material was measured by a three-point short beam bending method according to the standard for flexural strength detection GB-6569-1986 and was tested by a universal testing machine (Instron-1186). The size of a carbon/carbon composite material sample is 40mm multiplied by 4mm multiplied by 3mm (length multiplied by width multiplied by thickness), the surface of the sample needs to be ground flat after being cut into specified size by an inner diameter slicer, and chamfer processing needs to be carried out on the edge angle of the sample, so as to avoid measurement error caused by stress concentration. The test span of the experiment is 30mm, and the pressure head loading speed is 0.5 mm/min. Since the dispersion of the bending strength is taken into consideration, the average value of 6 test pieces per test specimen is taken as the bending strength of the material.
The tensile strength detection standard refers to the national standard GJB 6475-2008, samples are processed into dog-bone type standard tensile samples, the mechanical properties of the dog-bone type standard tensile samples are tested at room temperature at the tensile rate of 0.2mm/min, and in order to avoid damage of the test clamp to the samples, aluminum alloy reinforcing sheets with composite sizes are bonded at the two ends of the samples. Since the dispersion of the tensile strength is taken into consideration, the average value of 6 test pieces per test specimen is taken as the material tensile strength.
The results are shown in Table 1.
TABLE 1
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (9)
1. A wet needling process for preparing a carbon/carbon composite material is characterized by comprising the following steps:
step 1, dipping a carbon fiber net tire into slurry to obtain a carbon fiber net tire prefabricated body;
step 2, laminating the carbon fiber mesh prefabricated body and carbon fiber cloth to obtain a slurry-containing carbon fiber fabric; carrying out needling on the carbon fiber fabric containing the sizing agent to obtain the needled fabric containing the sizing agent; sequentially heating, curing and carbonizing the slurry-containing needled fabric to obtain a low-density carbon/carbon composite material blank;
step 3, repeatedly carrying out the processes of dipping, heating, curing and carbonizing on the low-density carbon/carbon composite material green body to obtain a high-density carbon/carbon composite material green body; carrying out high-temperature heat treatment on the high-density carbon/carbon composite material blank to obtain the carbon/carbon composite material;
in the step 1, the slurry is an ethanol suspension of asphalt and graphite powder.
2. The wet needling process for preparing the carbon/carbon composite material according to claim 1, wherein in the step 1, the mass ratio of the asphalt to the graphite powder in the slurry is 0.5-1.25: 1; the mass ratio of the total mass of the asphalt and the graphite powder to the mass of the ethanol is 2.5-3.5: 7.
3. The wet needling process for preparing the carbon/carbon composite material according to claim 1, wherein in step 1, the carbon fiber mesh accounts for 12-25% of the mass of the slurry.
4. The wet needling process for preparing the carbon/carbon composite material according to claim 1, wherein in the step 2, the heating temperature is 80-90 ℃ and the heating time is 8-12 h; the curing temperature is 400-600 ℃, and the curing time is 24-48 h; the carbonization temperature is 800-900 ℃, and the carbonization time is 2-4 h.
5. The wet needling process for preparing the carbon/carbon composite material according to claim 1, wherein the pressure of impregnation in the step 3 is 1-5 MPa, and the time is 6-8 h.
6. The wet needling process for preparing the carbon/carbon composite material according to claim 1, wherein in the step 3, the heating temperature is 80-90 ℃ and the heating time is 8-12 h; the curing temperature is 400-600 ℃, and the curing time is 24-48 h; the carbonization temperature is 800-900 ℃, and the carbonization time is 2-4 h.
7. The wet needling process for preparing the carbon/carbon composite material according to claim 1, wherein the repetition time in the step 3 is 3-5 times.
8. The wet needling process for preparing the carbon/carbon composite material according to claim 1, wherein in the step 3, the temperature of the high-temperature heat treatment is 1500-1800 ℃ and the time is 2 hours.
9. The carbon/carbon composite material prepared by the preparation process according to any one of claims 1 to 8.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114621020A (en) * | 2022-05-16 | 2022-06-14 | 浙江德鸿碳纤维复合材料有限公司 | Carbon-ceramic composite structure and preparation method thereof |
| CN115503299A (en) * | 2022-11-07 | 2022-12-23 | 浙江德鸿碳纤维复合材料有限公司 | Metal/carbon composite material plate and preparation method thereof |
| CN115894062A (en) * | 2022-12-26 | 2023-04-04 | 内蒙古航天红岗机械有限公司 | Low-cost carbon/graphite throat lining material and preparation method thereof |
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| CN115894062A (en) * | 2022-12-26 | 2023-04-04 | 内蒙古航天红岗机械有限公司 | Low-cost carbon/graphite throat lining material and preparation method thereof |
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