CN108517435B - Nano-carbon reinforced copper-based composite material for maglev train and preparation method thereof - Google Patents

Nano-carbon reinforced copper-based composite material for maglev train and preparation method thereof Download PDF

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CN108517435B
CN108517435B CN201810488620.2A CN201810488620A CN108517435B CN 108517435 B CN108517435 B CN 108517435B CN 201810488620 A CN201810488620 A CN 201810488620A CN 108517435 B CN108517435 B CN 108517435B
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copper
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CN108517435A (en
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蒋小松
舒锐
蒋佳芯
孙大明
邵甄胰
朱德贵
朱旻昊
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Southwest Jiaotong University
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    • C22C9/00—Alloys based on copper
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
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    • C22C9/00—Alloys based on copper
    • C22C9/02—Alloys based on copper with tin as the next major constituent
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    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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Abstract

The invention discloses a nano-carbon reinforced copper-based composite material, which is characterized in that: 0.1-5% of carbon nano tube subjected to surface modification, 0.1-5% of graphene subjected to surface modification, 2-10% of graphite powder, 1-4% of chromium powder, 1-8% of lead powder, 2-10% of tin powder, 0.1-1% of zirconium powder, 0.01-0.5% of lanthanum powder and the balance of copper powder; the surface-modified carbon nanotube is obtained by modifying the carbon nanotube with a gallic acid aqueous solution, and the surface-modified graphene is obtained by modifying graphene with a rutin aqueous solution. The copper-based composite material disclosed by the invention is low in impurity content, the structural integrity of the added reinforcing phase component is kept, a plurality of added components can play a role in co-reinforcement, and the strength, hardness and current-carrying frictional wear performance of the copper-based composite material are obviously improved. In addition, the invention also discloses a preparation method of the copper-based composite material, and the method has the advantages of simple process, easy production and wide application prospect.

Description

Nano-carbon reinforced copper-based composite material for maglev train and preparation method thereof
Technical Field
The invention relates to a copper-based composite material, in particular to a nanocarbon reinforced copper-based composite material and a preparation method thereof, belonging to the technical field of preparation of composite materials.
Background
Since the carbon nano tube and the graphene are respectively found, the carbon nano tube is researched by broad scholars, has excellent optical, thermal, electrical and mechanical properties due to the unique structure, and has the excellent characteristics of extremely high mechanical strength, ideal elasticity, low thermal expansion coefficient, small size and the like; graphene has high strength, large specific surface area and good elongation. Carbon nanotubes and graphene are ideal materials as the reinforcing phase of the composite material.
Carbon nanotubes and graphene are widely used as reinforcing phases for composites, and rapid development has been made in polymer-based composites. Among metal matrix composite materials, copper matrix composite materials are widely used as electronic materials, slider materials, contact materials, heat exchange materials, and the like, because of their excellent electrical and thermal conductivity. Therefore, nanocarbon has been attracting attention in reinforcing copper-based composite materials.
However, carbon nanotubes and graphene also present many difficulties in their application in reinforcing metal matrix composites. On one hand, since the carbon nanotubes and the graphene are all nano materials, the carbon nanotubes and the graphene have extremely large specific surface area and specific surface energy, and have large van der waals force, are easy to agglomerate and entangle, and are difficult to uniformly disperse in a metal matrix. On the other hand, the surface activity of the carbon nanotubes and graphene is low, and the wettability with the metal matrix is poor, so that the interface bonding strength between the carbon nanotubes and graphene and the metal matrix is poor. These factors seriously affect the mechanical, electrical, frictional and wear properties of the metal matrix composite.
In order to solve the above problems, a great deal of research has been carried out on chemical plating and molecular level mixing methods, but these methods have complex processes and high energy consumption, and the structures of carbon nanotubes and graphene are damaged to some extent during the pretreatment process, which will weaken the enhancement effect.
The carbon nano tube and the graphene are ideal reinforcing materials, but the reinforcing mechanisms of the one-dimensional carbon nano tube and the two-dimensional graphene are different, and the two carbon nano tube and the two graphene are mixed to be used as a reinforcing phase, so that the advantages of the two carbon nano tubes and the two graphene can be combined, and the reinforcing effect on the copper-based composite material is improved.
ChinaPatent application 201410354188.x discloses a carbon nanotube reinforced copper-based composite material and a preparation method thereof, wherein a gallic acid aqueous solution is firstly adopted to modify carbon nanotubes, and then the carbon nanotubes, copper powder, graphite powder and Ti are mixed3SiC2Ball milling the powder, and hot pressing and sintering to obtain the carbon nano tube reinforced copper-based composite material. However, the pressure loading direction is unidirectional during hot-pressing sintering, so that the copper-based composite material has certain anisotropy, and the performance of the copper-based composite material is different in different directions.
Chinese patent application 201510537320.5 discloses a method for preparing graphene reinforced copper-based composite material, which comprises the steps of firstly preparing graphene oxide, carrying out surface modification, then preparing graphene oxide-copper composite powder, and finally carrying out hot-pressing sintering to obtain the copper-based composite material. However, the pressure loading direction is unidirectional during hot-pressing sintering, so that the copper-based composite material has certain anisotropy, and the reinforcing effect of single graphene as a reinforcing material is single compared with that of the copper-based composite material.
Disclosure of Invention
The invention aims to solve the problem that in the prior art, carbon nanotubes and graphene are difficult to be fully matched with a matrix material to fully exert the reinforcing effect when applied to the composite material, and provides a nanocarbon reinforced copper-based composite material.
The reinforced copper-based composite material provided by the invention fully exerts the reinforcing effect of various raw material components, improves the strength and current-carrying frictional wear of the composite material, enables the copper-based composite material to realize better comprehensive performance, and further meets the requirements of different application conditions.
In order to achieve the above purpose, the invention provides the following technical scheme:
a nano-carbon reinforced copper-based composite material comprises the following components in percentage by weight:
0.1-5% of carbon nano tube subjected to surface modification, 0.1-5% of graphene subjected to surface modification, 2-10% of graphite powder, 1-4% of chromium powder, 1-8% of lead powder, 2-10% of tin powder, 0.1-1% of zirconium powder, 0.01-0.5% of lanthanum powder and the balance of copper powder.
Wherein the carbon nano tube subjected to surface modification is a carbon nano tube modified by gallic acid solution.
The graphene subjected to surface modification is graphene modified by a rutin solution.
The copper-based composite material disclosed by the invention combines two carbon nano materials as a nano reinforcing phase, and is designed by matching with graphite powder and various metal powder raw materials to obtain a novel copper-based alloy and nano carbon material composite reinforcing material. Through modification optimization, the carbon nano tube and graphene have good dispersibility, and can well play a role in reinforcing when being added and applied to a composite material, and then the overall raw material composition matching proportion design of the composite reinforced material is greatly optimized and adjusted, so that the comprehensive performance of the material is optimal, the effect of extremely low current-carrying wear can be realized, and the composite reinforced material can be better applied to the manufacture of special current-carrying friction workpieces.
Through extensive experimental research of the inventor, the performance of each component can generate a co-reinforcing effect when the weight percentage of each component in the copper-based composite material is the ratio. On one hand, the carbon nano tube, the graphene and the copper matrix form better interface combination, and the enhancement effect is obviously improved; on the other hand, the graphite self-lubricating effect is fully exerted, the current-carrying frictional wear mechanism of copper is changed, and the adhesive wear of pure copper is converted into the abrasive wear of the composite material; in addition, the carbon film can be formed between the friction pairs by adjusting and controlling the dosage proportion of the carbon nano tubes, the graphene and the graphite powder, so that the antifriction effect is achieved. And the addition proportions of other components, namely chromium powder, lead powder, tin powder, zirconium powder and lanthanum powder are optimized, so that on one hand, a solid solution can be formed with a copper matrix to realize a solid solution strengthening effect, on the other hand, the grain size of the copper matrix can be adjusted/reduced to play a fine grain strengthening effect, the wear consumption mechanism of the copper-based composite material between friction pairs is optimized, and the wear speed is obviously reduced.
Further, the carbon nano tube subjected to surface modification is a carbon nano tube modified by a gallic acid solution, the mass ratio of the carbon nano tube to the gallic acid is 1:0.5-8, and the gallic acid is calculated by the mass of the gallic acid dissolved in the gallic acid solution. Preferably, the mass ratio of the carbon nanotubes to the gallic acid is 1:2-6, and the proper mass ratio of the gallic acid ensures that the total amount of the gallic acid adsorbed on the carbon nanotubes is proper in the modification process, so that the dispersion effect and the performance reduction influence are balanced mutually.
Gallic acid, also called gallic acid, has chemical formula C6H2(OH)3COOH, belonging to the polyphenols. Hydroxyl groups connected to benzene rings in the gallic acid have extremely strong activity, are combined with the surfaces of the carbon nanotubes, and modify the surfaces of the carbon nanotubes; gallic acid can also be adsorbed to the surface of the carbon nanotubes by non-chemical action. The interaction of the two components not only helps to improve the dispersibility of the carbon nano tube, but also does not produce shearing action on the carbon nano tube to cause chemical damage.
Preferably, the gallic acid solution is a 1% to 100% saturated gallic acid solution.
Preferably, the gallic acid solution is an aqueous solution of gallic acid.
The gallic acid is dissolved in the solution in advance, and then the gallic acid and the carbon nano tube are mutually attracted to carry out uniform adsorption modification, so that the carbon nano tube is more fully modified, and the dispersion effect is better. The 1% -100% is calculated by taking the saturated solution of the gallic acid solution as 100% concentration, and the concentration of 1% is diluted by 100 times relative to the saturated solution of the gallic acid solution.
Preferably, the gallic acid solution is a 20% to 100% concentration gallic acid solution. The gallic acid solution with proper concentration is selected, and the higher solution concentration is favorable for the interaction of the gallic acid in the solution and the carbon nano tube to realize modification.
Preferably, the volume ratio of the mass of the carbon nano tube to the gallic acid aqueous solution is 0.05-0.4 g: 20-80 mL, preferably 0.05-0.2 g: 30-50 mL; more preferably, the ratio of the mass of the carbon nanotubes to the volume of the aqueous solution of gallic acid is 0.1g:40 mL. The concentration of the gallic acid aqueous solution is 0.3-1.15g/100 mL.
Further, the graphene subjected to surface modification is graphene modified by a rutin solution, and the mass ratio of the graphene to the rutin is 1: 0.5-8. Rutin is calculated by the mass of rutin dissolved in the solution. The proper amount of rutin forms proper modification strength on the graphene.
Rutin, also known as rutin, vitamin P, is a typical representative of flavonols. Due to the existence of the aromatic structure, rutin can generate pi-pi conjugated interaction with the surface of graphene, and is adsorbed on the surface of the graphene, and active groups are grafted on the surface of the graphene, so that the dispersion performance is improved; on the other hand, phenolic hydroxyl groups of rutin can interact with defect sites on the surface of graphene so as to modify the surface of the graphene, and meanwhile, more active groups and biological functional macromolecules can be grafted on the surface due to the existence of active groups such as hydroxyl groups. The combined action of the two aspects is more beneficial to improving the dispersion performance of the graphene, and the complete structure of the graphene is not damaged.
Preferably, the rutin solution is a rutin aqueous solution.
Preferably, the rutin solution is 1% -100% saturated rutin solution. The concentration of the rutin solution is relative to the 100% saturated rutin solution. Preferably, the rutin solution is 20% -100% saturated rutin solution.
Further, the volume ratio of the mass of the graphene to the volume of the rutin aqueous solution is 0.05-0.4 g: 20-80 mL. Preferably 0.05-0.2 g: 30-50 mL. The concentration of the rutin aqueous solution is 0.3-1.2g/100 mL. More preferably, the volume ratio of the mass of the graphene to the volume of the rutin aqueous solution is 0.1g to 40 mL.
The carbon nano tube subjected to surface modification has the characteristics of good dispersity and low impurity content of the carbon nano tube and the graphene subjected to surface modification, and the complete structure is maintained.
Further, the carbon nanotube subjected to surface modification is a carbon nanotube modified by a gallic acid solution, and the graphene subjected to surface modification is graphene modified by a rutin solution.
The modification process is as follows: and putting the carbon nano tube into a gallic acid solution, performing ultrasonic dispersion, standing, filtering and drying to obtain the modified carbon nano tube.
And putting the graphene into a rutin solution, performing ultrasonic dispersion, standing, filtering and drying to obtain the modified graphene.
Preferably, the ultrasonic dispersion time is 20-40 min, the standing time is 12-36 h, the vacuum drying temperature is 60-80 ℃, and the vacuum drying time is 1-8 h.
Preferably, the ultrasonic dispersion time is 20-30 min, the standing time is 18-30 h, the vacuum drying temperature is 60-70 ℃, and the vacuum drying time is 1-4 h.
Preferably, the ultrasonic dispersion time is 30min, the standing time is 24h, the vacuum drying temperature is 60 ℃, and the vacuum drying time is 2 h.
In the modification method of the carbon nano tube and the graphene, a brand-new modification method integrating physical adsorption and chemical adsorption is adopted, so that the method is efficient and reliable, does not generate pollutants such as wastewater, waste acid and the like, and is simple in process, easy to produce and stable and reliable in modification effect.
Further, the nanocarbon reinforced copper-based composite material comprises the following components in percentage by weight: 0.1-2% of carbon nano tube subjected to surface modification, 0.1-2% of graphene subjected to surface modification, 5-8% of graphite powder, 1-3% of chromium powder, 2-5% of lead powder, 5-8% of tin powder, 0.2-0.6% of zirconium powder, 0.01-0.2% of lanthanum powder and the balance of copper powder.
Further, the nanocarbon reinforced copper-based composite material comprises the following components in percentage by weight: 0.4-1.0% of carbon nano tube subjected to surface modification, 0.2-0.4% of graphene subjected to surface modification, 6-7% of graphite powder, 1.5-2.5% of chromium powder, 3.5-4.5% of lead powder, 6-7% of tin powder, 0.3-0.5% of zirconium powder, 0.05-0.13% of lanthanum powder and the balance of copper powder.
Further, the nanocarbon reinforced copper-based composite material comprises the following components in percentage by weight: 0.8% of carbon nano tube subjected to surface modification, 0.2% of graphene subjected to surface modification, 6.5% of graphite powder, 2% of chromium powder, 4% of lead powder, 6% of tin powder, 0.4% of zirconium powder, 0.1% of lanthanum powder and the balance of copper powder.
The invention also aims to provide a method for preparing the reinforced copper-based composite material, which ensures that the performance of the copper-based composite material obtained by matching various raw material components can better reach the expected design level by optimally designing the preparation method of the copper-based composite material, and meets the design and application requirements.
A preparation method of a copper-based composite material comprises the following steps:
(1) adding carbon nanotubes into a gallic acid aqueous solution, performing ultrasonic dispersion, standing, filtering, and vacuum drying filter residue to obtain surface-modified carbon nanotubes;
adding graphene into a rutin aqueous solution, performing ultrasonic dispersion, standing, filtering, and vacuum-drying filter residues to obtain surface-modified graphene;
(3) mixing the surface-modified carbon nano tube, the surface-modified graphene, copper powder, graphite powder, chromium powder, lead powder, tin powder, zirconium powder and lanthanum powder, and performing ball milling to obtain composite powder;
(4) carrying out cold press molding on the composite powder to obtain a composite material pressed compact;
(5) and carrying out hot isostatic pressing sintering on the composite material pressed compact, and cooling to obtain the nano-carbon reinforced copper-based composite material.
According to the method for preparing the copper-based composite material, the carbon nano tube and the graphene are firstly subjected to corresponding modification treatment to be converted into the carbon nano material with good dispersibility, then the carbon nano material and other raw materials are mixed and ball-milled to enable various raw material components to fully act to form a mixed material, and finally the composite powder is subjected to cold press molding and hot isostatic pressing sintering to obtain the nano carbon reinforced copper-based composite material. The whole preparation method is simple and easy to implement, strong in pertinence, high in pretreatment conversion efficiency of the nano carbon material, fully and uniformly dispersed in the ball milling of the mixed material, the enhancement effect of the carbon nano material is embodied and exerted to the maximum extent, the overall property performance of the composite material finally reaches the design expectation, the mechanical strength is higher, and the comprehensive wear resistance is more excellent.
Further, agate balls and agate ball tanks are adopted for ball milling in the step (3), the ball milling rotating speed is 200-450 r/min, and the ball milling time is 40-120 min.
Preferably, the ball mill in the step (3) adopts agate balls and agate ball tanks, the ball milling rotating speed is 300-400 r/min, and the ball milling time is 40-90 min. The ball milling rotating speed and the ball milling time are optimally adjusted, the ball milling mixing effect is better realized, the mixing uniformity of various raw materials is ensured, the stability of the raw material components is better, and the quality of the final sintered composite material is improved. More preferably, the ball milling in the step (3) adopts agate balls and agate ball tanks, the ball milling speed is 350 r/min, and the ball milling time is 60 min.
Further, the pressure of the cold press molding and pressing in the step (4) is 400-700 MPa.
According to the multiple experimental researches of the inventor, the cold press molding pressure reaches the range, so that the compact pressing of the composite powder raw material can be ensured, and the integrally sintered material has good compactness and high mechanical strength. Preferably, the pressure of the cold press molding in the step (4) is 500-600 MPa.
More preferably, the pressure of the cold press molding in the step (4) is 600 MPa.
Further, the hot isostatic pressing sintering temperature in the step (5) is 800-1000 ℃, the hot isostatic pressing sintering pressure is 80-100 MPa, and the hot isostatic pressing sintering time is 1-3 h. Through a plurality of experimental researches of the inventor, the sintering temperature, pressure and time parameters are adopted in the hot isostatic pressing sintering process, the final forming effect of the composite material is most favorably realized, and the density and the cohesion of the sintered composite material are optimal.
Preferably, the hot isostatic pressing sintering temperature in the step (5) is 850-950 ℃, the hot isostatic pressing sintering pressure is 90-100 MPa, and the hot isostatic pressing sintering time is 1-2 h. According to the invention, the hot isostatic pressing sintering temperature, pressure and time parameters are preferably selected, the reinforcing phase and the matrix in the sintered composite material are uniformly distributed in a staggered manner, elements are diffused mutually, and the effect of the reinforcing phase is improved. More preferably, the temperature of the hot isostatic pressing sintering in the step (5) is 900 ℃, the pressure of the hot isostatic pressing sintering is 100MPa, and the time of the hot isostatic pressing sintering is 2 h.
The new technical scheme provided by the invention can mainly realize the following technical effects:
1. the components of the nano-carbon reinforced copper-based composite material are subjected to long-term research and iteration by the inventor, and a brand new optimized component application and matching proportion relation are provided, so that the mechanical strength, the wear resistance, the current-carrying wear and other properties of the copper-based composite material are comprehensively optimized, and the application requirements of a conductive member of a magnetic suspension train are met.
2. The preparation raw material components of the copper-based composite material are subjected to brand-new optimal design and adjustment of mutual correlation of the content proportions of the components, so that the raw material components of the copper-based composite material can generate a synergistic cooperation and co-reinforcement effect, the metallographic phase of a metal material matrix in the copper-based composite material is changed, a brand-new alloy base phase is formed, the reinforcement effect of nano carbon is matched, the strength, current-carrying friction and wear and other properties of the copper-based composite material are obviously improved, and the density of the copper-based composite material is reduced.
3. In the nano-carbon reinforced copper-based composite material, the carbon nano-tube and the graphene are respectively subjected to surface modification, compared with the unmodified carbon nano-material, the nano-carbon reinforced copper-based composite material has better dispersibility and lower impurity content, keeps the structural integrity of the carbon nano-tube and the graphene, has good reinforcing effect when being applied to the composite material, and fully exerts the performance advantage characteristics of the nano-material.
4. The invention provides a preparation method of a copper-based composite material, which is matched with the formulation composition and the matching proportion of a brand-new optimized design, adopts a hot isostatic pressing process for sintering and forming, fully exerts the enhancement effect of the raw material component formulation on the performance of the copper-based composite material, controls the pressure in each direction to be equal in the sintering process, obtains the copper-based composite material with a uniform and compact structure, and effectively exerts the comprehensive performance advantages of a new material.
Description of the drawings:
FIG. 1 is an SEM image (magnification ×. 3000) of the composite powder after ball milling.
Fig. 2 is the BSE plot (x 1000 times) of the nanocarbon reinforced copper-based composite.
Fig. 3 is EDS results of nanocarbon reinforced copper-based composite matrix.
Fig. 4 is an SEM image (x 80000 times) of a compression fracture of the nanocarbon reinforced copper-based composite material.
Fig. 5 is an SEM image (x 20000 times) of shear fracture of the nanocarbon-reinforced copper-based composite material.
Detailed Description
The present invention will be described in further detail with reference to test examples and specific embodiments. It should be understood that the scope of the above-described subject matter is not limited to the following examples, and any techniques implemented based on the disclosure of the present invention are within the scope of the present invention. The carbon nanotubes and graphene involved in the examples of the present invention were purchased from the department of chemical delivery, organic chemistry, ltd, china academy of sciences.
< example 1>
Modified carbon nanotube
Adding carbon nanotubes into 10 μ g/mL gallic acid aqueous solution, and ultrasonically dispersing for 30min, wherein the ratio of the weight of the carbon nanotubes to the volume of the gallic acid aqueous solution is 0.1g:40 mL; standing for 24h, filtering, removing filter residue, and vacuum drying at 60 deg.C for 2h to obtain surface modified carbon nanotube.
By comparing the morphological characteristics of the carbon nanotubes with or without surface modification, the carbon nanotubes with or without surface modification are found to be flocculent or bundled and have poor dispersibility; the surface of the carbon nano tube after surface modification is smooth, a plurality of single carbon nano tubes can be observed, and the length-diameter ratio is not greatly changed.
0.1g of the surface-treated carbon nanotubes prepared in example 1 was uniformly dispersed in 100mL of deionized water, and after standing for 5 days, the deposition was gradually increased under the action of gravity, but the carbon nanotubes were still dispersed; meanwhile, carbon nanotubes which are not subjected to surface modification are used for comparison, and precipitation and agglomeration occur after standing for 1 day. It is shown that the surface-modified carbon nanotubes prepared in example 1 have excellent dispersibility.
< example 2>
Modified carbon nanotube
Surface-modified carbon nanotubes were obtained according to the method of example 1, except that the concentration of the aqueous solution of gallic acid was changed to 5. mu.g/mL or 15. mu.g/mL, and the same procedure as in example 1 was repeated.
0.1g of the carbon nanotubes prepared in example 2 and surface-treated with aqueous solutions of gallic acid at concentrations of 5. mu.g/mL and 15. mu.g/mL, respectively, was uniformly dispersed in 100mL of deionized water, and after standing for 2 to 3 days, the carbon nanotubes gradually precipitated under the action of gravity, but remained dispersed.
Combining the results of example 1 and example 2, the carbon nanotubes surface-modified with the aqueous solution of gallic acid have good dispersibility and reduced impurity content; and the surface modification effect is best when the concentration of the gallic acid aqueous solution is 10 μ g/mL.
< example 3>
Modified graphene
Adding graphene into 0.02 mu g/mL rutin aqueous solution, and performing ultrasonic dispersion for 30min, wherein the ratio of the weight of the graphene to the volume of the rutin aqueous solution is 0.1g:40 mL; standing for 24h, filtering, removing filter residues, and drying in vacuum at 60 ℃ for 2h to obtain the graphene subjected to surface modification.
By comparing SEM images of surface-modified graphene and graphene which is not subjected to surface modification, the graphene which is not subjected to surface modification is found to be flocculent or fasciculate, and the dispersibility is poor; the surface modified graphene is smooth in surface, so that a plurality of single graphene can be observed, and the size change is not large.
Uniformly dispersing 0.1g of the graphene subjected to surface treatment and prepared in the embodiment 3 in 100mL of deionized water, standing for 5 days, and gradually increasing the deposition under the action of gravity, wherein the graphene still keeps a dispersed state; meanwhile, graphene which is not subjected to surface modification is used for comparison, and precipitation and agglomeration occur after standing for 1 day. It is shown that the surface-modified graphene prepared in example 3 has excellent dispersibility.
< example 4>
Modified graphene
Surface-modified carbon nanotubes were obtained according to the method of example 3, except that the concentration of the aqueous solution of gallic acid was changed to 0.01. mu.g/mL or 0.04. mu.g/mL, and the same procedure as in example 3 was repeated.
0.1g of the carbon nanotubes prepared in example 4 and surface-treated with gallic acid aqueous solutions of 0.01. mu.g/mL and 0.04. mu.g/mL, respectively, were uniformly dispersed in 100mL of deionized water, and after standing for 2 to 3 days, the amount of the carbon nanotubes precipitated by gravity gradually increased, but the carbon nanotubes remained dispersed.
Combining the results of example 3 and example 4, the carbon nanotubes surface-modified with the aqueous solution of gallic acid have good dispersibility and reduced impurity content; and the surface modification effect is best when the concentration of the gallic acid aqueous solution is 0.02. mu.g/mL.
< example 5>
Copper-based composite material
(1) Taking the carbon nano tube subjected to surface modification in the embodiment 1; (2) according to parts by weight, 1 part of carbon nano tube subjected to surface modification, 6.5 parts of graphite powder, 2 parts of chromium powder, 4 parts of lead powder, 6 parts of tin powder, 0.4 part of zirconium powder, 0.1 part of lanthanum powder and 80 parts of copper powder are subjected to ball milling and powder mixing by adopting agate balls and an agate ball tank, wherein the rotating speed is 350 revolutions per minute, and the ball milling time is 50 minutes; (3) carrying out cold press molding on the composite powder at the pressure of 600 MPa; (4) and carrying out hot isostatic pressing on the obtained bulk material for 2h, wherein the hot isostatic pressing sintering temperature is 900 ℃, the pressure is 100MPa, and carrying out rapid cooling to obtain the nanocarbon reinforced copper-based composite material.
< example 6>
Copper-based composite material
Taking the surface-modified graphene in example 3; (2) according to parts by weight, 1 part of graphene subjected to surface modification, 6.5 parts of graphite powder, 2 parts of chromium powder, 4 parts of lead powder, 6 parts of tin powder, 0.4 part of zirconium powder, 0.1 part of lanthanum powder and 80 parts of copper powder are subjected to ball milling and powder mixing by adopting agate balls and an agate ball tank, wherein the rotating speed is 300 revolutions per minute, and the ball milling time is 60 minutes; (3) carrying out cold press molding on the composite powder at the pressure of 600 MPa; (4) and carrying out hot isostatic pressing on the obtained bulk material for 2h, wherein the hot isostatic pressing sintering temperature is 900 ℃, the pressure is 90MPa, and carrying out rapid cooling to obtain the nanocarbon reinforced copper-based composite material.
< example 7>
Copper-based composite material
Taking the surface-modified carbon nanotube in example 1 and taking the surface-modified graphene in example 3; (2) according to parts by weight, performing ball milling and powder mixing on 0.5 part of carbon nano tube subjected to surface modification, 0.5 part of graphene subjected to surface modification, 6.5 parts of graphite powder, 2 parts of chromium powder, 4 parts of lead powder, 6 parts of tin powder, 0.4 part of zirconium powder, 0.1 part of lanthanum powder and 80 parts of copper powder by using agate balls and an agate ball tank, wherein the rotating speed is 350 revolutions per minute, and the ball milling time is 60 minutes; (3) carrying out cold press molding on the composite powder at the pressure of 600 MPa; (4) and carrying out hot isostatic pressing on the obtained bulk material for 2h, wherein the hot isostatic pressing sintering temperature is 900 ℃, the pressure is 100MPa, and carrying out rapid cooling to obtain the nanocarbon reinforced copper-based composite material.
< example 8>
Copper-based composite material
Taking the surface-modified carbon nanotube in example 1 and taking the surface-modified graphene in example 3; (2) according to parts by weight, performing ball milling and powder mixing on 0.8 part of carbon nano tube subjected to surface modification, 0.1 part of graphene subjected to surface modification, 6.5 parts of graphite powder, 2 parts of chromium powder, 4 parts of lead powder, 6 parts of tin powder, 0.4 part of zirconium powder, 0.1 part of lanthanum powder and 80 parts of copper powder by using agate balls and an agate ball tank, wherein the rotating speed is 350 revolutions per minute, and the ball milling time is 60 minutes; (3) carrying out cold press molding on the composite powder at the pressure of 600 MPa; (4) and carrying out hot isostatic pressing on the obtained bulk material for 2h, wherein the hot isostatic pressing sintering temperature is 900 ℃, the pressure is 100MPa, and carrying out rapid cooling to obtain the nanocarbon reinforced copper-based composite material.
< comparative example 1>
Copper-based composite material
(1) According to parts by weight, 7.5 parts of graphite powder, 2 parts of chromium powder, 4 parts of lead powder, 6 parts of tin powder, 0.4 part of zirconium powder, 0.1 part of lanthanum powder and 80 parts of copper powder are subjected to ball milling and powder mixing by adopting agate balls and agate ball tanks, wherein the rotating speed is 350 revolutions per minute, and the ball milling time is 60 minutes; (2) carrying out cold press molding on the composite powder at the pressure of 600 MPa; (3) and carrying out hot isostatic pressing on the obtained bulk material for 2h, wherein the hot isostatic pressing sintering temperature is 900 ℃, the pressure is 100MPa, and carrying out rapid cooling to obtain the copper-based composite material.
< comparative example 2>
Copper-based composite material
(1) Mixing 2 parts by weight of the modified carbon nanotube prepared in example 1, 0.5 part by weight of the modified graphene prepared in example 3, 5 parts by weight of graphite powder, 3 parts by weight of chromium powder, 3.5 parts by weight of lead powder, 4 parts by weight of tin powder, 0.2 part by weight of lanthanum powder and 81.8 parts by weight of copper powder, and performing ball milling and powder mixing by using agate balls and agate ball tanks at the rotating speed of 350 revolutions per minute for 60 minutes; (2) carrying out cold press molding on the composite powder at the pressure of 600 MPa; (3) and carrying out hot isostatic pressing on the obtained bulk material for 2h, wherein the hot isostatic pressing sintering temperature is 900 ℃, the pressure is 100MPa, and carrying out rapid cooling to obtain the copper-based composite material.
< comparative example 3>
Copper-based composite material
(1) Ball-milling and mixing 2 parts by weight of the modified carbon nanotube prepared in example 1, 0.5 part by weight of the modified graphene prepared in example 3, 5 parts by weight of graphite powder, 4 parts by weight of lead powder, 6 parts by weight of tin powder, 0.4 part by weight of zirconium powder, 0.1 part by weight of lanthanum powder and 82 parts by weight of copper powder by using agate balls and an agate ball jar at the rotating speed of 350 revolutions per minute for 60 minutes; (2) carrying out cold press molding on the composite powder at the pressure of 600 MPa; (3) and carrying out hot isostatic pressing on the obtained bulk material for 2h, wherein the hot isostatic pressing sintering temperature is 900 ℃, the pressure is 100MPa, and carrying out rapid cooling to obtain the copper-based composite material.
< comparative example 4>
Copper-based composite material
(1) Ball-milling 2 parts by weight of the modified carbon nanotube prepared in example 1, 0.5 part by weight of the modified graphene prepared in example 3, 5 parts by weight of graphite powder, 2 parts by weight of chromium powder, 10 parts by weight of tin powder, 0.4 part by weight of zirconium powder, 0.1 part by weight of lanthanum powder and 80 parts by weight of copper powder by using agate balls and an agate ball jar at a rotation speed of 350 revolutions per minute for 60 minutes; (2) carrying out cold press molding on the composite powder at the pressure of 600 MPa; (3) and carrying out hot isostatic pressing on the obtained bulk material for 2h, wherein the hot isostatic pressing sintering temperature is 900 ℃, the pressure is 100MPa, and carrying out rapid cooling to obtain the copper-based composite material.
< comparative example 5>
Copper-based composite material
(1) Ball-milling and mixing 2 parts by weight of the modified carbon nanotube prepared in example 1, 0.5 part by weight of the modified graphene prepared in example 3, 5 parts by weight of graphite powder, 3 parts by weight of chromium powder, 5 parts by weight of lead powder, 0.4 part by weight of zirconium powder, 0.1 part by weight of lanthanum powder and 84 parts by weight of copper powder by using agate balls and an agate ball jar at the rotation speed of 350 revolutions per minute for 60 minutes; (2) carrying out cold press molding on the composite powder at the pressure of 600 MPa; (3) and carrying out hot isostatic pressing on the obtained bulk material for 2h, wherein the hot isostatic pressing sintering temperature is 900 ℃, the pressure is 100MPa, and carrying out rapid cooling to obtain the copper-based composite material.
< test 1>
The copper-based composite materials prepared in the above examples were tested by an electron microscope, etc., and the test results of some examples are as follows:
FIG. 1 is an SEM photograph of the ball-milled composite powder of example 5, in which surface-modified carbon nanotubes are uniformly dispersed between copper particles, and lamellar graphite is embedded in the copper particles; due to the mechanical action in the ball milling process, a series of changes such as particle deformation, cracking, cold welding and the like occur to form copper particle aggregates.
In examples 5 to 8, at higher magnification, some fragmentation of the reinforcing phase was observed, and the size of the reinforcing phase was reduced to some extent, due to the mechanical action of the ball mill; along with the increase of the ball milling rotating speed and the ball milling time, the uniform dispersion degree of the enhanced phase is increased, but the damage to the enhanced phase is also increased, and the optimal ball milling rotating speed is 350 r/min and the ball milling time is 60min under comprehensive consideration.
Fig. 2 is a BSE picture of the nanocarbon reinforced copper-based composite material obtained in example 7, and fig. 3 is an EDS result of the copper matrix in fig. 2. FIG. 2 shows that the nano-carbon, graphite and copper matrix are distributed in a staggered manner and are uniformly distributed as a whole. The EDS results shown in fig. 3 indicate that chromium, lead, tin, zirconium, lanthanum are solid-solubilized in the copper matrix, and the elements diffuse into each other during sintering and are uniformly distributed in the matrix.
Fig. 4 is an SEM picture of a compressed fracture of the copper-based composite material prepared in example 5, and it can be observed that some broken carbon nanotubes exist on the fracture and one end is embedded in the matrix, and broken carbon nanotubes and broken graphene are also observed on the fracture of the copper-based composite material prepared in other examples, and the broken carbon nanotubes and broken graphene play a role in bridging and load transfer in the copper-based composite material.
Fig. 5 is an SEM image (x 20000 times) of shear fracture of the nanocarbon reinforced copper-based composite material prepared in example 7. The SEM image is cut off, so that the carbon nano tube and the graphene are dispersed and embedded in the copper matrix to play a role in reinforcement; the lamellar graphite is also embedded in the copper matrix, and the frictional wear performance of the graphite can be obviously improved due to the self-lubricating effect of the graphite.
< test 2>
The density and the compactness of the copper-based composite materials obtained in the above examples and comparative examples were measured by the archimedes method, and the micro vickers hardness, the compressive strength and the shear strength were measured, and the results are shown in table 1.
TABLE 1 Experimental results for examples 5-8 and comparative examples
Group of Density of Compactness degree Vickers hardness Compressive strength Shear strength
Example 5 6.71 93.58 56.86 178.62 77.45
Example 6 6.92 96.51 58.94 194.36 78.64
Example 7 6.62 92.33 56.72 188.15 75.16
Example 8 6.78 94.56 60.12 215.89 82.23
Comparative example 1 6.83 95.13 36.89 126.35 48.12
Comparative example 2 6.68 93.25 42.61 147.63 52.08
Comparative example 3 6.75 94.06 44.32 153.06 56.86
Comparative example 4 6.78 94.82 44.42 149.16 51.40
Comparative example 5 6.61 92.19 40.89 143.25 50.75
In the table, the units of the test results are as follows: density (g/cm)3) Density (%), Vickers Hardness (HV), compressive strength (MPa), and shear strength (MPa).
As is clear from the results in Table 1, the copper-based composite material produced in example 8 has improved Vickers hardness by 3.26HV, 1.18HV, and 13.4HV, compressive strength by 37.27MPa, 21.53MPa, and 107.74MPa, and shear strength by 12.78MPa, 3.69MPa, and 10.07MPa, respectively, as compared with the copper-based composite materials produced in examples 5 to 7. Therefore, the copper-based composite material prepared in example 8 has more excellent hardness and strength than the copper-based composite materials prepared in examples 5 to 7, and example 8 is the best embodiment of the copper-based composite material.
Comparative examples 1 to 5 each lack part of the added components, resulting in a significant decrease in the mechanical properties of the copper-based composite material. Compared with the copper-based composite material prepared by the full formula prepared in the examples 5-8, the density difference is not great because the preparation process is the same. The Vickers hardness is reduced by 23.23HV to the maximum. The compression strength in the mechanical property is reduced by 89.54MPa to the maximum extent, and the shear strength is reduced by 34.11 MPa. Wherein, the performance of the copper-based composite material lacking two nano-carbons is reduced most obviously, which shows that the reinforcing effect of the nano-carbon is better than that of other components.
According to performance test results of examples and comparative examples, the effect of the invention can be achieved only when the copper-based composite material comprises, by weight, 0.1-5% of surface-modified carbon nanotubes, 0.1-5% of surface-modified graphene, 2-10% of graphite powder, 1-4% of chromium powder, 1-8% of lead powder, 2-10% of tin powder, 0.1-1% of zirconium powder, 0.01-0.5% of lanthanum powder, and the balance copper powder.
< test 3>
Processing the copper-based composite materials obtained in the above examples and comparative examples into standard parts, and testing the current-carrying wear coefficient of the copper-based composite materials obtained in different examples and comparative examples by a testing method of 5 m.s-1The current intensity was 20A, the pressure was 5N, 10N, 20N, 30N and 50N, respectively, and the results of the test are shown in Table 2 below.
TABLE 2 Current-carrying wear coefficient of copper-based composite materials of examples 5 to 8 and comparative examples
Rate of wear Pressure 5N Pressure 10N Pressure 20N Pressure 30N Pressure 50N
Example 5 0.24 0.36 0.55 0.80 1.11
Example 6 0.25 0.36 0.58 0.81 1.13
Example 7 0.23 0.35 0.56 0.79 1.16
Example 8 0.19 0.33 0.50 0.73 1.05
Comparative example 1 0.67 0.88 1.03 1.15 1.54
Comparative example 2 0.51 0.69 0.81 0.98 1.32
Comparative example 3 0.52 0.68 0.80 0.95 1.36
Comparative example 4 0.57 0.78 0.93 1.10 1.37
Comparative example 5 0.56 0.62 0.86 1.05 1.34
Wear rate units, mg · m-1。
The test results in the table show that the formula of the copper-based composite material prepared by the embodiment of the invention through optimized design realizes the optimized improvement of the matching relationship between different materials, the performance of each component generates the synergistic enhancement effect, the strength, current-carrying friction and wear and other performances of the copper-based composite material are obviously improved, and the density of the copper-based composite material is reduced. When the copper-based composite material is tested under different pressure conditions, the wear coefficient of the material is integrally kept at a lower level, and a large amount of wear increase caused by pressure change is not easy to occur, so that the current-carrying wear of the copper-based composite material and the wear mechanism of the traditional copper-based conductive material are essentially changed, and the comprehensive performance is greatly improved.
The copper-based composite material prepared by the comparative example scheme can see performance attenuation of different degrees according to the reduction of different components, the abrasion mechanism of the copper-based composite material is still similar to that of the traditional copper-based conductive material, and the abrasion amount is rapidly increased along with the change of current-carrying strength and pressure strength, so that the requirement of special application working conditions cannot be met.

Claims (2)

1. A nano-carbon reinforced copper-based composite material is characterized in that: 0.1-5% of carbon nano tube subjected to surface modification, 0.1-5% of graphene subjected to surface modification, 2-10% of graphite powder, 1-4% of chromium powder, 1-8% of lead powder, 2-10% of tin powder, 0.1-1% of zirconium powder, 0.01-0.5% of lanthanum powder and the balance of copper powder;
the carbon nano tube subjected to surface modification is prepared by the following method:
adding the carbon nano tube into a gallic acid aqueous solution of 5-15 mu g/mL, performing ultrasonic dispersion for 20-40 min, standing for 12-36 h, filtering, and performing vacuum drying on filter residue at 60-80 ℃ for 1-8 h to obtain a surface modified carbon nano tube;
the volume ratio of the mass of the carbon nano tube to the gallic acid aqueous solution is 0.05-0.4 g: 20-80 mL;
the mass ratio of the carbon nano tubes to the gallic acid is 1:0.5-8, and the gallic acid is calculated by the mass of the gallic acid dissolved in the gallic acid solution;
the surface-modified graphene is prepared by the following method:
adding graphene into 0.01-0.1 mu g/mL rutin aqueous solution, performing ultrasonic dispersion, standing, filtering, and vacuum drying filter residue to obtain surface-modified graphene;
the volume ratio of the mass of the graphene to the volume of the rutin aqueous solution is 0.05-0.4 g: 20-80 mL;
the mass ratio of the graphene to the rutin is 1:0.5-8, and the rutin is calculated by the mass of the rutin dissolved in the solution;
the preparation method of the copper-based composite material comprises the following steps:
(1) adding carbon nanotubes into a gallic acid aqueous solution, performing ultrasonic dispersion, standing, filtering, and vacuum drying filter residue to obtain surface-modified carbon nanotubes;
(2) adding graphene into a rutin aqueous solution, performing ultrasonic dispersion, standing, filtering, and vacuum-drying filter residues to obtain surface-modified graphene;
(3) performing ball milling on the surface-modified carbon nanotube and the surface-modified graphene with copper powder, graphite powder, chromium powder, lead powder, tin powder, zirconium powder and lanthanum powder to obtain composite powder; the ball milling adopts agate balls and agate ball tanks, the ball milling rotating speed is 200-450 r/min, and the ball milling time is 40-120 min;
(4) carrying out cold press molding on the composite powder to obtain a composite material pressed compact; the pressure of cold press molding pressing is 400-700 MPa;
(5) and carrying out hot isostatic pressing sintering on the composite material pressed compact, and cooling to obtain the nano-carbon reinforced copper-based composite material.
2. The nanocarbon-reinforced copper-based composite material according to claim 1, characterized in that: and (5) hot isostatic pressing sintering is carried out at the temperature of 800-1000 ℃, the pressure of hot isostatic pressing sintering is 80-100 MPa, and the time of hot isostatic pressing sintering is 1-3 h.
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