CN110157932A - A kind of preparation method of the graphene Modified Cu base electric contact material based on fabricated in situ - Google Patents
A kind of preparation method of the graphene Modified Cu base electric contact material based on fabricated in situ Download PDFInfo
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- CN110157932A CN110157932A CN201910299337.XA CN201910299337A CN110157932A CN 110157932 A CN110157932 A CN 110157932A CN 201910299337 A CN201910299337 A CN 201910299337A CN 110157932 A CN110157932 A CN 110157932A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/025—Composite material having copper as the basic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
- H01H1/027—Composite material containing carbon particles or fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The present invention relates to a kind of methods that growth in situ technique prepares graphene Modified Cu base electric contact material.The present invention passes through in-situ chemical vapor deposition technique first and prepares graphene coated fine copper powder, then uniformly mixes graphene coated fine copper powder, copper alloy powder, zinc stannate powder using mechanical ball mill technique, obtains composite granule.Electrical contact sintered body is then obtained using cold isostatic compaction technique, non-pressure sintering technology, obtains highly organized graphene Modified Cu base electric contact material finally by hot extrusion technique, cold-rolling process.The present invention introduces graphene reinforcement into copper-based electrical contact material by in-situ chemical vapor deposition technique, graphene raw material cost is greatly saved, it solves graphene process difficulties evenly dispersed in Copper substrate, the mechanical strength and arc resistant ablation property of contact contact material is significantly enhanced while not reducing contact material electrical and thermal conductivity performance.
Description
Technical field
The preparation method of the present invention relates to a kind of graphene Modified Cu base electric contact material based on fabricated in situ belongs to
In the preparation technical field of composite material.
Background technique
Electrical contact is one of the core component of electric switch, instrument and meter, is mainly responsible for disjunction, connects circuit and load
The vital task of electric current.The requirement of contact material be it is various, that is, require it have good electric conductivity, thermal conductivity, it is low and
Stable contact resistance has high damage tolerant corrosion, resistance fusion welding and good mechanical strength again.The conductive and heat-conductive of metallic silver
Performance is good, has good inoxidizability, is most important contact material at this stage.But due to silver-colored scarcity of resources, price is high
It is expensive, therefore carry out and have great importance without silver/section silver electric contact material development.Copper has good thermal conductivity and valence
Lattice are cheap, are the ideal materials for substituting Ag-based electrical contact.But traditional copper and its alloy mechanical property are poor, anti-melting welding and disjunction energy
Power is poor, limits it in the application in electrical contact field, powder metallurgical technique is industrially mostly used to prepare copper-based electrical contact composite wood
Material.
The reinforcement of traditional Cu-base composites mainly includes ceramic particle, carbon material etc., as silicon carbide, aluminium oxide,
Graphite, diamond etc..Ceramic particle high mechanical strength is non-conductive, and the electric conductivity of Copper substrate can be seriously undermined using it as reinforcement
Energy.Graphene one kind is by carbon atom with sp2The honeycomb planar nano material that hybrid form is formed has good lead
Electric, thermally conductive and mechanical property.It can not be weakened while improving the copper-based electrical contact strength of materials using graphene as reinforcement
Conductive, heating conduction, is the ideal reinforcement of copper-based electrical contact material.
A kind of preparation method of the copper-based electric contact material with graphene of existing patent of invention such as CN105719854A-,
A kind of electrical contact material of CN105525132A- and preparation method thereof, a kind of electrical contact material of CN105385883A- and its preparation side
A kind of copper-plated graphite alkene/copper-based electrical contact material of method, CN105551839A- and preparation method thereof, a kind of electricity of CN105483422A-
A kind of graphene enhancing copper-rare earth base electric contact material of contact material and preparation method thereof, CN105603247A- and its preparation side
Method is all made of powder metallurgical technique, graphene copper composite powders is prepared by copper powder and graphene powder ball milling mixing, due to stone
Black alkene and copper powder density difference are very big, and graphene itself is easy to reunite, and graphene is difficult in evenly dispersed and Copper substrate, serious shadow
Ring electrical contact performance.A kind of preparation method of growth in situ graphene enhancing copper-based electric contact material of patent CN105483641A-
Using gases such as methane as carbon source, using plasma chemical vapor deposition process is in 400 DEG C~800 DEG C conditions in Copper Powder Surface
Fabricated in situ graphene guarantees graphene dispersing uniformity in copper powder.But under the process conditions, copper powder is easily in hot conditions
Under sinter block into, cause subsequent powder metallurgical technique to be difficult to carry out.
Summary of the invention
The purpose of the present invention is: in view of the above-mentioned problems, the present invention is designed by ingredient first introduces rare earth element raising copper
Matrix antioxygenic property introduces zinc stannate particle and improves electrical contact fusion welding resisting ability.Secondly it uses high score for solid-state carbon source, passes through
Solution dipping-chemical gaseous phase technique solves graphene in the base evenly dispersed and asks in Copper Powder Surface fabricated in situ graphene
Topic.Meanwhile macromolecule may be implemented to the complete cladding of copper powder by solution impregnation technology, therefore copper powder can be prevented in high temperature
It is sintered in treatment process blocking.Finally, copper powder branch can will be coated on by carrying out ball-milling treatment to graphene coated electrolytic copper powder
Etype graphite alkene ball milling enters inside copper powder, and Copper Powder Surface only has part by graphene coated.This both realized graphene with it is copper-based
The good interface of body combines, and solves the problems, such as that graphene coated copper powder is difficult to sinter molding, and alloying element is easily being sintered
Homogenization is realized by diffusion at granular boundary in the process.
The technical scheme is that, anti-melting welding and disjunction energy poor for existing copper base electric contact material mechanical property
The problem of power difference provides a kind of preparation method of graphene Modified Cu base electric contact material based on fabricated in situ, it is therefore an objective to
The mechanical performance and resistance fusion welding energy that material is improved on the basis of Copper substrate electrical and thermal conductivity performance are not reduced.
A kind of preparation method of graphene Modified Cu base electric contact material based on fabricated in situ is provided, including is walked as follows
It is rapid:
Step 1, using polyethylene glycol or polyvinyl alcohol as solid-state polymer carbon source, and solid-state polymer carbon source is dissolved in wine
Essence forms homogeneous mixture solotion；It is preferred that solution temperature is 20~80 DEG C；
Copper powder is sufficiently stirred step 2 in the homogeneous mixture solotion, after filtering by the copper powder in solution and be dry,
It can be coated with the macromolecule layer of polyethylene glycol or polyvinyl alcohol in Copper Powder Surface, the copper powder for being coated with macromolecule layer is obtained, will wrap
The copper powder for being covered with macromolecule layer is placed in heating and calcining in high-temperature heater, and heating and calcining temperature is 500~1050 DEG C, and the time is
0.5~2 hour, the protective gas of heating was the mixed gas of hydrogen and argon gas, the polyethylene glycol or polyvinyl alcohol of Copper Powder Surface
Graphene is converted into protective gas；The copper powder is dendroid copper powder；
The copper powder for being coated with graphene, copper zirconium alloy powder, copper lanthanum alloy powder and stannic acid zinc powder are placed in ball milling and set by step 3
Standby middle carry out ball milling, the dendroid copper powder can extend after ball milling is deformed into flake copper powder, between the branch fork of dendroid copper powder
The graphene of package can be inside flake copper powder；Extension causes Copper Powder Surface to exist not by graphene coated part；Not by stone
There is good sinter molding, by the effect of mechanical ball mill, graphene and Copper substrate between the copper powder of black alkene covered section
It is preferably combined into one, improves interface bond strength；
Step 4, by the copper powder of the graphene after ball milling, copper zirconium alloy powder, copper lanthanum alloy powder and stannic acid zinc powder mixed powder
Body, which is fitted into jacket, carries out cold isostatic compaction, and molding blank obtains electrical contact sintered body by high temperature sintering, wherein being sintered
Atmosphere is nitrogen or argon inert atmosphere；Cold isostatic compaction pressure be 250MPa~300MPa, high temperature sintering temperature be 900~
950 DEG C, hot extrusion deformation is carried out after sintered body is kept the temperature, the modified copper-based electrical contact of graphene is obtained by cold-rolling deformation later
Material.
Further, the copper powder for being coated with graphene, copper zirconium alloy powder, copper lanthanum alloy powder and stannic acid zinc powder of step 3 is mixed
It closes in powder, the mass percent of lanthanum is 0.003%~0.006%, the mass percent of zirconium is 0.1%~0.3%, zinc stannate
Mass percent be 1.8%~2.3%, the mass percent of graphene is 0.05~1.0%, surplus is copper.
Further, the mass fraction of the polyethylene glycol in homogeneous mixture solotion or polyvinyl alcohol is 1.0%~25%.
Further, the partial size of the dendroid copper powder is 80~1000 mesh.
Further, the rotational speed of ball-mill of ball-grinding machine is 60~350 revs/min, and ratio of grinding media to material is 5:1~40~1.
Further, the temperature of the hot extrusion deformation is 800~850 DEG C, and extrusion ratio is 10:1~60:1, the cold rolling
The cold rolling single volume under pressure of deformation is 3%~10%.
The invention has the advantages that the 1, present invention can effectively improve Copper substrate antioxygenic property by adding rare-earth elements of lanthanum,
Significantly reduce contact resistor made of electrical contact material.Zinc stannate particle volatilizees during military service can effectively take away electrical contact on-off mistake
The heat generated in journey improves electrical contact fusion welding resisting ability.2, the present invention is solid-state carbon source on electrolytic copper powder surface using macromolecule
Fabricated in situ graphene, it is evenly dispersed in copper powder to realize graphene, saves graphene raw material cost.It is soaked by solution
Stain cladding process prepares graphene coated copper composite powders, and copper powder can be effectively prevented and burn during high temperature chemical vapor deposition
Form block.3, the present invention can will be coated on graphite between copper powder branch by carrying out ball-milling treatment to graphene coated electrolytic copper powder
Alkene ball milling enters inside copper powder, and Copper Powder Surface only has part by graphene coated, has both realized the good boundary of graphene and Copper substrate
Face combines, and solves the problems, such as that graphene coated copper powder is difficult to sinter molding, and alloying element easily passes through during the sintering process
Granular boundary realizes homogenization.
Specific embodiment
The present invention is described in further details below.
Embodiment 1
A kind of preparation method of graphene Modified Cu base electric contact material based on fabricated in situ is provided, including is walked as follows
It is rapid:
Step 1, using polyethylene glycol as solid-state polymer carbon source, and solid-state polymer carbon source is dissolved in alcohol and is formed uniformly
Mixed solution；Solution temperature is 50 DEG C；In the mixed solution, the mass fraction of polyethylene glycol is 5%, is stirred solution extremely
Make mixed solution uniform within few 0.5 hour.
200 mesh electrolytic copper powders are sufficiently stirred at least 0.5 hour step 2 in the homogeneous mixture solotion, will be in solution
Copper powder filtering and it is dry after, the macromolecule layer of polyethylene glycol or polyvinyl alcohol can be coated in Copper Powder Surface, be coated with
The copper powder of macromolecule layer；The copper powder for being coated with macromolecule layer is placed in heating and calcining in high-temperature heater, heating and calcining temperature is
850 DEG C, the time is 1 hour, and the protective gas of heating is the mixed gas of hydrogen and argon gas, and hydrogen-argon-mixed ratio is 1:4, gas
Body flow is 500sccm.The polyethylene glycol of Copper Powder Surface is converted into graphene in protective gas；
The copper powder for being coated with graphene, copper zirconium alloy powder, copper lanthanum alloy powder and stannic acid zinc powder are placed in ball milling and set by step 3
Standby middle carry out ball milling, Ball-milling Time 1 hour, obtains electrical contact composite granule by 300 revs/min of mechanical ball mill rotational speed of ball-mill.It is compound
Zirconium content 0.2% in powder, rare-earth elements of lanthanum content 0.004%, zirconium content 0.2%, stannic acid Zn content 2%, graphene content
0.3%, surplus is copper.The dendroid copper powder can extend after ball milling is deformed into flake copper powder, the branch fork of dendroid copper powder
Between the graphene that wraps up can be inside flake copper powder；Extension causes Copper Powder Surface to exist not by graphene coated part；Not by
Between the copper powder of graphene coated part have good sinter molding, by the effect of mechanical ball mill, graphene with it is copper-based
Body is preferably combined into one, and improves interface bond strength；
Step 4, by the copper powder of the graphene after ball milling, copper zirconium alloy powder, copper lanthanum alloy powder and stannic acid zinc powder mixed powder
Body, which is fitted into jacket, carries out cold isostatic compaction, and molding blank obtains electrical contact sintered body by high temperature sintering, wherein being sintered
Atmosphere is nitrogen or argon inert atmosphere；Cold isostatic compaction pressure is 250MPa, and pressure maintaining 1min, high temperature sintering temperature is 900
DEG C, sintering time 2h.Hot extrusion deformation is carried out after sintered body is kept the temperature, extrusion temperature is 830 DEG C, and hot extrusion ratio is 20:1
Graphene Modified Cu base electric contact material is obtained by cold-rolling deformation later, single pass volume under pressure is 5%, and total volume under pressure is
50%.
Embodiment graphene/Cu-base composites performance is as follows: the conductivity under room temperature is 92%IACS, and tension is strong
450MPa is spent, elongation percentage 15% has both good mechanical property and electric conductivity.
Claims (8)
1. a kind of preparation method of the graphene Modified Cu base electric contact material based on fabricated in situ, includes the following steps:
Step 1, using polyethylene glycol or polyvinyl alcohol as solid-state polymer carbon source, and solid-state polymer carbon source is dissolved in alcohol shape
At homogeneous mixture solotion；It is preferred that solution temperature is 20~80 DEG C；
Copper powder is sufficiently stirred step 2 in the homogeneous mixture solotion, after filtering by the copper powder in solution and is dry, in copper
Powder surface can be coated with the macromolecule layer of polyethylene glycol or polyvinyl alcohol, obtain the copper powder for being coated with macromolecule layer, will be coated with
The copper powder of macromolecule layer is placed in heating and calcining in high-temperature heater, and heating and calcining temperature is 500~1050 DEG C, and the time is 0.5~2
Hour, the protective gas of heating is the mixed gas of hydrogen and argon gas, and the polyethylene glycol or polyvinyl alcohol of Copper Powder Surface are being protected
Graphene is converted into gas；The copper powder is dendroid copper powder；
The copper powder for being coated with graphene, copper zirconium alloy powder, copper lanthanum alloy powder and stannic acid zinc powder are placed in ball-grinding machine by step 3
Ball milling is carried out, the dendroid copper powder can extend after ball milling is deformed into flake copper powder, wraps up between the branch fork of dendroid copper powder
Graphene can be inside the flake copper powder；Extension causes Copper Powder Surface to exist not by graphene coated part；Not by graphene
There is good sinter molding, by the effect of mechanical ball mill, graphene is more preferable with Copper substrate between the copper powder of covered section
Be combined into one, improve interface bond strength；
Step 4 fills the mixed powder of the copper powder of the graphene after ball milling, copper zirconium alloy powder, copper lanthanum alloy powder and stannic acid zinc powder
Enter and carry out cold isostatic compaction in jacket, molding blank obtains electrical contact sintered body by high temperature sintering, wherein sintering atmosphere
For nitrogen or argon inert atmosphere；Cold isostatic compaction pressure is 250MPa~300MPa, and high temperature sintering temperature is 900~950
DEG C, hot extrusion deformation is carried out after sintered body is kept the temperature, the modified copper-based electrical contact material of graphene is obtained by cold-rolling deformation later
Material.
2. a kind of preparation method of the graphene Modified Cu base electric contact material based on fabricated in situ as described in claim 1,
It is characterized by: the copper powder for being coated with graphene of step 3, copper zirconium alloy powder, copper lanthanum alloy powder and stannic acid zinc powder mixed powder
In body, the mass percent of lanthanum is 0.003%~0.006%, the mass percent of zirconium is 0.1%~0.3%, the matter of zinc stannate
Amount percentage is 1.8%~2.3%, the mass percent of graphene is 0.05~1.0%, and surplus is copper.
3. a kind of preparation method of the graphene Modified Cu base electric contact material based on fabricated in situ as described in claim 1,
It is characterized by: the mass fraction of polyethylene glycol or polyvinyl alcohol in homogeneous mixture solotion is 1.0%~25%.
4. a kind of preparation method of the graphene Modified Cu base electric contact material based on fabricated in situ as described in claim 1,
It is characterized by: the partial size of the dendroid copper powder is 80~1000 mesh.
5. a kind of preparation method of the graphene Modified Cu base electric contact material based on fabricated in situ as described in claim 1,
It is characterized by: the rotational speed of ball-mill of ball-grinding machine is 60~350 revs/min, ratio of grinding media to material is 5:1~40~1.
6. a kind of preparation method of the graphene Modified Cu base electric contact material based on fabricated in situ as described in claim 1,
It is characterized by: the temperature of the hot extrusion deformation is 800~850 DEG C, extrusion ratio is 10:1~60:1, the cold-rolling deformation
Cold rolling single volume under pressure is 3%~10%.
7. a kind of preparation method of the graphene Modified Cu base electric contact material based on fabricated in situ as described in claim 1,
It is characterized by: the temperature of the hot extrusion deformation is 820 DEG C, extrusion ratio is 10:1~60:1, the cold rolling of the cold-rolling deformation
Single volume under pressure is 3%~10%.
8. a kind of preparation method of the graphene Modified Cu base electric contact material based on fabricated in situ as described in claim 1,
It is characterized by: the temperature of the hot extrusion deformation is 830 DEG C, extrusion ratio is 10:1~60:1, the cold rolling of the cold-rolling deformation
Single volume under pressure is 3%~10%.
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| CN110424001A (en) * | 2019-08-29 | 2019-11-08 | 江西大乘汽车有限公司 | A kind of copper-based conductive contact method of modifying |
| CN110616352A (en) * | 2019-09-09 | 2019-12-27 | 四川大学 | Preparation method of high-strength high-conductivity copper-selenium multi-element alloy material |
| CN110695372A (en) * | 2019-10-10 | 2020-01-17 | 天津大学 | Preparation method for improving copper-graphene interface by using rare earth elements |
| CN111926205A (en) * | 2020-08-25 | 2020-11-13 | 宝鸡文理学院 | Preparation method of Cu-C-Ag alloy electrical contact material |
| CN114807682A (en) * | 2021-01-13 | 2022-07-29 | 中国科学院过程工程研究所 | Rare earth doped graphene-aluminum matrix composite material and preparation method thereof |
| CN115351277A (en) * | 2022-08-04 | 2022-11-18 | 国网智能电网研究院有限公司 | Graphene-copper composite material and preparation method and application thereof |
| CN117265314A (en) * | 2023-10-16 | 2023-12-22 | 靖江市海源有色金属材料有限公司 | Graphene reinforced copper-based composite electrical contact material and preparation method thereof |
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| CN110616352A (en) * | 2019-09-09 | 2019-12-27 | 四川大学 | Preparation method of high-strength high-conductivity copper-selenium multi-element alloy material |
| CN110695372A (en) * | 2019-10-10 | 2020-01-17 | 天津大学 | Preparation method for improving copper-graphene interface by using rare earth elements |
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| CN114807682A (en) * | 2021-01-13 | 2022-07-29 | 中国科学院过程工程研究所 | Rare earth doped graphene-aluminum matrix composite material and preparation method thereof |
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| CN115351277A (en) * | 2022-08-04 | 2022-11-18 | 国网智能电网研究院有限公司 | Graphene-copper composite material and preparation method and application thereof |
| CN115351277B (en) * | 2022-08-04 | 2024-02-06 | 国网智能电网研究院有限公司 | Graphene copper composite material and preparation method and application thereof |
| CN117265314A (en) * | 2023-10-16 | 2023-12-22 | 靖江市海源有色金属材料有限公司 | Graphene reinforced copper-based composite electrical contact material and preparation method thereof |
| CN117265314B (en) * | 2023-10-16 | 2024-04-16 | 靖江市海源有色金属材料有限公司 | Graphene reinforced copper-based composite electrical contact material and preparation method thereof |
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