CN105551839B - A kind of copper-plated graphite alkene/copper-based electrical contact material and preparation method thereof - Google Patents
A kind of copper-plated graphite alkene/copper-based electrical contact material and preparation method thereof Download PDFInfo
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- CN105551839B CN105551839B CN201610106144.4A CN201610106144A CN105551839B CN 105551839 B CN105551839 B CN 105551839B CN 201610106144 A CN201610106144 A CN 201610106144A CN 105551839 B CN105551839 B CN 105551839B
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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
-
- 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
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/101—Pretreatment of the non-metallic additives by coating
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
- H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
- H01H11/048—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
Abstract
The present invention relates to a kind of copper-plated graphite alkene/copper-based electrical contact materials and preparation method thereof.Electrical contact material includes the copper-plated graphite alkene and 98.0 99.9% Cu-RE alloys that weight content is 0.1 2.0%, and the weight ratio that rare earth accounts for Cu-RE alloys is 0.03 3.0%.Preparation method is：Graphene copper facing, powder by atomization, ball milling mix powder, cold moudling, vacuum arc melting.The present invention adds copper-plated graphite alkene reinforcement as skeleton in copper alloy, and material is made to have high rigidity, high-wearing feature, mechanical shock resistance, resistance fusion welding.The addition of rare earth improves the inoxidizability of copper alloy electric contact material and resistance to electrical arc erosion ability.
Description
Technical field
The present invention relates to a kind of electrical contact material more particularly to a kind of copper-plated graphite alkene/copper-based electrical contact material, Yi Jishang
State the preparation method of material.
Background technology
Electrical contact material is the critical component of instrument and meter, and the service life and functional reliability to instrument and meter play important
Effect.Copper-base contact material is since cheap, conductive, heat conductivility and silver are close, and part replaces silver-based contact in recent years,
Reduce the loss of noble silver.But since copper contact material easily aoxidizes, copper oxide and oxidation of the generation with low-resistivity
It is cuprous, increase the contact resistance of contact elements, make its in use easily fever, cause contact material reliability and
Service life reduces.
Existing patent document（Publication number 102385938A）, disclose a kind of metal matrix graphene composite electrical contact material and
Its preparation method, contact material, the graphene comprising 0.02-10wt%, remaining is metal matrix material.Since graphene increases
The addition of strong phase makes the composited contact material have conductive, thermal conductivity more better than other enhancing phase composited contact materials
It can be with higher hardness and wearability.But it is reducing agent because using poisonous and hazardous hydrazine hydrate, it is difficult to meet environmental requirement.
Rare earth accounts for the 80% of global rare earth reserves, the coloured conjunction of high-quality of exploitation rare earth element addition in China's rich reserves
Gold is the exclusive advantage in China.Rare earth element is more active, is added in metallic copper, and can deaerate slagging-off, crystal grain thinning, improves
The corrosion resistance and abrasion resistance properties of copper alloy.
Publication No. 105063413A, discloses a kind of copper-base contact material and preparation process, and copper-base contact material includes
Following weight composition, the magnesium of 0.2-0.6%, the antimony of 0.05-0.3%, the bismuth of 0.05-0.4%, the tin of 0.05- 0.3%,
The copper of the chromium of 0.05-0.3%, 0.005-0.05% boron, 0.02-0.1% lanthanums, 0.2-0.5% graphite and surplus, it is suitable by adding in
The intensity and wearability of electrical contact manufactured goods are improved in the boron of amount, tin, antimony powder end.
The Chinese patent of Publication No. 101145450 discloses a kind of special powder copper alloy electric contact material, feature
It is：The composition of the material, component by weight percentage are：Rare earth：0.1%~1%, boron：0.01%~0.1%,
Aluminium：0.1%~1%, silver：0.1%~1%, conductivity ceramics：0.2%~2%, bortz powder：0.2%~2%, surplus is copper
With inevitable impurity.
Above-mentioned two patents all improve the corrosion resistance of copper alloy, anti-oxidant by the addition of rare earth or rare earth oxide
Property, but simultaneously because the material addition of the low electric conductivities such as ceramic particle, chromium, reduces leading for copper contact material to a certain extent
Electricity, heat conductivility, therefore, it is difficult to obtain the copper-base contact material of excellent combination property.
The content of the invention
It conducts electricity very well it is an object of the invention to provide one kind, contact resistance is low and stablizes, the good, hardness of resistance fusion welding energy
Copper-plated graphite alkene/copper-based electrical contact material that is high and easily preparing.
Another object of the present invention is to provide the preparation method of above-mentioned material.
The present invention is realized by following technical solution.
A kind of copper-plated graphite alkene/copper-based electrical contact material, which is characterized in that including the copper facing that weight content is 0.1-2.0%
Copper-rare earth alloy of graphene and 98.0-99.9%, the weight ratio that rare earth accounts for copper-rare earth alloy are 0.03-3.0%.
Further, the copper-plated graphite alkene is in graphene surface deposited metal copper using direct current magnetron sputtering process
Into.
Further, the rare earth is one or more of lanthanum, cerium, yttrium, praseodymium and neodymium.Rare earth metal for lanthanum, cerium, praseodymium and
During the mixing of neodymium, it is known as norium.It common are：Lanthanum rich norium and rich cerium misch metal.Rich lanthanum
In norium, lanthanum accounts for the 40%~45% of total amount of rare earth, is respectively lower than 5%, 11%~13% and containing cerium, praseodymium, neodymium
33%~37%.In rich cerium misch metal, cerium accounts for the 50%~60% of total amount of rare earth, containing lanthanum 18%~28%, praseodymium 4%~
6% and neodymium 12%~20%.
The preparation method of above-mentioned electrical contact material, it is characterised in that comprise the following steps：
（1）Using direct current magnetron sputtering process in graphene surface deposited metal copper into copper-plated graphite alkene；
（2）200-300 mesh copper alloy powders are made using atomization in copper-rare earth alloy；
（3）Copper-plated graphite alkene and copper alloy powder are packed into ball mill and mix powder, uniformly mixed powder is made；
（4）By step（3）The powder of mixing is put into cold moudling in mold；
（5）Shaping blank carries out vacuum arc melting, and copper-plated graphite alkene/copper-based electrical contact material is made.
Further, the step（1）Middle graphene is N layers, N 1-10.
Further, the step（1）It is first polished, removed with fine sandpaper before the copper target installation that moderate purity is 99.99%
Surface film oxide, then cleaned with acetone is dried, and 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, using baffle by target
It is separated with graphene, removes the metal oxide of target material surface and other impurity, ensure follow-up graphene surface deposition copper film
Purity.The technological parameter of magnetically controlled DC sputtering is：Target is the copper target that purity is 99.99%, reaches 0.1*10 in vacuum degree-3-
1.0*10-3During Pa, the argon gas of purity 99.99%, operating air pressure 0.5-1.2Pa, sputtering power 100-150W, sedimentation time are passed through
For 5-30min.
Further, the step（2）Middle atomization is selected from the one of gas atomization, centrifugal atomization and ultrasonic atomizatio method
Kind.
Further, the step（3）The technological parameter of middle ball mill is：Ball grinder first vacuumizes is passed through argon gas guarantor again
Shield, rotating speed 100-250r/min, ball milling 15-20 minutes stop 5 minutes, alternate rotation clockwise, counterclockwise, when amounting to mixed powder
Between 2-6h.To prevent the oxidation of copper, ball grinder need to vacuumize before ball milling, and be passed through argon gas protection.In the ball milling parameter of the present invention
In the range of, the distribution of graphene and metal alloy mixed-powder can be controlled well.
Further, step（4）Described in cold moudling pressure be 400-600MPa, dwell time 3-5 minute.
Further, the step（5）The smelting furnace vacuum degree 1.0*10 of middle vacuum arc melting-3-3.0*10-3Pa, work
Make gas as argon gas, operating air pressure 0.02Pa-0.1Pa, smelting time 1-2 minutes.
The present invention useful achievement be：
（1）The present invention adds copper-plated graphite alkene reinforcement as skeleton in copper alloy, makes material resistance to high rigidity, height
Mill property, mechanical shock resistance, arc resistant ablation property.
（2）Copper is deposited in graphene surface by direct current magnetron sputtering process, graphene can be avoided and existed as nano particle
Reunite during mixed powder.
（3）Copper-plated graphite alkene improves graphene and intermetallic interfacial wettability, is conducive to obtain good interface combination,
Conductivity of composite material, heat conductivility, anti electric arc corrosion are further improved, preferably meets the performance requirement of electrical contact.
（4）The addition of rare earth improves the inoxidizability of copper alloy electric contact material and resistance to electrical arc erosion ability.
（5）Copper-rare earth alloy powder is prepared using atomization, rare earth alloy can be made to be uniformly distributed in Copper substrate, simultaneously
Cooling rate is very fast in atomization process, can be with crystal grain thinning tissue.
（6）Vacuum arc melting can reduce the oxidation during smelting copper alloy, while cooling velocity is fast, can obtain wear-resisting
The better contact material of property.
Specific embodiment
Embodiment 1
（1）Using direct current magnetron sputtering process in graphene（Number of plies 1-10）Surface deposited metal copper is prepared into copper-plated graphite
Alkene.Removal surface film oxide first is ground with fine sandpaper before the copper target material installation that purity is 99.99%, then is cleaned with acetone, is dried
It is dry, 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, remove the metal oxide of target material surface and other impurity, are ensured
The purity of follow-up graphene surface deposition copper film.The technological parameter of magnetically controlled DC sputtering is：Reach 0.1*10 in vacuum degree-3 Pa
When, it is passed through the argon gas of purity 99.99%, operating air pressure 0.5Pa, sputtering power 100W, sedimentation time 30min.
（2）200 mesh alloy powders are made using centrifugal atomization in copper-rare earth alloy, the rare earth in copper-rare earth is rich lanthanum
Norium, weight content are the 0.03% of copper-rare earth alloy.
（3）By copper-plated graphite alkene and alloy powder by weight 0.1:99.9 loading ball mills mix powder, are made uniformly mixed
Powder.The technological parameter of ball mill is：Ball grinder first vacuumizes is passed through argon gas protection again, and rotating speed 100r/min, ball milling 15 divides
Clock stops 5 minutes, alternate rotation clockwise, counterclockwise, amounts to mixed powder time 6h.
（4）By step（3）The powder of mixing is put into cold moudling in mold, pressure 400MPa, 5 minutes dwell times.
（5）Molding blank carries out vacuum arc melting, vacuum degree 1.0*10-3Pa, working gas are argon gas, operating air pressure
For 0.02Pa, copper-plated graphite alkene/copper-based electrical contact material is made in smelting time 2 minutes.
Embodiment 2
（1）Using direct current magnetron sputtering process in graphene（Number of plies 1-10）Surface deposited metal copper is into copper-plated graphite alkene.
Removal surface film oxide first is ground with fine sandpaper before the copper target material installation that purity is 99.99%, then is cleaned with acetone, is dried,
5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, remove the metal oxide of target material surface and other impurity, are ensured follow-up
Graphene surface deposits the purity of copper film.The technological parameter of magnetically controlled DC sputtering is：Reach 1*10 in vacuum degree-3During Pa, it is passed through
The argon gas of purity 99.99%, operating air pressure 1.2Pa, sputtering power 150W, sedimentation time 5min.
（2）300 mesh alloy powders are made using ultrasonic atomizatio method in copper-rare earth alloy, the rare earth in copper-rare earth is rich lanthanum
Norium, weight content are the 3.0% of copper-rare earth alloy.
（3）By copper-plated graphite alkene and alloy powder by weight 2.0：98.0 loading ball mills mix powder, are made uniformly mixed
Powder.The technological parameter of ball mill is：Ball grinder first vacuumizes is passed through argon gas protection again, and rotating speed 250r/min, ball milling 20 divides
Clock stops 5 minutes, alternate rotation clockwise, counterclockwise, amounts to mixed powder time 2h.
（4）By step（3）The powder of mixing is put into cold moudling in mold, pressure 600MPa, 3 minutes dwell times.
（5）Molding blank carries out vacuum arc melting, vacuum degree 3.0*10-3Pa, working gas are argon gas, operating air pressure
For 0.1Pa, copper-plated graphite alkene/copper-based electrical contact material is made in smelting time 1 minute.
Embodiment 3
（1）Using direct current magnetron sputtering process in graphene（Number of plies 1-10）Surface deposited metal copper is into copper-plated graphite alkene.
Removal surface film oxide first is ground with fine sandpaper before the copper target material installation that purity is 99.99%, then is cleaned with acetone, is dried,
5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, remove the metal oxide of target material surface and other impurity, are ensured follow-up
Graphene surface deposits the purity of copper film.The technological parameter of magnetically controlled DC sputtering is：Reach 0.3*10 in vacuum degree-3During Pa, lead to
Enter the argon gas of purity 99.99%, operating air pressure 0.8Pa, sputtering power 120W, sedimentation time 15min.
（2）200 mesh alloy powders are made using gas atomization in copper-rare earth alloy, the rare earth in copper-rare earth is rich lanthanum
Norium, weight content are the 0.3% of copper-rare earth alloy.
（3）By copper-plated graphite alkene and alloy powder by weight 1.0:99.0 loading ball mills mix powder, are made uniformly mixed
Powder.The technological parameter of ball mill is：Ball grinder first vacuumizes is passed through argon gas protection again, and rotating speed 150r/min, ball milling 20 divides
Clock stops 5 minutes, alternate rotation clockwise, counterclockwise, amounts to mixed powder time 3h.
（4）By step（3）The powder of mixing is put into cold moudling in mold, pressure 500MPa, 3 minutes dwell times.
（5）Molding blank carries out vacuum arc melting, vacuum degree 2.0*10-3Pa, working gas are argon gas, operating air pressure
For 0.03Pa, copper-plated graphite alkene/copper-based electrical contact material is made in smelting time 1 minute.
Embodiment 4
200 mesh alloy powders are made using gas atomization in copper-rare earth alloy, the rare earth in copper-rare earth is that rich cerium mixes
Rare earth metal is closed, weight content is the 1.0% of copper-rare earth alloy.Graphene is 0.5 with weight alloy ratio:99.5 other conditions
Copper-plated graphite alkene/copper-based electrical contact material is made with embodiment 3 in parameter.
Embodiment 5
200 mesh alloy powders are made using gas atomization in copper-rare earth alloy, the rare earth in copper-rare earth is that rich cerium mixes
Rare earth metal is closed, weight content is the 2.0% of copper-rare earth alloy.Graphene is 1.0 with weight alloy ratio:99.0 other conditions
Copper-plated graphite alkene/copper-rare earth base electric contact material is made with embodiment 3 in parameter.
Comparative example 1
The non-copper facing of graphene, 0.5wt% graphenes are added in fine copper, other conditions with embodiment 3, be made graphene/
Copper-based electrical contact material.
Comparative example 2
Graphene is not added with, copper-rare-earth-based electricity is made in copper-rare earth alloy that cerium-rich mischmetal weight content is 1.0%
Contact material.Preparation process is the same as embodiment 3.
Manufactured composite material parameters such as following table：
In embodiment, add in copper-plated graphite alkene/copper-based electrical contact material, with comparative example 1 made of copper-plated graphite alkene
Graphene is only added in, electrical contact material made of rare earth is not added in and compares, hardness improves；With only adding in comparative example 2
Enter rare earth, do not add in electrical contact material made of graphene and compare, hardness significantly improves, and electrical conductivity also improves.
The present invention improves hardness, electrical conductivity and the arc ablation resistance of electrical contact by adding copper-plated graphite alkene, by adding
Rare earth is added to substantially increase the inoxidizability of electrical contact material, obtains the good electrical contact material of comprehensive performance.
Claims (8)
1. a kind of copper-plated graphite alkene/copper-based electrical contact material, which is characterized in that it is 0.1- that electrical contact material, which includes weight content,
2.0% copper-plated graphite alkene and copper-rare earth alloy of 98.0-99.9%, the weight ratio that rare earth accounts for copper-rare earth alloy are 0.03-
3.0%；The copper-plated graphite alkene be using direct current magnetron sputtering process graphene surface deposited metal copper into;
It is characterized by comprising following steps：
（1）Using direct current magnetron sputtering process in graphene surface deposited metal copper into copper-plated graphite alkene；
（2）200-300 mesh copper alloy powders are made using atomization in copper-rare earth alloy；
（3）Copper-plated graphite alkene and copper alloy powder are packed into ball mill and mix powder, uniformly mixed powder is made；
（4）By step（3）The powder of mixing is put into cold moudling in mold；
（5）Shaping blank carries out vacuum arc melting, and copper-plated graphite alkene/copper-based electrical contact material is made.
2. electrical contact material according to claim 1, which is characterized in that the rare earth is in lanthanum, cerium, yttrium, praseodymium and neodymium
It is one or more of.
3. electrical contact material according to claim 1, which is characterized in that the step（1）Middle graphene is N layers, N 1-
10。
4. electrical contact material according to claim 1, which is characterized in that the step（1）The work of middle magnetically controlled DC sputtering
Skill parameter is：Target is the copper target that purity is 99.99%, reaches 0.1*10 in vacuum degree-3-1.0*10-3During Pa, purity is passed through
99.99% argon gas, operating air pressure 0.5-1.2Pa, sputtering power 100-150W, sedimentation time 5-30min.
5. electrical contact material according to claim 1, which is characterized in that the step（2）Middle atomization is selected from gas mist
One kind of change method, centrifugal atomization and ultrasonic atomizatio method.
6. electrical contact material according to claim 1, which is characterized in that the step（3）The technological parameter of middle ball mill
For：Ball grinder first vacuumizes and is passed through argon gas protection again, rotating speed 100-250r/min, and ball milling 15-20 minutes stops 5 minutes, up time
Pin, alternate rotation counterclockwise amount to mixed powder time 2-6h.
7. electrical contact material according to claim 1, which is characterized in that step（4）Described in cold moudling pressure be
400-600MPa, dwell time 3-5 minute.
8. electrical contact material according to claim 1, which is characterized in that the step（5）Middle vacuum arc melting is melted
Furnace vacuum degree 1.0*10-3-3.0*10-3Pa, working gas are argon gas, operating air pressure 0.02Pa-0.1Pa, smelting time 1-
2 minutes.
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| CN106367695A (en) * | 2016-08-31 | 2017-02-01 | 宁波新睦新材料有限公司 | Preparation method of copper-based composite material for cylinder sleeve |
| CN111676387A (en) * | 2020-06-08 | 2020-09-18 | 南昌航空大学 | Novel electrical contact material with RGO/Cu-Zr-La as component and preparation method thereof |
| CN112593112B (en) * | 2020-10-23 | 2021-09-24 | 淮阴工学院 | Multiphase friction-reducing resistance-increasing copper alloy and preparation method thereof |
| CN115786753B (en) * | 2023-02-02 | 2023-05-30 | 泰州泰锦合金材料有限公司 | Tellurium copper alloy material containing rare earth metal and preparation method thereof |
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| CN105140057A (en) * | 2015-07-03 | 2015-12-09 | 济南大学 | Nitride enhanced copper-based electrical contact composite material |
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