CN105575459A - Copper coated graphene reinforced copper base electric contact material preparation method - Google Patents
Copper coated graphene reinforced copper base electric contact material preparation method Download PDFInfo
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- CN105575459A CN105575459A CN201610106148.2A CN201610106148A CN105575459A CN 105575459 A CN105575459 A CN 105575459A CN 201610106148 A CN201610106148 A CN 201610106148A CN 105575459 A CN105575459 A CN 105575459A
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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
- 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
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Abstract
The invention relates to a copper coated graphene reinforced copper base electric contact material preparation method. The method comprises steps of graphene copper coating, copper smelting, adding rare earth and metal to a copper melt, graphene alloy melt copper coating, casting molding, stress relief annealing, and processing and forming. As the rare earth is added to the copper alloy, the oxidation resistance and the anti-arc burning ability of the copper alloy electric contact material are improved, the copper coated graphene improves the interfacial wettability between the graphene and the metal, good interface combination is acquired, the electrical conductivity, the thermal conductivity and the anti-arc erosion of the composite material are further improved, and performance requirements of the electric contact can be better met.
Description
Technical field
The present invention relates to a kind of preparation method of electrical contact material, particularly relate to the preparation method that a kind of copper-plated graphite alkene strengthens copper-based electrical contact material.
Background technology
Electrical contact material is the critical component of instrument and meter, plays an important role to life-span of instrument and meter and functional reliability.Copper-base contact material due to cheap, conduction, heat conductivility is close with silver, part replaces silver-based contact in recent years, the loss of minimizing noble silver.But, because copper contact material is very easily oxidized, generate cupric oxide and the cuprous oxide with low-resistivity, increase the contact resistance of contact elements, make it in use easily generate heat, cause the reliability of contact material and useful life to be reduced.
Existing patent documentation (publication number 102385938A), discloses a kind of metal matrix graphene composite electrical contact material and preparation method thereof, contact material, comprises the Graphene of 0.02-10wt%, and all the other are metal matrix material.Due to adding of Graphene wild phase, this composited contact material is had better conduct electricity than other wild phase composited contact materials, the hardness of heat conductivility and Geng Gao and resistance to wear.But because using poisonous and hazardous hydrazine hydrate for reducing agent, be difficult to meet environmental requirement.
Rare earth, at China's rich reserves, accounts for 80% of global rare earth reserves, and the high-quality non-ferrous alloy that exploitation rare earth element adds is the exclusive advantage of China.Rare earth element is relatively more active, adds in metallic copper, can degassedly remove the gred, crystal grain thinning, improves decay resistance and the abrasion resistance properties of copper alloy.
Publication number is 105063413A, discloses a kind of copper-base contact material and preparation technology, and copper-base contact material comprises 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 chromium of 0.05-0.3%, 0.005-0.05% boron, 0.02-0.1% lanthanum, the copper of 0.2-0.5% graphite and surplus, by adding appropriate boron, tin, antimony powder end, improve intensity and the resistance to wear of electrical contact manufactured goods.
Publication number is the Chinese patent of 101145450, disclose a kind of special powder copper alloy electric contact material, it is characterized in that: the composition of described material, component is by weight percentage: 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 and inevitable impurity.
Above-mentioned two patents all improve corrosion resistance, the non-oxidizability of copper alloy by the interpolation of rare earth or rare earth oxide, but simultaneously because the material of the low electric conductivity such as ceramic particle, chromium adds, reduce the conduction of copper contact material, heat conductivility to a certain extent, be therefore difficult to the copper-base contact material obtaining excellent combination property.
Summary of the invention
The object of the present invention is to provide a kind ofly to conduct electricity very well, contact resistance is low and stable, resistance fusion welding can good, hardness is high and the copper-plated graphite alkene of easy preparation strengthens the preparation method of copper-based electrical contact material.
The present invention is realized by technical scheme below.
Copper-plated graphite alkene strengthens a preparation method for copper-based electrical contact material, it is characterized in that comprising the following steps:
(1) direct current magnetron sputtering process is adopted to become copper-plated graphite alkene in graphenic surface plated metal copper;
(2) purity is copper melting in intermediate frequency furnace of 99.9%, adds weight of copper 0.05-2.0% rare earth and 0.5-5.0% metal X, fully stir in copper melts, and make copper-rare earth-X-alloy melt, described X is selected from one or more in zinc, aluminium, nickel, bismuth and antimony;
(3) copper-plated graphite alkene adds in copper-rare earth-X-alloy melt, and the weight ratio of copper-plated graphite alkene and copper-rare earth-X-alloy melt is 1.0-5.0:95-99.0, and after fully stirring, composite material is made in cast molding;
(4) composite material stress relief annealing, extruding or rolling machine-shaping, make copper-plated graphite alkene and strengthen copper-based electrical contact material.
Preferably, in described step (1), the number of plies of Graphene is N layer, and N is 1-10.
Described step (1) adopts direct current magnetron sputtering process to be prepared into copper-plated graphite alkene at Graphene (number of plies 1-10) surface deposition metallic copper.Purity is first carry out grinding with fine sandpaper before the copper target installation of 99.99% to remove surface film oxide, clean with acetone again, dry, 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, remove metal oxide and other impurity of target material surface, ensure the purity of follow-up graphenic surface depositing copper film.The technological parameter of magnetically controlled DC sputtering is: target to be purity be 99.99% copper target, reach 0.1*10 in vacuum degree
-3-1.0*10
-3during Pa, pass into the argon gas of purity 99.99%, operating air pressure is 0.8-1.5Pa, sputtering power 80-160W, and sedimentation time is 5-30min.
Preferably, described step (2) middle rare earth is selected from one or more in lanthanum, cerium, yttrium, praseodymium and neodymium, and rare earth adopts Copper Foil parcel to add, and adopts graphite cover to be directly pressed into below melt liquid level, keeps fully stirring after 3-5 minute.
More preferably, step (2) middle rare earth is selected from one or both in lanthanum, cerium.
Preferably, in step (4), annealing temperature is 200-300 DEG C, annealing time 2 hours.
Preferably, rolling machine-shaping after composite material annealing in step (4), rolling temperature is 600-850 DEG C, rolling reduction 80%-90%.
Preferably, in step (4), after composite material annealing, extrusion process is shaping, extrusion temperature 600-850 DEG C, extrusion ratio 50:1-150:1.
Useful achievement of the present invention is:
(1) the present invention adds Graphene reinforcement as skeleton in copper alloy, makes material have high rigidity, high-wearing feature, mechanical shock resistance, arc resistant ablation property.
(2) by direct current magnetron sputtering process at graphenic surface deposited copper, Graphene can be avoided and reunite in mixed powder process as nano particle.Meanwhile, copper-plated graphite alkene improves Graphene and intermetallic interface wet ability, is conducive to obtaining good interface and combines, conductivity of composite material, heat conductivility, anti electric arc corrosion are improved further, meets the performance requirement of electrical contact better.
(3) the adding of rare earth metal, the non-oxidizability of copper alloy electric contact material and resistance to electrical arc erosion ability is improved.
(4) conventional cast technique, technique is simple, is conducive to industrialized production.
Embodiment
Embodiment 1
(1) direct current magnetron sputtering process is adopted to be prepared into copper-plated graphite alkene at Graphene (number of plies 1-10) surface deposition metallic copper.Purity is first carry out grinding with fine sandpaper before the copper target installation of 99.99% to remove surface film oxide, clean with acetone again, dry, 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, remove metal oxide and other impurity of target material surface, ensure the purity of follow-up graphenic surface depositing copper film.The technological parameter of magnetically controlled DC sputtering is: reach 0.1*10 in vacuum degree
-3during Pa, pass into the argon gas of purity 99.99%, operating air pressure 0.8Pa, sputtering power 80W, sedimentation time is 30min.
(2) purity is copper melting in intermediate frequency furnace of 99.9%, add weight of copper content 0.05% cerium and 0.5% metallic zinc in copper melts, cerium adopts Copper Foil parcel to add, and adopts graphite cover to be directly pressed into below melt liquid level, keep fully stirring after 3-5 minute, make copper-cerium-kirsite melt.
(3) copper-plated graphite alkene adds in copper-cerium-kirsite melt, and the weight ratio of copper-plated graphite alkene and copper-cerium-kirsite melt is 1.0:99.0, and after fully stirring, composite material is made in cast molding.
(4) composite material stress relief annealing, annealing temperature is 200 DEG C, annealing time 2 hours.Material extrusion modling after annealing, extrusion temperature 600 DEG C, extrusion ratio 50:1, makes copper-plated graphite alkene and strengthens copper-based electrical contact material.
Embodiment 2
(1) direct current magnetron sputtering process is adopted to make copper-plated graphite alkene at Graphene (number of plies 1-10) surface deposition metallic copper.Purity is first carry out grinding with fine sandpaper before the copper target installation of 99.99% to remove surface film oxide, clean with acetone again, dry, 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, remove metal oxide and other impurity of target material surface, ensure the purity of follow-up graphenic surface depositing copper film.The technological parameter of magnetically controlled DC sputtering is: reach 1*10 in vacuum degree
-3during Pa, pass into the argon gas of purity 99.99%, operating air pressure is at 1.5Pa, and sputtering power is at 160W, and sedimentation time is 5min.
(2) purity is copper melting in intermediate frequency furnace of 99.9%, add weight of copper content 2.0% Rare Earth Lanthanum and 5.0% metallic zinc in copper melts, Rare Earth Lanthanum adopts Copper Foil parcel to add, and adopts graphite cover to be directly pressed into below melt liquid level, keep fully stirring after 3-5 minute, make copper-lanthanum-kirsite melt.
(3) copper-plated graphite alkene adds in copper-lanthanum-kirsite melt, and the weight ratio of copper-plated graphite alkene and copper-lanthanum-kirsite melt is 5.0:95.0, and after fully stirring, composite material is made in cast molding.
(4) composite material stress relief annealing, annealing temperature is 300 DEG C, annealing time 2 hours.Material extrusion modling after annealing, extrusion temperature 850 DEG C, extrusion ratio 150:1, makes copper-plated graphite alkene and strengthens copper-based electrical contact material.
Embodiment 3
(1) direct current magnetron sputtering process is adopted to make copper-plated graphite alkene at Graphene (number of plies 1-10) surface deposition metallic copper.Purity is first carry out grinding with fine sandpaper before the copper target installation of 99.99% to remove surface film oxide, clean with acetone again, dry, 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, remove metal oxide and other impurity of target material surface, ensure the purity of follow-up graphenic surface depositing copper film.The technological parameter of magnetically controlled DC sputtering is: reach 0.3*10 in vacuum degree
-3during Pa, pass into the argon gas of purity 99.99%, operating air pressure is at 1.0Pa, and sputtering power is at 100W, and sedimentation time is 15min.
(2) purity is copper melting in intermediate frequency furnace of 99.9%, add weight of copper content 0.5% Rare Earth Lanthanum and 1.0% metallic zinc in copper melts, Rare Earth Lanthanum adopts Copper Foil parcel to add, and adopts graphite cover to be directly pressed into below melt liquid level, keep fully stirring after 3-5 minute, make copper-lanthanum-kirsite melt.
(3) copper-plated graphite alkene adds in copper-lanthanum-kirsite melt, and the weight ratio of copper-plated graphite alkene and copper-lanthanum-kirsite melt is 2.0:98.0, and after fully stirring, composite material is made in cast molding.
(4) composite material stress relief annealing, annealing temperature is 300 DEG C, annealing time 2 hours.Composite material roll forming after annealing, temperature 600-850 DEG C, deflection is 80-90%, makes copper-plated graphite alkene and strengthens copper-based electrical contact material.
Embodiment 4
Copper-plated graphite alkene adds in copper-1.0% lanthanum-2.0% kirsite melt, and the weight ratio of copper-plated graphite alkene and copper-lanthanum-kirsite melt is 3.0:97.0, and other parameters, with embodiment 3, are made copper-plated graphite alkene and strengthened copper-based electrical contact material.
Embodiment 5
Copper-plated graphite alkene adds in copper-1.0% cerium-1.0% kirsite melt, and the weight ratio of copper-plated graphite alkene and copper-cerium-kirsite melt is 2.0:98.0, and other parameters, with embodiment 3, are made copper-plated graphite alkene and strengthened copper-based electrical contact material.
Comparative example 1
Not copper-plated Graphene adds in copper melts, and Graphene and weight of copper are than being 2.0:98.0, and other parameters, with embodiment 3, are made Graphene and strengthened copper-based electrical contact material.
Comparative example 2
Do not add Graphene, copper-1.0% cerium-1.0% kirsite melt makes copper-based electrical contact material according to embodiment 3 technique.
The composite material parameters made is as following table:
In embodiment, add the copper-plated graphite alkene that copper-plated graphite alkene makes and strengthen copper-based electrical contact material, and only add Graphene in comparative example 1, do not add the electrical contact material that rare earth metal makes and compare, hardness, conductivity all improve; Only add rare earth metal with comparative example 2, do not add the electrical contact material that Graphene makes and compare, hardness significantly improves, and conductivity also improves.
The present invention improves the hardness of electrical contact, conductivity and arc ablation resistance by adding copper-plated graphite alkene, improve the non-oxidizability of electrical contact material, obtaining the electrical contact material that combination property is good by adding rare earth metal.
Claims (8)
1. copper-plated graphite alkene strengthens a preparation method for copper-based electrical contact material, it is characterized in that comprising the following steps:
(1) direct current magnetron sputtering process is adopted to become copper-plated graphite alkene in graphenic surface plated metal copper;
(2) purity is copper melting in intermediate frequency furnace of 99.9%, adds weight of copper 0.05-2.0% rare earth and 0.5-5.0% metal X, fully stir in copper melts, and make copper-rare earth-X-alloy melt, described X is selected from one or more in zinc, aluminium, nickel, bismuth and antimony;
(3) copper-plated graphite alkene adds in copper-rare earth-X-alloy melt, and the weight ratio of copper-plated graphite alkene and copper-rare earth-X-alloy melt is 1.0-5.0:95-99.0, and after fully stirring, composite material is made in cast molding;
(4) composite material stress relief annealing, extruding or rolling machine-shaping, make copper-plated graphite alkene and strengthen copper-based electrical contact material.
2. preparation method according to claim 1, is characterized in that, in described step (1), the number of plies of Graphene is N layer, and N is 1-10.
3. preparation method according to claim 1, is characterized in that, the technological parameter of magnetically controlled DC sputtering is in described step (1): target to be purity be 99.99% copper target, reach 0.1*10 in vacuum degree
-3-1.0*10
-3during Pa, pass into the argon gas of purity 99.99%, operating air pressure is 0.8-1.5Pa, sputtering power 80-160W, and sedimentation time is 5-30min.
4. preparation method according to claim 1, it is characterized in that, step (2) middle rare earth is selected from one or more in lanthanum, cerium, yttrium, praseodymium and neodymium, and rare earth adopts Copper Foil parcel to add, adopt graphite cover to be directly pressed into below melt liquid level, keep fully stirring after 3-5 minute.
5. preparation method according to claim 1, is characterized in that, step (2) middle rare earth be selected from lanthanum, cerium one or both.
6. preparation method according to claim 1, is characterized in that, in step (4), annealing temperature is 200-300 DEG C, annealing time 2 hours.
7. preparation method according to claim 1, is characterized in that, rolling machine-shaping after the annealing of step (4) composite material, temperature is 600-850 DEG C, rolling reduction 80%-90%.
8. preparation method according to claim 1, is characterized in that, after the annealing of step (4) composite material, extrusion process is shaping, extrusion temperature 600-850 DEG C, extrusion ratio 50:1-150:1.
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Cited By (5)
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| CN112701513A (en) * | 2020-12-22 | 2021-04-23 | 慈溪市寅升电器有限公司 | Graphene copper alloy chemical nickel-plating power supply pin and preparation method thereof |
| CN114438365A (en) * | 2021-12-22 | 2022-05-06 | 厦门凯纳石墨烯技术股份有限公司 | High-thermal-conductivity carbon-based metal composite heat dissipation material and preparation method thereof |
| CN115786753A (en) * | 2023-02-02 | 2023-03-14 | 泰州泰锦合金材料有限公司 | Tellurium-copper alloy material containing rare earth metal and preparation method thereof |
| CN115948674A (en) * | 2023-03-14 | 2023-04-11 | 淄博国创中心先进车用材料技术创新中心 | Preparation method of graphene modified magnesium alloy hub |
| CN118492368A (en) * | 2024-07-17 | 2024-08-16 | 合肥工业大学 | Preparation method of reinforced aluminum bismuth alloy doped with surface copper-plated graphene |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN118492368A (en) * | 2024-07-17 | 2024-08-16 | 合肥工业大学 | Preparation method of reinforced aluminum bismuth alloy doped with surface copper-plated graphene |
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