CN116283332A - Preparation method of pitch-based carbon/carbon composite material with high thermal conductivity in thickness direction - Google Patents
Preparation method of pitch-based carbon/carbon composite material with high thermal conductivity in thickness direction Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 56
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000005087 graphitization Methods 0.000 claims abstract description 10
- 238000003763 carbonization Methods 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims description 26
- 239000000835 fiber Substances 0.000 claims description 20
- 239000011302 mesophase pitch Substances 0.000 claims description 20
- 239000011295 pitch Substances 0.000 claims description 17
- 239000011159 matrix material Substances 0.000 claims description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 13
- 238000005470 impregnation Methods 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000000945 filler Substances 0.000 claims description 8
- 239000002041 carbon nanotube Substances 0.000 claims description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000007731 hot pressing Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 229910003460 diamond Inorganic materials 0.000 claims description 4
- 239000010432 diamond Substances 0.000 claims description 4
- 230000006641 stabilisation Effects 0.000 claims description 4
- 238000011105 stabilization Methods 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000010030 laminating Methods 0.000 claims description 2
- 238000003475 lamination Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000003892 spreading Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 239000011231 conductive filler Substances 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- 239000010426 asphalt Substances 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 11
- 238000005336 cracking Methods 0.000 abstract description 4
- 238000005553 drilling Methods 0.000 abstract description 4
- 238000007598 dipping method Methods 0.000 abstract description 3
- 230000008595 infiltration Effects 0.000 abstract description 2
- 238000001764 infiltration Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 21
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 7
- 239000011153 ceramic matrix composite Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000009954 braiding Methods 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- IUHFWCGCSVTMPG-UHFFFAOYSA-N [C].[C] Chemical class [C].[C] IUHFWCGCSVTMPG-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000003733 fiber-reinforced composite Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000009958 sewing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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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
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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Abstract
The invention relates to a preparation method of a pitch-based carbon/carbon composite material with high thermal conductivity in the thickness direction, which comprises the steps of preparing a one-dimensional composite material preform by adopting a hot-press curing process, then carrying out laser drilling, dipping cracking carbonization and chemical vapor infiltration in the thickness direction, and finally carrying out graphitization treatment on the preform. Compared with the prior art, the invention realizes high heat conduction performance in the thickness direction, solves the problem of anisotropy of the heat conduction performance of the one-dimensional carbon/carbon composite material, and improves the designability of the structure and the material performance of the asphalt-based composite material.
Description
Technical Field
The invention belongs to the technical field of functional composite materials, and relates to a preparation method of a pitch-based carbon/carbon composite material with high thermal conductivity in the thickness direction.
Background
With the rapid development of aerospace, information industry and electronic industry, high thermal conductivity materials have become a key ring for restricting the development of industry, compared with common high thermal conductivity metal materials such as silver, copper and the like, asphalt-based carbon fibers have more excellent thermal conductivity (up to more than 1100W/(m.times.K)), more than four times of aluminum and more than two times of copper, and are expected to be applied to various fields. Therefore, the asphalt-based fiber-reinforced asphalt-based carbon-carbon composite material also becomes one of high-heat-conductivity materials with great application prospect.
Continuous fiber reinforced composite materials can be classified into three categories of linear (one-dimensional, 1D), planar (two-dimensional, 2D) and stereoscopic (three-dimensional, 3D) according to the weaving mode of the preform fibers. One-dimensional composites, sometimes referred to as unidirectional structural composites, are used in which all of the fibers in the composite are in the same direction, which is also generally the direction in which the composite is loaded. For pitch-based carbon-carbon composites, if one-dimensional preform braiding is chosen, the axial (along the fiber direction) thermal conductivity is the greatest (up to 800W/(m x K)), whereas two-or three-dimensional braiding is relatively low (typically < 400W/(m x K)). However, unidirectional pitch-based composites tend to have very low thermal conductivities (20-30W/(m x K)) in the thickness direction (perpendicular to the fiber direction), which becomes a short plate that limits the development and application of unidirectional pitch-based composites.
Patent CN202210159365.3 discloses a preparation method of a one-dimensional high-heat-conductivity C/C composite material, which adopts mesophase pitch-based carbon fibers as a reinforcement, performs one-dimensional directional laying by a mold with proper size, and performs sewing and fixing by the fibers to obtain a fiber preform. After the fiber preform is subjected to hot pressing, carbonization and graphitization treatment, the one-dimensional high-heat-conductivity C/C composite material with the density dimension of more than 1.8g/cm < 3 > can be obtained. The method adopts a hot pressing-pressurizing pre-oxidation process to improve the carbon residue rate of the asphalt adhesive in the liquid phase impregnation densification process, realizes the rapid densification of the C/C composite material, and greatly shortens the preparation period of the high-heat-conductivity C/C composite material. However, the C/C composite material prepared by the method still has the problem of overlarge heat conductivity difference along the axial direction and the radial direction of the fiber.
Patent CN201910083453.8 discloses a method for constructing directional heat conduction channels of a high heat conduction diamond modified silicon carbide ceramic matrix composite material, which prepares SiC-CMC with good mechanical properties and heat conductivity through the steps of preparing a porous preform, preparing slurry, laser drilling, dipping the slurry, curing and cracking resin, penetrating liquid silicon and the like. The thermal conductivity of the silicon carbide ceramic matrix composite material prepared by the method in the thickness direction can be expected to be improved by 10-20 times on the basis of the prior art, the silicon carbide ceramic matrix composite material has good heat transfer efficiency, can effectively conduct heat transfer, and prevents damage and failure of the material caused by heat concentration.
Disclosure of Invention
The invention aims to provide a preparation method of a pitch-based carbon/carbon composite material with high thermal conductivity in the thickness direction.
The aim of the invention can be achieved by the following technical scheme:
a preparation method of a pitch-based carbon/carbon composite material with high thermal conductivity in the thickness direction comprises the following steps:
(1) Taking and grinding mesophase pitch into powder, and dispersing the mesophase pitch into isopropanol solution to obtain matrix slurry;
(2) Arranging mesophase pitch fibers on a flexible graphite plate in an oriented manner, performing oxidation stabilization and low-temperature heat treatment, uniformly spraying the matrix slurry obtained in the step (1) in batches, uniformly spreading the obtained fiber tows in a mould in a unidirectional manner, laminating and hot-pressing to obtain a C/C composite material hot-pressed sample;
(3) Introducing an opening into the C/C composite material hot-pressed sample obtained in the step (2), and then performing ultrasonic cleaning and drying to obtain a porous C/C composite material preform with a directional heat conduction channel;
(4) Adding the heat-conducting filler powder into the matrix slurry obtained in the step (1), stirring and performing ultrasonic dispersion to obtain mesophase pitch/heat-conducting filler slurry;
(5) Placing the porous C/C composite material preform in the step (4) in a container, vacuumizing to negative pressure, then introducing the mesophase pitch/heat-conducting filler slurry, performing primary impregnation, and then boosting pressure to perform secondary impregnation, thus circulating for 0 times or more;
(6) And (3) sequentially carrying out high-temperature carbonization and graphitization treatment on the preform immersed in the step (5) to obtain a target product.
Further, in the step (1), the mass ratio of the mesophase pitch to the isopropanol is 1:1 to 1:3.
further, in the step (2), the oxidation stabilization is carried out by heat-treating the fiber at 200-250 ℃ under the protection of nitrogen.
Further, in the step (2), the low-temperature heat treatment process is to heat treat 300-350 ℃ under the protection of nitrogen.
Further, in the step (2), the mass ratio of the sprayed matrix slurry to the mesophase pitch fiber is 2:1.
further, in the step (2), the temperature in the lamination hot-pressing process is 300-500 ℃, the pressure is 2-4Mpa, and the time is 4-6h.
Further, in the step (3), a femtosecond laser processing technology is adopted for carrying out the hole opening, the aperture of the introduced hole opening is more than 3 times of the thickness of the C/C composite material hot-pressed sample, and the hole opening interval is more than or equal to the aperture.
Further, in the step (4), the heat conducting filler is micron-sized carbon nano tube, crystalline flake graphite or diamond powder, and the addition amount of the heat conducting filler is 1-10vol.% of the matrix slurry.
Further, in the step (5), the pressure in the primary impregnation process is 2-4MPa, and the time is 20-40minr.
Further, in the step (5), the pressure in the secondary impregnation process is 0.7-0.9Mpa, and the time is 20-40min.
Further, in the step (6), the process conditions of high-temperature carbonization are as follows: under the protection of inert gas, preserving heat for 2-4h at 750-900 ℃.
Further, in the step (6), the graphitizing process conditions are as follows: preserving heat at 2600-2800deg.C for 2-4h.
Further, in the step (5), when the number of cycles is 0, it means that only the primary impregnation and the secondary impregnation are performed.
Compared with the prior art, the invention can prepare the carbon-carbon composite material with good heat conduction performance in the fiber direction and the direction perpendicular to the fiber direction, solves the problem of anisotropy of the heat conduction performance of the one-dimensional carbon-carbon composite material, and improves the designability of the structure and the material performance of the asphalt-based composite material.
Detailed Description
The present invention will be described in detail with reference to specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
In the following examples, unless otherwise indicated, the starting materials or processing techniques are all conventional commercially available in the art.
Example 1
Preparation of one-dimensional asphalt-based carbon-carbon composite material plate
(1) Preparation of asphalt-based composite preform
Mixing ground mesophase pitch powder with isopropanol solution by using mesophase pitch as a matrix of the composite material, wherein the addition mass ratio of the mesophase pitch to the isopropanol is 1:2, preparing matrix slurry, hot-pressing unidirectional mesophase pitch-based fiber laminates, brushing the matrix slurry between fiber layers, wherein the mass ratio of the matrix slurry to the fibers is 2:1. the obtained preform is cured by heat preservation for 5 hours under the condition of 400 ℃ and 4MPa, and the size is 15-3 cm 3 The density is about 1.3-1.5g/cm 3 C/C composite of (C);
(2) Laser drilling
Introducing aperture to the thickness direction of the prepared semi-densified C/C composite material by using a femtosecond laser processing technology, wherein the aperture is more than 3 times of the thickness of the material, the aperture distance is more than or equal to the aperture, and carrying out ultrasonic cleaning and drying on the material after opening the aperture to obtain a porous C/C composite material preform with a directional heat conduction path;
(3) Configuration of thermally conductive paste
Adding 1-10vol.% of micron-sized carbon nanotube powder into the matrix slurry prepared in the step (1), magnetically stirring and ultrasonically dispersing the mixed solution, and finally obtaining uniformly dispersed mesophase pitch and carbon nanotube slurry;
(4) Immersion pyrolysis
Vacuum impregnation is first performed: firstly, placing a porous preform of a C/C composite material into a glass drying vessel, vacuumizing until the pressure in the vessel is less than 200Pa, maintaining for 25min, introducing slurry, immersing the preform into the slurry, and maintaining for 30min; and then carrying out pressure impregnation: placing the slurry and the preform into a closed container, pressurizing to 0.8MPa, keeping for 30min, taking out, wiping the surface of the preform, and drying; finally, placing the immersed preform in a high-temperature cracking furnace, carbonizing at 800 ℃ with nitrogen as a protective atmosphere for 3 hours, and repeating the steps for more than 3 times until the sample density reaches 1.8g/cm 3 ；
(5) Graphitization treatment
After the sample is subjected to the dipping and cracking process, the sample is placed in a graphitization furnace for graphitization treatment for improving the heat rate of the sample, wherein the graphitization temperature is 2700 ℃ and the graphitization time is 2-4 hours. And (5) sampling after the furnace temperature is cooled, and processing and polishing to obtain a finished product.
Example 2
The preparation method of the one-dimensional asphalt-based carbon-carbon composite board is the same as in example 1 except that carbon nanotube powder in the heat conduction slurry in step 3 in example 1 is changed to flake graphite.
Example 3
The preparation method of the one-dimensional asphalt-based carbon-carbon composite board is the same as in example 1 except that the carbon nanotube powder in the heat conduction slurry in the step 3 is changed to diamond powder in example 1.
Example 4
A preparation method of a one-dimensional asphalt-based carbon-carbon composite material plate comprises the steps of carrying out chemical vapor infiltration densification on a preform subjected to the impregnation and pyrolysis in the step 4 in the embodiment 1 to obtain a composite material with higher density, and carrying out other steps in the same manner as in the embodiment 1.
The following is a comparison of the thermal conductivity properties of the slabs obtained from the experimental and control groups, using example 1 as the experimental group, as a control group, without laser drilling, with reference to example 1, and is specifically as follows:
| sample model | Parallel thermal conductivity (W/(m.times.K)) | Vertical thermal conductivity (W/(m.times.K)) |
| Unpunched hole | 523.4 | 32.4 |
| Example 1 | ≥500 | ≥65 |
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. The preparation method of the pitch-based carbon/carbon composite material with high thermal conductivity in the thickness direction is characterized by comprising the following steps:
(1) Taking and grinding mesophase pitch into powder, and dispersing the mesophase pitch into isopropanol solution to obtain matrix slurry;
(2) Arranging mesophase pitch fibers on a flexible graphite plate in an oriented manner, performing oxidation stabilization and low-temperature heat treatment, uniformly spraying the matrix slurry obtained in the step (1) in batches, uniformly spreading the obtained fiber tows in a mould in a unidirectional manner, laminating and hot-pressing to obtain a C/C composite material hot-pressed sample;
(3) Introducing an opening into the C/C composite material hot-pressed sample obtained in the step (2), and then performing ultrasonic cleaning and drying to obtain a porous C/C composite material preform with a directional heat conduction channel;
(4) Adding the heat-conducting filler powder into the matrix slurry obtained in the step (1), stirring and performing ultrasonic dispersion to obtain mesophase pitch/heat-conducting filler slurry;
(5) Placing the porous C/C composite material preform in the step (4) in a container, vacuumizing to negative pressure, then introducing the mesophase pitch/heat-conducting filler slurry, performing primary impregnation, and then boosting pressure to perform secondary impregnation, thus circulating for 0 times or more;
(6) And (3) sequentially carrying out high-temperature carbonization and graphitization treatment on the preform immersed in the step (5) to obtain a target product.
2. The method for producing a pitch-based carbon/carbon composite material having a high thermal conductivity in the thickness direction according to claim 1, wherein in the step (1), the ratio of the addition mass of mesophase pitch to isopropyl alcohol is 1:1 to 1:3.
3. the method for producing a pitch-based carbon/carbon composite material having a high thermal conductivity in the thickness direction according to claim 1, wherein in the step (2), the oxidation stabilization is performed by: performing heat treatment at 200-250 ℃ in nitrogen protection atmosphere;
the low-temperature heat treatment process comprises the following steps: and heat treatment is carried out at 300-350 ℃ under the protection of nitrogen.
4. The method for producing a pitch-based carbon/carbon composite material having a high thermal conductivity in the thickness direction according to claim 1, wherein in the step (2), the mass ratio of the sprayed matrix slurry to the mesophase pitch fiber is 2:1.
5. the method for preparing a pitch-based carbon/carbon composite material having high thermal conductivity in a thickness direction according to claim 1, wherein in the step (2), the temperature during lamination hot pressing is 300 to 500 ℃, the pressure is 2 to 4Mpa, and the time is 4 to 6 hours.
6. The method for preparing a pitch-based carbon/carbon composite material with high thermal conductivity in the thickness direction according to claim 1, wherein in the step (3), the holes are formed by a femtosecond laser processing technology, the aperture of the introduced holes is 3 times greater than the thickness of a hot pressed sample of the C/C composite material, and the aperture interval is greater than or equal to the aperture.
7. The method for producing a pitch-based carbon/carbon composite material having a high thermal conductivity in the thickness direction according to claim 1, wherein in the step (4), the heat conductive filler is a micron-sized carbon nanotube, flake graphite or diamond powder added in an amount of 1 to 10vol.% of the matrix slurry.
8. The method for preparing a pitch-based carbon/carbon composite material having high thermal conductivity in a thickness direction according to claim 1, wherein in the step (5), the pressure in the primary impregnation process is 2 to 4MPa for 20 to 40 minutes;
the pressure in the secondary soaking process is 0.7-0.9Mpa, and the time is 20-40min.
9. The method for producing a pitch-based carbon/carbon composite material having a high thermal conductivity in the thickness direction according to claim 1, wherein in the step (6), the process conditions for high-temperature carbonization are as follows: under the protection of inert gas, preserving heat for 2-4h at 750-900 ℃.
10. The method for preparing a pitch-based carbon/carbon composite material having high thermal conductivity in a thickness direction according to claim 1, wherein in the step (6), graphitization is performed under the following process conditions: preserving heat at 2600-2800 ℃.
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