CN105428097B - A kind of Ag-based electrical contact composite and preparation method thereof - Google Patents
A kind of Ag-based electrical contact composite and preparation method thereof Download PDFInfo
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- CN105428097B CN105428097B CN201510983345.8A CN201510983345A CN105428097B CN 105428097 B CN105428097 B CN 105428097B CN 201510983345 A CN201510983345 A CN 201510983345A CN 105428097 B CN105428097 B CN 105428097B
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- electrical contact
- silver
- contact composite
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- graphite alkene
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Classifications
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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
- H01H1/023—Composite material having a noble metal 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
-
- 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
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- 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
Abstract
The present invention relates to a kind of Ag-based electrical contact composite, and the preparation method of this material.Ag-based electrical contact composite is made up of the silvering graphite alkene and 95.0 99.9% silver of weight 0.1 5.0%.Its preparation method is：Graphene is silver-plated, ball milling mix powder, cold moudling, sintering, plastic working shaping.The Ag-based electrical contact composite of the present invention, silvering graphite alkene is added in silver as skeleton, while making material that there is high rigidity, mechanical shock resistance and arc resistant ablation property, avoids the reduction of electric conductivity, thermal conductivity.
Description
Technical field
The present invention relates to a kind of electrical contact material and preparation method thereof, more particularly to a kind of Ag-based electrical contact composite and
Preparation method.
Background technology
Silver/carbon electrical contact material with performances such as fabulous resistance fusion welding, low contact resistances have been supplied in it is low in bear
In load relay and signaling switch, still, because its relatively low mechanical strength, low wearability and anti electric arc corrosion limit
It is more widely applied.
Chinese patent literature 101763956A, it is open（Bulletin）Day 2010.06.30, disclose in silver/graphite material
Method by adding cermet and rare earth element improves its hardness and abrasion resistance properties.
Chinese patent literature 101707146A, it is open（Bulletin）Day 2010.05.12, disclose and pass through carbon material（Buddha's warrior attendant
Stone, graphite, carbon）Deposits tungsten and Argent grain, solve the problems, such as that graphite and matrix wetability are bad, improve hardness and resistance to electric arc
It is ablative.
Chinese patent literature 101866761A, it is open（Bulletin）Day 2010.10.20, disclose and be squeezed into by proprietary
Type technique prepares high-performance silver/graphite composite material.
Existing patent document（Publication number 102385938A）, disclose a kind of metal matrix graphene composite electrical contact material
And preparation method thereof, contact material, the graphene comprising 0.02-10wt%, remaining is metal matrix material.Due to graphene
Strengthen the addition of phase, the composited contact material is had than other more preferable conductive, heat conduction of enhancing phase composited contact material
The hardness and wearability of performance and Geng Gao.
Electrical contact material performance has the space further lifted.
The content of the invention
Present invention aims at a kind of Ag-based electrical contact composite is provided, by adding silver-plated stone in silver alloy
Black alkene reinforcement, while its electric conductivity, thermal conductivity is not reduced, improve hardness, wearability and the resistance to arc erosion of silver.
Present invention also offers the preparation method of above-mentioned electrical contact material simultaneously.
Technical scheme of the invention for the proposition that solves the above problems：
A kind of Ag-based electrical contact composite, it is characterised in that by weight than the silvering graphite alkene for 0.1-5.0% and
95.0-99.9% silver composition, silver-colored particle diameter is 10-80 microns.
Preferably, graphene is N layers, N 1-10.
The preparation method of above-mentioned Ag-based electrical contact composite, it is characterised in that comprise the following steps：
（1）Argent is deposited on by graphenic surface using direct current magnetron sputtering process, silvering graphite alkene is made.Direct magnetic control
The technological parameter of sputtering deposition device is：Vacuum reaches 0.1*10-3-1.0*10-3During Pa, high-purity argon gas, vacuum chamber gas are passed through
Press 0.8-1.5Pa, sputtering power 80-160W, sedimentation time 5-20min.
（2）Silvering graphite alkene and snow cover enter ball mill ball milling, and silvering graphite alkene and the mixed uniformly powder of silver is made.Ball milling
Machine working condition is：Using alumina balls ink tank and agate ball, ratio of grinding media to material 3:1, vacuumize, be filled with the argon that purity is 99.99%
Gas, rotating speed 150-250r/min, alternate run clockwise, counterclockwise, ball milling 10-15 minutes, stop 5 minutes, the mixed powder time is
4-8 hours.
（3）By step（2）Powder is put into mould cold moudling after mixing, is carried out under pressure 100-300MPa, during pressurize
Between be sintered after 2-5 minutes, sintering temperature is 750-900 DEG C, soaking time 2-4 hours, preferably 880 DEG C of sintering temperature.
（4）Composite plastic working is molded, using fashion of extrusion, 300-500 DEG C of temperature, extrusion ratio 50：1-200：
1, Ag-based electrical contact composite is made.
The present invention useful achievement be：
（1）Ag-based electrical contact composite, in silver add graphene nano powder, be remarkably improved material hardness and
Wearability, silvering graphite alkene improve the interface binding power of graphene and matrix silver, can make electric conductivity, the heat conduction of electrical contact material
Performance, anti electric arc corrosion further improve.
（2）In the preparation method of electrical contact, using direct current magnetron sputtering process in graphenic surface deposition of silver, formation nucleocapsid
Structure, aggregation of the graphene as nano particle during mixed powder is avoided, ensures that graphene is evenly distributed in the base.Simultaneously
Large scale electrical contact material can be prepared, is adapted to industrialization large-scale production.
Embodiment
Embodiment 1
（1）Using direct current magnetron sputtering process in graphene（The number of plies is 1-10 layers）Surface deposited metal silver is prepared into silver-plated stone
Black alkene.First polished before the silver-colored target installation that purity is 99.99% with fine sandpaper, remove surface film oxide, then cleaned with acetone,
Dry, carry out 5 minutes pre-sputterings before Deposited By Dc Magnetron Sputtering, remove the metal oxide of target material surface and other impurity, protect
Demonstrate,prove the purity of follow-up graphenic surface deposition silverskin.Sputtering parameter is as follows：Vacuum reaches 0.1*10-3During Pa, high-purity argon is passed through
Gas, gas pressure in vacuum 0.8Pa, sputtering power 160W, sedimentation time 5min.
（2）Silvering graphite alkene and 10 micro-silver powders press 0.1:99.9 weight ratio is fitted into ball mill, using alumina balls
Ink tank and agate ball, ratio of grinding media to material 3:1.Ball grinder first vacuumize be passed through again 99.99% argon gas protection, rotating speed 150r/min, ball milling
During mixed powder, ball milling clockwise 15 minutes, stop 5 minutes, ball milling counterclockwise 15 minutes, stop 5 minutes, according to this alternately work
Make, Ball-milling Time 4 hours, obtain silvering graphite alkene and the mixed uniformly powder of silver.
（3）By step（2）Powder is put into mould after mixing, and cold moudling, dwell time 5 are carried out under pressure 100MPa
Minute, cold moudling part, 880 DEG C of sintering temperature, soaking time 2 hours are sintered under hydrogen shield.
（4）Extrusion process, 300 DEG C of temperature, extrusion ratio 50：1, Ag-based electrical contact composite is made.
Embodiment 2
（1）Using direct current magnetron sputtering process in graphene（The number of plies is 1-10 layers）Surface deposited metal silver is prepared into silver-plated stone
Black alkene.First polished before the silver-colored target installation that purity is 99.99% with fine sandpaper, remove surface film oxide, then cleaned with acetone,
Dry, carry out 5 minutes pre-sputterings before Deposited By Dc Magnetron Sputtering, remove the metal oxide of target material surface and other impurity, protect
Demonstrate,prove the purity of follow-up graphenic surface deposition silverskin.Sputtering parameter is as follows：Vacuum reaches 1.0*10-3During Pa, high-purity argon is passed through
Gas, gas pressure in vacuum 1.5Pa, sputtering power 80W, sedimentation time 20min.
（2）Silvering graphite alkene and 10 micro-silver powders press 0.5:99.5 weight ratio is fitted into ball mill, using alumina balls
Ink tank and agate ball, ratio of grinding media to material 3:1.Ball grinder first vacuumize be passed through again 99.99% argon gas protection, rotating speed 250r/min, ball milling
During mixed powder, ball milling clockwise 10 minutes, stop 5 minutes, ball milling counterclockwise 10 minutes, stop 5 minutes, according to this alternately work
Make, Ball-milling Time 8 hours, obtain silvering graphite alkene and the mixed uniformly powder of silver.
（3）By step（2）Powder is put into mould after mixing, and cold moudling, dwell time 2 are carried out under pressure 300MPa
Minute, cold moudling part, 880 DEG C of sintering temperature, soaking time 4 hours are sintered under hydrogen shield.
（4）Extrusion process, 500 DEG C of temperature, extrusion ratio 200：1, Ag-based electrical contact composite is made.
Embodiment 3
（1）Using direct current magnetron sputtering process in graphene（The number of plies is 1-10 layers）Surface deposited metal silver is prepared into silver-plated stone
Black alkene.First polished before the silver-colored target installation that purity is 99.99% with fine sandpaper, remove surface film oxide, then cleaned with acetone,
Dry, carry out 5 minutes pre-sputterings before Deposited By Dc Magnetron Sputtering, remove the metal oxide of target material surface and other impurity, protect
Demonstrate,prove the purity of follow-up graphenic surface deposition silverskin.Sputtering parameter is as follows：Vacuum reaches 0.3*10-3During Pa, high-purity argon is passed through
Gas, gas pressure in vacuum 1.0Pa, sputtering power 110W, sedimentation time 5min.
（2）Silvering graphite alkene and 40 micro-silver powders press 5.0:95.0 weight ratio is fitted into ball mill, using alumina balls
Ink tank and agate ball, ratio of grinding media to material 3:1.Ball grinder first vacuumize be passed through again 99.99% argon gas protection, rotating speed 200r/min, ball milling
During mixed powder, ball milling clockwise 10 minutes, stop 5 minutes, ball milling counterclockwise 10 minutes, stop 5 minutes, according to this alternately work
Make, Ball-milling Time 4 hours, obtain silvering graphite alkene and the mixed uniformly powder of silver.
（3）By step（2）Powder is put into mould after mixing, and cold moudling, dwell time 3 are carried out under pressure 100MPa
Minute, cold moudling part, 880 DEG C of sintering temperature, soaking time 2 hours are sintered under hydrogen shield.
（4）Extrusion process, 450 DEG C of temperature, extrusion ratio 100：1, Ag-based electrical contact composite is made.
Embodiment 4
（1）Using direct current magnetron sputtering process in graphene（The number of plies is 1-10）Surface deposited metal silver is prepared into silvering graphite
Alkene.First polished before the silver-colored target installation that purity is 99.99% with fine sandpaper, remove surface film oxide, then cleaned with acetone, 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 graphenic surface deposition silverskin.Sputtering parameter is as follows：Vacuum reaches 0.2*10-3During Pa, high-purity argon gas is passed through,
Gas pressure in vacuum 1.2Pa, sputtering power 100W, sedimentation time 10min.
（2）Silvering graphite alkene and 80 micro-silver powders press 2.0:98.0 weight ratio is fitted into ball mill, using alumina balls
Ink tank and agate ball, ratio of grinding media to material 3:1.Ball grinder first vacuumize be passed through again 99.99% argon gas protection, rotating speed 250r/min, ball milling
During mixed powder, ball milling clockwise 10 minutes, stop 5 minutes, ball milling counterclockwise 10 minutes, stop 5 minutes, according to this alternately work
Make, Ball-milling Time 4 hours, obtain silvering graphite alkene and the mixed uniformly powder of silver.
（3）By step（2）Powder is put into mould after mixing, and cold moudling, dwell time 3 are carried out under pressure 100MPa
Minute, cold moudling part, 880 DEG C of sintering temperature, soaking time 2 hours are sintered under hydrogen shield.
（4）Extrusion process, 450 DEG C of temperature, extrusion ratio 100：1, Ag-based electrical contact composite is made.
Embodiment 5
Silvering graphite alkene：Silver powder is pressed by weight 5.0:95.0 are fitted into ball mill, and other specification is made with embodiment 4
Graphene strengthens Ag-based electrical contact composite.
Comparative example 1
By graphene with silver by weight 0.1:99.9, which load ball mill, mixes powder, and silver-based is made with embodiment 3 in other parameters
Electrical contact material.
Comparative example 2
Snow cover is entered into ball mill and mixes powder, Ag-based electrical contact material is made with embodiment 3 in other parameters.
Manufactured composite parameters such as following table：
Addition silvering graphite alkene is made in graphene enhancing Ag-based electrical contact composite, with comparative example 1 and adds graphene
Manufactured electrical contact material is compared, and hardness significantly improves 60%, and electrical conductivity also improves.With silver in comparative example 2 made of electricity
Contact material is compared, and hardness significantly improves, and up to 200%, electrical conductivity also significantly improves.
Claims (6)
1. a kind of Ag-based electrical contact composite, it is characterised in that by the silvering graphite alkene and 95.0- that weight is 0.1-5.0%
99.9% silver composition, silver-colored particle diameter is 10-80 microns；
The preparation method of the Ag-based electrical contact composite, comprises the following steps：
（1）Argent is deposited on by graphenic surface using direct current magnetron sputtering process, silvering graphite alkene is made；
（2）Silvering graphite alkene and snow cover enter ball mill ball milling, and silvering graphite alkene and the mixed uniformly powder of silver is made；
（3）By step（2）Powder is put into mould cold moudling after mixing, sintering；
（4）Composite plastic working is molded, Ag-based electrical contact composite is made.
2. a kind of Ag-based electrical contact composite according to claim 1, it is characterised in that graphene is N layers, N 1-
10。
3. electric contact composite material according to claim 1, it is characterised in that the step（1）Middle magnetically controlled DC sputtering
The technological parameter of depositing device is：Vacuum reaches 0.1*10-3-1.0*10-3During Pa, high-purity argon gas, gas pressure in vacuum are passed through
0.8-1.5Pa, sputtering power 80-160W, sedimentation time 5-20min.
4. electric contact composite material according to claim 1, it is characterised in that the step（2）Middle ball mill work shape
State is：Using alumina balls ink tank and agate ball, ratio of grinding media to material 3:1, vacuumize, be filled with the argon gas that purity is 99.99%, rotating speed
150-250r/min, alternate run clockwise, counterclockwise, ball milling 10-15 minutes, stop 5 minutes, it is 4-8 hours to mix the powder time.
5. electric contact composite material according to claim 1, it is characterised in that the step（3）Middle cold moudling is being pressed
Carried out under power 100-300MPa, minute dwell time 2-5, sintering temperature is 750-900 DEG C, soaking time 2-4 hours.
6. electric contact composite material according to claim 1, it is characterised in that step（4）It is middle to use extruding Plastic Forming,
300-500 DEG C of temperature, extrusion ratio 50：1-200：1.
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| CN105838914A (en) * | 2016-04-16 | 2016-08-10 | 苏州思创源博电子科技有限公司 | Preparation method of silver-based contact material containing graphene |
| CN105895418A (en) * | 2016-04-16 | 2016-08-24 | 苏州思创源博电子科技有限公司 | Preparation method of silver based electric contact material |
| CN105719854A (en) * | 2016-04-16 | 2016-06-29 | 苏州思创源博电子科技有限公司 | Preparation method for copper-based electric contact material with graphene |
| CN105950904B (en) * | 2016-07-07 | 2018-04-27 | 济南大学 | A kind of preparation method of silvering graphite alkene enhancing copper-based electric contact material |
| CN107267795B (en) * | 2017-06-20 | 2019-12-10 | 华北水利水电大学 | High-conductivity silver-based melt material and smelting method thereof |
| CN108677048B (en) * | 2018-04-20 | 2020-11-17 | 西安理工大学 | Nitrogen-doped graphene silver-based composite material and preparation method thereof |
| CN109811177A (en) * | 2018-11-19 | 2019-05-28 | 昆明贵金属研究所 | A kind of preparation method of highly conductive high-intensitive silver-graphene composite material |
| CN110541150B (en) * | 2019-08-22 | 2024-05-03 | 沈阳科友真空技术有限公司 | Multilayer film structure for reed switch relay contact and preparation method thereof |
| CN111118326A (en) * | 2020-02-24 | 2020-05-08 | 江苏新奥碳纳米材料应用技术研究院有限公司 | Graphene aluminum-coated/aluminum-based heat dissipation material and preparation method thereof |
| CN112366107B (en) * | 2020-11-11 | 2021-12-10 | 福达合金材料股份有限公司 | Preparation method of silver metal oxide sheet-shaped electrical contact |
| CN113131307B (en) * | 2021-03-26 | 2023-01-24 | 上海联影医疗科技股份有限公司 | Slip ring carbon brush preparation method and slip ring carbon brush |
| CN114101666B (en) * | 2021-09-03 | 2023-08-01 | 叶浩博 | Graphene-based silver-saving electrical contact material and manufacturing method thereof |
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