CN105428097A - Silver-based electrical contact composite material and preparation method therefor - Google Patents
Silver-based electrical contact composite material and preparation method therefor Download PDFInfo
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- CN105428097A CN105428097A CN201510983345.8A CN201510983345A CN105428097A CN 105428097 A CN105428097 A CN 105428097A CN 201510983345 A CN201510983345 A CN 201510983345A CN 105428097 A CN105428097 A CN 105428097A
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- silver
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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
-
- 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 invention relates to a silver-based electrical contact composite material and a preparation method therefor. The silver-based electrical contact composite material is prepared from 0.1-5.0% of silver plated graphene and 95.0-99.9% of silver in percentage by weight; and the silver-based electrical contact composite material is prepared by steps of graphene silver plating, ball milling and powder mixing, cold pressing molding, sintering and plastic processing and molding. According to the silver-based electrical contact composite material, the silver plated graphene is added to silver to be used as the skeleton so as to endow the material with high hardness, mechanical impact resistance and electric arc ablation resistance, and meanwhile, the reduction of electrical conductivity and thermal conductivity is avoided.
Description
Technical field
The present invention relates to a kind of electrical contact material and preparation method thereof, particularly relate to a kind of Ag-based electrical contact composite material and preparation method.
Background technology
Silver/the carbon electrical contact material with the performance such as fabulous resistance fusion welding, low contact resistance has been applied in low middle load relay and signaling switch, but, apply more widely because its lower mechanical strength, low resistance to wear and anti electric arc corrosion limit it.
Chinese patent literature 101763956A, open (bulletin) day 2010.06.30, discloses and improve its hardness and abrasion resistance properties by the method for adding cermet and rare earth element in silver/graphite material.
Chinese patent literature 101707146A, open (bulletin) day 2010.05.12, disclose by material with carbon element (diamond, graphite, carbon) deposits tungsten and Argent grain, solve graphite and the bad problem of matrix wetability, improve hardness and arc ablation resistance.
Chinese patent literature 101866761A, open (bulletin) day 2010.10.20, discloses and prepares high-performance silver/graphite composite material by proprietary extrusion forming process.
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.
Electrical contact material performance has the space promoted further.
Summary of the invention
The object of the invention is to provide a kind of Ag-based electrical contact composite material, by adding silvering graphite alkene reinforcement in silver alloy, while not reducing its conductivity, thermal conductivity, improves the hardness of silver, resistance to wear and resistance to arc erosion.
Present invention also offers the preparation method of above-mentioned electrical contact material simultaneously.
The present invention is the technical scheme proposed that solves the problem:
A kind of Ag-based electrical contact composite material, it is characterized in that, be that the silvering graphite alkene of 0.1-5.0% and the silver of 95.0-99.9% form by weight ratio, and the particle diameter of silver is 10-80 micron.
Preferably, Graphene is N layer, and N is 1-10.
The preparation method of above-mentioned Ag-based electrical contact composite material, is characterized in that comprising the following steps:
(1) adopt direct current magnetron sputtering process that argent is deposited on graphenic surface, make silvering graphite alkene.The technological parameter of Deposited By Dc Magnetron Sputtering equipment is: vacuum degree reaches 0.1*10
-3-1.0*10
-3during Pa, pass into high-purity argon gas, gas pressure in vacuum 0.8-1.5Pa, sputtering power 80-160W, sedimentation time is 5-20min.
(2) silvering graphite alkene and snow cover enter ball mill ball milling, make silvering graphite alkene and the mixed uniformly powder of silver.Ball mill operating state is: adopt alumina balls ink tank and agate ball, ratio of grinding media to material 3:1, vacuumizes, be filled with the argon gas that purity is 99.99%, rotating speed 150-250r/min, clockwise, counterclockwise alternate run, ball milling 10-15 minute, stops 5 minutes, and the mixed powder time is 4-8 hour.
(3) powder after step (2) mixing is put into mold cold molded, carry out under pressure 100-300MPa, sinter after dwell time 2-5 minute, sintering temperature is 750-900 DEG C, temperature retention time 2-4 hour, sintering temperature preferably 880 DEG C.
(4) by shaping for composite material plastic working, adopt fashion of extrusion, temperature 300-500 DEG C, extrusion ratio 50:1-200:1, make Ag-based electrical contact composite material.
Useful achievement of the present invention is:
(1) Ag-based electrical contact composite material, graphene nano powder is added in silver, can significantly improve hardness and the resistance to wear of material, silvering graphite alkene improves the interface binding power of Graphene and matrix silver, and the conductivity of electrical contact material, heat conductivility, anti electric arc corrosion can be made to improve further.
(2) in the preparation method of electrical contact, adopt direct current magnetron sputtering process at graphenic surface depositing silver, form nucleocapsid structure, avoid Graphene as the gathering of nano particle in mixed powder process, ensure that Graphene is evenly distributed in the base.Large size electro contact material can be prepared simultaneously, be applicable to industrialization large-scale production.
Embodiment
Embodiment 1
(1) direct current magnetron sputtering process is adopted to be prepared into silvering graphite alkene at Graphene (number of plies is 1-10 layer) surface deposition argent.Purity is first polish with fine sandpaper before the silver-colored target installation of 99.99%, removes surface film oxide, then cleans with acetone, dry, carry out 5 minutes pre-sputterings before Deposited By Dc Magnetron Sputtering, remove metal oxide and other impurity of target material surface, ensure the purity of follow-up graphenic surface deposition silverskin.Sputtering parameter is as follows: vacuum degree reaches 0.1*10
-3during Pa, pass into high-purity argon gas, gas pressure in vacuum 0.8Pa, sputtering power 160W, sedimentation time is 5min.
(2) weight ratio that silvering graphite alkene and 10 micro-silver powders press 0.1:99.9 loads in ball mill, adopts alumina balls ink tank and agate ball, ratio of grinding media to material 3:1.Ball grinder first vacuumizes the argon shield passing into 99.99% again; rotating speed 150r/min; ball milling mixes in powder process; clockwise ball milling 15 minutes, stops 5 minutes, counterclockwise ball milling 15 minutes; stop 5 minutes; alternation according to this, Ball-milling Time 4 hours, obtains silvering graphite alkene and the mixed uniformly powder of silver.
(3) powder after step (2) mixing is put into mould, under pressure 100MPa, carry out cold moudling, 5 minutes dwell times, under hydrogen shield, sintering is cold-pressed into shaped piece, sintering temperature 880 DEG C, temperature retention time 2 hours.
(4) extrusion process, temperature 300 DEG C, extrusion ratio 50:1, makes Ag-based electrical contact composite material.
Embodiment 2
(1) direct current magnetron sputtering process is adopted to be prepared into silvering graphite alkene at Graphene (number of plies is 1-10 layer) surface deposition argent.Purity is first polish with fine sandpaper before the silver-colored target installation of 99.99%, removes surface film oxide, then cleans with acetone, dry, carry out 5 minutes pre-sputterings before Deposited By Dc Magnetron Sputtering, remove metal oxide and other impurity of target material surface, ensure the purity of follow-up graphenic surface deposition silverskin.Sputtering parameter is as follows: vacuum degree reaches 1.0*10
-3during Pa, pass into high-purity argon gas, gas pressure in vacuum 1.5Pa, sputtering power 80W, sedimentation time is 20min.
(2) weight ratio that silvering graphite alkene and 10 micro-silver powders press 0.5:99.5 loads in ball mill, adopts alumina balls ink tank and agate ball, ratio of grinding media to material 3:1.Ball grinder first vacuumizes the argon shield passing into 99.99% again; rotating speed 250r/min; ball milling mixes in powder process; clockwise ball milling 10 minutes, stops 5 minutes, counterclockwise ball milling 10 minutes; stop 5 minutes; alternation according to this, Ball-milling Time 8 hours, obtains silvering graphite alkene and the mixed uniformly powder of silver.
(3) powder after step (2) mixing is put into mould, under pressure 300MPa, carry out cold moudling, 2 minutes dwell times, under hydrogen shield, sintering is cold-pressed into shaped piece, sintering temperature 880 DEG C, temperature retention time 4 hours.
(4) extrusion process, temperature 500 DEG C, extrusion ratio 200:1, makes Ag-based electrical contact composite material.
Embodiment 3
(1) direct current magnetron sputtering process is adopted to be prepared into silvering graphite alkene at Graphene (number of plies is 1-10 layer) surface deposition argent.Purity is first polish with fine sandpaper before the silver-colored target installation of 99.99%, removes surface film oxide, then cleans with acetone, dry, carry out 5 minutes pre-sputterings before Deposited By Dc Magnetron Sputtering, remove metal oxide and other impurity of target material surface, ensure the purity of follow-up graphenic surface deposition silverskin.Sputtering parameter is as follows: vacuum degree reaches 0.3*10
-3during Pa, pass into high-purity argon gas, gas pressure in vacuum 1.0Pa, sputtering power 110W, sedimentation time is 5min.
(2) weight ratio that silvering graphite alkene and 40 micro-silver powders press 5.0:95.0 loads in ball mill, adopts alumina balls ink tank and agate ball, ratio of grinding media to material 3:1.Ball grinder first vacuumizes the argon shield passing into 99.99% again; rotating speed 200r/min; ball milling mixes in powder process; clockwise ball milling 10 minutes, stops 5 minutes, counterclockwise ball milling 10 minutes; stop 5 minutes; alternation according to this, Ball-milling Time 4 hours, obtains silvering graphite alkene and the mixed uniformly powder of silver.
(3) powder after step (2) mixing is put into mould, under pressure 100MPa, carry out cold moudling, 3 minutes dwell times, under hydrogen shield, sintering is cold-pressed into shaped piece, sintering temperature 880 DEG C, temperature retention time 2 hours.
(4) extrusion process, temperature 450 DEG C, extrusion ratio 100:1, makes Ag-based electrical contact composite material.
Embodiment 4
(1) direct current magnetron sputtering process is adopted to be prepared into silvering graphite alkene at Graphene (number of plies is 1-10) surface deposition argent.Purity is first polish with fine sandpaper before the silver-colored target installation of 99.99%, removes surface film oxide, then cleans with acetone, dry, carry out 5 minutes pre-sputterings before Deposited By Dc Magnetron Sputtering, remove metal oxide and other impurity of target material surface, ensure the purity of follow-up graphenic surface deposition silverskin.Sputtering parameter is as follows: vacuum degree reaches 0.2*10
-3during Pa, pass into high-purity argon gas, gas pressure in vacuum 1.2Pa, sputtering power 100W, sedimentation time is 10min.
(2) weight ratio that silvering graphite alkene and 80 micro-silver powders press 2.0:98.0 loads in ball mill, adopts alumina balls ink tank and agate ball, ratio of grinding media to material 3:1.Ball grinder first vacuumizes the argon shield passing into 99.99% again; rotating speed 250r/min; ball milling mixes in powder process; clockwise ball milling 10 minutes, stops 5 minutes, counterclockwise ball milling 10 minutes; stop 5 minutes; alternation according to this, Ball-milling Time 4 hours, obtains silvering graphite alkene and the mixed uniformly powder of silver.
(3) powder after step (2) mixing is put into mould, under pressure 100MPa, carry out cold moudling, 3 minutes dwell times, under hydrogen shield, sintering is cold-pressed into shaped piece, sintering temperature 880 DEG C, temperature retention time 2 hours.
(4) extrusion process, temperature 450 DEG C, extrusion ratio 100:1, makes Ag-based electrical contact composite material.
Embodiment 5
Silvering graphite alkene: silver powder loads in ball mill by by weight 5.0:95.0, other parameters, with embodiment 4, are made Graphene and are strengthened Ag-based electrical contact composite material.
Comparative example 1
Graphene is loaded ball mill with silver by weight 0.1:99.9 and mixes powder, other parameter, with embodiment 3, makes Ag-based electrical contact material.
Comparative example 2
Snow cover is entered ball mill and mixes powder, other parameter, with embodiment 3, makes Ag-based electrical contact material.
The composite material parameters made is as following table:
Add silvering graphite alkene to make Graphene and strengthen Ag-based electrical contact composite material, and add compared with electrical contact material that Graphene makes in comparative example 1, hardness significantly improves 60%, and conductivity also improves.Compared with the electrical contact material made with silver in comparative example 2, hardness significantly improves, and can reach 200%, conductivity also significantly improves.
Claims (7)
1. an Ag-based electrical contact composite material, is characterized in that, is that the silvering graphite alkene of 0.1-5.0% and the silver of 95.0-99.9% form by weight, and the particle diameter of silver is 10-80 micron.
2. a kind of Ag-based electrical contact composite material according to claim 1, is characterized in that, Graphene is N layer, and N is 1-10.
3. a preparation method for Ag-based electrical contact composite material described in claim 1, is characterized in that comprising the following steps:
(1) adopt direct current magnetron sputtering process that argent is deposited on graphenic surface, make silvering graphite alkene;
(2) silvering graphite alkene and snow cover enter ball mill ball milling, make silvering graphite alkene and the mixed uniformly powder of silver;
(3) powder after step (2) mixing is put into mold cold molded, sintering;
(4) by shaping for composite material plastic working, Ag-based electrical contact composite material is made.
4. preparation method according to claim 3, is characterized in that, in described step (1), the technological parameter of Deposited By Dc Magnetron Sputtering equipment is: vacuum degree reaches 0.1*10
-3-1.0*10
-3during Pa, pass into high-purity argon gas, gas pressure in vacuum 0.8-1.5Pa, sputtering power 80-160W, sedimentation time is 5-20min.
5. preparation method according to claim 3, it is characterized in that, in described step (2), ball mill operating state is: adopt alumina balls ink tank and agate ball, ratio of grinding media to material 3:1, vacuumizes, be filled with the argon gas that purity is 99.99%, rotating speed 150-250r/min, clockwise, counterclockwise alternate run, ball milling 10-15 minute, stop 5 minutes, the mixed powder time is 4-8 hour.
6. preparation method according to claim 3, is characterized in that, in described step (3), cold moudling is carried out under pressure 100-300MPa, and dwell time 2-5 minute, sintering temperature is 750-900 DEG C, temperature retention time 2-4 hour, sintering temperature preferably 880 DEG C.
7. preparation method according to claim 3, is characterized in that, adopts extruding Plastic Forming, temperature 300-500 DEG C, extrusion ratio 50:1-200:1 in step (4).
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Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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 |
CN105950904A (en) * | 2016-07-07 | 2016-09-21 | 济南大学 | Preparing method for silver plating graphene enhanced copper-based electric contact material |
CN107267795A (en) * | 2017-06-20 | 2017-10-20 | 华北水利水电大学 | A kind of high conductivity silver-based melt material and its method of smelting |
CN108677048A (en) * | 2018-04-20 | 2018-10-19 | 西安理工大学 | A kind of silver-based composite material of nitrogen-doped graphene 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 |
CN110541150A (en) * | 2019-08-22 | 2019-12-06 | 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 |
CN113131307A (en) * | 2021-03-26 | 2021-07-16 | 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 |
CN114101666A (en) * | 2021-09-03 | 2022-03-01 | 叶浩博 | Graphene-based silver-saving electrical contact material and manufacturing method thereof |
WO2022099854A1 (en) * | 2020-11-11 | 2022-05-19 | 浙江福达合金材料科技有限公司 | Preparation method for silver metal oxide sheet-like electrical contact |
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 |
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CN105950904A (en) * | 2016-07-07 | 2016-09-21 | 济南大学 | Preparing method for silver plating graphene enhanced copper-based electric contact material |
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 |
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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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