CN106367785A - Cyanide-free silver-graphene composite coating and preparation method - Google Patents
Cyanide-free silver-graphene composite coating and preparation method Download PDFInfo
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- CN106367785A CN106367785A CN201610836024.XA CN201610836024A CN106367785A CN 106367785 A CN106367785 A CN 106367785A CN 201610836024 A CN201610836024 A CN 201610836024A CN 106367785 A CN106367785 A CN 106367785A
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- silver
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Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/46—Electroplating: Baths therefor from solutions of silver
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
Abstract
The invention discloses a cyanide-free silver-graphene composite coating and a preparation method. The surface of a copper base material is electroplated with a silver coating and a silver-graphene coating. The preparation method of the cyanide-free silver-graphene composite coating comprises the steps of base body treatment, silver-graphene composite plating solution preparing, silver preplating and silver-graphene composite coating preparing. The cyanide-free silver-graphene composite coating has good electrical conductivity, good thermal conductivity, good abrasion resistance, a long service life, good corrosion resistance and good anti-sulfuration capacity, wherein the contact resistance is 15-30 [mu]omega (the external torque is 5-20 N.m); the heat conductivity rate is 350-500 W.m<1>.K<1>; the friction coefficient is 0.06-0.22 when the load at the normal temperature and pressure is 280 g; and the service life meet the standard between the M1 level and the M2 level of disconnector mechanical life levels in a mechanical life experiment (the clamping force is 400-600 N). The cyanide-free silver-graphene composite coating has good comprehensive performance, can meet outdoor working conditions of high-voltage disconnectors and has large application value.
Description
Technical field
The present invention relates to a kind of functional coating of no cyanogen silver Graphene, the particularly functional design of coating and its preparation
Method, belongs to electrical contact protective material technical field.
Background technology
At present, the dynamic and static contact of outdoor high-voltage isolating switch protects position many using there being cyanogen plating fine silver design, and this electricity connects
Tactile material can provide good electric conductivity, heat conductivity and low and stable contact resistance.But traditional cyaniding plant of silver system
Big for environment pollution, and there is the shortcomings of wear extent is big, resistance fusion welding is poor in coating, ultimately result in the heating event of disconnecting switch
Barrier.Because the self lubricity of crystalline flake graphite, non-oxidizability, good stability and specific surface area and surface energy are larger and promote metal
The characteristics such as ion deposition, the silver-graphitic composited contact material that Siemens is prepared by cyaniding plant of silver system can be significantly
Improve the wearability of contact material and service life, and easily form one layer of graphite on contact material surface during using
Layer protecting film, plays the effect reducing contact material surface contacted resistance.But its cyanide using has severe toxicity, with environment
Friendly is disagreed, and graphite, poor thermal conductivity certainly will affect the conduction of composite deposite, heat conductivity, be badly in need of a kind of electric conductivity,
Heat conductivity and the excellent material of self-lubricating are replacing graphite.Britain geim in 2004 et al. is prepared by " micromechanical forces disintegrating method "
Graphene, a kind of contact material band being announced to the world splendidly as preparing high connductivity, heat conduction, wear-resisting, anti-corrosion, anti-melting welding of Graphene
Carry out dawn.(in Graphene, the conduction velocity of electronics is 8 × 10 to the high electric conductivity of Graphene5M/s), heat conductivity (5300 w
m-1·k-1), specific surface area (theoretical specific surface area be 2600 m2/ g) and superior lubrication and protective value, it is that instead of graphite
Optimal material.Silver-colored Graphene coating not only can improve the property such as the wearability of coating, antioxidation, corrosion resistance, resistance fusion welding
Can, conduction, the heat conductivity of coating can also be improved.In order to solve high-voltage switch gear problems of excessive heat, it is badly in need of a kind of design height of invention and leads
Electricity, heat conductivility, have the environment of the silver-plated contact material of new type functional Graphene of the performance such as well wear-resisting, anti-corrosion simultaneously
Friendly method.
Content of the invention
Present invention aim at preparing a kind of feature composite deposite of high voltage isolator electrical contact material, using electricity
Plating method prepares a kind of feature composite deposite of silver Graphene on Copper substrate, and this composite deposite has excellent electric conductivity, leads
The hot, performance such as wearability, non-oxidizability, sulfuration resistant ability.One kind of the present invention no cyanogen silver Graphene composite deposite and preparation side
Method, described silver-colored Graphene composite deposite is electroplate with silvering and silver-colored Graphene coating respectively for Copper base material surface；Described system
Preparation Method is as follows:
Solution is prepared
Contain in the pre- silver plating solution prepared: the agno of 5 ~ 50g/l3, the ki of 50 ~ 400g/l, 10 ~ 200 g/l
na2s2o3, the hno of 1 ~ 10g/l3, ph value 1 ~ 7；
Contain in the composite plating bath prepared: the agno of 5 ~ 90 g/l3, the ki of 60 ~ 600 g/l, 10 ~ 400 g/l
na2s2o3, the hno of 1 ~ 10g/l3, the dispersant of 1 ~ 50g/l, the nano-graphene piece of 5 ~ 100 g/l, ph value 1 ~ 7；
3. prepare except containing in oil solution: the naoh of 50 ~ 600 g/l, the naco of 20 ~ 100 g/l3, 5 ~ 80 g/l
na3po4；
4. contain in the Acidwash solution prepared: the hno of 20 ~ 200g/l3, the h of 30 ~ 150g/l2so4.
Prepared by coating
In electroplating process, negative electrode adopts the anaerobic copper sheet of purity >=99.95% as plating substrate, and anode using purity is
99.99% plating silver plate；
Polishing: using 400 ~ 3000# waterproof abrasive paper uniform grinding anaerobic copper sheet substrate；
3. oil removing: anaerobic copper sheet substrate is placed in except, in oil solution, immersion 5 ~ 10min carries out oil removing；
4. clean: the anaerobic copper sheet substrate deionized water after oil removing is cleaned up；
5. pickling: the anaerobic copper sheet substrate cleaned is put into immersion 5 ~ 15 s in Acidwash solution, then deionized water is cleaned；
6. pre- silver-plated: after circuit ON, the anaerobic copper sheet substrate after pickling is directly placed in pre- silver plating solution, reaction 30 ~
600s, electric current density is 0.1 ~ 1.5 a/dm2, 25 ~ 80 DEG C of temperature, time 30 ~ 600s；
7. silver-colored Graphene composite plating: pre- silver-plated anaerobic copper sheet substrate is put in composite plating bath after deionization washing, electric current
Density is 0.1 ~ 2.5a/dm2, magnetic stirring speed 300 ~ 1500r/min, 25 ~ 80 DEG C of temperature, mixing time 20 ~ 60 min,
Electroplating time 1 ~ 5 h；
Post processing: through deionized water wash, drying, obtain surface has silver-colored Graphene composite deposite to step plated item 7.
Copper base material.
Described dispersion. formulation is: the sodium polyacrylate of 0.3 wt% ~ 10 wt%, the carboxymethyl of 0.3 wt% ~ 10 wt%
The alkylphenol polyoxyethylene of sodium cellulosate, 1 wt% ~ 10wt%.
The number of plies 10 ~ 50 of described nano-graphene piece, 5 ~ 10 μm of median particle diameter.
The solution have the advantages that: (1) plating solution adopts ki and na of green non-pollution2s2o3As chelating agent, facilitate back
Receive and reprocess the conversion it is achieved that environmentally friendly；(2) production technology is efficient；(3) the double-deck coating prepared has good knot
Make a concerted effort, reach the requirement of GB gb/t 5270-2005；(4) resistance to SO_2 of coating reaches navigation mark qj485-1988 and requires；(5) plate
The coefficient of friction when normal temperature and pressure load is 280 g for the layer is 0.06 ~ 0.22, (folder in the mechanical life experiment under actual condition
Clamp force 400 ~ 600 n) reaches between disconnecting switch mechanical life grade m1 and m2 level standard that (division is tested 4500 ~ 6500 times, plating
5 ~ 10 μm of layer loss)；(6) contact resistance of coating is 15 ~ 30 μ ω (external torque 5 ~ 20 n m)；(7) thermal conductivity 350 ~
500 w·m-1·k-1.To sum up, the silver-colored Graphene composite deposite of invention has excellent combination property, fully meets high_voltage isolation
The outwork condition of switch, has larger using value.
Brief description
The adhesion test photomacrograph of the silver-colored Graphene composite deposite of Fig. 1 embodiment of the present invention 1.
The photomacrograph of the silver-colored Graphene composite deposite of Fig. 2 embodiment of the present invention 2.
Specific embodiment:
Below in conjunction with the accompanying drawings present example is further described.
Embodiment 1
(1) solution allocation
1. pre- silver-plated main component in solution is: agno310 g/l, ki 200 g/l, na2s2o380 g/l, hno35 g/l,
25 DEG C of temperature, time 30 s, ph value 4.
2. composite plating bath main component is: agno320 g/l, ki 260 g/l, na2s2o380 g/l, hno35 g/l,
Dispersant 5 g/l, nano-graphene piece 20 g/l, mixing speed 700 r/min, mixing time 40 min, ph value 4.
Dispersion. formulation is: sodium polyacrylate 2 wt%, sodium carboxymethyl cellulose 1 wt%, alkylphenol polyoxyethylene 3
wt%；
(2) coating preparation
Polishing: using 400# waterproof abrasive paper uniform grinding matrix.
Highly basic oil removing: test piece is placed in except, in oil solution, immersion 5 min carry out highly basic oil removing.
3. the test piece deionized water after oil removing is cleaned up.
4. pickling: clean test piece is put into and soaks 5 s in Acidwash solution, then deionized water is cleaned.
5. pre- silver-plated: after circuit ON, the test piece after light corrosion is directly placed in pre- silver plating solution, reacts 30 s,
Electric current density is 0.1 a/dm2.
6. silver-colored Graphene composite plating: the test piece after deionization washing is directly placed in composite plating solution, and electric current is close
Spend for 0.3 a/dm2, magnetic stirring speed 700 r/min, time 1 h.
7. through deionized water rinsing after test piece is taken out, it is dried.
Prepare 14 μm of coating of thickness, Graphene content 15 %, contact resistance 19.9 μ ω (external torque 10 n m),
Thermal conductivity 365.662 w m-1·k-1, the coefficient of friction when normal temperature and pressure load is 280 g is 0.17, mechanical endurance test
After (clamping force 500 n) 5000 times, coating loses 6 μm.
Embodiment 2
(1) solution allocation
1. pre- silver-plated main component in solution is: agno310 g/l, ki 200 g/l, na2s2o380 g/l, hno35 g/l,
25 DEG C of temperature, time 30 s, ph value 4.
2. composite plating bath main component is: agno320 g/l, ki 260 g/l, na2s2o380 g/l, hno35 g/l,
Dispersant 5 g/l, nano-graphene piece 30 g/l, mixing speed 700 r/min, mixing time 40 min, ph value 4.
Dispersion. formulation is:: sodium polyacrylate 1 wt%, sodium carboxymethyl cellulose 2 wt%, alkylphenol polyoxyethylene 3
wt%；
(2) coating preparation
Polishing: using 800# waterproof abrasive paper uniform grinding matrix.
Highly basic oil removing: test piece is placed in except, in oil solution, immersion 5 min carry out highly basic oil removing.
3. the test piece deionized water after oil removing is cleaned up.
4. pickling: clean test piece is put into and soaks 5 s in Acidwash solution, then deionized water is cleaned.
5. pre- silver-plated: after circuit ON, the test piece after light corrosion is directly placed in pre- silver plating solution, reacts 30 s,
Electric current density is 0.1 a/dm2.
6. silver-colored Graphene composite plating: the test piece after deionization washing is directly placed in composite plating solution, and electric current is close
Spend for 0.3 a/dm2, magnetic stirring speed 700 r/min, time 1 h.
7. through deionized water rinsing after test piece is taken out, it is dried.
Prepare 14 μm of coating of thickness, Graphene content 18 %, contact resistance 18.9 μ ω (external torque 10 n m),
Thermal conductivity 405.568 w m-1·k-1, the coefficient of friction when normal temperature and pressure load is 280 g is 0.15, mechanical endurance test
After (clamping force 500 n) 5000 times, coating loses 4 μm.
Claims (3)
1. one kind no cyanogen silver Graphene composite deposite and preparation method it is characterised in that: described silver-colored Graphene composite deposite is
Copper base material surface is electroplate with silvering and silver-colored Graphene coating respectively；Described preparation method is as follows:
A () solution is prepared
(1) contain in the pre- silver plating solution prepared: the agno of 5 ~ 50g/l3, the ki of 50 ~ 400g/l, 10 ~ 200 g/l
na2s2o3, the hno of 1 ~ 10g/l3, ph value 1 ~ 7；
(2) contain in the composite plating bath prepared: the agno of 5 ~ 90 g/l3, the ki of 60 ~ 600 g/l, 10 ~ 400 g/l
na2s2o3, the hno of 1 ~ 10g/l3, the dispersant of 1 ~ 50g/l, the nano-graphene piece of 5 ~ 100 g/l, ph value 1 ~ 7；
(3) prepare except containing in oil solution: the naoh of 50 ~ 600 g/l, the naco of 20 ~ 100 g/l3, 5 ~ 80 g/l
na3po4；
(4) contain in the Acidwash solution prepared: the hno of 20 ~ 200g/l3, the h of 30 ~ 150g/l2so4；
Prepared by (b) coating
(1), in electroplating process, negative electrode adopts the anaerobic copper sheet of purity >=99.95% as plating substrate, and anode using purity is
99.99% plating silver plate；
(2) polish: using 400 ~ 3000# waterproof abrasive paper uniform grinding anaerobic copper sheet substrate；
(3) oil removing: anaerobic copper sheet substrate is placed in except, in oil solution, immersion 5 ~ 10min carries out oil removing；
(4) clean: the anaerobic copper sheet substrate deionized water after oil removing is cleaned up；
(5) pickling: the anaerobic copper sheet substrate cleaned is put into immersion 5 ~ 15 s in Acidwash solution, then deionized water is cleaned；
(6) pre- silver-plated: after circuit ON, the anaerobic copper sheet substrate after pickling is directly placed in pre- silver plating solution, reaction 30 ~
600s, electric current density is 0.1 ~ 1.5 a/dm2, 25 ~ 80 DEG C of temperature, time 30 ~ 600s；
(7) silver-colored Graphene composite plating: pre- silver-plated anaerobic copper sheet substrate is put in composite plating bath after deionization washing, electricity
Current density is 0.1 ~ 2.5a/dm2, magnetic stirring speed 300 ~ 1500r/min, 25 ~ 80 DEG C of temperature, mixing time 20 ~ 60
Min, electroplating time 1 ~ 5 h；
(8) post processing: through deionized water wash, drying, obtain surface has silver-colored Graphene composite deposite to the plated item of step (7)
Copper base material.
2. one kind according to claim 1 no cyanogen silver Graphene composite deposite and preparation method it is characterised in that: described
Dispersion. formulation is: the sodium polyacrylate of 0.3 wt% ~ 10 wt%, the sodium carboxymethyl cellulose of 0.3 wt% ~ 10 wt%, 1 wt% ~
The alkylphenol polyoxyethylene of 10wt%.
3. one kind according to claim 1 no cyanogen silver Graphene composite deposite and preparation method it is characterised in that: described
The number of plies 10 ~ 50 of nano-graphene piece, 5 ~ 10 μm of median particle diameter.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107574470A (en) * | 2017-08-24 | 2018-01-12 | 南京理工大学 | A kind of preparation method of the silver-colored graphene composite deposite of nickeliferous transition zone |
| CN109267124A (en) * | 2018-10-19 | 2019-01-25 | 西安西电电气研究院有限责任公司 | A kind of silver coated graphite composite deposite and preparation method thereof |
| CN110923785A (en) * | 2019-12-11 | 2020-03-27 | 哈尔滨东大高新材料股份有限公司 | Method for preparing silver alloy/copper alloy composite contact material for circuit breaker by codeposition |
| CN111235608A (en) * | 2020-03-10 | 2020-06-05 | 国网浙江省电力有限公司电力科学研究院 | Cyanide-free silver-based composite plating solution, silver-based composite plating layer and preparation method thereof |
| CN111519232A (en) * | 2020-04-20 | 2020-08-11 | 国网江西省电力有限公司电力科学研究院 | Silver/graphene composite plating solution, use method thereof and silver/graphene composite plating layer |
| CN112368422A (en) * | 2018-07-05 | 2021-02-12 | 罗森伯格高频技术有限公司 | Silver electrolyte for depositing a silver dispersion layer and a contact surface with a silver dispersion layer |
| CN112805412A (en) * | 2018-10-11 | 2021-05-14 | Abb电网瑞士股份公司 | Silver-graphene composite coating for sliding contactor and electroplating method thereof |
| CN114197017A (en) * | 2021-12-08 | 2022-03-18 | 国网江西省电力有限公司电力科学研究院 | Composite coating and preparation method and application thereof |
| CN114507887A (en) * | 2022-02-25 | 2022-05-17 | 全球能源互联网研究院有限公司 | Composite coating and preparation method thereof |
| EP4089697A1 (en) * | 2021-05-10 | 2022-11-16 | ABB Schweiz AG | Metal-graphene coated electrical contact |
| CN117292873A (en) * | 2022-06-16 | 2023-12-26 | 温州泰钰新材料科技有限公司 | electrical contact conductor |
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| CN107574470A (en) * | 2017-08-24 | 2018-01-12 | 南京理工大学 | A kind of preparation method of the silver-colored graphene composite deposite of nickeliferous transition zone |
| US20210254230A1 (en) * | 2018-07-05 | 2021-08-19 | Rosenberger Hochfrequenztechnik Gmbh & Co. Kg | Silver electrolyte for depositing dispersion silver layers and contact surfaces with dispersion silver layers |
| CN112368422A (en) * | 2018-07-05 | 2021-02-12 | 罗森伯格高频技术有限公司 | Silver electrolyte for depositing a silver dispersion layer and a contact surface with a silver dispersion layer |
| CN112805412A (en) * | 2018-10-11 | 2021-05-14 | Abb电网瑞士股份公司 | Silver-graphene composite coating for sliding contactor and electroplating method thereof |
| US11542616B2 (en) | 2018-10-11 | 2023-01-03 | Hitachi Energy Switzerland Ag | Silver-graphene composite coating for sliding contact and electroplating method thereof |
| CN112805412B (en) * | 2018-10-11 | 2022-02-11 | Abb电网瑞士股份公司 | Silver-graphene composite coating for sliding contactor and electroplating method thereof |
| CN109267124A (en) * | 2018-10-19 | 2019-01-25 | 西安西电电气研究院有限责任公司 | A kind of silver coated graphite composite deposite and preparation method thereof |
| CN110923785B (en) * | 2019-12-11 | 2022-04-22 | 哈尔滨东大高新材料股份有限公司 | Method for preparing silver alloy/copper alloy composite contact material for circuit breaker by codeposition |
| CN110923785A (en) * | 2019-12-11 | 2020-03-27 | 哈尔滨东大高新材料股份有限公司 | Method for preparing silver alloy/copper alloy composite contact material for circuit breaker by codeposition |
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| WO2022238055A1 (en) * | 2021-05-10 | 2022-11-17 | Abb Schweiz Ag | Metal-graphene coated electrical contact |
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| CN114197017B (en) * | 2021-12-08 | 2023-10-20 | 国网江西省电力有限公司电力科学研究院 | Composite coating and preparation method and application thereof |
| CN114507887A (en) * | 2022-02-25 | 2022-05-17 | 全球能源互联网研究院有限公司 | Composite coating and preparation method thereof |
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