CN105609159B - A kind of copper-plated graphite alkene enhancing copper-based electrical contact material and preparation method thereof - Google Patents
A kind of copper-plated graphite alkene enhancing copper-based electrical contact material and preparation method thereof Download PDFInfo
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- CN105609159B CN105609159B CN201610106143.XA CN201610106143A CN105609159B CN 105609159 B CN105609159 B CN 105609159B CN 201610106143 A CN201610106143 A CN 201610106143A CN 105609159 B CN105609159 B CN 105609159B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
- H01R13/02—Contact members
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
- H01R13/02—Contact members
- H01R13/03—Contact members characterised by the material, e.g. plating, or coating materials
Abstract
The present invention relates to a kind of copper-plated graphite alkene enhancing copper-based electrical contact material and preparation method thereof.Electrical contact material includes the copper-plated graphite alkene and 95.0 99.9% Cu-RE alloys that weight content is 0.1 5.0%, and the weight ratio that rare earth accounts for Cu-RE alloys is 0.03 2.0%.Preparation method is：Graphene copper facing, powder by atomization, ball milling mix powder, cold moudling, sintering, post forming, sintering.The present invention adds copper-plated graphite alkene reinforcement as skeleton in copper alloy, material is had high rigidity, high-wearing feature, mechanical shock resistance, resistance fusion welding.The addition of rare earth, improves the inoxidizability and resistance to electrical arc erosion ability of copper alloy electric contact material.
Description
Technical field
Strengthen copper-based electrical contact material the present invention relates to a kind of electrical contact material, more particularly to a kind of copper-plated graphite alkene, with
And the preparation method of above-mentioned material.
Background technology
Electrical contact material is the critical component of instrument and meter, and the life-span and functional reliability to instrument and meter play important
Effect.Copper-base contact material is close due to cheap, conductive, heat conductivility and silver, partly replaces silver-based contact in recent years,
Reduce the loss of noble silver.But, because copper contact material is easily aoxidized, cupric oxide and oxidation of the generation with low-resistivity
It is cuprous, increase the contact resistance of contact elements, make its in use easily heating, cause contact material reliability and
Service life is reduced.
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.Because graphene increases
The addition of strong phase, makes the composited contact material have than other more preferable conductive, thermal conductivity of enhancing phase composited contact material
Can be with higher hardness and wearability.But because the use of poisonous and hazardous hydrazine hydrate being reducing agent, 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 of China.Rare earth element is more active, is added in metallic copper, and can deaerate slagging-off, crystal grain thinning, improves
The decay resistance and abrasion resistance properties of copper alloy.
Publication No. 105063413A, discloses a kind of copper-base contact material and preparation technology, and copper-base contact material is included
Following weight composition, 0.2-0.6% magnesium, 0.05-0.3% antimony, 0.05-0.4% bismuth, 0.05- 0.3% tin,
The copper of 0.05-0.3% chromium, 0.005-0.05% boron, 0.02-0.1% lanthanums, 0.2-0.5% graphite and surplus, it is suitable by adding
The boron of amount, tin, antimony powder end, improve the intensity and wearability of electrical contact manufactured goods.
The Chinese patent of Publication No. 101145450, discloses a kind of special powder copper alloy electric contact material, its feature
It is：The composition of the material, component by weight percentage is：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, anti-oxidant of copper alloy by the addition of rare earth or rare earth oxide
Property, but simultaneously because the material addition of the low electric conductivity 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
Conducted electricity very well it is an object of the invention to provide one kind, contact resistance it is low and stably, resistance fusion welding can good, hardness
Copper-plated graphite alkene enhancing 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 scheme.
A kind of copper-plated graphite alkene strengthens copper-based electrical contact material, it is characterised in that including weight content be 0.1-5.0%'s
Copper-rare earth alloy of copper-plated graphite alkene and 95.0-99.9%, the weight ratio that rare earth accounts for copper-rare earth alloy is 0.03-2.0%.
Preferably, the copper-plated graphite alkene be using direct current magnetron sputtering process graphenic surface deposited metal copper into.
Preferably, one or more of the rare earth in lanthanum, cerium, yttrium, praseodymium and neodymium.Rare earth metal be lanthanum, cerium, praseodymium and
During the mixing of neodymium, referred to 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 graphenic 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 loaded into ball mill and mix powder, mixed uniformly powder is made；
（4）By step（3）The powder of mixing is put into cold moudling in mould, sintering；
（5）Graphene enhancing copper-rare earth base electric contact material is made in post forming, sintering.
Preferably, the step（1）Middle graphene is N layers, and N is 1-10.
The step（1）In, purity is first polished before being installed for 99.99% copper target with fine sandpaper, removes surface oxidation
Film, then cleaned with acetone, is dried, and 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, using baffle plate by target and graphene
Separate, remove the metal oxide and other impurity of target material surface, it is ensured that follow-up graphenic surface deposits the purity of copper film.Direct current
The technological parameter of magnetron sputtering is：Target is the copper target that purity is 99.99%, and 0.1*10 is reached in vacuum-3-1.0*10-3Pa
When, it is passed through the argon gas of purity 99.99%, operating air pressure 0.5-1.2Pa, sputtering power 100-150W, sedimentation time is 5-30min.
Preferably, the step（2）Middle atomization is selected from the one of gas atomization, centrifugal atomization and ultrasonic atomizatio method
Kind.
Preferably, the step（3）The technological parameter of middle ball mill is：Ball grinder is first vacuumized is passed through argon gas protection again,
Rotating speed 100-250r/min, ball milling 15-20 minutes stops 5 minutes, alternate rotation clockwise, counterclockwise, amounts to mixed powder time 2-
6h.To prevent that ball grinder need to be vacuumized before the oxidation of copper, ball milling, and it is passed through argon gas protection.In the ball milling parameter scope of the present invention
It is interior, the distribution of graphene and metal alloy mixed-powder can be controlled well.
Preferably, step（4）Described in cold moudling pressure be 400-600MPa, dwell time 3-5 minute, cold moudling
Part is sintered under argon gas or hydrogen shield, vacuum 1.0*10-3-5.0*10-1Pa, 700-900 DEG C of sintering temperature, soaking time
2-4 hours.
Preferably, it is characterised in that the step（5）Middle post forming pressure is 200-500MPa, dwell time 3-5 point
Clock, post forming part is sintered under argon gas or hydrogen shield, vacuum 1.0*10-3-5.0*10-1Pa, sintering temperature 700-900
DEG C, soaking time 2-4 hours.
The present invention useful achievement be：
（1）The present invention adds graphene reinforcement as skeleton in copper alloy, material is had high rigidity, high abrasion
Property, mechanical shock resistance, arc resistant ablation property.
（2）Copper is deposited in graphenic 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 interface wet ability, is conducive to obtaining good interface combination,
Conductivity of composite material, heat conductivility, anti electric arc corrosion is further improved, preferably meet the performance requirement of electrical contact.
（4）The addition of rare earth, improves the inoxidizability and resistance to electrical arc erosion ability of copper alloy electric contact material.
（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）Copper prepared by repressing and re-sintering-rare earth base composite material consistency is high, is conducive to obtaining high combination property.
（7）Cold moudling sintering preparation technology is simple, and production cost is low, is adapted to large-scale mass production.
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.Purity is first ground removal surface film oxide before being installed for 99.99% copper target material with fine sandpaper, then is cleaned with acetone, dries
It is dry, 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, are separated target with graphene using baffle plate, target material surface is removed
Metal oxide and other impurity, it is ensured that follow-up graphenic surface deposits the purity of copper film.The technique ginseng of magnetically controlled DC sputtering
Number is：0.1*10 is reached in vacuum-3During Pa, the argon gas of purity 99.99%, operating air pressure 0.5Pa, sputtering power are passed through
100W, sedimentation time is 30min.
（2）Rare earth copper-rare earth alloy being made of centrifugal atomization in 200 mesh alloy powders, copper-rare earth is rich cerium
Norium, weight content is the 0.03% of copper-rare earth alloy.
（3）By copper-plated graphite alkene and alloy powder by weight 0.1:99.9, which load ball mill, mixes powder, is made well mixed
Powder.The technological parameter of ball mill is：Ball grinder is first vacuumized is passed through argon gas protection, rotating speed 100r/min, 15 points of ball milling again
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 mould, and pressure is 400MPa, 5 minutes dwell times,
Cold moudling part is sintered under argon gas protection, vacuum 1.0*10-3Pa, 900 DEG C of sintering temperature, soaking time 2 hours.
（5）Blank post forming, pressure is 200MPa, and 5 minutes dwell times, post forming part burns under argon gas protection
Knot, vacuum 1.0*10-3Copper-plated graphite alkene enhancing copper-based electrical contact material is made in Pa, 900 DEG C of sintering temperature, soaking time 2 hours
Material.
Embodiment 2
（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.Purity is first ground removal surface film oxide before being installed for 99.99% copper target material with fine sandpaper, then is cleaned with acetone, dries
It is dry, 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, are separated target with graphene using baffle plate, target material surface is removed
Metal oxide and other impurity, it is ensured that follow-up graphenic surface deposits the purity of copper film.The technique ginseng of magnetically controlled DC sputtering
Number is：1*10 is reached in vacuum-3During Pa, the argon gas of purity 99.99% is passed through, operating air pressure 1.2Pa, sputtering power 150W,
Sedimentation time is 5min.
（2）Rare earth copper-rare earth alloy being made of ultrasonic atomizatio method in 300 mesh alloy powders, copper-rare earth is rich lanthanum
Norium, weight content is the 2% of copper-rare earth alloy.
（3）By copper-plated graphite alkene and alloy powder by weight 5.0：95.0, which load ball mill, mixes powder, is made well mixed
Powder.The technological parameter of ball mill is：Ball grinder is first vacuumized is passed through argon gas protection, rotating speed 250r/min, 20 points of ball milling again
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 mould, and pressure is 600MPa, 3 minutes dwell times,
Cold moudling part is sintered under hydrogen shield, vacuum 5.0*10-1Pa, 700 DEG C of sintering temperature, soaking time 4 hours.
（5）Blank post forming, pressure is 500MPa, and 3 minutes dwell times, post forming part burns under hydrogen shield
Knot, vacuum 5.0*10-1Copper-plated graphite alkene enhancing copper-based electrical contact material is made in Pa, 700 DEG C of sintering temperature, soaking time 4 hours
Material.
Embodiment 3
（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.Purity is first ground removal surface film oxide before being installed for 99.99% copper target material with fine sandpaper, then is cleaned with acetone, dries
It is dry, 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, are separated target with graphene using baffle plate, target material surface is removed
Metal oxide and other impurity, it is ensured that follow-up graphenic surface deposits the purity of copper film.The technique ginseng of magnetically controlled DC sputtering
Number is：When vacuum reaches 0.3*10-3 Pa, the argon gas of purity 99.99%, operating air pressure 0.8Pa, sputtering power are passed through
120W, sedimentation time is 5min.
（2）Rare earth copper-rare earth alloy being made of gas atomization in 200 mesh alloy powders, copper-rare earth is rich cerium
Norium, weight content is the 0.5% of copper-rare earth alloy.
（3）By copper-plated graphite alkene and alloy powder by weight 0.5:99.5, which load ball mill, mixes powder, is made well mixed
Powder.The technological parameter of ball mill is：Ball mill is first vacuumized is passed through argon gas protection, rotating speed 150r/min, 20 points of ball milling again
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 mould, and pressure is 500MPa, 3 minutes dwell times,
Cold moudling part is sintered under argon gas protection, vacuum 1.0*10-1Pa, 750 DEG C of sintering temperature, soaking time 2 hours.
（5）Blank post forming, pressure is 500MPa, and 3 minutes dwell times, post forming part burns under argon gas protection
Knot, vacuum 1.0*10-3Copper-plated graphite alkene enhancing copper-based electrical contact material is made in Pa, 750 DEG C of sintering temperature, soaking time 2 hours
Material.
Embodiment 4
200 mesh alloys are made using gas atomization for 1.0% copper-rare earth alloy in cerium-rich mischmetal weight content
Powder, graphene is 0.5 with weight alloy ratio:99.5, copper-plated graphite alkene enhancing copper is made in other conditions parameter be the same as Example 3
Base electric contact material.
Embodiment 5
200 mesh alloys are made using gas atomization for 0.5% copper-rare earth alloy in cerium-rich mischmetal weight content
Powder, graphene is 1.0 with weight alloy ratio:99.0, other conditions parameter be the same as Example 3, be made copper-plated graphite alkene enhancing copper-
Rare earth base electric contact material.
Comparative example 1
The non-copper facing of graphene, the graphene of weight content 0.5% is added in fine copper, and other conditions be the same as Example 3 is made
Graphene strengthens copper-based electrical contact material.
Comparative example 2
Graphene is not added with, copper-rare earth is made for 0.5% copper-rare earth alloy in rich cerium misch metal weight content
Base electric contact material.Preparation technology be the same as Example 3.
The composite parameters such as following table being made：
In embodiment, copper-plated graphite alkene enhancing copper-rare earth base electric contact material that copper-plated graphite alkene is made is added, with contrast
Graphene is only added in example 1, the electrical contact material that rare earth is made is not added and is compared, hardness improves；With comparative example 2
In only add rare earth metal, the electrical contact material that graphene is made is not added and is compared, hardness is significantly improved, and electrical conductivity also has necessarily
Raising.
The present invention improves hardness, electrical conductivity and the arc ablation resistance of electrical contact by adding copper-plated graphite alkene, by adding
Plus rare earth improves the inoxidizability of electrical contact material, the good electrical contact material of combination property is obtained.
Claims (9)
1. a kind of copper-plated graphite alkene strengthens the preparation method of copper-based electrical contact material, it is characterised in that electrical contact material includes weight
It is 0.1-0.5% copper-plated graphite alkene and 99.5-99.9% copper-rare earth alloy to measure content, and rare earth accounts for the weight of copper-rare earth alloy
Than for 0.03-2.0%；
The preparation method of electrical contact material, comprises the following steps：（1）Deposited using direct current magnetron sputtering process in graphenic surface
Copper-plated graphite alkene is made in metallic copper；（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 loaded into ball mill and mix powder, well mixed powder is made；（4）By step（3）Mixing
Powder is put into cold moudling in mould, sintering；（5）Blank post forming, sintering is made graphene enhancing copper-rare-earth-based electricity and touched
Head material.
2. the preparation method of electrical contact material according to claim 1, it is characterised in that the copper-plated graphite alkene is to use
Direct current magnetron sputtering process graphenic surface deposited metal copper into.
3. the preparation method of electrical contact material according to claim 1, it is characterised in that the rare earth be lanthanum, cerium, yttrium,
One or more in praseodymium and neodymium.
4. the preparation method of electrical contact material according to claim 1, it is characterised in that the step（1）Middle graphene
For N layers, N is 1-10.
5. the preparation method of electrical contact material according to claim 1, it is characterised in that the step（1）Middle DC magnetic
Controlling the technological parameter sputtered is：Target is the copper target that purity is 99.99%, and 0.1*10 is reached in vacuum-3-1.0*10-3During Pa,
It is passed through the argon gas of purity 99.99%, operating air pressure 0.5-1.2Pa, sputtering power 100-150W, sedimentation time is 5-30min.
6. the preparation method of electrical contact material according to claim 1, it is characterised in that the step（2）Middle atomization
One kind selected from gas atomization, centrifugal atomization and ultrasonic atomizatio method.
7. the preparation method of electrical contact material according to claim 1, it is characterised in that the step（3）Middle ball mill
Technological parameter be：Ball grinder first vacuumizes and is passed through argon gas protection again, and rotating speed 100-250r/min, ball milling 15-20 minutes stops
5 minutes, alternate rotation clockwise, counterclockwise amounted to mixed powder time 2-6h.
8. the preparation method of electrical contact material according to claim 1, it is characterised in that step（4）Described in be cold-pressed into
Type pressure is 400-600MPa, and dwell time 3-5 minute, cold moudling part is sintered under vacuum, argon gas or hydrogen shield, vacuum
Spend 1.0*10-3-5.0*10-1Pa, 700-900 DEG C of sintering temperature, soaking time 2-4 hours.
9. the preparation method of electrical contact material according to claim 1, it is characterised in that the step（5）In it is secondary into
Type pressure is 200-500MPa, and dwell time 3-5 minute, cold moudling part is sintered under vacuum, argon gas or hydrogen shield, vacuum
Spend 1.0*10-3-5.0*10-1Pa, 700-900 DEG C of sintering temperature, soaking time 2-4 hours.
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| CN107755703A (en) * | 2017-09-13 | 2018-03-06 | 大同新成新材料股份有限公司 | A kind of method for preparing pantograph graphene composite material |
| CN108817727A (en) * | 2018-07-19 | 2018-11-16 | 河南科技大学 | Pyrolysismethod synthesis is by force in conjunction with the high-strength Sn-Ag-Cu-RE system composite soldering and preparation method of the enhancing of copper-plated graphite alkene |
| CN112349667A (en) * | 2019-08-09 | 2021-02-09 | 昆山微电子技术研究院 | Preparation method of graphene/copper composite metal interconnection line |
| CN110695372B (en) * | 2019-10-10 | 2022-05-06 | 天津大学 | Preparation method for improving copper-graphene interface by using rare earth elements |
| CN112239350B (en) * | 2020-10-19 | 2022-08-05 | 西安工程大学 | Preparation method of copper tin oxide contact material |
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| CN102779988A (en) * | 2012-08-06 | 2012-11-14 | 常州大学 | Composite negative electrode material coating modification method of lithium ion battery |
| CN102925741A (en) * | 2012-11-08 | 2013-02-13 | 镇江中孚复合材料有限公司 | Copper base solid self-lubricating composite material and method for preparing the same |
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