CN110157932B - Preparation method of graphene modified copper-based electrical contact material based on in-situ synthesis - Google Patents

Preparation method of graphene modified copper-based electrical contact material based on in-situ synthesis Download PDF

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CN110157932B
CN110157932B CN201910299337.XA CN201910299337A CN110157932B CN 110157932 B CN110157932 B CN 110157932B CN 201910299337 A CN201910299337 A CN 201910299337A CN 110157932 B CN110157932 B CN 110157932B
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copper
graphene
powder
electrical contact
copper powder
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CN110157932A (en
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李秀辉
燕绍九
洪起虎
陈翔
王楠
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AECC Beijing Institute of Aeronautical Materials
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F1/00Special treatment of metallic powder, e.g. to facilitate working, to improve properties; Metallic powders per se, e.g. mixtures of particles of different composition
    • B22F1/0003Metallic powders per se; Mixtures of metallic powders; Metallic powders mixed with a lubricating or binding agent
    • B22F1/0007Metallic powder characterised by its shape or structure, e.g. fibre structure
    • B22F1/0055Flake form powders
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F1/00Special treatment of metallic powder, e.g. to facilitate working, to improve properties; Metallic powders per se, e.g. mixtures of particles of different composition
    • B22F1/02Special treatment of metallic powder, e.g. to facilitate working, to improve properties; Metallic powders per se, e.g. mixtures of particles of different composition comprising coating of the powder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/04Making alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00Contacts
    • H01H1/02Contacts characterised by the material thereof
    • H01H1/021Composite material
    • H01H1/025Composite material having copper as the basic material
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01HELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00Contacts
    • H01H1/02Contacts characterised by the material thereof
    • H01H1/021Composite material
    • H01H1/027Composite material containing carbon particles or fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
    • B22F2999/00Aspects linked to processes or compositions used in powder metallurgy

Abstract

The invention relates to a method for preparing a graphene modified copper-based electrical contact material by an in-situ growth process. According to the method, the graphene-coated pure copper powder is prepared by an in-situ chemical vapor deposition process, and then the graphene-coated pure copper powder, the copper alloy powder and the zinc stannate powder are uniformly mixed by adopting a mechanical ball milling process to obtain the composite powder. And then, obtaining an electrical contact sintering blank by adopting a cold isostatic pressing process and a pressureless sintering process, and finally obtaining the graphene modified copper-based electrical contact material with a good structure by adopting a hot extrusion process and a cold rolling process. According to the invention, the graphene reinforcement is introduced into the copper-based electrical contact material through the in-situ chemical vapor deposition process, so that the cost of graphene raw materials is greatly saved, the process problem that graphene is uniformly dispersed in a copper matrix is solved, and the mechanical strength and the arc ablation resistance of the contact material are obviously enhanced while the electric and thermal conductivity of the contact material is not reduced.

Description

Preparation method of graphene modified copper-based electrical contact material based on in-situ synthesis
Technical Field
The invention relates to a preparation method of a graphene modified copper-based electrical contact material based on in-situ synthesis, and belongs to the technical field of preparation of composite metal materials.
Background
The electrical contact is one of the core components of electrical switches and instruments and meters, and is mainly responsible for the important tasks of breaking and connecting circuits and load currents. The requirements of the contact material are manifold, i.e. it has good electrical and thermal conductivity, low and stable contact resistance, high resistance to erosion, welding and good mechanical strength. The silver metal has good electric conduction and heat conduction performance and good oxidation resistance, and is the most main electric contact material at the present stage. However, the development of silver-free/silver-saving electrical contact materials is of great significance because silver resources are scarce and the price is high. Copper has good heat conduction and electric conduction performance and low price, and is an ideal material for replacing silver-based electrical contacts. However, the traditional copper and copper alloy have poor mechanical properties and poor fusion welding resistance and breaking capacity, so that the application of the copper and copper alloy in the field of electrical contacts is limited, and the copper-based electrical contact composite material is prepared by adopting a powder metallurgy process in industry.
The reinforcement of the conventional copper-based composite material mainly comprises ceramic particles, carbon materials and the like, such as silicon carbide, aluminum oxide, graphite, diamond and the like. The ceramic particles have high mechanical strength but are not conductive, and the conductive performance of the copper matrix is seriously weakened by taking the ceramic particles as reinforcing bodies. Graphene is prepared from carbon atoms in sp2The honeycomb planar two-dimensional nano material formed by the hybridization mode has good electric conduction, heat conduction and mechanical properties. The graphene is used as the reinforcement, so that the strength of the copper-based electrical contact material can be improved, and the electric conduction and heat conduction performance of the copper-based electrical contact material can not be weakened, and the graphene is an ideal reinforcement for the copper-based electrical contact material.
The existing invention patents include, for example, CN 105719854A-a preparation method of a copper-based electrical contact material with graphene, CN 105525132A-an electrical contact material and a preparation method thereof, CN 105385883A-an electrical contact material and a preparation method thereof, CN 105551839A-a copper-plated graphene/copper-based electrical contact material and a preparation method thereof, CN 105483422A-an electrical contact material and a preparation method thereof, and CN 105603247A-a graphene-reinforced copper-rare earth-based electrical contact material and a preparation method thereof, all adopt powder metallurgy processes, and graphene copper composite powder is prepared by ball-milling and mixing copper powder and graphene powder. The patent CN 105483641A-a method for preparing an in-situ growth graphene reinforced copper-based electric contact material, uses gas such as methane as a carbon source, and adopts a plasma chemical vapor deposition process to synthesize graphene in situ on the surface of copper powder at 400-800 ℃, so as to ensure the dispersion uniformity of the graphene in the copper powder. However, under the process conditions, copper powder is very easy to sinter into blocks under the high-temperature condition, so that the subsequent powder metallurgy process is difficult to perform.
Disclosure of Invention
The purpose of the invention is: aiming at the problems, the invention firstly introduces rare earth elements to improve the oxidation resistance of the copper matrix through component design and introduces zinc stannate particles to improve the fusion welding resistance of the electrical contact. Secondly, a high-molecular solid carbon source is adopted, graphene is synthesized in situ on the surface of the copper powder through a solution impregnation-chemical vapor phase process, and the problem of uniform dispersion of the graphene in a matrix is solved. Meanwhile, the complete coating of the copper powder by the polymer can be realized through the solution dipping process, so that the copper powder can be prevented from being sintered into blocks in the high-temperature treatment process. And finally, performing ball milling treatment on the graphene-coated electrolytic copper powder, wherein the graphene coated between the copper powder and the dendrite can enter the copper powder through ball milling, and the surface of the copper powder is only partially coated by the graphene. The method not only realizes good interface combination of the graphene and the copper matrix, but also solves the problem that the graphene coated copper powder is difficult to sinter and mold, and the alloy elements are easy to diffuse at the particle interface in the sintering process to realize homogenization.
The technical scheme of the invention is as follows: aiming at the problems of poor mechanical property and poor fusion welding resistance and breaking capacity of the existing copper-based electrical contact material, the preparation method of the graphene modified copper-based electrical contact material based on in-situ synthesis is provided, and the purpose is to improve the mechanical property and fusion welding resistance of the material on the basis of not reducing the electric and heat conductivity of a copper matrix.
The preparation method of the graphene modified copper-based electrical contact material based on in-situ synthesis comprises the following steps:
step 1, taking polyethylene glycol or polyvinyl alcohol as a solid polymer carbon source, and dissolving the solid polymer carbon source in alcohol to form a uniform mixed solution; preferably, the dissolving temperature is 20-80 ℃;
step 2, fully stirring copper powder in the uniformly mixed solution, filtering and drying the copper powder in the solution, coating a macromolecular layer of polyethylene glycol or polyvinyl alcohol on the surface of the copper powder to obtain the macromolecular layer coated copper powder, placing the macromolecular layer coated copper powder in a high-temperature heating furnace for heating and calcining at the temperature of 500-1050 ℃ for 0.5-2 hours, wherein the heated protective gas is a mixed gas of hydrogen and argon, and the polyethylene glycol or polyvinyl alcohol on the surface of the copper powder is converted into graphene in the protective gas; the copper powder is dendritic copper powder;
step 3, placing the copper powder, the copper-zirconium alloy powder, the copper-lanthanum alloy powder and the zinc stannate powder coated with the graphene in ball milling equipment for ball milling, wherein the dendritic copper powder can extend and deform into flaky copper powder after ball milling, and the graphene wrapped among branches of the dendritic copper powder can be positioned inside the flaky copper powder; extending to cause that the surface of the copper powder has a part which is not coated by the graphene; the copper powder which is not coated by the graphene has good sintering formability, and the graphene and the copper matrix are better combined into a whole under the action of mechanical ball milling, so that the interface bonding strength is improved;
step 4, putting the ball-milled mixed powder of copper powder, copper-zirconium alloy powder, copper-lanthanum alloy powder and zinc stannate powder of graphene into a sheath for cold isostatic pressing, and sintering the molded blank at a high temperature to obtain an electrical contact sintered blank, wherein the sintering atmosphere is nitrogen or argon inert atmosphere; and (3) carrying out cold isostatic pressing at a pressure of 250-300 MPa and a high-temperature sintering temperature of 900-950 ℃, carrying out thermal extrusion deformation on the sintered blank after heat preservation, and then carrying out cold rolling deformation to obtain the graphene modified copper-based electrical contact material.
Further, in the mixed powder of the graphene-coated copper powder, the copper-zirconium alloy powder, the copper-lanthanum alloy powder and the zinc stannate powder in the step 3, the mass percent of lanthanum is 0.003-0.006%, the mass percent of zirconium is 0.1-0.3%, the mass percent of zinc stannate is 1.8-2.3%, the mass percent of graphene is 0.05-1.0%, and the balance is copper.
Further, the mass fraction of the polyethylene glycol or the polyvinyl alcohol in the uniformly mixed solution is 1.0-25%.
Furthermore, the particle size of the dendritic copper powder is 80-1000 meshes.
Furthermore, the ball milling rotation speed of the ball milling equipment is 60-350 revolutions per minute, and the ball-material ratio is 5: 1-40-1.
Further, the temperature of hot extrusion deformation is 800-850 ℃, the extrusion ratio is 10: 1-60: 1, the single-time pressing amount of cold rolling of the cold rolling deformation is 3-10%.
The invention has the advantages that: 1. according to the invention, the rare earth element lanthanum is added, so that the oxidation resistance of the copper matrix can be effectively improved, and the contact resistance of the electrical contact material is obviously reduced. The zinc stannate particles volatilize in the service process, so that heat generated in the on-off process of the electrical contact can be effectively taken away, and the fusion welding resistance of the electrical contact is improved. 2. According to the method, the graphene is synthesized in situ on the surface of the electrolytic copper powder by taking the polymer as the solid carbon source, so that the graphene is uniformly dispersed in the copper powder, and the cost of the graphene raw material is saved. The graphene-coated copper composite powder is prepared by a solution dipping coating process, so that the copper powder can be effectively prevented from being sintered into blocks in the high-temperature chemical vapor deposition process. 3. According to the invention, through carrying out ball milling treatment on the graphene-coated electrolytic copper powder, the graphene coated between copper powder branches can enter the copper powder through ball milling, and the surface of the copper powder is only partially coated by the graphene, so that not only is good interface combination of the graphene and a copper matrix realized, but also the problem that the graphene-coated copper powder is difficult to sinter and form is solved, and the alloy elements are easy to realize homogenization through particle interfaces in the sintering process.
Detailed Description
The present invention is described in further detail below.
Example 1
The preparation method of the graphene modified copper-based electrical contact material based on in-situ synthesis comprises the following steps:
step 1, taking polyethylene glycol as a solid polymer carbon source, and dissolving the solid polymer carbon source in alcohol to form a uniform mixed solution; the dissolution temperature is 50 ℃; in the mixed solution, the mass fraction of the polyethylene glycol is 5%, and the mixed solution is stirred for at least 0.5 hour to ensure that the mixed solution is uniform.
Step 2, fully stirring 200-mesh electrolytic copper powder in the uniformly mixed solution for at least 0.5 hour, filtering and drying the copper powder in the solution, and coating a macromolecular layer of polyethylene glycol or polyvinyl alcohol on the surface of the copper powder to obtain the copper powder coated with the macromolecular layer; the copper powder coated with the polymer layer is placed in a high-temperature heating furnace for heating and calcining, the heating and calcining temperature is 850 ℃, the heating and calcining time is 1 hour, the heated protective gas is mixed gas of hydrogen and argon, and the proportion of the hydrogen and argon mixed gas is 1: 4, the gas flow rate is 500 sccm. Polyethylene glycol on the surface of the copper powder is converted into graphene in protective gas;
and 3, placing the copper powder, the copper-zirconium alloy powder, the copper-lanthanum alloy powder and the zinc stannate powder coated with the graphene into ball milling equipment for ball milling, wherein the mechanical ball milling rotation speed is 300 revolutions per minute, and the ball milling time is 1 hour, so that the electric contact composite powder is obtained. The composite powder contains 0.2% of zirconium, 0.004% of lanthanum as a rare earth element, 0.2% of zirconium, 2% of zinc stannate, 0.3% of graphene and the balance of copper. The dendritic copper powder can be extended and deformed into flake copper powder after ball milling, and graphene wrapped between branches of the dendritic copper powder can be positioned inside the flake copper powder; extending to cause that the surface of the copper powder has a part which is not coated by the graphene; the copper powder which is not coated by the graphene has good sintering formability, and the graphene and the copper matrix are better combined into a whole under the action of mechanical ball milling, so that the interface bonding strength is improved;
step 4, putting the ball-milled mixed powder of copper powder, copper-zirconium alloy powder, copper-lanthanum alloy powder and zinc stannate powder of graphene into a sheath for cold isostatic pressing, and sintering the molded blank at a high temperature to obtain an electrical contact sintered blank, wherein the sintering atmosphere is nitrogen or argon inert atmosphere; and keeping the pressure of the cold isostatic pressing at 250MPa for 1min, and sintering at the high-temperature sintering temperature of 900 ℃ for 2 h. And (3) carrying out thermal extrusion deformation on the sintered blank after heat preservation, wherein the thermal extrusion temperature is 830 ℃, the thermal extrusion ratio is 20:1, then carrying out cold rolling deformation to obtain the graphene modified copper-based electrical contact material, and the single-rolling pressing amount is 5% and the total pressing amount is 50%.
The performance of the graphene/copper-based composite material of the embodiment is as follows: the conductivity at normal temperature is 92% IACS, the tensile strength is 450MPa, the elongation is 15%, and the composite material has good mechanical property and conductivity.

Claims (9)

1. A preparation method of a graphene modified copper-based electrical contact material based on in-situ synthesis comprises the following steps:
step 1, taking polyethylene glycol or polyvinyl alcohol as a solid polymer carbon source, and dissolving the solid polymer carbon source in alcohol to form a uniform mixed solution;
step 2, fully stirring copper powder in the uniformly mixed solution, filtering and drying the copper powder in the solution, coating a macromolecular layer of polyethylene glycol or polyvinyl alcohol on the surface of the copper powder to obtain the macromolecular layer coated copper powder, placing the macromolecular layer coated copper powder in a high-temperature heating furnace for heating and calcining at the temperature of 500-1050 ℃ for 0.5-2 hours, wherein the heated protective gas is a mixed gas of hydrogen and argon, and the polyethylene glycol or polyvinyl alcohol on the surface of the copper powder is converted into graphene in the protective gas; the copper powder is dendritic copper powder;
step 3, placing the copper powder, the copper-zirconium alloy powder, the copper-lanthanum alloy powder and the zinc stannate powder coated with the graphene in ball milling equipment for ball milling, wherein the dendritic copper powder can extend and deform into flaky copper powder after ball milling, and the graphene wrapped among branches of the dendritic copper powder can be positioned inside the flaky copper powder; extending to cause that the surface of the copper powder has a part which is not coated by the graphene; the copper powder which is not coated by the graphene has good sintering formability, and the graphene and the copper matrix are better combined into a whole under the action of mechanical ball milling, so that the interface bonding strength is improved;
step 4, putting the ball-milled mixed powder of copper powder, copper-zirconium alloy powder, copper-lanthanum alloy powder and zinc stannate powder of graphene into a sheath for cold isostatic pressing, and sintering the molded blank at a high temperature to obtain an electrical contact sintered blank, wherein the sintering atmosphere is nitrogen or argon inert atmosphere; and (3) carrying out cold isostatic pressing at a pressure of 250-300 MPa and a high-temperature sintering temperature of 900-950 ℃, carrying out thermal extrusion deformation on the sintered blank after heat preservation, and then carrying out cold rolling deformation to obtain the graphene modified copper-based electrical contact material.
2. The method for preparing the graphene-modified copper-based electrical contact material based on in-situ synthesis according to claim 1, wherein the method comprises the following steps: in the mixed powder of the copper powder, the copper-zirconium alloy powder, the copper-lanthanum alloy powder and the zinc stannate powder coated with the graphene in the step 3, the mass percent of lanthanum is 0.003-0.006%, the mass percent of zirconium is 0.1-0.3%, the mass percent of zinc stannate is 1.8-2.3%, the mass percent of graphene is 0.05-1.0%, and the balance is copper.
3. The method for preparing the graphene-modified copper-based electrical contact material based on in-situ synthesis according to claim 1, wherein the method comprises the following steps: the mass fraction of the polyethylene glycol or the polyvinyl alcohol in the uniformly mixed solution is 1.0-25%.
4. The method for preparing the graphene-modified copper-based electrical contact material based on in-situ synthesis according to claim 1, wherein the method comprises the following steps: the particle size of the dendritic copper powder is 80-1000 meshes.
5. The method for preparing the graphene-modified copper-based electrical contact material based on in-situ synthesis according to claim 1, wherein the method comprises the following steps: the ball milling rotation speed of the ball milling equipment is 60-350 r/min, and the ball-material ratio is 5: 1-40-1.
6. The method for preparing the graphene-modified copper-based electrical contact material based on in-situ synthesis according to claim 1, wherein the method comprises the following steps: the temperature of hot extrusion deformation is 800-850 ℃, the extrusion ratio is 10: 1-60: 1, the single-time pressing amount of cold rolling of the cold rolling deformation is 3-10%.
7. The method for preparing the graphene-modified copper-based electrical contact material based on in-situ synthesis according to claim 1, wherein the method comprises the following steps: the temperature of hot extrusion deformation is 820 ℃, the extrusion ratio is 10: 1-60: 1, the single-time pressing amount of cold rolling of the cold rolling deformation is 3-10%.
8. The method for preparing the graphene-modified copper-based electrical contact material based on in-situ synthesis according to claim 1, wherein the method comprises the following steps: the temperature of hot extrusion deformation is 830 ℃, the extrusion ratio is 10: 1-60: 1, the single-time pressing amount of cold rolling of the cold rolling deformation is 3-10%.
9. The method for preparing the graphene-modified copper-based electrical contact material based on in-situ synthesis according to claim 1, wherein the method comprises the following steps: in the step 1, a solid polymer carbon source is dissolved in alcohol to form a uniform mixed solution, wherein the dissolving temperature is 20-80 ℃.
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