CN101256903A - Silver-graphitic electrical contact composite plating layer and method of preparing the same - Google Patents
Silver-graphitic electrical contact composite plating layer and method of preparing the same Download PDFInfo
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- CN101256903A CN101256903A CNA2008100348368A CN200810034836A CN101256903A CN 101256903 A CN101256903 A CN 101256903A CN A2008100348368 A CNA2008100348368 A CN A2008100348368A CN 200810034836 A CN200810034836 A CN 200810034836A CN 101256903 A CN101256903 A CN 101256903A
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Abstract
Silver -black lead electrical contact composite plating and manufacture method thereof, which belongs to metallic material technology field. The steps are: confecting compound plating solution, black lead granule dispersing, and substrate preprocess, compound plating solution ingredient: methane sulfonic acid silver 0.05M/L, succinimide 0.15M/L-1.5M/L, composite plating. boracic acid 0.5M/L-0.5M/L, black lead content in solution 2g/L-50g/L. The composite plating is made up of silver and black lead, wherein the black lead volume percent is: 1-15%, silver volume fraction 85%-99%, contact resistance 1.2-2m Omega, hardness 70-100Hv, density more than 99.9%. The present invention plating solution is protection environment and non-toxic; the ultrasonic energy promoting adequate distribution of black lead granule, the produced composite plating has smooth surface and high density.
Description
Technical field
Invention relates to a kind of silver-graphitic composite material and preparation method thereof, particularly a kind of silver-graphitic electrical contact composite plating layer and preparation method thereof, belongs to the metal material technical field.
Background technology
Industrial extensive use silver is as contact material, but fine silver hardness is low, resistance to wear is relatively poor, resistance fusion welding is relatively poor.Silver and the compound of graphite not only have excellent lubrication, and can significantly improve the non-oxidizability and the resistance fusion welding of silver, are therefore needing to have special application advantage on the parts of sliding contact.Industrial main employing powder metallurgy method prepares the silver-graphitic composite material at present, and the problem material density of existence is poor, and Graphite Distribution is inhomogeneous, and the contact electric life is relatively poor, and can not prepare complex-shaped part.In addition according to statistics, the present silver that is used for contact material in the world accounts for 1/4th of whole silver consuming amounts.And silver-colored in a kind of noble metal, the cost height adopts composite electric plating method to prepare slider material, can reduce the loss of silver, and the preparation method is simple, and significant meaning is arranged economically.
Through new to the tea of prior art, Germany Siemens company has developed the process that composite plating prepares the silver-graphitic composite deposite under the cyaniding plant of silver system, but the problem that exists is that the coating surface of preparation is coarse, loose porous, causes wear extent big, and useful life is not long.Because cyanide is hypertoxic, environment is caused huge pollution simultaneously, soon on the verge of being replaced.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of silver-graphitic electrical contact composite plating layer and preparation method thereof is provided, make it on the copper matrix surface, prepare silver-graphitic electrical contact composite plating layer with ultrasonic assisted recombination galvanoplastic.The electroplate liquid nonhazardous that the present invention uses, environmentally friendly, can save in a large number with silver, and technology is simple, easy operating, low for equipment requirements, production cost is low; The coating surface of preparation is bright and clean, density is high, and graphite granule is uniformly dispersed, and contact resistance is low, the hardness height.
The present invention is achieved by the following technical solutions:
Silver-graphitic electrical contact composite plating layer involved in the present invention, by silver and graphite two phase compositions, wherein the graphite volume fraction is 1%-15%, the volume fraction of silver is 85%-99%.Physical property is contact resistance 1.2m Ω-2m Ω, hardness 70Hv-100Hv, and density reaches more than 99.9%.
The preparation method of silver-graphitic electrical contact composite plating layer involved in the present invention may further comprise the steps:
The first step, preparation composite plating solution.
The composite plating solution main component is: utilized as silver methane sulfonate 0.05M/L-0.5M/L, succimide 0.15M/L-1.5M/L, boric acid 0.5M/L-0.5M/L, pH value 8-11, content of graphite 2g/L-50g/L in the solution.
Second step, graphite granule disperse.
Obtain to such an extent that add the dispersant of dodecyl APEO (BRIJ35) 2g/L in the electroplate liquid in the first step as the graphite colloid, stir then and it was fully dissolved in 10 minutes-30 minutes, then composite plating solution was placed the ultrasonic tank sonicated 10 minutes-30 minutes, the graphite colloid in the solution is fully disperseed.
The 3rd step, substrate pretreated.
Configuration oxide film dissolving mixed acid: percent by volume is: H
2SO
4: HNO
3: HCl=90: 9: 1.
Matrix copper spare is placed acetone soln, and oil removing is 5 minutes-15 minutes in ultrasonic tank.
Oxide film dissolving in mixed acid then, the pickling time is 1 second-5 seconds.
The 4th step, composite plating
To place prepared composite plating solution of second step through pretreated copper spare of the 3rd step as negative electrode, and adopt ultrasonication at cathode surface, supersonic frequency 20KHz-45KHz, ultrasonic power are 5W/cm
2-250W/cm
2, current density range 0.5-6A/dm
2, temperature 35-80 ℃, pH 8-11, electroplating time 10-60 minute, anode adopted silver plate.Electroplate and finish to obtain silver-graphitic electrical contact composite plating layer.
The present invention adopts the environment-friendly type composite plating process to prepare that silver-graphitic is compound to electrically contact coating, and thickness can reach 10-100 μ m, and hardness is 70-100Hv.This technology major advantage is: electroplate liquid environment-protecting asepsis evil, ultrasonic energy promotes the even distribution of graphite granule, the composite deposite surfacing for preparing, density height under ultrasonication.Adopt the silver-graphitic composite material of composite electric plating method preparation can save in a large number with silver with respect to methods such as powder metallurgy, extruding sintering, technology is simple, and production cost is low.
Embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The first step, the preparation composite plating solution: the electroplate liquid parameter of preparation is: utilized as silver methane sulfonate 0.05M/L, succimide 0.25M/L, boric acid 0.05M/L, content of graphite 10g/L, pH 8.
Second step, the dispersion of graphite granule: in composite plating solution, add dispersant 2g/L (dodecyl APEO), stir then and it was fully dissolved in 10 minutes, composite plating solution was placed the ultrasonic tank sonicated 10 minutes then, the graphite colloid in the solution is fully disperseed.
The 3rd step, substrate pretreated:
Configuration oxide film dissolving mixed acid: percent by volume is: H
2SO
4: HNO
3: HCl=90: 9: 1.
Matrix copper spare is placed acetone soln, and oil removing is 5 minutes in ultrasonic tank, then 1 second oxide film dissolving of pickling in mixed acid.
The 4th step, composite plating:
Pretreated copper spare as negative electrode, is placed the scattered composite plating solution of graphite granule, adopt ultrasonication at cathode surface.Supersonic frequency 20KHz, ultrasonic power density 200W/cm
2, current density 0.5A/dm
2, 35 ℃ of temperature, anode adopts silver plate, and electroplating time 60 minutes obtains graphite percent by volume 1%, and hardness is 97Hv, the composite deposite of contact resistance 1.6m Ω.
Embodiment 2
The first step, the electroplate liquid parameter of preparation is:
Utilized as silver methane sulfonate 0.15M/L, succimide 0.75M/L, boric acid 0.15M/L, content of graphite 30g/L, pH 10.
Second step, the dispersion of graphite granule:
In composite plating solution, add dispersant 2g/L (dodecyl APEO), stir then and it was fully dissolved in 20 minutes, composite plating solution was placed the ultrasonic tank sonicated 20 minutes then, the graphite colloid in the solution is fully disperseed.
The 3rd step, substrate pretreated:
Configuration oxide film dissolving mixed acid: percent by volume is: H
2SO
4: HNO
3: HCl=90: 9: 1.
Matrix copper spare is placed acetone soln, and oil removing is 10 minutes in ultrasonic tank, then 3 seconds oxide film dissolvings of pickling in mixed acid.
The 4th step, composite plating:
Pretreated copper spare as negative electrode, is placed the scattered composite plating solution of graphite granule, adopt ultrasonication at cathode surface.Supersonic frequency 30KHz, ultrasonic power density 5W/cm
2, current density 3A/dm
2, 50 ℃ of temperature, anode adopts silver plate, and electroplating time 20 minutes obtains graphite percent by volume 15%, and hardness is 77Hv, the composite deposite of contact resistance 1.7m Ω.
Embodiment 3
The first step, the electroplate liquid parameter of preparation is: utilized as silver methane sulfonate 0.5M/L, succimide 1.5M/L, boric acid 0.5M/L, content of graphite 50g/L, pH11.
Second step, the dispersion of graphite granule:
In composite plating solution, add dispersant 2g/L (dodecyl APEO), stir then and it was fully dissolved in 30 minutes, composite plating solution was placed the ultrasonic tank sonicated 30 minutes then, the graphite colloid in the solution is fully disperseed.
The 3rd step, substrate pretreated:
Configuration oxide film dissolving mixed acid: percent by volume is: H
2SO
4: HNO
3: HCl=90: 9: 1.
Matrix copper spare is placed acetone soln, and oil removing is 15 minutes in ultrasonic tank, then 5 seconds oxide film dissolvings of pickling in mixed acid.
The 4th step, composite plating:
Pretreated copper spare as negative electrode, is placed the scattered composite plating solution of graphite granule, adopt ultrasonication at cathode surface.Current density 4A/dm
2, 80 ℃ of temperature, electroplating time 15 minutes, supersonic frequency 45KHz, ultrasonic power density 21W/cm
2, anode adopts high-purity silver plate, obtains graphite percent by volume 7%, and hardness is 84Hv, the composite deposite of contact resistance 1.3m Ω.
Embodiment 4
The first step, the electroplate liquid parameter of preparation is: utilized as silver methane sulfonate 0.1M/L, succimide 0.25M/L, boric acid 0.1M/L, content of graphite 40g/L, pH 10.
Second step, the dispersion of graphite granule:
In composite plating solution, add dispersant 2g/L (dodecyl APEO), stir then and it was fully dissolved in 30 minutes, composite plating solution was placed the ultrasonic tank sonicated 30 minutes then, the graphite colloid in the solution is fully disperseed.
The 3rd step, substrate pretreated:
Configuration oxide film dissolving mixed acid: percent by volume is: H
2SO
4: HNO
3: HCl=90: 9: 1.
Matrix copper spare is placed acetone soln, and oil removing is 15 minutes in ultrasonic tank, then 5 seconds oxide film dissolvings of pickling in mixed acid.
The 4th step, composite plating:
Pretreated copper spare as negative electrode, is placed the scattered composite plating solution of graphite granule, adopt ultrasonication at cathode surface.Current density 6A/dm
2, 80 ℃ of temperature, electroplating time 15 minutes, supersonic frequency 20KHz, ultrasonic power density 100W/cm
2, anode adopts high-purity silver plate, obtains graphite percent by volume 2%, and hardness is 100Hv, the composite deposite of contact resistance 1.5m Ω.
Claims (10)
1, a kind of silver-graphitic electrical contact composite plating layer is characterized in that, by silver and graphite two phase compositions, wherein the graphite volume fraction is 1%-15%, and the volume fraction of silver is 85%-99%.
2, silver-graphitic electrical contact composite plating layer according to claim 1 is characterized in that, contact resistance is 1.2m Ω-2m Ω, and hardness is 70Hv-100Hv, and density reaches more than 99.9%.
3, a kind of preparation method of silver-graphitic electrical contact composite plating layer as claimed in claim 1 is characterized in that, may further comprise the steps:
The first step, the preparation composite plating solution: the composite plating solution composition is: utilized as silver methane sulfonate 0.05M/L-0.5M/L, succimide 0.15M/L-1.5M/L, boric acid 0.5M/L-0.5M/L, content of graphite 2g/L-50g/L in the solution;
Second step, graphite granule disperses: obtain to such an extent that add the dispersant of dodecyl APEO as the graphite colloid in the electroplate liquid in the first step, stirring is fully dissolved it, then composite plating solution is placed the ultrasonic tank sonicated, and the graphite colloid in the solution is fully disperseed;
The 3rd step, substrate pretreated: matrix copper spare is placed acetone soln, oil removing in ultrasonic tank, oxide film dissolving in mixed acid then;
In the 4th step, composite plating: will place prepared composite plating solution of second step through pretreated copper spare of the 3rd step as negative electrode, and adopt ultrasonication at cathode surface, anode adopts silver plate, electroplates and finishes to obtain silver-graphitic electrical contact composite plating layer.
4, the preparation method of silver-graphitic electrical contact composite plating layer according to claim 3 is characterized in that, in second step, and described composite plating solution, its pH value is 8-11.
5, the preparation method of silver-graphitic electrical contact composite plating layer according to claim 3 is characterized in that, in second step, dodecyl APEO addition is 2g/L, and mixing time is 10 minutes-30 minutes, and the sonicated time is 10 minutes-30 minutes.
6, the preparation method of silver-graphitic electrical contact composite plating layer according to claim 3 is characterized in that, in the 3rd step, the oil removing time is 5 minutes-15 minutes; Oxide film dissolving in mixed acid, the pickling time is 1 second-5 seconds.
According to the preparation method of claim 3 or 6 described silver-graphitic electrical contact composite plating layers, it is characterized in that 7, in the 3rd step, described mixed acid percent by volume is: H
2SO
4: HNO
3: HCl=90: 9: 1.
8, the preparation method of silver-graphitic electrical contact composite plating layer according to claim 3 is characterized in that, in the 4th step, and described composite plating, its supersonic frequency is 20KHz-45KHz, ultrasonic power is 5W/cm
2-250W/cm
2
9, according to the preparation method of claim 3 or 8 described silver-graphitic electrical contact composite plating layers, it is characterized in that, in the 4th step, described composite plating, its current density range 0.5-6A/dm
2, temperature range 35-80 ℃.
10, according to the preparation method of claim 3 or 8 described silver-graphitic electrical contact composite plating layers, it is characterized in that, in the 4th step, described composite plating, its pH value 8-11, electroplating time 10 minutes-60 minutes.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102061495A (en) * | 2010-11-15 | 2011-05-18 | 沈阳工业大学 | Graphite dispersant agent in cyanide-free electrodeposition silver-graphite alloy plating solution and preparation method |
| CN104694997A (en) * | 2015-03-13 | 2015-06-10 | 哈尔滨工程大学 | Method for obtaining nano Cu-Sn-graphite composite coating and Cu-Sn-graphite electroplating solution |
| CN104746113A (en) * | 2015-04-27 | 2015-07-01 | 南京宁美表面技术有限公司 | Cyanide-free silver plating solution and electroplating method |
| CN105006383A (en) * | 2015-07-13 | 2015-10-28 | 青海大学 | Novel silver-based low-voltage contact material |
| CN105297095A (en) * | 2015-12-14 | 2016-02-03 | 南昌航空大学 | Functional coating of pure silver layer/pure-graphite composite layer and preparation method of functional coating |
| CN105386091A (en) * | 2015-12-24 | 2016-03-09 | 南昌航空大学 | Graphite dispersion composite additive |
| CN106367785A (en) * | 2016-09-21 | 2017-02-01 | 南昌航空大学 | Cyanide-free silver-graphene composite coating and preparation method |
| CN107164791A (en) * | 2017-06-08 | 2017-09-15 | 广东电网有限责任公司电力科学研究院 | Silver/graphite composite silver plating liquor and preparation method thereof and electrodeposition technology |
| CN107749364A (en) * | 2017-09-27 | 2018-03-02 | 国家电网公司 | A kind of high voltage isolation switch contact fingertip and its production technology |
| CN108468017A (en) * | 2018-03-20 | 2018-08-31 | 西安福莱电工合金有限公司 | A kind of magnetically controlled sputter method preparing silver-colored graphite composite deposite in copper contact surfaces |
| CN109137011A (en) * | 2018-09-20 | 2019-01-04 | 吕莉 | A kind of preparation method of high voltage isolator contact material |
| CN111180102A (en) * | 2020-01-04 | 2020-05-19 | 浙江大学 | Preparation method of conductive silver paste based on silver-coated graphite conductive agent |
| JP2020152929A (en) * | 2019-03-18 | 2020-09-24 | Ｄｏｗａメタルテック株式会社 | Composite plated material, and method of producing the same |
| CN114144544A (en) * | 2019-08-01 | 2022-03-04 | 同和金属技术有限公司 | Composite plated article and method for producing the same |
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2008
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102061495A (en) * | 2010-11-15 | 2011-05-18 | 沈阳工业大学 | Graphite dispersant agent in cyanide-free electrodeposition silver-graphite alloy plating solution and preparation method |
| CN102061495B (en) * | 2010-11-15 | 2012-07-04 | 沈阳工业大学 | Graphite dispersant agent in cyanide-free electrodeposition silver-graphite alloy plating solution and preparation method |
| CN104694997A (en) * | 2015-03-13 | 2015-06-10 | 哈尔滨工程大学 | Method for obtaining nano Cu-Sn-graphite composite coating and Cu-Sn-graphite electroplating solution |
| CN104746113A (en) * | 2015-04-27 | 2015-07-01 | 南京宁美表面技术有限公司 | Cyanide-free silver plating solution and electroplating method |
| CN105006383A (en) * | 2015-07-13 | 2015-10-28 | 青海大学 | Novel silver-based low-voltage contact material |
| CN105297095A (en) * | 2015-12-14 | 2016-02-03 | 南昌航空大学 | Functional coating of pure silver layer/pure-graphite composite layer and preparation method of functional coating |
| CN105386091A (en) * | 2015-12-24 | 2016-03-09 | 南昌航空大学 | Graphite dispersion composite additive |
| CN106367785A (en) * | 2016-09-21 | 2017-02-01 | 南昌航空大学 | Cyanide-free silver-graphene composite coating and preparation method |
| CN107164791A (en) * | 2017-06-08 | 2017-09-15 | 广东电网有限责任公司电力科学研究院 | Silver/graphite composite silver plating liquor and preparation method thereof and electrodeposition technology |
| CN107749364A (en) * | 2017-09-27 | 2018-03-02 | 国家电网公司 | A kind of high voltage isolation switch contact fingertip and its production technology |
| CN108468017A (en) * | 2018-03-20 | 2018-08-31 | 西安福莱电工合金有限公司 | A kind of magnetically controlled sputter method preparing silver-colored graphite composite deposite in copper contact surfaces |
| CN109137011A (en) * | 2018-09-20 | 2019-01-04 | 吕莉 | A kind of preparation method of high voltage isolator contact material |
| JP2020152929A (en) * | 2019-03-18 | 2020-09-24 | Ｄｏｗａメタルテック株式会社 | Composite plated material, and method of producing the same |
| CN111705340A (en) * | 2019-03-18 | 2020-09-25 | 同和金属技术有限公司 | Composite plated article and method of making same |
| JP7233991B2 (en) | 2019-03-18 | 2023-03-07 | Ｄｏｗａメタルテック株式会社 | Composite plated material and its manufacturing method |
| CN114144544A (en) * | 2019-08-01 | 2022-03-04 | 同和金属技术有限公司 | Composite plated article and method for producing the same |
| CN111180102A (en) * | 2020-01-04 | 2020-05-19 | 浙江大学 | Preparation method of conductive silver paste based on silver-coated graphite conductive agent |
| CN111180102B (en) * | 2020-01-04 | 2020-12-15 | 浙江大学 | Preparation method of conductive silver paste based on silver-coated graphite conductive agent |
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