CN117802347A - Preparation method of carbon-copper composite material with good heat dissipation and wear resistance - Google Patents
Preparation method of carbon-copper composite material with good heat dissipation and wear resistance Download PDFInfo
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- AHADSRNLHOHMQK-UHFFFAOYSA-N methylidenecopper Chemical compound [Cu].[C] AHADSRNLHOHMQK-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 230000017525 heat dissipation Effects 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
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- 239000007788 liquid Substances 0.000 claims description 96
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- 239000001257 hydrogen Substances 0.000 claims description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims description 20
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 19
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
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- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 abstract description 20
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method of a carbon-copper composite material with good heat dissipation and wear resistance, which comprises the following steps: carrying out graphene oxide loading treatment on the surface of the foamy copper to obtain pretreated foamy copper; filling carbon fibers into the pores of the pretreated foamy copper to obtain a foamy copper-carbon preform; carrying out cracking carbonization on the foam copper-carbon preform by adopting an isothermal chemical vapor infiltration process to obtain a carbon-copper composite material precursor; graphitizing the carbon-copper composite material precursor, and preparing the carbon-copper composite material precursor with good heat dissipation and wear resistance after graphitizationCarbon-copper composite material of (a). The carbon-copper composite material prepared by the invention has excellent mechanical property, heat conduction property and wear resistance, and the thermal conductivity of the fiber axial direction is more than or equal to 100W (m.k) ‑1 ) The thermal conductivity perpendicular to the axial direction of the fiber is more than or equal to 300W (m.k) ‑1 ) The wear resistance of the carbon-carbon composite material is about 1.5 times that of the carbon-carbon composite material.
Description
Technical Field
The invention relates to the technical field of carbon composite materials. In particular to a preparation method of a carbon-copper composite material with good heat dissipation and wear resistance.
Background
The Carbon-Carbon composite material (Carbon-Carbon composite mater ial) is a full-Carbon composite material which is prepared by taking graphite Carbon as a matrix phase, taking Carbon fibers as a reinforcing phase and adopting a certain special processing preparation process, can still keep the strength at the room temperature at 2500 ℃, has excellent anti-ablation performance, and has a specific gravity of small (1.7-2.0 g/cm 3 ) The steel has the advantages of high strength (7-9 times of steel), low thermal expansion coefficient, high temperature resistance, corrosion resistance and the like, is mainly used for light-weight and high-efficiency design in the structure, and has been used for replacing metal materials in various fields and widely applied. However, the carbon-carbon composite material has poor heat conduction capability, and the in-plane heat conduction of the carbon fiber is about 54W (m.k) -1 ) The vertical fiber surface heat conduction was 22W (m.k -1 )。
Copper metal is one of the earliest metals used by human beings, mineral resources are rich, and the smelting process is mature. The ductility is good, the thermal conductivity is extremely high (about 400W/(mK)), the thermal conductivity is the highest metal after noble metal, and furthermore, the copper alloy has excellent mechanical properties. Therefore, copper can be used as a metal matrix of the composite material, on one hand, the high heat conduction performance of the matrix is ensured, and on the other hand, the mechanical property of the composite material can be greatly improved by adding a proper amount of alloy elements into copper, so that the composite material has excellent comprehensive performance.
Copper-based composite materials have been widely used in devices with high requirements for thermal and electrical conductivity. To further enhance the overall properties, specific reinforcement phases are typically added to improve the properties of the copper-based composite in one or more aspects, and commonly used materials include carbides (silicon carbide, etc.), carbon materials (diamond, graphite fibers, graphite flakes, etc.), metals (tungsten, molybdenum, etc.), and the like. The Carbon material has extremely high thermal conductivity and excellent mechanical properties, and has a plurality of isomerides, so the Carbon material reinforced copper-based composite material is widely focused, and mainly comprises Diamond/Cu Diamond/copper composite material (D/Cu), carbon nano tube/Cu Carbon nano tube/copper composite material (CNT/Cu), graphene/Cu Graphene/copper composite material (GNS/Cu), graphene/Cu flake Graphite/copper composite material, graphene/Cu Graphite film/copper composite material, carbon fiber/Cu Carbon fiber/copper composite material (Cf/Cu) and the like.
The composite material formed by combining the carbon-carbon material and the copper material can improve the abrasion resistance and the overall heat conduction performance of the carbon-carbon composite material while ensuring the performance of the carbon-carbon composite material, and can greatly expand the application range of the carbon-carbon composite material, but how to compound the carbon-carbon material and the copper material to prepare the carbon-copper composite material with the mechanical property, the heat conduction performance and the wear resistance reaching ideal states still needs to be solved.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a preparation method of the carbon-carbon foam copper composite material with good heat dissipation and wear resistance, so as to solve the problem that the mechanical property, the heat conductivity and the wear resistance of the traditional carbon-copper composite material cannot reach ideal conditions and limit the application of the carbon-foam copper composite material.
In order to solve the technical problems, the invention provides the following technical scheme:
the preparation method of the carbon-copper composite material with good heat dissipation and wear resistance comprises the following steps:
carrying out graphene oxide loading treatment on the surface of the foamy copper to obtain pretreated foamy copper;
filling carbon fibers into the pores of the pretreated foam copper to obtain a foam copper-carbon preform;
step (3), cracking and carbonizing the foam copper-carbon preform by adopting an isothermal chemical vapor infiltration process to obtain a carbon-copper composite material precursor;
and (4) graphitizing the precursor of the carbon-copper composite material, and preparing the carbon-copper composite material with good heat dissipation and wear resistance after graphitization is finished.
In the step (1), the graphene oxide loading treatment is performed on the surface of the foam copper by adopting an electroplating method or an immersion method. In the process of loading graphene oxide by an electroplating method, copper ions and GO are simultaneously deposited on the surface of the foam copper, and the deposition of the copper ions further enhances the interfacial bonding force between the GO and the foam copper substrate; compared with the dipping method, the electroplating method can lead the surface coating property of the foamy copper to be better and more uniform, but the electroplating method has more complex operation flow and longer period. The graphene oxide is deposited by the dipping method, the deposited layer is thicker, the whole body is covered on the surface of the foam copper in a multi-layer mode, compared with an electroplating method, the dipping method is simple in equipment and convenient to operate, and the whole coating effect is slightly lower than that of the electroplating method.
The preparation method of the carbon-copper composite material with good heat dissipation and wear resistance comprises the following operation methods of: dispersing graphene oxide into an ethanol solution, adding 3-aminopropyl triethoxysilane KH550, and uniformly mixing to obtain a mixed dispersion liquid A; using foam copper as an anode, using the mixed dispersion liquid A as electroplating liquid, and adopting constant current electricity to carry out electroplating deposition; drying after electroplating, and performing heat treatment on the dried foamy copper, wherein the pretreated foamy copper is prepared after the heat treatment is finished;
the operation method of the dipping method comprises the following steps: dispersing graphene oxide into an organic solvent, and obtaining a mixed dispersion liquid B after uniform dispersion; immersing the foam copper in the mixed dispersion liquid B, placing the mixed dispersion liquid B under ultrasonic conditions for ultrasonic deposition, and vacuum drying after the deposition is finished; and carrying out heat treatment on the dried foamy copper, and preparing the pretreated foamy copper after the heat treatment is finished.
The carbon-carbon with good heat dissipation and wear resistanceThe preparation method of the copper composite material comprises the following steps of: the mass ratio of graphene oxide to 3-aminopropyl triethoxysilane KH550 to ethanol solution is (1-2), 1-2, 8-9, and the particle size of the graphene oxide is 20-40 μm; the volume fraction of ethanol in the ethanol solution is 95-99%; constant current density of 5-15 mA/cm 2 The electroplating deposition time is 10-30 min (wherein, too low current density can lead to low surface density of an electroplated layer, poor surface flatness and smoothness, too high current density can lead to aggregation of graphene oxide to affect material performance, too short electroplating deposition time can lead to uneven thickness of the electroplated layer or insufficient overall thickness of the electroplated layer, after the electroplating deposition time exceeds 30 min, the thickness of the electroplated layer is slowly increased, the preparation efficiency is reduced, and meanwhile, the performance of the electroplated layer is not obviously improved), the drying temperature is 100-120 ℃ when the electroplated layer is dried, and the drying time is 2-4 h; the conditions of the heat treatment are as follows: in the argon atmosphere, the temperature rising rate of the foam copper material is increased to 850-950 ℃ at the speed of 5 ℃/min, and the temperature is kept for 1.5-2.5 h (the temperature rising rate of the heat treatment is too fast, so that the temperature gradient in the material is large, the stress is easy to generate, the strength and toughness of the material are affected, the preparation time is prolonged, the preparation efficiency is affected, the heat treatment temperature is not too high in the process, the foam metal matrix is melted at a high temperature, the temperature requirement of the heat treatment process cannot be met, the heat preservation time is maintained within the range of 1.5-2.5 h, the temperature uniformity of the material is ensured, and the ideal heat treatment effect is achieved); the high-temperature heat treatment can remove oxygen-containing functional groups on the surface of the graphene oxide, and reduce the graphene oxide into reduced graphene oxide (rGO) so as to improve the interface bonding capacity of the material and the heat conduction property of the material.
When the graphene oxide is loaded by the impregnation method, the following steps are carried out: the organic solvent is formed by mixing absolute ethyl alcohol and acetone according to the volume ratio of 1:1; the mass concentration of the graphene oxide in the mixed dispersion liquid B is 300mg/L, the particle size of the graphene oxide is 20-40 mu m (the graphene oxide concentration is too low to cause poor continuity and uniformity of a graphene oxide layer loaded on the surface of the foam copper, and the too high concentration can cause thicker graphene oxide layer to influence the subsequent high-temperature oxidation reduction); the times of ultrasonic deposition are 1 to 5 times; the conditions of ultrasonic deposition are: the ultrasonic frequency is 35-45 kHz, the ultrasonic power is 100-300W, and the ultrasonic deposition time is 10-30 min; after the deposition is finished, the vacuum drying temperature is 80-100 ℃ and the drying time is 2-4 h; the conditions of the heat treatment are as follows: under argon atmosphere, the temperature rising rate of the foam copper material is increased to 850-950 ℃ at the speed of 5 ℃/min, and the temperature is kept for 1.5-2.5 h.
The preparation method of the carbon-copper composite material with good heat dissipation and wear resistance comprises the following steps of:
filling by adopting long carbon fiber with the length range of 1.8-2.5 mm, wherein the filling mode is as follows: implanting long carbon fibers into the pores of the pretreated foam copper in an ultrasonic vibration mode;
Or, short carbon fibers with the length ranging from 0.8 mm to 1.0mm are adopted for filling, and the filling mode is as follows: implanting short carbon fibers into the pores of the pretreated foam copper in an ultrasonic vibration mode;
or, long carbon fibers with the length of 1.8-2.5 mm and short carbon fibers with the length of 0.8-1.0 mm are mixed to form long/short mixed fibers for filling, and the filling mode is as follows: filling long/short mixed fibers into the pretreated foam copper pores in a colloid suction filtration mode;
the diameter of the long carbon fiber with the diameter of 1.8-2.5 mm is 6-7 mu m, and the diameter of the short carbon fiber with the diameter of 0.8-1.0 mm is 6-7 mu m; the foam copper holes with the specification of 10ppi are filled to form loose foam copper-carbon preformed bodies taking foam copper as a framework.
The preparation method of the carbon-copper composite material with good heat dissipation and wear resistance comprises the following steps of: dispersing long carbon fibers into a fiber dispersing agent to form a long carbon fiber dispersing liquid A, then completely immersing pretreated foam copper into the long carbon fiber dispersing liquid A for ultrasonic vibration filling, and drying at 100 ℃ for 2-4 hours after filling; the mass fraction of the long carbon fibers in the long carbon fiber dispersion liquid A is 4-6wt%; the ultrasonic frequency is 45kHz, the ultrasonic power is 100-300W, and the ultrasonic time is 10-30 min;
When short carbon fibers are used for filling: firstly dispersing short carbon fibers into a fiber dispersing agent to form a short carbon fiber dispersing liquid A, then completely immersing pretreated foam copper into the short carbon fiber dispersing liquid A for ultrasonic vibration filling, and drying at 100 ℃ for 2-4 h after filling; the mass fraction of the short carbon fibers in the short carbon fiber dispersion liquid A is 4-6wt%; the ultrasonic frequency is 45kHz, the ultrasonic power is 100-300W, and the ultrasonic time is 10-30 min;
when filling with long/short mixed fibers: the colloid suction filtration mode is mixed suction filtration or layered suction filtration, and the colloid suction filtration is dried for 2 to 4 hours at the temperature of 100 ℃ after the suction filtration is finished;
when mixing and suction filtering, firstly mixing long carbon fibers and short carbon fibers according to the mass ratio of 1:1, and then pre-dispersing the long carbon fibers and the short carbon fibers into a fiber dispersing agent by ultrasonic, wherein the pre-dispersing time of the ultrasonic is 10mi < n >, so as to obtain a long/short mixed fiber dispersing liquid, and the mass fraction of the long carbon fibers in the long/short mixed fiber dispersing liquid is 4-6wt%; then carrying out mixed suction filtration under the pressure of 0.02-0.05 MPa, and repeatedly carrying out suction filtration until the quality of the pretreated foamy copper is not increased any more, wherein the repeated suction filtration is generally required for 3-5 times;
when the layering suction filtration is carried out, the long carbon fiber is firstly subjected to ultrasonic pre-dispersion into a fiber dispersing agent to obtain a long carbon fiber dispersing liquid B, and the short carbon fiber is subjected to ultrasonic pre-dispersion into the fiber dispersing agent to obtain a short carbon fiber dispersing liquid B; the ultrasonic pre-dispersion time is 10mi n; the mass fraction of the long carbon fibers in the long carbon fiber dispersion liquid B and the mass fraction of the short carbon fibers in the short carbon fiber dispersion liquid B are 4-6wt%; then, under the condition of the pressure of 0.02-0.05 MPa, carrying out suction filtration of the short carbon fiber dispersion liquid B and then carrying out suction filtration of the long carbon fiber dispersion liquid B; repeatedly carrying out suction filtration until the quality of the pretreated foamy copper is not increased any more, wherein the suction filtration is generally required to be carried out for 3 to 5 times; the ratio of the layer thicknesses of the long carbon fiber layer and the short carbon fiber layer in the obtained foam copper-carbon preform is 1:1-2, the layer thickness ratio is controlled by the same or different mass fiber aqueous solutions through the same suction filtration method, and the material formability after suction filtration and drying is poor due to the fact that the layer thickness ratio is too large or too small;
The fiber dispersing agents for dispersing the long carbon fibers, the short carbon fibers and the long/short mixed fibers are all hydroxyethyl cellulose aqueous solutions, and the mass ratio of the hydroxyethyl cellulose to water in the fiber dispersing agents is 1:100; hydroxyethyl cellulose HEC belongs to nonionic soluble cellulose ethers, and the decomposition temperature is 205-210 ℃, and the hydroxyethyl cellulose HEC can be heated and decomposed in the subsequent high-temperature heat treatment process.
The preparation method of the carbon-copper composite material with good heat dissipation and wear resistance comprises the following steps:
covering the outer surface of the foam copper filled with the carbon fibers in the gaps with a carbon fiber braided fabric and a carbon fiber felt preform; namely: completely coating the foam copper filled with the carbon fibers in the gaps in the carbon fiber braided fabric and the carbon fiber felt preform to form a foam copper-carbon preform; or only the single surface of the foam copper filled with the carbon fibers in the gaps is covered by the carbon fiber braided fabric and the carbon fiber felt preform;
the weaving method of the carbon fiber braided fabric and the carbon fiber felt preform comprises the following steps: sequentially and alternately laying a single-layer carbon fiber braided fabric and a carbon fiber felt, and orthogonally layering the carbon fiber braided fabric according to [0/90] n; fixing the carbon fiber braided fabric and the carbon fiber felt by adopting a needle punching method to prepare a carbon fiber braided fabric and a carbon fiber felt preform with the thickness of 10-15 mm. After methane and hydrogen are cracked and carbonized, the carbon fiber braided fabric and the carbon fiber felt preform are combined with the foam copper filled with carbon fibers in the gaps, so that the foam copper is processed into a carbon-foam copper composite surface material, and the wear resistance and the heat conductivity of the carbon-carbon composite material are improved.
The carbon fiber braided fabric and the carbon fiber felt are coated outside the foam copper filled with the carbon fibers, so that the internal foam copper skeleton cannot be heated and melted to flow out (the melting point of the foam copper is 900 ℃) under the high-temperature condition while the cracking gas is carbonized into the prefabricated body, and meanwhile, the internal carbon fibers are combined through pyrolytic carbon to form the carbon/carbon composite material.
The preparation method of the carbon-copper composite material with good heat dissipation and wear resistance comprises the following steps:
sewing long carbon fiber tows in the direction perpendicular to the foam copper and carbon layered prefabricated plane, wherein the diameter of each long carbon fiber filament is 6-8 mu m, and the diameter of each long carbon fiber tow is 0.5-0.8 mm; sewing long carbon fiber tows into foam copper holes filled with carbon fibers with the specification of 10pp < i > by manual sewing, wherein the stitch spacing is 3mm, and the row spacing is 1-3 mm, so as to obtain a foam copper-carbon preform with a loose porous structure; too large stitch spacing and row spacing can cause too large pores to influence the loading effect of the material on pyrolytic carbon, and too small pores can cause hole sealing of the material in the process of depositing pyrolytic carbon to influence the deposition efficiency. The long carbon fiber tows are sewn in the direction perpendicular to the prefabrication plane of the foam copper and the carbon layered prefabrication plane, so that carbon fibers filled in the foam copper and carbon fiber materials added to the surface of the foam copper can be combined with the foam copper more stably, a carbon-carbon composite material combined with the foam copper stably is formed in subsequent high-temperature heat treatment, and the bonding force between the carbon-carbon material and the foam copper is increased while the heat conducting performance of the carbon-copper composite material in the direction perpendicular to the fiber direction is improved.
In the preparation method of the carbon-copper composite material with good heat dissipation and wear resistance, in the step (3), the isothermal chemical vapor infiltration process conditions are as follows: methane and hydrogen are used as gas phases; the gas cracking temperature is 1050-1100 ℃, the atmosphere pressure is 20-40 kPa, the flow ratio of methane to hydrogen is 3:2, and the flow of methane is 20-30 g/h; the densification time is 70-100 h, wherein the too low gas cracking temperature can lead to the incomplete cracking of the gas into alkane activated carbon small molecules which are deposited on the surface of the foam copper, and the too high cracking temperature can lead to the complete melting of the foam copper matrix skeleton; the surface of the material is crusted due to the overlarge atmospheric pressure in the cracking process, the overall density of the material is poor due to the overlarge atmospheric pressure, the density of the material is reduced due to the overlarge flow rate ratio of methane and hydrogen, and the danger such as explosion is easy to occur due to the overlarge flow rate ratio; too short a densification time also results in a low density.
In the preparation method of the carbon-copper composite material with good heat dissipation and wear resistance, in the step (4), the graphitization temperature is 2000-2300 ℃, the graphitization time is 10-20 h, the poor interatomic bonding force can be caused by the too low graphitization temperature or the too short graphitization time, the overall electric conduction and heat conduction performance of the composite material can be reduced, and the too high temperature or the too long time can increase energy consumption to influence industrial production.
The technical scheme of the invention has the following beneficial technical effects:
1. the carbon-copper composite material prepared by the method has high heat conduction and high wear resistance. The graphene is used as an interface material, so that the bonding strength of the carbon-copper material can be enhanced, and the interface thermal resistance is effectively lower. The carbon fibers with different sizes are filled in the foam copper framework to form an interlocking structure, so that the continuity of the pyrolytic carbon layer and the carbon fiber matrix in the three-dimensional direction can be effectively ensured, the bonding strength and the mechanical property of the carbon-copper composite material are ensured, and the foam copper is communicated in the three-dimensional direction, so that the crack expansion of the carbon-copper composite material can be effectively inhibited, the heat conduction effect is well achieved, and the heat conduction property of the carbon-copper composite material in the vertical fiber direction is improved.
2. Because the interface bonding capability of the pyrolytic carbon and the foam copper is weaker, after the graphene layer is loaded on the surface of the foam copper, the graphene layer is used as an interface bonding medium, and a composite structure of the foam copper-graphene layer-pyrolytic carbon layer can be finally formed; because the graphene layer has high heat conduction capacity, the interface thermal resistance can be reduced by being attached to the foam copper, and the interface bonding capacity and the heat conductivity of the material are further enhanced through the composite structure. The bonding between the foamy copper and the graphene layers is mainly mechanical interlocking bonding, and the bonding between the pyrolytic carbon and the graphene layers in the pyrolytic carbon process is mainly bonding through covalent bonds between C atoms in the graphene and active carbon atoms in the pyrolytic carbon so as to improve the interface bonding strength of the material.
3. The carbon-copper composite material prepared by the invention has excellent mechanical property, heat conduction property and wear resistance, and the thermal conductivity of the fiber axial direction is more than or equal to 100W (m.k) -1 ) The thermal conductivity perpendicular to the axial direction of the fiber is more than or equal to 300W (m.k) -1 ) The wear resistance of the carbon-carbon composite material is about 1.5 times that of the carbon-carbon composite material. The carbon-copper composite material prepared by the invention has great application potential in the fields of friction materials, pantograph slide plate materials, electric brush materials, oil-containing bearings, electric contact materials, electronic packaging materials, conductive materials, mechanical part materials and the like.
Drawings
FIG. 1 is a schematic illustration of the preparation flow of the carbon-copper composite material in example 3 of the present invention;
FIG. 2 is a schematic illustration of the preparation flow of the carbon-copper composite material in example 6 of the present invention;
FIG. 3 is a photograph of copper foam prior to filling in examples 1-7 and comparative example of the present invention;
FIG. 4 is a photograph of a carbon-copper composite material prepared according to a comparative example of the present invention;
FIG. 5 is a photograph of a carbon-copper composite material prepared in example 6 of the present invention.
Detailed Description
Example 1
In this embodiment, the preparation method of the carbon-copper composite material with good heat dissipation and wear resistance includes the following steps:
carrying out graphene oxide loading treatment on the surface of the foam copper by adopting an electroplating method to obtain pretreated foam copper; the operation method of the electroplating method comprises the following steps:
Dispersing graphene oxide with the particle size of 20-40 mu m into an ethanol solution, adding 3-aminopropyl triethoxysilane KH550, and uniformly mixing to obtain a mixed dispersion liquid A, wherein the mass ratio of the graphene oxide to the 3-aminopropyl triethoxysilane KH550 to the ethanol solution in the mixed dispersion liquid A is 1:1:9; the volume fraction of ethanol in the ethanol solution is 95%;
step (1-2) using copper foam with a specification of 10ppi as an anode, using the mixed dispersion liquid A as a plating solution, and using a current density of 10mA/cm 2 Is subjected to electroplating deposition by constant current; the time of electroplating deposition is 30mi n; drying for 3h at 110 ℃ after electroplating deposition;
after the steps (1-3) and drying are finished, carrying out heat treatment on the foam copper deposited by electroplating, wherein the heat treatment conditions are as follows: under argon atmosphere, raising the temperature of the foam copper material to 850 ℃ at a heating rate of 5 ℃/min, and preserving heat for 2.5h; after the heat treatment is finished, preparing pretreated foamy copper;
filling carbon fibers into the pores of the pretreated foam copper to obtain a foam copper-carbon preform; the method for filling the carbon fiber comprises the following steps: filling with long carbon fiber of length 1.8-2.5 mm and diameter of 1.8-2.5 mm of 6-7 microns; the filling mode is as follows: the long carbon fiber is implanted into the pores of the pretreated foam copper in an ultrasonic vibration mode, and specifically: dispersing long carbon fibers into a fiber dispersing agent to form a long carbon fiber dispersing liquid A, completely immersing pretreated foam copper into the long carbon fiber dispersing liquid A for ultrasonic vibration filling, and drying at 100 ℃ for 4 hours after filling; the fiber dispersing agent for dispersing the long carbon fibers is hydroxyethyl cellulose water solution, and the mass ratio of the hydroxyethyl cellulose to water in the fiber dispersing agent is 1:100; the mass fraction of the long carbon fibers in the long carbon fiber dispersion liquid A is 6wt%; the ultrasonic frequency is 45kHz, the ultrasonic power is 300W, and the ultrasonic time is 20 min;
Step (3), cracking and carbonizing the foam copper-carbon preform by adopting an isothermal chemical vapor infiltration process to obtain a carbon-copper composite material precursor; the isothermal chemical vapor infiltration process conditions were: methane and hydrogen are used as gas phases; the gas cracking temperature is 1050 ℃, the atmosphere pressure is 40kPa, the flow ratio of methane to hydrogen is 3:2, and the flow of methane is 30g/h; the densification time is 100h;
step (4), graphitizing the carbon-copper composite material precursor, wherein the graphitization temperature is 2000 ℃, and the graphitization time is 20 hours; and after graphitization is finished, preparing the carbon-copper composite material with good heat dissipation and wear resistance.
Example 2
In this embodiment, the preparation method of the carbon-copper composite material with good heat dissipation and wear resistance includes the following steps:
carrying out graphene oxide loading treatment on the surface of the foam copper by adopting an impregnation method to obtain pretreated foam copper; the operation method of the dipping method comprises the following steps:
step (1-1), dispersing graphene oxide with the particle size of 20-40 mu m into an organic solvent, and uniformly mixing to obtain a mixed dispersion liquid B; the organic solvent is formed by mixing absolute ethyl alcohol and acetone according to the volume ratio of 1:1; the mass concentration of the graphene oxide in the mixed dispersion liquid B is 300mg/L;
Immersing the foam copper with the specification of 10 ppi in the mixed dispersion liquid B, and placing the mixed dispersion liquid B under ultrasonic conditions for ultrasonic deposition, and drying in vacuum after the deposition is finished; the times of ultrasonic deposition are 3 times, and the time of each ultrasonic deposition is 15 min; the conditions of ultrasonic deposition are: the ultrasonic frequency is 45kHz, and the ultrasonic power is 200W; the temperature of vacuum drying after deposition is 100 ℃ and the drying time is 4 hours;
step (1-3), carrying out heat treatment on the dried foamy copper, wherein the heat treatment conditions are as follows: under argon atmosphere, raising the temperature of the foam copper material to 950 ℃ at a heating rate of 5 ℃/min, and preserving heat for 1.5h; after the heat treatment is finished, preparing pretreated foamy copper;
filling carbon fibers into the pores of the pretreated foam copper to obtain a foam copper-carbon preform; the method for filling the carbon fiber comprises the following steps: filling with short carbon fiber of length 0.8-1.0 mm and short carbon fiber of diameter 6-7 microns in length 0.8-1.0 mm; the filling mode is as follows: the short carbon fibers are implanted into the pores of the pretreated foam copper in an ultrasonic vibration mode, and specifically: firstly dispersing short carbon fibers into a fiber dispersing agent to form a short carbon fiber dispersing liquid A, and then completely immersing pretreated foam copper into the short carbon fiber dispersing liquid A for ultrasonic vibration filling; the fiber dispersing agent for dispersing the short carbon fibers is prepared by dissolving hydroxyethyl cellulose in water, and the mass ratio of the hydroxyethyl cellulose to the water in the fiber dispersing agent is 1:100; the mass fraction of the short carbon fibers in the short carbon fiber dispersion liquid A is 5wt%; the ultrasonic frequency is 45kHz, the ultrasonic power is 150W, and the ultrasonic time is 30 min; and drying after the ultrasonic vibration filling is finished, wherein the drying temperature is 100 ℃, and the drying time is 4 hours.
Step (3), cracking and carbonizing the foam copper-carbon preform by adopting an isothermal chemical vapor infiltration process to obtain a carbon-copper composite material precursor; the isothermal chemical vapor infiltration process conditions were: methane and hydrogen are used as gas phases; the gas cracking temperature is 1100 ℃, the atmosphere pressure is 20kPa, the flow ratio of methane to hydrogen is 3:2, and the flow of methane is 20g/h; the densification time is 70h;
step (4), graphitizing the carbon-copper composite material precursor, wherein the graphitization temperature is 2100 ℃, and the graphitization time is 15 hours; and after graphitization is finished, preparing the carbon-copper composite material with good heat dissipation and wear resistance.
Example 3
In this embodiment, the preparation method of the carbon-copper composite material with good heat dissipation and wear resistance includes the following steps:
carrying out graphene oxide loading treatment on the surface of the foam copper by adopting an electroplating method to obtain pretreated foam copper; the operation method of the electroplating method comprises the following steps:
dispersing graphene oxide with the particle size of 20-40 mu m into an ethanol solution, adding 3-aminopropyl triethoxysilane KH550, and uniformly mixing to obtain a mixed dispersion liquid A, wherein the mass ratio of the graphene oxide to the 3-aminopropyl triethoxysilane KH550 to the ethanol solution in the mixed dispersion liquid A is 1:1:8; the volume fraction of ethanol in the ethanol solution is 99%;
Step (1-2) using copper foam with a specification of 10ppi as an anode, using the mixed dispersion liquid A as a plating solution, and using a current density of 10mA/cm 2 Is subjected to electroplating deposition by constant current; the time of electroplating deposition is 10mi n;
after the electroplating is finished, carrying out heat treatment on the foam copper deposited by electroplating, wherein the heat treatment conditions are as follows: under argon atmosphere, raising the temperature of the foam copper material to 900 ℃ at a heating rate of 5 ℃/min, and preserving heat for 2 hours; after the heat treatment is finished, preparing pretreated foamy copper;
filling carbon fibers into the pores of the pretreated foam copper to obtain a foam copper-carbon preform; the method for filling the carbon fiber comprises the following steps: mixing long carbon fibers with the diameter of between 1.8 and 2.5mm and short carbon fibers with the diameter of between 0.8 and 1.0mm to form long/short mixed fibers for filling, wherein the diameter of the long carbon fibers with the diameter of between 1.8 and 2.5mm is between 6 and 7 mu m, and the diameter of the short carbon fibers with the diameter of between 0.8 and 1.0mm is between 6 and 7 mu m; the filling mode is as follows: filling long/short mixed fibers into the pretreated foam copper pores by adopting a colloid mixed suction filtration mode; specifically: firstly, mixing long carbon fibers and short carbon fibers according to a mass ratio of 1:1, and then pre-dispersing the long carbon fibers and the short carbon fibers into a fiber dispersing agent by ultrasonic, wherein the pre-dispersing time of the ultrasonic is 10 min, so as to obtain a long/short mixed fiber dispersing liquid, and the mass fraction of the long carbon fibers in the long/short mixed fiber dispersing liquid is 4wt%; then carrying out mixed suction filtration under the condition of the pressure of 0.05MPa, and repeating the suction filtration for 3-5 times until the quality of the pretreated foam copper is not increased; the fiber dispersing agent for dispersing the long/short mixed fibers is prepared by dissolving hydroxyethyl cellulose in water, and the mass ratio of the hydroxyethyl cellulose to the water in the fiber dispersing agent is 1:100; and (5) drying after the mixed suction filtration filling is finished, wherein the drying temperature is 100 ℃, and the drying time is 4 hours.
Step (3), cracking and carbonizing the foam copper-carbon preform by adopting an isothermal chemical vapor infiltration process to obtain a carbon-copper composite material precursor; the isothermal chemical vapor infiltration process conditions were: methane and hydrogen are used as gas phases; the gas cracking temperature is 1080 ℃, the atmosphere pressure is 30kPa, the flow ratio of methane to hydrogen is 3:2, and the flow of methane is 25g/h; the densification time is 80h;
step (4), graphitizing the carbon-copper composite material precursor, wherein the graphitization temperature is 2300 ℃, and the graphitization time is 10 hours; and after graphitization is finished, preparing the carbon-copper composite material with good heat dissipation and wear resistance.
Example 4
In this embodiment, the preparation method of the carbon-copper composite material with good heat dissipation and wear resistance includes the following steps:
carrying out graphene oxide loading treatment on the surface of the foam copper by adopting an electroplating method to obtain pretreated foam copper; the operation method of the electroplating method comprises the following steps:
dispersing graphene oxide with the particle size of 20-40 mu m into an ethanol solution, adding 3-aminopropyl triethoxysilane KH550, and uniformly mixing to obtain a mixed dispersion liquid A, wherein the mass ratio of the graphene oxide to the 3-aminopropyl triethoxysilane KH550 to the ethanol solution in the mixed dispersion liquid A is 2:2:9; the volume fraction of ethanol in the ethanol solution is 97%;
Step (1-2) using copper foam with a specification of 10ppi as an anode, using the mixed dispersion liquid A as a plating solution, and using a current density of 10mA/cm 2 Is subjected to electroplating deposition by constant current; the time of electroplating deposition is 20mi n;
after the electroplating is finished, carrying out heat treatment on the foam copper deposited by electroplating, wherein the heat treatment conditions are as follows: under argon atmosphere, raising the temperature of the foam copper material to 950 ℃ at a heating rate of 5 ℃/min, and preserving heat for 2 hours; after the heat treatment is finished, preparing pretreated foamy copper;
filling carbon fibers into the pores of the pretreated foam copper to obtain a foam copper-carbon preform; the method for filling the carbon fiber comprises the following steps: mixing long carbon fibers with the diameter of between 1.8 and 2.5mm and short carbon fibers with the diameter of between 0.8 and 1.0mm to form long/short mixed fibers for filling, wherein the diameter of the long carbon fibers with the diameter of between 1.8 and 2.5mm is between 6 and 7 mu m, and the diameter of the short carbon fibers with the diameter of between 0.8 and 1.0mm is between 6 and 7 mu m; the filling mode is as follows: respectively filling long carbon fibers and short carbon fibers into the pretreated foam copper pores in a colloid layering suction filtration mode; namely:
firstly, pre-dispersing long carbon fibers into a fiber dispersing agent in an ultrasonic manner to obtain a long carbon fiber dispersing liquid B, and pre-dispersing short carbon fibers into the fiber dispersing agent in an ultrasonic manner to obtain a short carbon fiber dispersing liquid B; the ultrasonic pre-dispersion time is 10mi n; the mass fraction of the long carbon fibers in the long carbon fiber dispersion liquid B and the mass fraction of the short carbon fibers in the short carbon fiber dispersion liquid B are 5wt%; then carrying out suction filtration of the short carbon fiber dispersion liquid B under the condition of the pressure of 0.02MPa, and then carrying out suction filtration of the long carbon fiber dispersion liquid B; repeatedly carrying out suction filtration until the quality of the pretreated foamy copper is not increased; after layering and suction filtration, the layer thickness ratio of a long carbon fiber layer to a short carbon fiber layer in the foam copper-carbon preform is 1:1; the fiber dispersing agents for dispersing the long carbon fibers and the short carbon fibers are all obtained by dissolving hydroxyethyl cellulose in water, and the mass ratio of the hydroxyethyl cellulose to the water in the fiber dispersing agents is 1:100; and drying after the layering, suction filtration and filling are finished, wherein the drying temperature is 100 ℃, and the drying time is 4 hours.
Step (3), cracking and carbonizing the foam copper-carbon preform by adopting an isothermal chemical vapor infiltration process to obtain a carbon-copper composite material precursor; the isothermal chemical vapor infiltration process conditions were: methane and hydrogen are used as gas phases; the gas cracking temperature is 1100 ℃, the atmosphere pressure is 35kPa, the flow ratio of methane to hydrogen is 3:2, and the flow of methane is 30g/h; the densification time is 90 hours;
step (4), graphitizing the carbon-copper composite material precursor, wherein the graphitization temperature is 2200 ℃, and the graphitization time is 17 hours; and after graphitization is finished, preparing the carbon-copper composite material with good heat dissipation and wear resistance.
Example 5
In this embodiment, the preparation method of the carbon-copper composite material with good heat dissipation and wear resistance includes the following steps:
carrying out graphene oxide loading treatment on the surface of the foam copper by adopting an electroplating method to obtain pretreated foam copper; the operation method of the electroplating method comprises the following steps:
dispersing graphene oxide with the particle size of 20-40 mu m into an ethanol solution, adding 3-aminopropyl triethoxysilane KH550, and uniformly mixing to obtain a mixed dispersion liquid A, wherein the mass ratio of the graphene oxide to the 3-aminopropyl triethoxysilane KH550 to the ethanol solution in the mixed dispersion liquid A is 2:2:9; the volume fraction of ethanol in the ethanol solution is 96%;
Step (1-2) using copper foam with a specification of 10ppi as an anode, using the mixed dispersion liquid A as a plating solution, and using a current density of 10mA/cm 2 Is subjected to electroplating deposition by constant current; the time of electroplating deposition is 20mi n;
after the electroplating is finished, carrying out heat treatment on the foam copper deposited by electroplating, wherein the heat treatment conditions are as follows: under argon atmosphere, raising the temperature of the foam copper material to 950 ℃ at a heating rate of 5 ℃/min, and preserving heat for 2 hours; after the heat treatment is finished, preparing pretreated foamy copper;
filling carbon fibers into the pores of the pretreated foam copper to obtain a foam copper-carbon preform; the method for filling the carbon fiber comprises the following steps: mixing long carbon fibers with the diameter of between 1.8 and 2.5mm and short carbon fibers with the diameter of between 0.8 and 1.0mm to form long/short mixed fibers for filling, wherein the diameter of the long carbon fibers with the diameter of between 1.8 and 2.5mm is between 6 and 7 mu m, and the diameter of the short carbon fibers with the diameter of between 0.8 and 1.0mm is between 6 and 7 mu m; the filling mode is as follows: respectively filling long carbon fibers and short carbon fibers into the pretreated foam copper pores in a colloid layering suction filtration mode; namely:
firstly, pre-dispersing long carbon fibers into a fiber dispersing agent in an ultrasonic manner to obtain a long carbon fiber dispersing liquid B, and pre-dispersing short carbon fibers into the fiber dispersing agent in an ultrasonic manner to obtain a short carbon fiber dispersing liquid B; the ultrasonic pre-dispersion time is 10mi n; the mass fraction of the long carbon fibers in the long carbon fiber dispersion liquid B and the mass fraction of the short carbon fibers in the short carbon fiber dispersion liquid B are 5wt%; then carrying out suction filtration of the short carbon fiber dispersion liquid B under the condition of the pressure of 0.02MPa, and then carrying out suction filtration of the long carbon fiber dispersion liquid B; repeatedly carrying out suction filtration until the quality of the pretreated foamy copper is not increased; after layering and suction filtration, the layer thickness ratio of a long carbon fiber layer to a short carbon fiber layer in the foam copper-carbon preform is 1:1.5; the fiber dispersing agents for dispersing the long carbon fibers and the short carbon fibers are all obtained by dissolving hydroxyethyl cellulose in water, and the mass ratio of the hydroxyethyl cellulose to the water in the fiber dispersing agents is 1:100; and drying after the layering, suction filtration and filling are finished, wherein the drying temperature is 100 ℃, and the drying time is 4 hours.
Then covering the outer surface of the foam copper with the carbon fibers filled in the pores with a carbon fiber braided fabric and a carbon fiber felt preform; namely: completely coating the foam copper filled with the carbon fibers in the gaps in the carbon fiber braided fabric and the carbon fiber felt preform to form a foam copper-carbon preform; the weaving method of the carbon fiber braided fabric and the carbon fiber felt preform comprises the following steps: sequentially and alternately laying a single-layer carbon fiber braided fabric and a carbon fiber felt, and orthogonally layering the carbon fiber braided fabric according to [0/90] n; fixing a carbon fiber braided fabric and a carbon fiber felt by adopting a needle punching method to prepare a carbon fiber braided fabric and a carbon fiber felt preform with the thickness of 10 mm; the carbon fiber braided fabric is TC33-3k 240 g plain weave carbon fiber cloth of Guangdong Taili carbon fiber liability Co., ltd, and the carbon fiber felt is a non-woven felt formed after short carbon fibers are uniformly flicked in the embodiment, and multiple layers are overlapped when in use.
Step (3), cracking and carbonizing the foam copper-carbon preform by adopting an isothermal chemical vapor infiltration process to obtain a carbon-copper composite material precursor; the isothermal chemical vapor infiltration process conditions were: methane and hydrogen are used as gas phases; the gas cracking temperature is 1100 ℃, the atmosphere pressure is 35kPa, the flow ratio of methane to hydrogen is 3:2, and the flow of methane is 30g/h; the densification time is 90 hours;
Step (4), graphitizing the carbon-copper composite material precursor, wherein the graphitization temperature is 2200 ℃, and the graphitization time is 17 hours; and after graphitization is finished, preparing the carbon-copper composite material with good heat dissipation and wear resistance.
Example 6
In this embodiment, the preparation method of the carbon-copper composite material with good heat dissipation and wear resistance includes the following steps:
carrying out graphene oxide loading treatment on the surface of the foam copper by adopting an electroplating method to obtain pretreated foam copper; the operation method of the electroplating method comprises the following steps:
dispersing graphene oxide with the particle size of 20-40 mu m into an ethanol solution, adding 3-aminopropyl triethoxysilane KH550, and uniformly mixing to obtain a mixed dispersion liquid A, wherein the mass ratio of the graphene oxide to the 3-aminopropyl triethoxysilane KH550 to the ethanol solution in the mixed dispersion liquid A is 2:2:9; the volume fraction of ethanol in the ethanol solution is 96%;
step (1-2) using copper foam with a specification of 10ppi as an anode, using the mixed dispersion liquid A as a plating solution, and using a current density of 10mA/cm 2 Is subjected to electroplating deposition by constant current; the time of electroplating deposition is 20mi n;
after the electroplating is finished, carrying out heat treatment on the foam copper deposited by electroplating, wherein the heat treatment conditions are as follows: under argon atmosphere, raising the temperature of the foam copper material to 950 ℃ at a heating rate of 5 ℃/min, and preserving heat for 2 hours; after the heat treatment is finished, preparing pretreated foamy copper;
Filling carbon fibers into the pores of the pretreated foam copper to obtain a foam copper-carbon preform; the method for filling the carbon fiber comprises the following steps: mixing long carbon fibers with the diameter of between 1.8 and 2.5mm and short carbon fibers with the diameter of between 0.8 and 1.0mm to form long/short mixed fibers for filling, wherein the diameter of the long carbon fibers with the diameter of between 1.8 and 2.5mm is between 6 and 7 mu m, and the diameter of the short carbon fibers with the diameter of between 0.8 and 1.0mm is between 6 and 7 mu m; the filling mode is as follows: respectively filling long carbon fibers and short carbon fibers into the pretreated foam copper pores in a colloid layering suction filtration mode; namely:
firstly, pre-dispersing long carbon fibers into a fiber dispersing agent in an ultrasonic manner to obtain a long carbon fiber dispersing liquid B, and pre-dispersing short carbon fibers into the fiber dispersing agent in an ultrasonic manner to obtain a short carbon fiber dispersing liquid B; the ultrasonic pre-dispersion time is 10mi n; the mass fraction of the long carbon fibers in the long carbon fiber dispersion liquid B and the mass fraction of the short carbon fibers in the short carbon fiber dispersion liquid B are 5wt%; then carrying out suction filtration of the short carbon fiber dispersion liquid B under the condition of the pressure of 0.02MPa, and then carrying out suction filtration of the long carbon fiber dispersion liquid B; repeatedly carrying out suction filtration until the quality of the pretreated foamy copper is not increased; after layering and suction filtration, the layer thickness ratio of a long carbon fiber layer to a short carbon fiber layer in the foam copper-carbon preform is 1:1.5; the fiber dispersing agents for dispersing the long carbon fibers and the short carbon fibers are all obtained by dissolving hydroxyethyl cellulose in water, and the mass ratio of the hydroxyethyl cellulose to the water in the fiber dispersing agents is 1:100; and drying after the layering, suction filtration and filling are finished, wherein the drying temperature is 100 ℃, and the drying time is 4 hours.
Then covering the outer surface of the foam copper with the carbon fibers filled in the pores with a carbon fiber braided fabric and a carbon fiber felt preform; namely: completely coating the foam copper filled with the carbon fibers in the gaps in the carbon fiber braided fabric and the carbon fiber felt preform; then sewing long carbon fiber tows in the direction perpendicular to the foam copper and carbon-carbon layered prefabricated plane, wherein the diameter of each long carbon fiber filament is 6-8 mu m, and the diameter of each long carbon fiber tow is 0.5-0.8 mm; when in sewing, sewing long carbon fiber tows into foam copper holes with the specification of 10ppi and filled with carbon fibers, wherein the stitch spacing is 3mm, and the row spacing is 3mm, so as to obtain a foam copper-carbon preform with a loose porous structure; the weaving method of the carbon fiber braided fabric and the carbon fiber felt preform comprises the following steps: sequentially and alternately laying a single-layer carbon fiber braided fabric and a carbon fiber felt, and orthogonally layering the carbon fiber braided fabric according to [0/90] n; fixing a carbon fiber braided fabric and a carbon fiber felt by adopting a needle punching method to prepare a carbon fiber braided fabric and a carbon fiber felt preform with the thickness of 12 mm; the carbon fiber braided fabric is TC33-3k 240 g plain weave carbon fiber cloth of Guangdong Taili carbon fiber liability Co., ltd, and the carbon fiber felt is a non-woven felt formed after short carbon fibers are uniformly flicked in the embodiment, and multiple layers are overlapped when in use.
Step (3), cracking and carbonizing the foam copper-carbon preform by adopting an isothermal chemical vapor infiltration process to obtain a carbon-copper composite material precursor; the isothermal chemical vapor infiltration process conditions were: methane and hydrogen are used as gas phases; the gas cracking temperature is 1100 ℃, the atmosphere pressure is 35kPa, the flow ratio of methane to hydrogen is 3:2, and the flow of methane is 25g/h; the densification time is 90 hours;
step (4), graphitizing the carbon-copper composite material precursor, wherein the graphitization temperature is 2200 ℃, and the graphitization time is 17 hours; and after graphitization is finished, preparing the carbon-copper composite material with good heat dissipation and wear resistance.
Example 7
In this embodiment, the preparation method of the carbon-copper composite material with good heat dissipation and wear resistance includes the following steps:
carrying out graphene oxide loading treatment on the surface of the foam copper by adopting an electroplating method to obtain pretreated foam copper; the operation method of the electroplating method comprises the following steps:
dispersing graphene oxide with the particle size of 20-40 mu m into an ethanol solution, adding 3-aminopropyl triethoxysilane KH550, and uniformly mixing to obtain a mixed dispersion liquid A, wherein the mass ratio of the graphene oxide to the 3-aminopropyl triethoxysilane KH550 to the ethanol solution in the mixed dispersion liquid A is 2:2:9; the volume fraction of ethanol in the ethanol solution is 96%;
Step (1-2) using copper foam with a specification of 10ppi as an anode, using the mixed dispersion liquid A as a plating solution, and using a current density of 10mA/cm 2 Is subjected to electroplating deposition by constant current; the time of electroplating deposition is 20mi n;
after the electroplating is finished, carrying out heat treatment on the foam copper deposited by electroplating, wherein the heat treatment conditions are as follows: under argon atmosphere, raising the temperature of the foam copper material to 950 ℃ at a heating rate of 5 ℃/min, and preserving heat for 2 hours; after the heat treatment is finished, preparing pretreated foamy copper;
filling carbon fibers into the pores of the pretreated foam copper to obtain a foam copper-carbon preform; the method for filling the carbon fiber comprises the following steps: mixing long carbon fibers with the diameter of between 1.8 and 2.5mm and short carbon fibers with the diameter of between 0.8 and 1.0mm to form long/short mixed fibers for filling, wherein the diameter of the long carbon fibers with the diameter of between 1.8 and 2.5mm is between 6 and 7 mu m, and the diameter of the short carbon fibers with the diameter of between 0.8 and 1.0mm is between 6 and 7 mu m; the filling mode is as follows: respectively filling long carbon fibers and short carbon fibers into the pretreated foam copper pores in a colloid layering suction filtration mode; namely:
firstly, pre-dispersing long carbon fibers into a fiber dispersing agent in an ultrasonic manner to obtain a long carbon fiber dispersing liquid B, and pre-dispersing short carbon fibers into the fiber dispersing agent in an ultrasonic manner to obtain a short carbon fiber dispersing liquid B; the ultrasonic pre-dispersion time is 10mi n; the mass fraction of the long carbon fibers in the long carbon fiber dispersion liquid B and the mass fraction of the short carbon fibers in the short carbon fiber dispersion liquid B are 6wt%; then carrying out suction filtration of the short carbon fiber dispersion liquid B under the condition of the pressure of 0.02MPa, and then carrying out suction filtration of the long carbon fiber dispersion liquid B; repeatedly carrying out suction filtration until the quality of the pretreated foamy copper is not increased; after layering and suction filtration, the layer thickness ratio of a long carbon fiber layer to a short carbon fiber layer in the foam copper-carbon preform is 1:2; the fiber dispersing agents for dispersing the long carbon fibers and the short carbon fibers are all obtained by dissolving hydroxyethyl cellulose in water, and the mass ratio of the hydroxyethyl cellulose to the water in the fiber dispersing agents is 1:100; and drying after the layering, suction filtration and filling are finished, wherein the drying temperature is 100 ℃, and the drying time is 4 hours.
Then covering the outer surface of the foam copper with the carbon fibers filled in the pores with a carbon fiber braided fabric and a carbon fiber felt preform; namely: covering the carbon fiber braided fabric and the carbon fiber felt preform on the single surface of the foam copper filled with the carbon fibers in the gaps; then sewing long carbon fiber tows in the direction perpendicular to the foam copper and carbon-carbon layered prefabricated plane, wherein the diameter of each long carbon fiber filament is 6-8 mu m, and the diameter of each long carbon fiber tow is 0.5-0.8 mm; when in sewing, sewing long carbon fiber tows into foam copper holes with the specification of 10ppi and filled with carbon fibers, wherein the stitch spacing is 3mm, and the row spacing is 3mm, so as to obtain a foam copper-carbon preform with a loose porous structure; the weaving method of the carbon fiber braided fabric and the carbon fiber felt preform comprises the following steps: sequentially and alternately laying a single-layer carbon fiber braided fabric and a carbon fiber felt, and orthogonally layering the carbon fiber braided fabric according to [0/90] n; fixing a carbon fiber braided fabric and a carbon fiber felt by adopting a needle punching method to prepare a carbon fiber braided fabric and a carbon fiber felt preform with the thickness of 15 mm; the carbon fiber braided fabric is TC33-3k 240 g plain weave carbon fiber cloth of Guangdong Taili carbon fiber liability Co., ltd, and the carbon fiber felt is a non-woven felt formed after short carbon fibers are uniformly flicked in the embodiment, and multiple layers are overlapped when in use.
Step (3), cracking and carbonizing the foam copper-carbon preform by adopting an isothermal chemical vapor infiltration process to obtain a carbon-copper composite material precursor; the isothermal chemical vapor infiltration process conditions were: methane and hydrogen are used as gas phases; the gas cracking temperature is 1100 ℃, the atmosphere pressure is 35kPa, the flow ratio of methane to hydrogen is 3:2, and the flow of methane is 30g/h; the densification time is 90 hours;
step (4), graphitizing the carbon-copper composite material precursor, wherein the graphitization temperature is 2200 ℃, and the graphitization time is 17 hours; and after graphitization is finished, preparing the carbon-copper composite material with good heat dissipation and wear resistance.
Comparative example
The preparation method of the carbon-copper composite material of the comparative example comprises the following steps:
step (1), directly filling carbon fibers into the pores of the foam copper to obtain a foam copper-carbon preform; the carbon fiber filling method of this example is identical to that of example 1, and the raw materials used are identical;
step (2), carrying out cracking carbonization on the foam copper-carbon preform by adopting an isothermal chemical vapor infiltration process to obtain a carbon-copper composite material precursor; the procedure and parameters for this step are exactly the same as in example 1;
step (3), graphitizing the precursor of the carbon-copper composite material, and preparing the carbon-copper composite material after graphitization is finished; the procedure and parameters for this step are exactly the same as in example 1;
Respectively carrying out comparative tests on the mechanical properties, the heat conduction properties and the wear resistance of the carbon-copper composite materials prepared in the examples 1 to 7 and the comparative examples, wherein the mechanical properties are tested by a tensile test, the heat conduction properties are tested by a flat plate method, and the wear resistance is tested by a friction and wear test; the test results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the carbon-copper composite materials prepared by the methods of the different examples except example 2 have a thermal conductivity in the fiber axis direction of more than 100W (m.k -1 ) The method comprises the steps of carrying out a first treatment on the surface of the Except for comparison, the thermal conductivity of the carbon-copper composite material prepared by all the examples in the axial direction of the fiber is more than 300W (m.k) -1 ) The carbon-copper composite material prepared by the method has good heat dissipation. In addition, the wear resistance of the carbon-copper composite material prepared by the method is about 1.5 times of that of a common carbon-carbon composite material.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While the obvious variations or modifications which are extended therefrom remain within the scope of the claims of this patent application.
Claims (10)
1. The preparation method of the carbon-copper composite material with good heat dissipation and wear resistance is characterized by comprising the following steps:
carrying out graphene oxide loading treatment on the surface of the foamy copper to obtain pretreated foamy copper;
filling carbon fibers into the pores of the pretreated foam copper to obtain a foam copper-carbon preform;
step (3), cracking and carbonizing the foam copper-carbon preform by adopting an isothermal chemical vapor infiltration process to obtain a carbon-copper composite material precursor;
and (4) graphitizing the precursor of the carbon-copper composite material, and preparing the carbon-copper composite material with good heat dissipation and wear resistance after graphitization is finished.
2. The method for producing a carbon-copper composite material having excellent heat dissipation and wear resistance according to claim 1, wherein in the step (1), the graphene oxide is carried out on the surface of the copper foam by an electroplating method or an immersion method.
3. The method for preparing a carbon-copper composite material with good heat dissipation and wear resistance according to claim 2, wherein the operation method of the electroplating method is as follows: dispersing graphene oxide into an ethanol solution, adding 3-aminopropyl triethoxysilane KH550, and uniformly mixing to obtain a mixed dispersion liquid A; using foam copper as an anode, using the mixed dispersion liquid A as electroplating liquid, and adopting constant current electricity to carry out electroplating deposition; drying after electroplating, and performing heat treatment on the dried foamy copper, wherein the pretreated foamy copper is prepared after the heat treatment is finished;
The operation method of the dipping method comprises the following steps: dispersing graphene oxide into an organic solvent, and obtaining a mixed dispersion liquid B after uniform dispersion; immersing the foam copper in the mixed dispersion liquid B, placing the mixed dispersion liquid B under ultrasonic conditions for ultrasonic deposition, and vacuum drying after the deposition is finished; and carrying out heat treatment on the dried foamy copper, and preparing the pretreated foamy copper after the heat treatment is finished.
4. The method for preparing a carbon-copper composite material with good heat dissipation and wear resistance according to claim 3, wherein when the graphene oxide is loaded by an electroplating method: the mass ratio of graphene oxide to 3-aminopropyl triethoxysilane KH550 to ethanol solution is (1-2), 1-2, 8-9, and the particle size of the graphene oxide is 20-40 μm; the volume fraction of ethanol in the ethanol solution is 95-99%; constant current density of 5-15 mA/cm 2 The time of electroplating deposition is 10-30 min, the drying temperature is 100-120 ℃ and the drying time is 2-4 h after the electroplating deposition; the conditions of the heat treatment are as follows: under argon atmosphere, raising the temperature of the foam copper material to 850-950 ℃ at a heating rate of 5 ℃/min, and preserving heat for 1.5-2.5 h;
when the graphene oxide is loaded by the impregnation method, the following steps are carried out: the organic solvent is formed by mixing absolute ethyl alcohol and acetone according to the volume ratio of 1:1; the mass concentration of the graphene oxide in the mixed dispersion liquid B is 300mg/L, and the particle size of the graphene oxide is 20-40 mu m; the times of ultrasonic deposition are 1 to 5 times; the conditions of ultrasonic deposition are: the ultrasonic frequency is 35-45 kHz, the ultrasonic power is 100-300W, and the ultrasonic deposition time is 10-30 min; after the deposition is finished, the vacuum drying temperature is 80-100 ℃ and the drying time is 2-4 h; the conditions of the heat treatment are as follows: under argon atmosphere, the temperature rising rate of the foam copper material is increased to 850-950 ℃ at 5 ℃/min, and the temperature is kept for 1.5-2.5 h.
5. The method for preparing a carbon-copper composite material with good heat dissipation and wear resistance according to claim 1, wherein in the step (2), the method for filling carbon fibers is as follows:
filling by adopting long carbon fiber with the length range of 1.8-2.5 mm, wherein the filling mode is as follows: implanting long carbon fibers into the pores of the pretreated foam copper in an ultrasonic vibration mode;
or, short carbon fibers with the length ranging from 0.8 mm to 1.0mm are adopted for filling, and the filling mode is as follows: implanting short carbon fibers into the pores of the pretreated foam copper in an ultrasonic vibration mode;
or, long carbon fibers with the length of 1.8-2.5 mm and short carbon fibers with the length of 0.8-1.0 mm are mixed to form long/short mixed fibers for filling, and the filling mode is as follows: filling long/short mixed fibers into the pretreated foam copper pores in a colloid suction filtration mode;
the diameter of the long carbon fiber with the diameter of 1.8-2.5 mm is 6-7 mu m, and the diameter of the short carbon fiber with the diameter of 0.8-1.0 mm is 6-7 mu m; the pore size of the copper foam was 10ppi.
6. The method for preparing a carbon-copper composite material with good heat dissipation and wear resistance according to claim 5, wherein when long carbon fibers are used for filling: dispersing long carbon fibers into a fiber dispersing agent to form a long carbon fiber dispersing liquid A, then completely immersing pretreated foam copper into the long carbon fiber dispersing liquid A for ultrasonic vibration filling, and drying at 100 ℃ for 2-4 hours after filling; the mass fraction of the long carbon fibers in the long carbon fiber dispersion liquid A is 4-6wt%; the ultrasonic frequency is 45kHz, the ultrasonic power is 100-300W, and the ultrasonic time is 10-30 min;
When short carbon fibers are used for filling: firstly dispersing short carbon fibers into a fiber dispersing agent to form a short carbon fiber dispersing liquid A, then completely immersing pretreated foam copper into the short carbon fiber dispersing liquid A for ultrasonic vibration filling, and drying at 100 ℃ for 2-4 h after filling; the mass fraction of the short carbon fibers in the short carbon fiber dispersion liquid A is 4-6wt%; the ultrasonic frequency is 45kHz, the ultrasonic power is 100-300W, and the ultrasonic time is 10-30 min;
when filling with long/short mixed fibers: the colloid suction filtration mode is mixed suction filtration or layered suction filtration, and the colloid suction filtration is dried for 2 to 4 hours at the temperature of 100 ℃ after the suction filtration is finished;
when mixing and suction filtering, firstly mixing long carbon fibers and short carbon fibers according to the mass ratio of 1:1, and then pre-dispersing the long carbon fibers and the short carbon fibers into a fiber dispersing agent by ultrasonic, wherein the pre-dispersing time of ultrasonic is 10min, so as to obtain a long/short mixed fiber dispersing liquid, and the mass fraction of the long carbon fibers in the long/short mixed fiber dispersing liquid is 4-6wt%; then mixing and suction filtering are carried out under the condition that the pressure is 0.02-0.05 MPa, and the suction filtering is repeated until the quality of the pretreated foam copper is not increased any more;
when the layering suction filtration is carried out, the long carbon fiber is firstly subjected to ultrasonic pre-dispersion into a fiber dispersing agent to obtain a long carbon fiber dispersing liquid B, and the short carbon fiber is subjected to ultrasonic pre-dispersion into the fiber dispersing agent to obtain a short carbon fiber dispersing liquid B; the ultrasonic pre-dispersion time is 10min; the mass fraction of the long carbon fibers in the long carbon fiber dispersion liquid B and the mass fraction of the short carbon fibers in the short carbon fiber dispersion liquid B are 4-6wt%; then, under the condition of the pressure of 0.02-0.05 MPa, carrying out suction filtration of the short carbon fiber dispersion liquid B and then carrying out suction filtration of the long carbon fiber dispersion liquid B; repeatedly carrying out suction filtration until the quality of the pretreated foamy copper is not increased; after layering and suction filtration, the layer thickness ratio of the long carbon fiber layer to the short carbon fiber layer in the foam copper-carbon preform is 1:1-2;
The fiber dispersing agents for dispersing the long carbon fibers, the short carbon fibers and the long/short mixed fibers are all hydroxyethyl cellulose aqueous solutions, and the mass ratio of the hydroxyethyl cellulose to water in the fiber dispersing agents is 1:100.
7. The method for producing a carbon-copper composite material having excellent heat dissipation and wear resistance according to claim 5, wherein the step (2) further comprises the steps of:
covering the outer surface of the foam copper filled with the carbon fibers in the gaps with a carbon fiber braided fabric and a carbon fiber felt preform; namely: completely coating the foam copper filled with the carbon fibers in the gaps in the carbon fiber braided fabric and the carbon fiber felt preform to form a foam copper-carbon preform; or only the single surface of the foam copper filled with the carbon fibers in the gaps is covered by the carbon fiber braided fabric and the carbon fiber felt preform;
the weaving method of the carbon fiber braided fabric and the carbon fiber felt preform comprises the following steps: sequentially and alternately laying a single-layer carbon fiber braided fabric and a carbon fiber felt, and orthogonally layering the carbon fiber braided fabric according to [0/90] n; fixing the carbon fiber braided fabric and the carbon fiber felt by adopting a needle punching method to prepare a carbon fiber braided fabric and a carbon fiber felt preform with the thickness of 10-15 mm.
8. The method for producing a carbon-copper composite material having excellent heat dissipation and wear resistance according to claim 7, wherein the step (2) further comprises the steps of:
Sewing long carbon fiber tows in the direction perpendicular to the foam copper and carbon layered prefabricated plane, wherein the diameter of each long carbon fiber filament is 6-8 mu m, and the diameter of each long carbon fiber tow is 0.5-0.8 mm; when in sewing, the stitch interval is 3mm, and the row interval is 1-3 mm.
9. The method for preparing a carbon-copper composite material with good heat dissipation and wear resistance according to claim 1, wherein in the step (3), the isothermal chemical vapor infiltration process conditions are: methane and hydrogen are used as gas phases; the gas cracking temperature is 1050-1100 ℃, the atmosphere pressure is 20-40 kPa, the flow ratio of methane to hydrogen is 3:2, and the flow of methane is 20-30 g/h; the densification time is 70-100 h.
10. The method for producing a carbon-copper composite material having excellent heat dissipation and wear resistance according to claim 1, wherein in the step (4), the graphitization temperature is 2000 to 2300 ℃ and the graphitization time is 10 to 20 hours.
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