CN105779801A - Graphene enhanced silver nickel electric contact composite material and preparation method thereof - Google Patents
Graphene enhanced silver nickel electric contact composite material and preparation method thereof Download PDFInfo
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- C22C1/00—Making non-ferrous alloys
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- C22C5/06—Alloys based on silver
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- H—ELECTRICITY
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- H01H1/00—Contacts
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a graphene enhanced silver nickel electric contact composite material and a preparation method thereof. The method comprises the following steps: preparing by using a chemical method to obtain silver oxidized graphene composite powder; mixing metal nickel powder and the silver oxidized graphene composite powder; and carrying out reduction treatment, powder metallurgy and hot extrusion technologies to obtain the graphene enhanced silver nickel electric contact composite material. While the original performance of AgNi is kept, the conductivity and welding resistance of the graphene enhanced silver nickel electric contact composite material can be improved, and contact resistance is reduced. The preparation method is easy to operate, the technology is easy to control, and large-scale production is easy to implement.
Description
Technical field
The preparation method that the present invention relates to the metal-base composites of a kind of field of material technology, specifically, refers to a kind of Graphene and strengthens silver nickel electric contact composite material and preparation method thereof.
Background technology
Graphene is because of its unusual conduction, heat conductivility, high hardness, intensity and corrosion resistance etc. and become study hotspot, and along with the progressively breakthrough of the difficult problem such as mass production and large scale, Graphene will be applied to the fields such as mobile equipment, Aero-Space, new forms of energy battery at first.Although the research and development of graphene reinforced metal-matrix composite is slow, but the conduction of Graphene excellence, heat conduction and mechanical performance will bring major transformation to metal-base composites performance boost.Correlational study report was continuously increased in recent years.
Publication number is the Chinese invention patent of CN1848323A, provide a kind of silver-nickel electric contact producing technology, it is application " co-precipitation-ball-milling method " preparation silver nickel electric contact raw material powder, and powder body preparation engineering includes getting the raw materials ready, displacement reaction, powder cleaning and drying is sieved, liquid waste processing, ball mill pulverizing and reduction treatment operation;Then through pressed compact, sintering, multiple pressure and extrusion process, obtain silver nickel composite material.This present invention is complicated, especially in its powder body preparation process, very easily brings impurity, and this material resistance is high, and electrical contact performance is not good, it is necessary to improve further.
Publication number is the Chinese invention patent of CN103466611B, the preparation method providing a kind of graphene load nano silver-nickel alloy composite granule, adopt oxidation-reduction method to be prepared for graphene oxide, then reduce through reducing agent after Graphene is mixed with silver ion and nickel ion and obtain graphene nano silver-nickel composite granule.This invention is simple, and without any coating material, Graphene distribution is relatively uniform.But, in the composite powder that the method obtains nickel due to granule tiny, very easily oxidized, be unfavorable for store and application, largely limit the application of this composite.
Publication number is the Chinese invention patent of CN104700961A, provide a kind of graphene/silver composite material and preparation method thereof, graphene oxide solution successively adds reducing agent and silver nitrate, the argentum powder that reduction prepares graphene oxide compound directly and in solution, tentatively obtain graphene oxide/argentum composite powder, it is dried reduction and obtains Graphene/argentum composite powder, obtain the compound bulk of Graphene/silver, composite wire material, composite strip again through powder metallurgy, hot extrusion, rolling technique.In composite prepared by this invention, graphene dispersion is uniform, and matrix and reinforcement interface cohesion good.But simple with Graphene for strengthening phase, the anti electric arc corrosion ability of composite, materials loss rate is high, it is impossible to large-scale application, can be only applied to specified conditions
Although the addition of Graphene can improve the conduction of material, heat conduction and mechanical performance to a certain extent in the studies above, but its aspect such as process controllability, material property still needs to further improvement.
Therefore, realize High-performance graphene with a kind of environmental protection, low cost, production technology means that controllability is good and strengthen the preparation of silver nickel contact material not only there is important scientific research value, and be with a wide range of applications.
Summary of the invention
The present invention is directed to deficiency and defect that above-mentioned prior art exists, it is provided that a kind of Graphene strengthens silver nickel electric contact composite material and preparation method thereof.The present invention adopts silver as matrix material, and Graphene strengthens phase as first, and metallic nickel strengthens phase as second, prepare consistency height, conduct electricity very well, anti-melting welding ability strong, the silver/graphite alkene that contact resistance is low/nickel (AgGRNi) composite.Meanwhile, the method is simple, and process controllability is good, and cost is low, easily accomplishes scale production, described silver-based composite material even tissue, stable performance.
The present invention is achieved by the following technical solutions:
The present invention first uses chemical method to prepare silver graphene oxide composite powder, then is mixed with silver graphene oxide composite powder by metal nickel powder, obtains preparation AgGRNi composite by reduction treatment, powder metallurgy, Hot-extrusion.AgGRNi composite is while keeping the original performance of AgNi, it is possible to improve its electrical conductivity and anti-melting welding ability, reduces contact resistance, and this preparation method is simple to operate, technique is easily-controllable, easily accomplishes scale production.
For achieving the above object, the preparation method that Graphene of the present invention strengthens silver nickel electric contact composite material, comprise the steps:
The first step, mixes silver/graphene oxide composite powder with nikel powder, obtains silver/graphene oxide/nickle composite powder;
Second step, reduces silver/graphene oxide/nickle composite powder, obtains AgGRNi composite powder;
3rd step, adopts PM technique, is shaped by described AgGRNi composite powder, sintering processes, obtain the AgGRNi composite of high-compactness, and namely Graphene strengthens silver nickel electric contact composite material.
Preferably, in the first step: described silver/graphene oxide composite powder is to be prepared by chemical synthesis.Specifically, graphene oxide solution mixes with reductant solution, then this mixed liquor mixes with silver nitrate solution, and then is sufficiently mixed the suspension of reaction acquisition silver/graphene oxide composite powder, obtains pure silver/graphene oxide composite powder through settling, wash, drying.
It is furthermore preferred that described reducing agent is one or more in the non-toxic, environmental friendly reducing agents such as ascorbic acid, glucose, citric acid, oxalic acid.The concentration of reductant solution and silver nitrate solution is 0.1mol/L-1mol/L, and the mass concentration of graphene oxide solution is 0.5%-1.8%, and graphene oxide addition accounts for the 0.3wt%-5wt% of composite gross mass.
Preferably, in the described first step, silver/graphene oxide composite powder is mixed with nikel powder: using V-type batch mixer or ball mill to be mixed homogeneously with metallic nickel powder body by silver/graphite alkene composite powder, mixing time is 3-8 hour, and wherein the addition of nickel accounts for the 1wt%-30wt% of composite gross mass.
Preferably, in described second step, owing to the oxy radical of surface of graphene oxide can hinder the transmission of electronics, reduce the electric conductivity of composite, it is necessary to silver/graphene oxide composite powder is carried out reduction treatment.This process heat reduction in a hydrogen atmosphere, heating-up temperature is 450 DEG C-700 DEG C, 3-12 hour heat time heating time, obtains silver/graphite alkene composite powder.
Preferably, in described 3rd step, powder metallurgy process includes isostatic cool pressing and sintering process, and hydrostatic pressure is 0.6GPa-6GPa, and sintering temperature is 500 DEG C-900 DEG C, and sintering time is 3-12 hour, and sintering atmosphere is hydrogen.
As an optimal way, after the 3rd step, farther include the 4th step: described AgGRNi composite is carried out extrusion process, the further densification of material structure, obtain AgGRNi silk material.
Preferably, in described 4th step, the temperature of hot extrusion is 500 DEG C-800 DEG C, and extrusion ratio is 20-80.
The present invention also provides for a kind of AgGRNi composite prepared by said method.
In the present invention, it is possible to conveniently control the pattern particle diameter of Graphene, the addition of Ni and silver matrix, it is preferred that, graphene oxide addition is the addition of 0.3wt%-5wt%, Ni is 1wt%-30wt%, and surplus is silver, morphologies prepared by electronation is spherical, and particle diameter is 0.2 μm-8 μm.Graphene reinforced effects is obvious, can meet different application demands preferably.Further, graphene oxide addition is preferably the addition of 0.5wt%-0.8wt%, Ni and is preferably 10wt%-35wt%.
Compared with prior art, the invention have the benefit that
(1) adopting hydrogen silver/graphene oxide/nickle composite powder to reduce, obtain silver/graphite alkene/nickel composite powder, the oxide of part of nickel, while redox graphene, has been also carried out reduction by this process, is conducive to improving the electric conductivity of composite.
(2) sintering processes in powder metallurgy process, omnidistance employing hydrogen shield, it is ensured that the structure of Graphene is not destroyed, and also ensure that nickel is not oxidized.
(3) addition of Graphene, effectively improves tradition the resistance fusion welding energy of AgNi material, temperature characteristic etc., and reduces its contact resistance.
(4) further, adopt chemical method to prepare silver/graphene oxide composite powder, it is ensured that graphene oxide dispersed, and composite effect is good.
The present invention is cooperated by the technology such as between PM technique, chemical synthesising technology and Hot-extrusion, it is possible to prepares the AgGRNi composite of excellent performance, breaches a series of problem in science and technical barrier.Comparing the AgNi electric contact composite material strengthened without Graphene, the electric life of AgGRNi composite contact improves 15%~30%, and contact resistance reduces 5%~20%, and melting welding power reduces by 15%~30%.
The present invention realizes High-performance graphene strengthen the preparation of silver nickel contact material with a kind of environmental protection, low cost, production technology means that controllability is good, not only has important scientific research value, and is with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is the preparation technology flow chart of the AgGRNi composite of preferred embodiment of the present invention.
Detailed description of the invention
Hereinafter technical scheme being further described, the following description is only the use understanding technical solution of the present invention, is not used in restriction the scope of the present invention, and protection scope of the present invention is as the criterion with claims.
As it is shown in figure 1, this figure is the preparation technology flow chart of the AgGRNi composite of preferred embodiment of the present invention, the preparation technology of AgGRNi composite can be sequentially carried out according to this flow process, it is possible to according to practical application request, selects to carry out separate step therein.
Embodiment one
The basic operational steps that the present embodiment 1 prepares AgGRNi composite is as follows:
I) material composition of AgGRNi composite
The material composition of AgGRNi composite is mainly argent, metallic nickel and Graphene, and wherein graphene oxide addition is 0.5wt%, and the addition of nickel is 10wt%, and surplus is silver.
II) basic step (accompanying drawing 1 is shown in technological process) of AgGRNi composite is prepared
1) preparation 0.1mol/L silver nitrate solution and 0.1mol/L ascorbic acid solution (or glucose or citric acid or oxalic acid one or more);
2) taking 2.5L ascorbic acid solution with 24.6g mass concentration is that 0.5% graphene oxide solution mixes, and ion stirs 5-10 minute, takes 2L silver nitrate solution and joins in above-mentioned mixed liquor, continues ion stirring.Silver nitrate and ascorbic acid generation reduction reaction, generate Argent grain, and graphene oxide is adsorbed by argentum powder, obtains silver/graphene oxide suspension.By silver/graphene oxide suspension centrifuge washing 5-10 time, lyophilization, obtain silver/graphene oxide composite powder.
3) using V-type batch mixer, mixed with 2.5g nikel powder by gained silver/graphene oxide composite powder, the mixed powder time is 5 hours, obtains silver/graphene oxide/nickel composite powder.
4) by silver/graphene oxide/nickel composite powder in a hydrogen atmosphere, 450 DEG C of heat reductions 3 hours, obtain AgGRNi composite powder.
5) utilizing isostatic cool pressing technology by compressing for AgGRNi composite powder, obtain AgGRNi billet, this billet is positioned over sintering furnace, lower 850 DEG C of hydrogen atmosphere sinters 10 hours, obtains the AgGRNi composite of high compaction.
Embodiment 2
Main difference is that with embodiment 1: the present embodiment 2 adds hot extrusion process, obtain AgGRNi composite wire material.
I) material composition of AgGRNi composite
The material composition of AgGRNi composite is mainly argent, stannum oxide and Graphene, and wherein graphene oxide addition is 0.3wt%, and the addition of nickel is 15wt%, and surplus is silver.
II) basic step (accompanying drawing 1 is shown in technological process) of AgGRNi composite is prepared
1) preparation 0.2mol/L silver nitrate solution and 0.2mol/L ascorbic acid solution;
2) taking 2.5L ascorbic acid solution with 25.1g mass concentration is that 0.6% graphene oxide solution mixes, and ion stirs 5-10 minute, takes 2L silver nitrate solution and joins in above-mentioned mixed liquor, continues ion stirring.Silver nitrate and ascorbic acid generation reduction reaction, generate Argent grain, and graphene oxide is adsorbed by argentum powder, obtains silver/graphene oxide suspension.By silver/graphene oxide suspension centrifuge washing 5-10 time, lyophilization, obtain silver/graphene oxide composite powder.
3) using V-type batch mixer, mixed with 7.5g nikel powder by gained silver/graphite alkene composite powder, the mixed powder time is 6.5 hours, obtains silver/graphene oxide/nickel composite powder.
4) by silver/graphene oxide/nickel composite powder in a hydrogen atmosphere, 500 DEG C of heat reductions 4 hours, obtain AgGRNi composite powder.
5) utilizing isostatic cool pressing technology by compressing for AgGRNi composite powder, obtain AgGRNi billet, this billet is positioned over sintering furnace, lower 850 DEG C of hydrogen atmosphere sinters 12 hours, obtains the AgGRNi composite of high compaction.
6) the AgGRNi composite after high density powder metallurgy being carried out hot extrusion, extrusion temperature is 500 DEG C, and extrusion ratio is 40, obtains AgGRNi composite wire material.Resulting materials is carried out basic physics performance test, it has been found that resistivity is 2.2;Vickers hardness hv is 90;Hot strength is 210MPa;Elongation percentage is 19%.It addition, after this material prepares into rivet contact, its electric life compares AgNi15Promoting 20%, contact resistance reduces by 10%.
Embodiment 3
Main difference is that with embodiment 2: in the present embodiment 3, reducing agent adopts the mixing reductant solution of ascorbic acid and glucose, changes the addition of Graphene and nickel simultaneously, obtains AgGRNi composite wire material.
I) material composition of AgGRNi composite
The material composition of AgGRNi composite is mainly argent, metallic nickel and Graphene, and wherein graphene oxide addition is 0.8wt%, and the addition of nickel is 35wt%, and surplus is silver.
II) basic step (accompanying drawing 1 is shown in technological process) of AgGRNi composite is prepared
1) the mixing reductant solution of preparation 0.2mol/L silver nitrate solution and 0.2mol/L ascorbic acid and glucose, wherein ascorbic acid and glucose quality ratio is for 2:1;
2) taking 2.5L mixing reductant solution with 50g mass concentration is that 0.8% graphene oxide solution mixes, and ion stirs 5-10 minute, takes 2L silver nitrate solution and joins in above-mentioned mixed liquor, continues ion stirring.Silver nitrate and ascorbic acid generation reduction reaction, generate Argent grain, and graphene oxide is adsorbed by argentum powder, obtains silver/graphene oxide suspension.By silver/graphene oxide suspension centrifuge washing 5-10 time, lyophilization, obtain silver/graphene oxide composite powder.
3) using V-type batch mixer, mixed with 21g nikel powder by gained silver/graphite alkene composite powder, the mixed powder time is 7 hours, obtains silver/graphene oxide/nickel composite powder.
4) by silver/graphene oxide/nickel composite powder in a hydrogen atmosphere, 700 DEG C of heat reductions 5 hours, obtain AgGRNi composite powder.
5) utilizing isostatic cool pressing technology by compressing for AgGRNi composite powder, obtain AgGRNi billet, this billet is positioned over sintering furnace, lower 900 DEG C of hydrogen atmosphere sinters 8 hours, obtains the AgGRNi composite of high compaction.
6) the AgGRNi composite after high density powder metallurgy being carried out hot extrusion, extrusion temperature is 750 DEG C, and extrusion ratio is 60, obtains AgGRNi composite wire material.Resulting materials is carried out basic physics performance test, it has been found that resistivity is 2.6;Vickers hardness hv is 115;Hot strength is 210MPa;Elongation percentage is 15%.It addition, after this material prepares into rivet contact, its melting welding power compares AgNi30Reducing by 20%, contact resistance reduces by 16%.
Embodiment 4
Main difference is that with embodiment 3: the present embodiment 4 changes the addition of Graphene and nickel, obtain the AgGRNi composite wire material of high Graphene content.
I) material composition of AgGRNi composite
The material composition of AgGRNi composite is mainly argent, metallic nickel and Graphene, and wherein graphene oxide addition is 5wt%, and the addition of nickel is 1wt%, and surplus is silver.
II) basic step (accompanying drawing 1 is shown in technological process) of AgGRNi composite is prepared
1) the mixing reductant solution of preparation 0.2mol/L silver nitrate solution and 0.2mol/L ascorbic acid and glucose, wherein ascorbic acid and glucose quality ratio is for 2:1;
2) taking 2.5L mixing reductant solution with 167g mass concentration is that 1.5% graphene oxide solution mixes, and ion stirs 5-10 minute, takes 2L silver nitrate solution and joins in above-mentioned mixed liquor, continues ion stirring.Silver nitrate and ascorbic acid generation reduction reaction, generate Argent grain, and graphene oxide is adsorbed by argentum powder, obtains silver/graphene oxide suspension.By silver/graphene oxide suspension centrifuge washing 5-10 time, lyophilization, obtain silver/graphene oxide composite powder.
3) using V-type batch mixer, mixed with 0.5g nikel powder by gained silver/graphite alkene composite powder, the mixed powder time is 7 hours, obtains silver/graphene oxide/nickel composite powder.
4) by silver/graphene oxide/nickel composite powder in a hydrogen atmosphere, 600 DEG C of heat reductions 5 hours, obtain AgGRNi composite powder.
5) utilizing isostatic cool pressing technology by compressing for AgGRNi composite powder, obtain AgGRNi billet, this billet is positioned over sintering furnace, lower 500 DEG C of hydrogen atmosphere sinters 8 hours, obtains the AgGRNi composite of high compaction.
6) the AgGRNi composite after high density powder metallurgy being carried out hot extrusion, extrusion temperature is 550 DEG C, and extrusion ratio is 80, obtains AgGRNi composite wire material.Resulting materials is carried out basic physics performance test, it has been found that resistivity is 2.1;Vickers hardness hv is 90;Hot strength is 180MPa;Elongation percentage is 19%.It addition, after this material prepares into rivet contact, its melting welding power compares AgNi30Reducing by 30%, contact resistance reduces by 20%.
Should be understood that, above-described embodiment is only a part of embodiment of the present invention, Graphene of the present invention strengthens silver nickel electric contact composite material and includes all systems suitable in this product, as change matrix silver prepare formula, can also is that the combination of other silver salt solutions and reducing agent, Graphene and nickel reinforcement can also be any other a kind of feed postition, and the formula of final composite should be designed according to practical application request.
Although present disclosure has been made to be discussed in detail already by above preferred embodiment, but it should be appreciated that the description above should not be regarded as limitation of the present invention.After those skilled in the art have read foregoing, multiple amendment and replacement for the present invention all will be apparent from.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. the preparation method that a Graphene strengthens silver nickel electric contact composite material, it is characterised in that comprise the following steps:
The first step, mixes silver/graphene oxide composite powder with nikel powder, obtains silver/graphene oxide/nickle composite powder;
Second step, reduces silver/graphene oxide/nickle composite powder, obtains AgGRNi composite powder;
3rd step, adopts PM technique, is shaped by described AgGRNi composite powder, sintering processes, obtain the AgGRNi composite of high-compactness, and namely Graphene strengthens silver nickel electric contact composite material.
2. the preparation method that Graphene as claimed in claim 1 strengthens silver nickel electric contact composite material, it is characterised in that in the first step, described silver/graphene oxide composite powder is to be prepared by chemical synthesis.
3. the preparation method that Graphene as claimed in claim 2 strengthens silver nickel electric contact composite material, it is characterized in that, described chemical synthesis refers to: graphene oxide solution mixed with reductant solution, then this mixed liquor mixes with silver nitrate solution, and then it is sufficiently mixed the suspension reacting acquisition silver/graphene oxide composite powder, through sedimentation, washing, dry silver/graphene oxide composite powder that acquisition is pure.
4. the preparation method that Graphene as claimed in claim 3 strengthens silver nickel electric contact composite material, it is characterised in that described reducing agent is one or more in ascorbic acid, glucose, citric acid, oxalic acid non-toxic, environmental friendly reducing agent;The concentration of described reductant solution and silver nitrate solution is 0.1mol/L-1mol/L.
5. the preparation method that Graphene as claimed in claim 3 strengthens silver nickel electric contact composite material, it is characterised in that the mass concentration of described graphene oxide solution is 0.5%-1.8%, and graphene oxide addition accounts for the 0.3wt%-5wt% of composite gross mass.
6. the preparation method that Graphene as claimed in claim 1 strengthens silver nickel electric contact composite material, it is characterized in that, in the first step, described silver/graphene oxide composite powder is mixed with nikel powder, incorporation time is 3-8 hour, and wherein the addition of nickel accounts for the 1wt%-30wt% of composite gross mass.
7. the preparation method that Graphene as claimed in claim 1 strengthens silver nickel electric contact composite material, it is characterised in that in second step, described silver/graphene oxide composite powder is reduced, referring to: heat reduction in a hydrogen atmosphere, heating-up temperature is 450 DEG C-700 DEG C, 3-12 hour heat time heating time.
8. the preparation method that Graphene as claimed in claim 1 strengthens silver nickel electric contact composite material, it is characterized in that, in 3rd step, described PM technique includes isostatic cool pressing and sintering process, hydrostatic pressure is 0.6GPa-6GPa, sintering temperature is 500 DEG C-900 DEG C, and sintering time is 3-12 hour, and sintering atmosphere is hydrogen.
9. the preparation method that the Graphene as described in any one of claim 1-8 strengthens silver nickel electric contact composite material, it is characterized in that, after the 3rd step, farther include the 4th step: described AgGRNi composite is carried out extrusion process, the further densification of material structure, obtains AgGRNi silk material.
10. the Graphene enhancing silver nickel electric contact composite material that prepared by a method as described in any one of claim 1-9.
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CN106363190A (en) * | 2016-09-18 | 2017-02-01 | 东莞市中合金科技有限公司 | Silver-nickel-graphene alloy material and preparation method thereof |
CN108218412A (en) * | 2017-12-23 | 2018-06-29 | 南京悠谷新材料科技有限公司 | A kind of preparation method of zinc-silver metallic composite |
CN108441668A (en) * | 2018-04-13 | 2018-08-24 | 上海和伍复合材料有限公司 | A kind of silver tungsten contact material and preparation method thereof |
CN108531764A (en) * | 2018-04-13 | 2018-09-14 | 上海和伍复合材料有限公司 | A kind of silver tungsten carbide carbon alkene contact material and preparation method thereof |
CN112620640A (en) * | 2020-12-09 | 2021-04-09 | 温州宏丰电工合金股份有限公司 | Preparation method of AgNi electrical contact material based on recycling of AgC scrap |
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