CN105551860A - Preparation method of nickel-plated graphene/silver-nickel electrical contact material - Google Patents
Preparation method of nickel-plated graphene/silver-nickel electrical contact material Download PDFInfo
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- CN105551860A CN105551860A CN201610106140.6A CN201610106140A CN105551860A CN 105551860 A CN105551860 A CN 105551860A CN 201610106140 A CN201610106140 A CN 201610106140A CN 105551860 A CN105551860 A CN 105551860A
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- nickel
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Classifications
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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
-
- 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
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- 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
Abstract
The invention relates to a preparation method of a nickel-plated graphene/silver-nickel electrical contact material. The preparation method comprises the following steps: performing direct-current magnetron sputtering and nickel plating of graphene, ball-milling and mixing nickel-plated graphene, silver powder and nickel powder, cold pressing and forming, sintering, and processing and forming, wherein the material comprises 0.1-5.0 wt% of nickel-plated graphene, 10-40 wt% of nickel powder and the rest of silver powder ball-milled mixed powder. A nickel-plated graphene reinforcing body is added into the silver powder and the nickel powder, such that the hardness, the abrasive resistance and the melting-welding resistance of silver are improved while the electrical conductivity and the thermal conductivity of the electrical contact material prepared by the invention are not decreased.
Description
Technical field
The present invention relates to a kind of preparation method of electrical contact material, particularly relate to the preparation method of a kind of Ni-coated graphite alkene/silver-colored nickel electric contact material.
Background technology
AgNi material has good processing characteristics, good mar proof, contact resistance low and stable wait excellent properties be used on various small current relay, master switch and probe of contactor, but due to its resistance fusion welding poor, have impact on its broader applications.There are some researches show, graphite adds in silver-colored nickel material can stop the melting welding of contact and bonding, reduces the contact resistance of contact, improves conductivity and resistance fusion welding.
Existing patent (publication number 102808098A) discloses a kind of preparation method of silver/nickel/graphite contact material, adopt the method for chemical plating, after Graphite Coating nickel, coated with silver is prepared into intermediate composite particles again, then employing tradition mixes powder, sintering process prepares silver/nickel/graphite contact material.But graphite plating process complex process preparation technology, plating solution has certain contaminative to human body, and coating quality is wayward, is not suitable for suitability for industrialized production.Meanwhile, add graphite and adopt micron order, particle size is comparatively large, reduces the mechanical strength of electrical contact material to a certain extent, and resistance to arc erosion is poor simultaneously, is difficult to obtain the electrical contact material that combination property meets user demand.
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.
Therefore, realize the preparation of electrical contact with the production technology of a kind of environmental protection, low cost, material property is promoted further.
Summary of the invention
The object of the invention is the preparation method providing a kind of Ni-coated graphite alkene/silver-colored nickel electric contact material, by adding Ni-coated graphite alkene reinforcement in silver powder, nickel powder, while not reducing its conductivity, thermal conductivity, improve the hardness of silver, resistance to wear and resistance fusion welding.
The present invention is the technical scheme proposed that solves the problem:
A preparation method for Ni-coated graphite alkene/silver-colored nickel electric contact material, is characterized in that, comprise the following steps:
(1) direct current magnetron sputtering process is adopted to make Ni-coated graphite alkene at graphenic surface plated metal nickel.Graphene is N layer, and N is 1-10.Purity is first polish with fine sandpaper before the nickel target installation of 99.99%, remove surface film oxide, clean with acetone again, dry, 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, adopt baffle plate target and Graphene to be separated, remove metal oxide and other impurity of target material surface, ensure the purity of follow-up graphenic surface nickel deposited film.The concrete technology of Deposited By Dc Magnetron Sputtering equipment is: target to be purity be 99.99% nickel 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 at 0.8-1.2Pa, and sputtering power is at 80-120W, and sedimentation time is 5-20min.
(2) by 0.1-5.0wt% Ni-coated graphite alkene, 10%-40wt% nickel powder, surplus is that silver is put into ball mill ball milling and mixed powder, nickel powder granularity 300 order-450 order, silver powder granularity 200 order-300 order.Ball milling mixes in powder process, and adopt alumina balls grinding jar and agate ball, ratio of grinding media to material 3:1, vacuumizes 10 minutes; pass into the argon shield of purity 99.99% again, rotating speed 150-350 rev/min, every ball milling 10-15 minute; stop 5 minutes, exchange rotation clockwise and counterclockwise, amount to mixed powder time 4-8 hour.Alternately ball milling mixes powder, is conducive to the full and uniform mixing of metal dust.
For preventing the oxidation of copper, before ball milling, ball grinder need vacuumize, and passes into argon shield.Within the scope of ball milling parameter of the present invention, well can control the distribution of Graphene and metal alloy mixed-powder.
(3) powder after step (2) mixing is put into mould cold moudling, pressure 150-350MPa, dwell time 2-5 minute, sinter under the hydrogen shield of purity 99.9%, sintering temperature 800-1000 DEG C, temperature retention time 2-4 hour.
(4) extruding or rolling mill practice make Ni-coated graphite alkene/silver-colored nickel electric contact material.
Cold-rolled sintered blank extrudes in (4) by described step, and extrusion temperature 600-850 DEG C, extrusion ratio 50:1-150:1 make the section bar of needs.
Cold-rolled sintered blank is rolled in (4) by described step, rolling temperature 600-850 DEG C, and rolling reduction 80%-90% makes section bar, sheet material, tubing.
Useful achievement of the present invention is:
(1) silver-colored nickel electric contact material adds the Graphene with ultra-high conductivity, thermal conductivity, hardness, can reduce the contact resistance of contact, improves thermal conductivity and resistance fusion welding.
(2) adopt magnetron sputtered deposition technology in graphenic surface nickel deposited, the structure formed, improve the interface cohesion of Graphene and matrix silver, good interface bonding energy can make contact material obtain higher conductivity, thermal conductivity, it also avoid the gathering of graphene nano powder in matrix silver, ensure Graphene distributing homogeneity in the base, coating process is pollution-free simultaneously, and deposition process easily controls.
(3) in silver matrix, add nickel, improve the hardness of material, resistance fusion welding and non-oxidizability.
Embodiment
Embodiment 1
(1) direct current magnetron sputtering process is adopted to be prepared into Ni-coated graphite alkene at Graphene (number of plies is 1-10 layer) surface deposition metallic nickel.Purity is first polish with fine sandpaper before the nickel target installation of 99.99%, remove surface film oxide, clean with acetone again, dry, 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, adopt baffle plate target and Graphene to be separated, remove metal oxide and other impurity of target material surface, ensure the purity of follow-up graphenic surface nickel deposited film.Sputtering parameter is as follows: vacuum degree reaches 0.1*10
-3during Pa, pass into the argon gas of purity 99.99%, gas pressure in vacuum 0.8Pa, sputtering power 120W, sedimentation time is 5min.
(2) Ni-coated graphite alkene: nickel powder: the weight ratio that 0.1:10:89.9 pressed by silver powder 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 150 revs/min, and ball milling mixes in powder process, clockwise ball milling 15 minutes; stop 5 minutes, counterclockwise ball milling 15 minutes, stop 5 minutes; alternation according to this, amounts to the mixed 4 hours powder time, obtains mixed uniformly powder.
(3) powder after step (2) mixing is put into mould, under pressure 150MPa, carry out cold moudling, 5 minutes dwell times, under hydrogen shield, sintering is cold-pressed into shaped piece, sintering temperature 800 DEG C, temperature retention time 4 hours.
(4) extrusion process, temperature 600 DEG C, extrusion ratio 50:1, makes Ni-coated graphite alkene/silver-colored nickel electric contact material.
Embodiment 2
(1) direct current magnetron sputtering process is adopted to be prepared into Ni-coated graphite alkene at Graphene (number of plies is 1-10 layer) surface deposition metallic nickel.Purity is first polish with fine sandpaper before the nickel target installation of 99.99%, remove surface film oxide, clean with acetone again, dry, 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, adopt baffle plate target and Graphene to be separated, remove metal oxide and other impurity of target material surface, ensure the purity of follow-up graphenic surface nickel deposited film.Sputtering parameter is as follows: vacuum degree reaches 1.0*10
-3during Pa, pass into the argon gas of purity 99.99%, gas pressure in vacuum 1.2Pa, sputtering power 80W, sedimentation time is 20min.
(2) Ni-coated graphite alkene: nickel powder: the weight ratio that 5:40:55 pressed by silver powder 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 350 revs/min, and ball milling mixes in powder process, clockwise ball milling 10 minutes; stop 5 minutes, counterclockwise ball milling 10 minutes, stop 5 minutes; alternation according to this, amounts to the mixed 8 hours powder time, obtains mixed uniformly powder.
(3) powder after step (2) mixing is put into mould, under pressure 350MPa, carry out cold moudling, 2 minutes dwell times, under hydrogen shield, sintering is cold-pressed into shaped piece, sintering temperature 1000 DEG C, temperature retention time 2 hours.
(4) extrusion process, temperature 850 DEG C, extrusion ratio 150:1, makes Ni-coated graphite alkene/silver-colored nickel electric contact material.
Embodiment 3
(1) direct current magnetron sputtering process is adopted to be prepared into Ni-coated graphite alkene at Graphene (number of plies is 1-10 layer) surface deposition metallic nickel.Purity is first polish with fine sandpaper before the nickel target installation of 99.99%, remove surface film oxide, clean with acetone again, dry, 5 minutes pre-sputterings are carried out before Deposited By Dc Magnetron Sputtering, adopt baffle plate target and Graphene to be separated, remove metal oxide and other impurity of target material surface, ensure the purity of follow-up graphenic surface nickel deposited film.Sputtering parameter is as follows: vacuum degree reaches 0.3*10
-3during Pa, pass into the argon gas of purity 99.99%, gas pressure in vacuum 1.0Pa, sputtering power 110W, sedimentation time is 5min.
(2) Ni-coated graphite alkene: nickel powder: the weight ratio that 2:10:88 pressed by silver powder 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 200 revs/min, and ball milling mixes in powder process, clockwise ball milling 10 minutes; stop 5 minutes, counterclockwise ball milling 10 minutes, stop 5 minutes; alternation according to this, amounts to the mixed 5 hours powder time, obtains mixed uniformly powder.
(3) powder after step (2) mixing is put into mould, under pressure 200MPa, carry out cold moudling, 3 minutes dwell times, under hydrogen shield, sintering is cold-pressed into shaped piece, sintering temperature 850 DEG C, temperature retention time 3 hours.
(4) extrusion process, temperature 750 DEG C, extrusion ratio 100:1, makes Ni-coated graphite alkene/silver-colored nickel electric contact material.
Embodiment 4
Ni-coated graphite alkene: nickel powder: the weight ratio that 2:20:78 pressed by silver powder loads in ball mill, and other conditional parameters are with embodiment 3, and adopt rolling machine-shaping, temperature 600 DEG C, deformation rate is 80%, makes Ni-coated graphite alkene/silver-colored nickel electric contact material.
Embodiment 5
Ni-coated graphite alkene: nickel powder: the weight ratio that 5:20:75 pressed by silver powder loads in ball mill, and other conditional parameters are with embodiment 3, and adopt rolling machine-shaping, temperature 850 DEG C, deformation rate is 90%, makes Ni-coated graphite alkene/silver-colored nickel electric contact material.
Comparative example 1
Silver powder: nickel powder loads ball mill by the weight ratio of 20:80 and mixes powder, and other parameter, with embodiment 3, makes silver-colored nickel electric contact material.
Comparative example 2
Silver powder: nickel powder loads ball mill by the weight ratio of 10:90 and mixes powder, and other parameter, with embodiment 3, makes silver-colored nickel electric contact material.
Comparative example 3
Graphene and silver powder are by weight: 0.5:99.5 loads ball mill grinding, and other parameter, with embodiment 3, is made Graphene and strengthened silver-colored nickel electric contact material.
The composite material parameters made is as following table:
Add Ni-coated graphite alkene to make Graphene and strengthen silver-colored nickel electric contact material, with do not add in comparative example 1,2 that Graphene makes silver-colored nickel electric contact material compared with, though hardness, conductivity all significantly improve or conductivity does not improve, hardness significantly improves.With add in comparative example 3 that Graphene makes silver-colored nickel electric contact material compared with, hardness significantly improves, and obtains better combination property.
Claims (7)
1. a preparation method for Ni-coated graphite alkene/silver-colored nickel electric contact material, is characterized in that, comprise the following steps:
(1) direct current magnetron sputtering process is adopted to make Ni-coated graphite alkene at graphenic surface plated metal nickel;
(2) by 0.1-5.0wt% Ni-coated graphite alkene, 10%-40wt% nickel powder, surplus is that silver is put into ball mill ball milling and mixed powder, nickel powder granularity 300 order-450 order, silver powder granularity 200 order-300 order;
(3) powder after step (2) mixing is put into mould cold moudling, sintering;
(4) extruding or rolling mill practice make Ni-coated graphite alkene/silver-colored nickel electric contact material.
2. preparation method according to claim 1, is characterized in that, in step (1), Graphene is N layer, and N is 1-10.
3. preparation method according to claim 1, is characterized in that, the concrete technology of Deposited By Dc Magnetron Sputtering equipment is in step (1): target to be purity be 99.99% nickel 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 at 0.8-1.2Pa, and sputtering power is at 80-120W, and sedimentation time is 5-20min.
4. preparation method according to claim 1; it is characterized in that, in step (2), ball milling mixes in powder process, adopts alumina balls grinding jar and agate ball; ratio of grinding media to material 3:1; vacuumize 10 minutes, then pass into the argon shield of purity 99.99%, rotating speed 150-350 rev/min; every ball milling 10-15 minute; stop 5 minutes, exchange rotation clockwise and counterclockwise, amount to mixed powder time 4-8 hour.
5. preparation method according to claim 1, is characterized in that, cold moudling pressure 150-350MPa, dwell time 2-5 minute in step (3), sinter, sintering temperature 800-1000 DEG C, temperature retention time 2-4 hour under the hydrogen shield of purity 99.9%.
6. preparation method according to claim 1, is characterized in that, in step (4), cold-rolled sintered blank extrusion process is shaping, extrusion temperature 600-850 DEG C, extrusion ratio 50:1-150:1.
7. preparation method according to claim 1, is characterized in that, cold-rolled sintered blank rolling machine-shaping in step (4), rolling temperature 600-850 DEG C, rolling reduction 80%-90%.
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| CN109207780A (en) * | 2018-09-17 | 2019-01-15 | 南昌大学 | A kind of milling method enhancing AZ31 magnesium alloy |
| CN114101666A (en) * | 2021-09-03 | 2022-03-01 | 叶浩博 | Graphene-based silver-saving electrical contact material and manufacturing method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108941966A (en) * | 2018-08-20 | 2018-12-07 | 苏州大学张家港工业技术研究院 | A kind of graphene strengthens the welding method of steel Al dissimilar materials weld seam |
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| CN109207780A (en) * | 2018-09-17 | 2019-01-15 | 南昌大学 | A kind of milling method enhancing AZ31 magnesium alloy |
| CN109207780B (en) * | 2018-09-17 | 2020-07-14 | 南昌大学 | Rolling method for reinforcing AZ31 magnesium alloy |
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