CN108193148B - Preparation method of carbon fiber reinforced metal matrix composite - Google Patents
Preparation method of carbon fiber reinforced metal matrix composite Download PDFInfo
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- CN108193148B CN108193148B CN201711443722.4A CN201711443722A CN108193148B CN 108193148 B CN108193148 B CN 108193148B CN 201711443722 A CN201711443722 A CN 201711443722A CN 108193148 B CN108193148 B CN 108193148B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/02—Pretreatment of the fibres or filaments
- C22C47/04—Pretreatment of the fibres or filaments by coating, e.g. with a protective or activated covering
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/04—Electroplating: Baths therefor from solutions of chromium
- C25D3/08—Deposition of black chromium, e.g. hexavalent chromium, CrVI
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
Abstract
The invention discloses a preparation method of a carbon fiber reinforced metal matrix composite, which comprises the following specific steps: step 1, pretreating the surface of carbon fiber; step 2, plating metal copper, nickel or chromium on the surface of the carbon fiber by adopting an electroplating method; step 3, weighing a certain amount of metal powder and metal-coated carbon fibers, and mechanically mixing the metal powder and the metal-coated carbon fibers in a wine barrel type mixer; step 4, the mixed material in the step 3 is placed in a steel pressing die for cold press molding; step 5, the green body formed by cold pressing in the step 4 is arranged in a three-high graphite die for hot pressing and sintering; and 6, placing the composite material sintered in the step 5 into a solid sand blasting machine for surface treatment to obtain the carbon fiber reinforced metal matrix composite material. The preparation method solves the problems of premature fiber pulling, breakage and failure caused by poor bonding of the reinforcing phase and the matrix due to the interface wetting problem of the existing fiber reinforced composite material.
Description
Technical Field
The invention belongs to the technical field of composite material preparation methods, and particularly relates to a preparation method of a carbon fiber reinforced metal matrix composite material.
Background
The composite material is composed of a matrix material, a reinforcement and an interface therebetween, and the performance of the composite material depends on the ratio of the reinforcement to the matrix and the performance of the three components. The composite material can exert the advantages of the materials of the respective components, the components of the composite material mutually make up for the deficiencies to generate a synergistic effect to have new characteristics, and meanwhile, the composite material can design special performance and comprehensive performance meeting the actual requirements and is increasingly highly valued by countries in the world. Compared with other materials, the metal matrix composite material has higher specific strength, specific rigidity, excellent conductivity, heat resistance, high toughness and high impact property. The method is widely applied to various fields of aerospace, automobile shipbuilding, bridge construction, electric machinery, medical treatment, sports and the like.
The reinforcement of the metal matrix composite material mainly comprises fibers, whiskers and particles, wherein the fibers are the first choice of the reinforcement due to the characteristics of high strength, high modulus, high temperature resistance, environment resistance, friction resistance, chemical resistance and the like. In particular, carbon fiber is usually used as a main reinforcing phase of a composite material due to its low density, high strength and excellent electrical and thermal properties. However, when the carbon fiber is compounded with the metal matrix, the non-metallic property of the carbon fiber, the wettability of the interface, the bonding state and the like become bottlenecks in the development of the composite material. If the mechanical and physical bonding interface strength is low, the carbon fibers are often pulled out, peeled or shed when bearing load, and the performance of the composite material is greatly influenced. Therefore, it is inevitable to modify the surface of the carbon fiber to control the bonding state of the metal and the carbon fiber. The composite material prepared by the modified carbon fiber can make up the problems of the current materials.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon fiber reinforced metal matrix composite, which solves the problems of premature extraction, fracture and failure of fibers caused by poor bonding of a reinforcing phase and a matrix due to the interface wetting problem of the conventional fiber reinforced composite.
The invention adopts the technical scheme that a preparation method of a carbon fiber reinforced metal matrix composite material comprises the following specific steps:
step 1, pretreating the surface of carbon fiber;
step 2, plating metal copper, nickel or chromium on the surface of the carbon fiber by adopting an electroplating method;
step 3, weighing a certain amount of metal powder and carbon fiber coated with metal copper, nickel or chromium, and mechanically mixing in a wine barrel type mixer for 30-80 min;
step 4, putting the mixed material obtained in the step 3 into a steel pressing die for cold press molding, wherein the selected pressing pressure is 300-500 MPa;
step 5, the green body formed by cold pressing in the step 4 is arranged in a three-high graphite die for hot pressing and sintering;
and 6, placing the composite material sintered in the step 5 into a solid sand blasting machine for surface treatment to obtain the carbon fiber reinforced metal matrix composite material.
The present invention is also characterized in that,
the pretreatment process of the carbon fiber surface in the step 1 is as follows: placing the carbon fiber in a heating furnace, burning for 30-60 min at 480-500 ℃ for thermal degreasing, soaking in acetone for 1h, washing with water, placing in a drying oven for drying for 6-8 h at 35-45 ℃, placing the dried carbon fiber in 68 wt% concentrated nitric acid, coarsening for 60-90 min at 90 ℃, and washing with deionized water to be neutral.
In the step 2, the specific process of plating metal copper, nickel or chromium on the surface of the carbon fiber by adopting an electroplating method is as follows: taking the carbon fiber treated in the step 1 as a cathode, taking a nickel sheet, a copper sheet or a lead sheet as an anode, placing the anode in an electroplating solution for electroplating, then washing the anode for 3-5 times, and placing the anode in a drying oven for drying for 6-8 hours at the temperature of 35-45 ℃; after the surface of the carbon fiber is plated with the metal copper, passivation treatment is needed.
In step 2, the electroplating solution for plating metal copper on the surface of the carbon fiber comprises the following components: 30-50 g/L of copper sulfate, 10-25 g/L of sodium tartrate, 60-90 g/L of sodium citrate and 8-12 g/L of potassium nitrate, wherein the electroplating process conditions are as follows: electroplating temperature: 25-45 ℃, current density: 1.0 to 3.5A/dm2And electroplating time: 20-40 min.
In step 2, the electroplating solution for plating metallic nickel on the surface of the carbon fiber comprises the following components: 200-270 g/L of nickel sulfate, 60-70 g/L of nickel chloride, 32-40 g/L of boric acid and 0.01-0.1 g/L of sodium dodecyl sulfate, wherein the electroplating process conditions are as follows: electroplating temperature: 25-40 ℃, current density: 0.1 to 0.5A/dm2And electroplating time: 4-20 min.
In step 2, the electroplating solution for plating metal chromium on the surface of the carbon fiber comprises the following components: 230-250 g/L of chromic anhydride, 1.25-5 mL/L of concentrated sulfuric acid and 5-10 g/L of boric acid, wherein the electroplating process conditions are as follows: electroplating temperature: and (3) electroplating time at 40-60 ℃: 10-30 min, current density: 24 to 30A/dm2。
In the step 3, the volume of the carbon fiber coated with the metal copper, nickel or chromium accounts for 1-50% of the total volume of the mixed material.
And 3, the metal powder in the step 3 is copper powder, iron powder, aluminum powder or tungsten powder.
In step 5, the hot-pressing sintering process comprises the following steps: slowly heating to 0.7-0.8 times of the melting point of the metal in a high-temperature atmosphere protection hot-pressing furnace, simultaneously pressurizing to 20-30 MPa, standing for 60-90 min, and cooling along with the furnace, wherein the used protective atmosphere is argon or nitrogen, and the gas flow is 1-2L/h.
In step 6, the used sand grains have a grain size of about 0.1-0.5 mm and an impact velocity of 1-3 m/s.
The invention has the beneficial effects that:
(1) the mechanical property and the physical property of the composite material can be greatly improved by pre-coating metal on the surface of the carbon fiber and then mixing, hot-pressing and sintering;
(2) the method for preparing the carbon fiber reinforced metal matrix composite material has the advantages of simple operation, low energy consumption, low cost, high production efficiency and easy industrial production.
Drawings
FIG. 1 is an SEM image of an electro-coppered carbon fiber prepared by the method of the present invention;
FIG. 2 is an SEM image of an electroplated nickel carbon fiber prepared by the method of the present invention;
FIG. 3 is an SEM image of an electro-chromic carbon fiber prepared by the method of the present invention;
FIG. 4 is a macroscopic structural morphology of a carbon fiber reinforced copper-based composite material with a volume fraction of 3% plated with chromium prepared by the method of the present invention;
FIG. 5 is a macroscopic structural morphology of a 10% volume fraction chromium-plated carbon fiber reinforced copper-based composite material prepared by the method of the present invention;
FIG. 6 is a macroscopic structural morphology of a carbon fiber reinforced copper-based composite material with a volume fraction of 15% plated with chromium prepared by the method of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a carbon fiber reinforced metal matrix composite, which comprises the following specific steps:
step 1, surface pretreatment of carbon fibers
The carbon fiber is placed in a heating furnace and burned for 30-60 min at 480-500 ℃ for thermal degreasing (the burning temperature and the burning time depend on the specific carbon fiber because the organic glue components on the surface of the purchased carbon fiber are different, for example, the commercial TC-35 type carbon fiber can be thermally degreased after being burned for 60min at 480 ℃), then the carbon fiber is soaked in acetone for 1h to dissolve the coke and clean the surface of the carbon fiber, and after being washed for multiple times, the carbon fiber is placed in a drying oven for drying for 6-8 h at 35-45 ℃. And then placing the dried carbon fiber in 68 wt% concentrated nitric acid, coarsening for 60-90 min at 90 ℃, and washing with deionized water to be neutral.
Step 2, plating copper, nickel or chromium on the surface of the carbon fiber by adopting an electroplating method
And (3) taking the carbon fiber treated in the step (1) as a cathode, taking a nickel sheet, a copper sheet or a lead sheet as an anode, and placing the anode in electroplating solution for electroplating. And washing with deionized water for multiple times, and drying in a drying oven at 35-45 ℃ for 6-8 h for later use. The plating solution composition and process parameters are shown in Table 1. It is worth proposing that copper is easy to oxidize, and after the copper electroplating is finished, passivation treatment needs to be carried out in time (namely, carbon fibers plated with copper are placed in 15% of disodium ethylene diamine tetraacetate solution for passivation for 15min), and then washing and drying are carried out.
TABLE 1 electroplating bath composition and Process parameters
Step 3, mixing the materials
The respective amounts of the metal powder and the metal-coated carbon fiber (the coated metal layer is negligible) are calculated from the metal powder having a particle size of about 60 to 80 μm (200 mesh) in accordance with the ratio of the composite material to be produced (the calculation method is the ratio of the theoretical density G of the part volume G to be added). According to the volume percentage, the theoretical density of the composite material is the volume ratio of the metal density G added to the metal powder plus the volume ratio of the metal-coated carbon fiber to the metal-coated carbon fiber. Typically the metal matrix is copper, with copper or nickel coated carbon fibers; the metal matrix is of iron or tungsten, and nickel-coated carbon fibers are suggested.
Step 4, mixing
And (4) mechanically mixing the metal powder calculated in the step (3) and the metal-coated carbon fiber in a wine barrel type mixer for 30-80 min. When mixing, 10-20 mL/kg of alcohol is added, so that the mixing efficiency is accelerated, and dust emission is avoided. The volume of the carbon fiber coated with the metal copper, nickel or chromium accounts for 1 to 50 percent of the total volume of the mixed material.
Step 5, forming
And (2) weighing a certain amount of the material mixed in the step (4) (the weighed amount depends on the components of the composite material and the size of a pressed blank, and the general calculation method is that the weighed mass is the volume G of the pressed blank and the density of the composite material of the components) is placed in a steel die (the size and the shape of the part are determined and designed in advance) for cold pressing and forming, wherein the selected pressing pressure is 300-500 MPa.
Step 6, hot-pressing sintering
And (3) loading the green body subjected to cold press molding in the step (5) into a three-high graphite (high-strength, high-density and high-conductivity) mold (similar to a steel pressing mold in size and shape). And then slowly heating (the heating speed is 200-300 ℃/h) in a high-temperature atmosphere protection hot-pressing furnace to the sintering temperature (generally 0.7-0.8 time of the melting point of the metal), simultaneously pressurizing to the pressure of 20-30 MPa, standing at high temperature for 60-90 min, and then cooling along with the furnace. The protective atmosphere is argon or nitrogen, and the gas flow is 1-2L/h.
Step 7, post-treatment
And (4) placing the carbon fiber reinforced metal matrix composite sintered in the step (6) into a solid sand blasting machine for surface treatment, wherein the grain size of the used sand grains is about 0.1-0.5 mm, and the impact speed is 1-3 m/s. Removing some attachments attached to the surface and improving the stress state of the surface.
It can be seen from fig. 1 that the metal copper particles on the surface of the carbon fiber are more uniform and the coating is completely covered, but the particles are larger;
as seen from FIG. 2, the metallic nickel layer on the surface of the carbon fiber has small particles and is uniformly coated, but the surface of the coating has a small amount of micropores;
from FIG. 3, it can be seen that the metal chromium particles on the surface of the carbon fiber are dense and uniform but are relatively large compared with the chemical chromium plating particles;
from fig. 4-6, it can be seen that the carbon fibers in the carbon fiber reinforced copper-based composite material prepared from the chromium-plated carbon fibers with the volume fractions of 3%, 10% and 15% are uniformly distributed in the matrix, the segregation phenomenon is avoided, the material has no obvious holes, and the matrix structure is compact.
Example 1
A preparation method of a carbon fiber reinforced copper-based composite material comprises the following specific steps:
step 1, surface pretreatment of carbon fibers
Placing the carbon fiber in a heating furnace, burning for 60min at 480 ℃ for thermal degreasing, soaking in acetone for 1h to dissolve coke, cleaning the surface of the carbon fiber, washing with water for multiple times, and placing in a drying oven for drying for 8 hours at 35 ℃. And then placing the dried carbon fiber in 68 wt% concentrated nitric acid, coarsening for 60min at 90 ℃, and washing with deionized water to be neutral.
Step 2, plating metal copper on the surface of the carbon fiber by adopting an electroplating method
And (3) placing the carbon fiber treated in the step (1) as a cathode and 99.99% of pure copper sheets as an anode in electroplating solution for electroplating. Washing with deionized water for 3 times, and drying in a drying oven at 35 deg.C for 8 hr. The plating bath composition and process parameters are shown in Table 2. It is worth proposing that copper is easy to oxidize, and after the copper electroplating is finished, passivation treatment needs to be carried out in time (namely, carbon fibers plated with copper are placed in 15% of disodium ethylene diamine tetraacetate solution for passivation for 15min), and then washing and drying are carried out.
TABLE 2 electroplating bath composition and Process parameters
Step 3, mixing
Weighing a certain amount of copper powder with the particle size of 60 microns and carbon fiber coated with metal copper, mechanically mixing the copper powder and the carbon fiber in a wine barrel type mixer for 30min, and adding 10mL/kg of alcohol during mixing to accelerate mixing efficiency and avoid dust; wherein, the volume ratio of the copper powder to the carbon fiber coated with the metal copper is as follows: 85:15
Step 4, forming
And (4) putting the mixed material obtained in the step (3) into a steel pressing die for cold press molding, wherein the selected pressing pressure is 300 MPa.
Step 5, hot-pressing sintering
And (3) loading the green body subjected to cold press molding in the step (4) into a three-high graphite (high-strength, high-density and high-conductivity) mold (similar to a steel pressing mold in size and shape). Then slowly heating (the heating rate is 200 ℃/h) in a high-temperature atmosphere protection hot-pressing furnace to the sintering temperature (0.7 time of the melting point of metal copper), simultaneously pressurizing to the pressure of 20MPa, standing at the high temperature for 60min, and then cooling along with the furnace. The protective atmosphere used was argon or nitrogen, and the gas flow was 1L/h.
Step 6, post-treatment
And (5) placing the carbon fiber reinforced metal matrix composite sintered in the step (5) into a solid sand blasting machine for surface treatment, wherein the grain size of the used sand grains is about 0.1mm, and the impact speed is 1 m/s. Removing some attachments attached to the surface and improving the stress state of the surface.
Example 2
A preparation method of a carbon fiber reinforced copper-based composite material comprises the following specific steps:
step 1, surface pretreatment of carbon fibers
Placing the carbon fiber in a heating furnace, burning for 30min at 500 ℃ for thermal degreasing, soaking in acetone for 1h to dissolve coke, cleaning the surface of the carbon fiber, washing with water for multiple times, and placing in a drying oven for drying at 45 ℃ for 6 h. And then placing the dried carbon fiber in 68 wt% concentrated nitric acid, coarsening for 90min at 90 ℃, and washing with deionized water to be neutral.
Step 2, plating metal copper on the surface of the carbon fiber by adopting an electroplating method
And (3) placing the carbon fiber treated in the step (1) as a cathode and 99.99% of pure copper sheets as an anode in electroplating solution for electroplating. Washing with deionized water for 5 times, and drying in a drying oven at 45 deg.C for 8 hr. The plating bath composition and process parameters are shown in Table 3. It is worth proposing that copper is easy to oxidize, and after the copper electroplating is finished, passivation treatment needs to be carried out in time (namely, carbon fibers plated with copper are placed in 15% of disodium ethylene diamine tetraacetate solution for passivation for 15min), and then washing and drying are carried out.
TABLE 3 electroplating bath composition and Process parameters
Step 3, mixing
Weighing a certain amount of copper powder with the particle size of 80 microns and carbon fiber coated with metal copper, mechanically mixing the copper powder and the carbon fiber in a wine barrel type mixer for 80min, and adding 20mL/kg of alcohol during mixing to accelerate mixing efficiency and avoid dust; wherein, the volume ratio of the copper powder to the carbon fiber coated with the metal copper is as follows: 99:1
Step 4, forming
And (4) putting the mixed material obtained in the step (3) into a steel pressing die for cold press molding, wherein the selected pressing pressure is 500 MPa.
Step 5, hot-pressing sintering
And (3) loading the green body subjected to cold press molding in the step (4) into a three-high graphite (high-strength, high-density and high-conductivity) mold (similar to a steel pressing mold in size and shape). Then slowly heating (the heating rate is 300 ℃/h) in a high-temperature atmosphere protection hot-pressing furnace to the sintering temperature (0.8 time of the melting point of the metal copper), simultaneously pressurizing to the pressure of 30MPa, standing at the high temperature for 90min, and then cooling along with the furnace. The protective atmosphere used was argon, the gas flow was 2L/h.
Step 6, post-treatment
And (5) placing the carbon fiber reinforced metal matrix composite sintered in the step (5) into a solid sand blasting machine for surface treatment, wherein the grain size of the used sand grains is about 0.5mm, and the impact speed is 3 m/s. Removing some attachments attached to the surface and improving the stress state of the surface.
Example 3
A preparation method of a carbon fiber reinforced copper-based composite material comprises the following specific steps:
step 1, surface pretreatment of carbon fibers
Placing the carbon fiber in a heating furnace, burning for 40min at 490 ℃ for thermal degreasing, soaking in acetone for 1h to dissolve coke, cleaning the surface of the carbon fiber, washing with water for multiple times, and placing in a drying oven for drying for 7 hours at 40 ℃. And then placing the dried carbon fiber in 68 wt% concentrated nitric acid, coarsening for 65min at 90 ℃, and washing with deionized water to be neutral.
Step 2, plating metal copper on the surface of the carbon fiber by adopting an electroplating method
And (3) placing the carbon fiber treated in the step (1) as a cathode and 99.99% of pure copper sheets as an anode in electroplating solution for electroplating. Washing with deionized water for 4 times, and drying in a drying oven at 40 deg.C for 7 hr. The plating bath composition and process parameters are shown in Table 4. It is worth proposing that copper is easy to oxidize, and after the copper electroplating is finished, passivation treatment needs to be carried out in time (namely, carbon fibers plated with copper are placed in 15% of disodium ethylene diamine tetraacetate solution for passivation for 15min), and then washing and drying are carried out.
TABLE 4 electroplating bath composition and Process parameters
Step 3, mixing
Weighing a certain amount of copper powder with the particle size of 70 microns and carbon fiber coated with metal copper, mechanically mixing for 70min in a wine barrel type mixer, and adding 15mL/kg of alcohol during mixing to accelerate mixing efficiency and avoid dust; wherein, the volume ratio of the copper powder to the carbon fiber coated with the metal copper is as follows: 95:5
Step 4, forming
And (4) putting the mixed material obtained in the step (3) into a steel pressing die for cold press molding, wherein the selected pressing pressure is 400 MPa.
Step 5, hot-pressing sintering
And (3) loading the green body subjected to cold press molding in the step (4) into a three-high graphite (high-strength, high-density and high-conductivity) mold (similar to a steel pressing mold in size and shape). Then slowly heating (the heating rate is 250 ℃/h) in a high-temperature atmosphere protection hot-pressing furnace to the sintering temperature (0.75 time of the melting point of the metal copper), simultaneously pressurizing to 25MPa, staying at the high temperature for 80min, and then cooling along with the furnace. The protective atmosphere used was argon or nitrogen, the gas flow was 1.5L/h.
Step 6, post-treatment
And (5) placing the carbon fiber reinforced metal matrix composite sintered in the step (5) into a solid sand blasting machine for surface treatment, wherein the grain size of the used sand grains is about 0.4mm, and the impact speed is 2.5 m/s. Removing some attachments attached to the surface and improving the stress state of the surface.
Example 4
A preparation method of a carbon fiber reinforced iron-based composite material comprises the following specific steps:
step 1, surface pretreatment of carbon fibers
Placing the carbon fiber in a heating furnace, burning for 30min at 500 ℃ for thermal degreasing, soaking in acetone for 1h to dissolve coke, cleaning the surface of the carbon fiber, washing with water for multiple times, and placing in a drying oven for drying at 45 ℃ for 6 h. And then placing the dried carbon fiber in 68 wt% concentrated nitric acid, coarsening for 90min at 90 ℃, and washing with deionized water to be neutral.
Step 2, plating metallic nickel on the surface of the carbon fiber
And (3) placing the carbon fiber treated in the step (1) as a cathode and 99.99% of pure nickel sheets as an anode in electroplating solution for electroplating, washing and drying. The bath composition and parameters of the electroplated nickel are shown in Table 5.
TABLE 5 plating bath composition and parameters for nickel electroplating
Step 3, mixing
Weighing a certain amount of iron powder with the particle size of 60 microns and carbon fiber coated with metal nickel, mechanically mixing the iron powder and the carbon fiber in a wine barrel type mixer for 30min, and adding 10mL/kg of alcohol during mixing to accelerate the mixing efficiency and avoid dust; wherein, the volume ratio of the iron powder to the carbon fiber coated with the metallic nickel is as follows: 50: 50
Step 4, forming
And (4) putting the mixed material obtained in the step (3) into a steel pressing die for cold press molding, wherein the selected pressing pressure is 300 MPa.
Step 5, hot-pressing sintering
And (3) loading the green body subjected to cold press molding in the step (4) into a three-high graphite (high-strength, high-density and high-conductivity) mold (similar to a steel pressing mold in size and shape). Then slowly heating (the heating rate is 250 ℃/h) in a high-temperature atmosphere protection hot-pressing furnace to the sintering temperature (0.75 time of the melting point of iron), simultaneously pressurizing to 25MPa, staying at the high temperature for 80min, and then cooling along with the furnace. The protective atmosphere used was argon, the gas flow was 1.5L/h.
Step 6, post-treatment
And (5) placing the carbon fiber reinforced metal matrix composite sintered in the step (5) into a solid sand blasting machine for surface treatment, wherein the grain size of the used sand grains is about 0.4mm, and the impact speed is 2.5 m/s. Removing some attachments attached to the surface and improving the stress state of the surface.
Example 5
A preparation method of a carbon fiber reinforced tungsten-based composite material comprises the following specific steps:
step 1, surface pretreatment of carbon fibers
Placing the carbon fiber in a heating furnace, burning for 60min at 480 ℃ for thermal degreasing, soaking in acetone for 1h to dissolve coke, cleaning the surface of the carbon fiber, washing with water for multiple times, and placing in a drying oven for drying for 8 hours at 35 ℃. And then placing the dried carbon fiber in 68 wt% concentrated nitric acid, coarsening for 60min at 90 ℃, and washing with deionized water to be neutral.
Step 2, plating nickel on the surface of the carbon fiber by adopting an electroplating method
And (3) placing the carbon fiber treated in the step (1) as a cathode and 99.99% of pure nickel sheets as an anode in electroplating solution for electroplating. Washing with deionized water for 3 times, and drying in a drying oven at 35 deg.C for 8 hr. The plating bath composition and process parameters are shown in Table 6.
TABLE 6 electroplating bath composition and Process parameters
Step 3, mixing
Weighing a certain amount of tungsten powder with the particle size of 70 microns and carbon fiber coated with metal nickel, mechanically mixing for 50min in a wine barrel type mixer, and adding 15mL/kg of alcohol during mixing to accelerate mixing efficiency and avoid dust; wherein, the volume ratio of the tungsten powder to the carbon fiber coated with the metallic nickel is as follows: 75:25
Step 4, forming
And (4) putting the mixed material obtained in the step (3) into a steel pressing die for cold press molding, wherein the selected pressing pressure is 400 MPa.
Step 5, hot-pressing sintering
And (3) loading the green body subjected to cold press molding in the step (4) into a three-high graphite (high-strength, high-density and high-conductivity) mold (similar to a steel pressing mold in size and shape). Then slowly heating (the heating rate is 300 ℃/h) in a high-temperature atmosphere protection hot-pressing furnace to the sintering temperature (0.8 time of the tungsten melting point), simultaneously pressurizing to the pressure of 20MPa, standing at the high temperature for 90min, and cooling along with the furnace. The protective atmosphere used was argon, and the gas flow was 1L/h.
Step 6, post-treatment
And (5) placing the carbon fiber reinforced metal matrix composite sintered in the step (5) into a solid sand blasting machine for surface treatment, wherein the grain size of the used sand grains is about 0.1mm, and the impact speed is 1 m/s. Removing some attachments attached to the surface and improving the stress state of the surface.
Example 6
A preparation method of a carbon fiber reinforced copper-based composite material comprises the following specific steps:
step 1, surface pretreatment of carbon fibers
Placing the carbon fiber in a heating furnace, burning for 40min at 490 ℃ for thermal degreasing, soaking in acetone for 1h to dissolve coke, cleaning the surface of the carbon fiber, washing with water for multiple times, and placing in a drying oven for drying for 7 hours at 40 ℃. And then placing the dried carbon fiber in 68 wt% concentrated nitric acid, coarsening for 65min at 90 ℃, and washing with deionized water to be neutral.
Step 2, plating nickel on the surface of the carbon fiber by adopting an electroplating method
And (3) placing the carbon fiber treated in the step (1) as a cathode and 99.99% of pure nickel sheets as an anode in electroplating solution for electroplating. Washing with deionized water for 5 times, and drying in a drying oven at 45 deg.C for 8 hr. The plating bath composition and process parameters are shown in Table 7.
TABLE 7 electroplating bath composition and Process parameters
Step 3, mixing
Weighing a certain amount of copper powder with the particle size of 80 microns and carbon fiber coated with metal nickel, mechanically mixing the copper powder and the carbon fiber in a wine barrel type mixer for 80min, and adding 20mL/kg of alcohol during mixing to accelerate mixing efficiency and avoid dust; wherein the volume ratio of the copper powder to the carbon fiber coated with the metal nickel is as follows: 97:3
Step 4, forming
And (4) putting the mixed material obtained in the step (3) into a steel pressing die for cold press molding, wherein the selected pressing pressure is 500 MPa.
Step 5, hot-pressing sintering
And (3) loading the green body subjected to cold press molding in the step (4) into a three-high graphite (high-strength, high-density and high-conductivity) mold (similar to a steel pressing mold in size and shape). Then slowly heating (the heating rate is 200 ℃/h) in a high-temperature atmosphere protection hot-pressing furnace to the sintering temperature (0.7 time of the melting point of copper), simultaneously pressurizing to the pressure of 30MPa, standing at the high temperature for 60min, and then cooling along with the furnace. The protective atmosphere used was argon or nitrogen, the gas flow was 2L/h.
Step 6, post-treatment
And (5) placing the carbon fiber reinforced metal matrix composite sintered in the step (5) into a solid sand blasting machine for surface treatment, wherein the grain size of the used sand grains is about 0.5mm, and the impact speed is 3 m/s. Removing some attachments attached to the surface and improving the stress state of the surface.
Example 7
A preparation method of a carbon fiber reinforced aluminum matrix composite material comprises the following specific steps:
step 1, surface pretreatment of carbon fibers
Placing the carbon fiber in a heating furnace, burning for 30min at 500 ℃ for thermal degreasing, soaking in acetone for 1h to dissolve coke, cleaning the surface of the carbon fiber, washing with water for multiple times, and placing in a drying oven for drying at 45 ℃ for 6 h. And then placing the dried carbon fiber in 68 wt% concentrated nitric acid, coarsening for 90min at 90 ℃, and washing with deionized water to be neutral.
Step 2, plating metal chromium on the surface of the carbon fiber by adopting an electroplating method
And (3) placing the carbon fiber treated in the step (1) as a cathode and 99.99% of pure lead sheets as an anode in electroplating solution for electroplating. Washing with deionized water for 3 times, and drying in a drying oven at 35 deg.C for 8 hr. The plating bath composition and process parameters are shown in Table 8.
TABLE 8 electroplating bath composition and Process parameters
Step 3, mixing
Weighing a certain amount of aluminum powder with the particle size of 60 microns and carbon fiber coated with metal chromium, mechanically mixing the aluminum powder and the carbon fiber in a wine barrel type mixer for 30min, and adding 10mL/kg of alcohol during mixing to accelerate the mixing efficiency and avoid dust; wherein the volume ratio of the aluminum powder to the carbon fiber coated with the metal chromium is as follows: 90:10
Step 4, forming
Putting the mixed material obtained in the step (3) into a steel pressing die for cold press molding, wherein the selected pressing pressure is 300 MPa;
step 5, hot-pressing sintering
And (3) loading the green body subjected to cold press molding in the step (4) into a three-high graphite (high-strength, high-density and high-conductivity) mold (similar to a steel pressing mold in size and shape). Then slowly heating (the heating rate is 200 ℃/h) in a high-temperature atmosphere protection hot-pressing furnace to the sintering temperature (0.7 time of the melting point of aluminum), simultaneously pressurizing to the pressure of 20MPa, standing at the high temperature for 60min, and cooling along with the furnace. The protective atmosphere used was argon or nitrogen, and the gas flow was 1L/h.
Step 6, post-treatment
And (5) placing the carbon fiber reinforced metal matrix composite sintered in the step (5) into a solid sand blasting machine for surface treatment, wherein the grain size of the used sand grains is about 0.1mm, and the impact speed is 1 m/s. Removing some attachments attached to the surface and improving the stress state of the surface.
Example 8
A preparation method of a carbon fiber reinforced aluminum matrix composite material comprises the following specific steps:
step 1, surface pretreatment of carbon fibers
Placing the carbon fiber in a heating furnace, burning for 60min at 480 ℃ for thermal degreasing, soaking in acetone for 1h to dissolve coke, cleaning the surface of the carbon fiber, washing with water for multiple times, and placing in a drying oven for drying for 8 hours at 35 ℃. And then placing the dried carbon fiber in 68 wt% concentrated nitric acid, coarsening for 70min at 90 ℃, and washing with deionized water to be neutral.
Step 2, plating metal chromium on the surface of the carbon fiber by adopting an electroplating method
And (3) placing the carbon fiber treated in the step (1) as a cathode and 99.99% of pure lead sheets as an anode in electroplating solution for electroplating. Washing with deionized water for several times, and drying in a drying oven at 45 deg.C for 8 hr. The plating bath composition and process parameters are shown in Table 9.
TABLE 9 electroplating bath composition and Process parameters
Step 3, mixing
Weighing a certain amount of aluminum powder with the particle size of 80 microns and carbon fiber coated with metal chromium, mechanically mixing in a wine barrel type mixer for 80min, and adding 20mL/kg of alcohol during mixing to accelerate mixing efficiency and avoid dust; wherein the volume ratio of the aluminum powder to the carbon fiber coated with the metal chromium is as follows: 80:20
Step 4, forming
Putting the mixed material obtained in the step (3) into a steel pressing die for cold press molding, wherein the selected pressing pressure is 500 MPa;
step 5, hot-pressing sintering
And (3) loading the green body subjected to cold press molding in the step (4) into a three-high graphite (high-strength, high-density and high-conductivity) mold (similar to a steel pressing mold in size and shape). Then slowly heating (the heating rate is 300 ℃/h) in a high-temperature atmosphere protection hot-pressing furnace to the sintering temperature (0.8 time of the melting point of aluminum), simultaneously pressurizing to 30MPa, standing at the high temperature for 90min, and cooling along with the furnace. The protective atmosphere used was argon or nitrogen, the gas flow was 2L/h.
Step 6, post-treatment
And (5) placing the carbon fiber reinforced metal matrix composite sintered in the step (5) into a solid sand blasting machine for surface treatment, wherein the grain size of the used sand grains is about 0.5mm, and the impact speed is 3 m/s. Removing some attachments attached to the surface and improving the stress state of the surface.
Example 9
A preparation method of a carbon fiber reinforced copper-based composite material comprises the following specific steps:
step 1, surface pretreatment of carbon fibers
Placing the carbon fiber in a heating furnace, burning for 50min at 490 ℃ for thermal degreasing, soaking in acetone for 1h to dissolve coke, cleaning the surface of the carbon fiber, washing with water for multiple times, and placing in a drying oven for drying at 40 ℃ for 7 h. And then placing the dried carbon fiber in 68 wt% concentrated nitric acid, coarsening for 65min at 90 ℃, and washing with deionized water to be neutral.
Step 2, plating metal chromium on the surface of the carbon fiber by adopting an electroplating method
And (3) placing the carbon fiber treated in the step (1) as a cathode and 99.99% of pure lead sheets as an anode in electroplating solution for electroplating. Washing with deionized water for 4 times, and drying in a drying oven at 40 deg.C for 7 hr. The plating bath composition and process parameters are shown in Table 10.
TABLE 10 electroplating bath composition and Process parameters
Step 3, mixing
Weighing a certain amount of copper powder with the particle size of 70 microns and carbon fiber coated with metal chromium, mechanically mixing for 70min in a wine barrel type mixer, and adding 15mL/kg of alcohol during mixing to accelerate mixing efficiency and avoid dust; wherein the volume ratio of the copper powder to the carbon fiber coated with the metal chromium is 82:18
Step 4, forming
Putting the mixed material obtained in the step (3) into a steel pressing die for cold press molding, wherein the selected pressing pressure is 400 MPa;
step 5, hot-pressing sintering
And (3) loading the green body subjected to cold press molding in the step (4) into a three-high graphite (high-strength, high-density and high-conductivity) mold (similar to a steel pressing mold in size and shape). Then slowly heating (the heating rate is 250 ℃/h) in a high-temperature atmosphere protection hot-pressing furnace to the sintering temperature (0.75 time of the melting point of copper), simultaneously pressurizing to 25MPa, staying at the high temperature for 80min, and then cooling along with the furnace. The protective atmosphere used was argon or nitrogen, the gas flow was 1.5L/h.
Step 6, post-treatment
And (5) placing the carbon fiber reinforced metal matrix composite sintered in the step (5) into a solid sand blasting machine for surface treatment, wherein the grain size of the used sand grains is about 0.4mm, and the impact speed is 2.5 m/s. Removing some attachments attached to the surface and improving the stress state of the surface.
The invention has the advantages that:
(1) the mechanical property and the physical property of the composite material can be greatly improved by pre-coating metal on the surface of the carbon fiber and then mixing, hot-pressing and sintering;
(2) the method for preparing the carbon fiber reinforced metal matrix composite material has the advantages of simple operation, low energy consumption, low cost, high production efficiency and easy industrial production.
Claims (8)
1. The preparation method of the carbon fiber reinforced metal matrix composite is characterized by comprising the following specific steps of:
step 1, pretreating the surface of carbon fiber;
the pretreatment process of the carbon fiber surface in the step 1 is as follows: placing carbon fibers in a heating furnace, firing for 30-60 min at 480-500 ℃ for thermal degreasing, soaking in acetone for 1h, washing with water, placing in a drying oven for drying for 6-8 h at 35-45 ℃, placing the dried carbon fibers in 68 wt% concentrated nitric acid, coarsening for 60-90 min at 90 ℃, and washing with deionized water to be neutral;
step 2, plating metal copper, nickel or chromium on the surface of the carbon fiber by adopting an electroplating method;
step 3, weighing a certain amount of metal powder and carbon fiber coated with metal copper, nickel or chromium, and mechanically mixing in a wine barrel type mixer for 30-80 min;
step 4, putting the mixed material obtained in the step 3 into a steel pressing die for cold press molding, wherein the selected pressing pressure is 300-500 MPa;
step 5, the green body formed by cold pressing in the step 4 is arranged in a three-high graphite die for hot pressing and sintering;
in step 5, the hot-pressing sintering process comprises the following steps: slowly heating to 0.7-0.8 times of the melting point of the metal in a high-temperature atmosphere protection hot-pressing furnace, simultaneously pressurizing to 20-30 MPa, standing for 60-90 min, and cooling along with the furnace, wherein the used protective atmosphere is argon or nitrogen, and the gas flow is 1-2L/h;
and 6, placing the composite material sintered in the step 5 into a solid sand blasting machine for surface treatment to obtain the carbon fiber reinforced metal matrix composite material.
2. The method for preparing a carbon fiber reinforced metal matrix composite material according to claim 1, wherein in the step 2, the specific process of plating the metal copper, nickel or chromium on the surface of the carbon fiber by using an electroplating method is as follows: taking the carbon fiber treated in the step 1 as a cathode, taking a nickel sheet, a copper sheet or a lead sheet as an anode, placing the anode in an electroplating solution for electroplating, then washing the anode for 3-5 times, and placing the anode in a drying oven for drying for 6-8 hours at the temperature of 35-45 ℃; after the surface of the carbon fiber is plated with the metal copper, passivation treatment is needed.
3. The method for preparing a carbon fiber reinforced metal matrix composite material as recited in claim 2, wherein in the step 2, the plating solution for plating the metal copper on the surface of the carbon fiber comprises the following components: 30-50 g/L of copper sulfate, 10-25 g/L of sodium tartrate, 60-90 g/L of sodium citrate and 8-12 g/L of potassium nitrate, wherein the electroplating process conditions are as follows: electroplating temperature: 25-45 ℃, current density: 1.0E3.5A/dm2And electroplating time: 20-40 min.
4. The method for preparing a carbon fiber reinforced metal matrix composite material as recited in claim 2, wherein in the step 2, the plating solution for plating the metal nickel on the surface of the carbon fiber comprises the following components: 200-270 g/L of nickel sulfate, 60-70 g/L of nickel chloride, 32-40 g/L of boric acid and 0.01-0.1 g/L of sodium dodecyl sulfate, wherein the electroplating process conditions are as follows: electroplating temperature: 25-40 ℃, current density: 0.1 to 0.5A/dm2And electroplating time: 4-20 min.
5. The method for preparing a carbon fiber reinforced metal matrix composite material as recited in claim 2, wherein in the step 2, the plating solution for plating metal chromium on the surface of the carbon fiber comprises the following components: 230-250 g/L of chromic anhydride, 1.25-5 mL/L of concentrated sulfuric acid and 5-10 g/L of boric acid, wherein the electroplating process conditions are as follows: electroplating temperature: and (3) electroplating time at 40-60 ℃: 10-30 min, current density: 24 to 30A/dm2。
6. The method for preparing a carbon fiber reinforced metal matrix composite material according to claim 1, wherein in the step 3, the volume of the carbon fiber coated with the metal copper, nickel or chromium accounts for 1-50% of the total volume of the mixture.
7. The method for preparing a carbon fiber reinforced metal matrix composite according to claim 1, wherein the metal powder in step 3 is copper powder, iron powder, aluminum powder or tungsten powder.
8. The method for preparing a carbon fiber reinforced metal matrix composite material according to claim 1, wherein in the step 6, the sand grain used has a grain size of 0.1-0.5 mm and an impact velocity of 1-3 m/s.
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| CN110343977B (en) * | 2019-07-22 | 2021-03-30 | 陕西理工大学 | Preparation method of continuous carbon fiber reinforced aluminum matrix composite |
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