CN107217292A - Composite silver plating liquor and preparation method thereof, electrodeposition technology and application - Google Patents
Composite silver plating liquor and preparation method thereof, electrodeposition technology and application Download PDFInfo
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- CN107217292A CN107217292A CN201710487117.0A CN201710487117A CN107217292A CN 107217292 A CN107217292 A CN 107217292A CN 201710487117 A CN201710487117 A CN 201710487117A CN 107217292 A CN107217292 A CN 107217292A
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- composite
- silver
- silver plating
- plating liquor
- electrodeposition technology
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/46—Electroplating: Baths therefor from solutions of silver
Abstract
The invention belongs to field of electroplating, more particularly to composite silver plating liquor and preparation method thereof and electrodeposition technology.The invention provides a kind of composite silver plating liquor, including following component：Water miscible Ag-containing compound is that 20 60g/L, sodium thiosulfate are that 150 300g/L, potassium metabisulfite are that 20 60g/L, polyethyleneimine are that 0.2 1g/L, thiosemicarbazide are that 0.2 1g/L, graphene oxide are that 0.1~2g/L, CTAB are 0.05~1g/L.The invention also discloses a kind of electrodeposition technology.Composite silver plating liquor disclosed by the invention and preparation method thereof and electrodeposition technology can effectively solve graphene in silver-colored graphene composite deposite prepared by current composite silver plating liquor and not be attached to the not good technological deficiency of coating performance that composite deposite causes well.
Description
Technical field
The invention belongs to field of electroplating, more particularly to composite silver plating liquor and preparation method thereof, electrodeposition technology and application.
Background technology
High voltage isolator is one of most power transmission and transforming equipment of usage amount in power system, is also important control and guarantor
Protection unit, its operation conditions whether normal relation to whole power network safety and stably.Operate failure, Insulator detection, conduction
Loop is overheated and corrosion is 4 subject matters reflected during current disconnecting switch is run.
Selecting copper the dynamic and static contact material of country's disconnecting switch at present, good conductive surface is typically carried out for guarantee more
Silver-plated process, i.e., make anode with fine silver plate, and copper contact makees negative electrode, and electro-deposition is carried out under cyaniding plant of silver system.But with electricity
The construction of fast development, particularly super-pressure, extra high voltage line and intelligent grid that power is built, the use longevity of common silver coating
Life has been difficult the actual demand for meeting the power transmission and transforming equipments such as high voltage isolator, and common silver coating matter is soft, wears no resistance, resistance
The problems such as color and not strong automatical cleaning ability, is urgently to be resolved hurrily.Moreover, cyanide is severe toxicity, to ecological environment and the health of producers
There is great harm, while the technology and cost requirement to liquid waste processing are higher.
At present, scholar proposes that preparation silver-graphene composite material prepares novel silver and crosses solution, but current composite silver plating is molten
Liquid prepare silver-graphitic composite deposite in graphene be not attached to well in composite deposite, cause composite deposite hardness,
The hydraulic performance declines such as thickness.
The content of the invention
In view of this, composite silver plating liquor disclosed by the invention and preparation method thereof, electrodeposition technology and application can be effective
Solve graphite in silver-graphitic composite deposite prepared by current composite silver plating liquor and be not attached to composite deposite well, cause
Check the technological deficiency of coating performance decline.
Present invention also offers a kind of composite silver plating liquor, it is characterised in that including following component：
Preferably, including following component：
Preferably, the water miscible Ag-containing compound is silver nitrate.
Wherein, the solvent of the composite silver plating liquor is water.
Present invention also offers a kind of preparation method of composite silver plating liquor, including：
1) water miscible Ag-containing compound, sodium thiosulfate, potassium metabisulfite, polyethyleneimine and thiosemicarbazide are mixed
Close, obtain mixed solution；
2) by step 1) mixed solution mixed with graphene oxide and cetyl trimethylammonium bromide, in ultrasound condition
Under dissolve graphene oxide, obtain composite silver plating liquor.
Preferably, the graphene oxide is bought from Changzhou No.6 Element Material Technology Co., Ltd..
Preferably, step 1) PH of the mixed solution is 5-6.
Present invention also offers a kind of electrodeposition technology, including：
1) composite silver plating liquor) is prepared；
2)) copper sheet and silver plate are set；
3)) by step 2)) copper sheet and silver plate be placed in step 1)) composite silver plating liquor in carry out electro-deposition, obtain silver-
Graphite composite deposite.
Preferably, the current density of the electro-deposition is 0.3-0.6A/dm2。
More preferably, the current density of the electro-deposition is 0.5A/dm2。
Preferably, the mixing speed of the electro-deposition is 1000-1200r/min.
More preferably, the mixing speed of the electro-deposition is 1200r/min.
Preferably, the plating temperature of the electro-deposition is 20-50 DEG C.
More preferably, the plating temperature of the electro-deposition is 25 DEG C.
Preferably, the parameter of the electro-deposition is：Current density is 0.5A/dm2；Mixing speed is 1200r/min；Apply
It is 25 DEG C to plate temperature.
The preparation method of described composite silver plating liquor and/or described composite silver plating liquor disclosed by the invention and/or
Application of the described electrodeposition technology in silver-graphene composite deposite is prepared.
The invention provides a kind of composite silver plating liquor, the composite silver plating liquor includes：Water miscible Ag-containing compound,
Sodium thiosulfate, potassium metabisulfite, polyethyleneimine, thiosemicarbazide, graphene oxide and cetyl trimethylammonium bromide,
Graphene can cause scattered well combine in coating in silver-graphene composite deposite prepared by the composite silver plating liquor of the present invention
In, the performance of the coating greatly improved.The invention also discloses a kind of electrodeposition technology, compared to traditional electrodeposition technology, sheet
The electrodeposition technology of disclosure of the invention is simple, and controllability is good so that graphene, silver particles can be combined with metallic plate well,
So as to obtain the metal composite cladding of excellent performance.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described.
Fig. 1 shows the performance evaluation of coating prepared by different mixing speeds；
Fig. 2 shows the performance evaluation of coating prepared by different current densities；
Fig. 3 shows the performance evaluation of coating prepared by different electroplating temperatures；
Fig. 4 shows the performance evaluation of coating prepared by the different pH value of composite silver plating liquor；
Fig. 5 shows the microscopic appearance of silver-graphene composite deposite, wherein, left figure is the microscopic appearance of 200 times of amplification, right figure
For 6000 times of microscopic appearance of amplification.
Embodiment
The invention provides composite silver plating liquor and preparation method thereof, electrodeposition technology and application, can effectively it solve current
Graphite is not attached to the technological deficiency of composite deposite well in silver-graphitic composite deposite prepared by composite silver plating liquor.
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
Wherein, the raw material and reagent of following examples are commercially available, and CTAB is cetyl trimethylammonium bromide.The oxygen
Graphite alkene is bought from Changzhou No.6 Element Material Technology Co., Ltd..
Embodiment 1
Test group 1 to experiment 6：40g/L silver nitrates, 200g/L sodium thiosulfate, 40g/L potassium metabisulfites, 1g/L oxidations
Graphene, 0.5g/LCTAB, polyethyleneimine 0.8g/L, thiosemicarbazide 0.8g/L, ultrasound 1h after being sufficiently stirred for are made compound
Silver-colored plating liquor.
The copper sheet substrate and silver strip that carry out oil removing, polishing, ultrasonic wave cleaning, alkali cleaning and pickling are placed in above-mentioned test group 1
After the composite silver plating liquor of~test group 6, carry out composite electrodeposition and prepare silver-graphene composite deposite.
The parameter of composite electrodeposition is set to：
Test group 1：Mixing speed：400r/min；Current density：0.5A/dm2；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5；
Test group 2：Mixing speed：600r/min；Current density：0.5A/dm2；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5；；
Test group 3：Mixing speed：800r/min；Current density：0.5A/dm2；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5；
Test group 4：Mixing speed：1000r/min；Current density：0.5A/dm2；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5；
Test group 5：Mixing speed：1200r/min；Current density：0.5A/dm2；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5；
Test group 6：Mixing speed：1400r/min；Current density：0.5A/dm2；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5.
The thickness and hardness of the silver-graphene composite deposite of test group 1~6 are detected, as a result as shown in figure 1, mixing speed
Little to the thickness effect of silver-graphene composite deposite, the thickness of the silver-graphene composite deposite of test group 1~6 is at 9.5 μm
Near, and hardness influence of the mixing speed on silver-graphene composite deposite is larger, when mixing speed is in 1200r/min, its is hard
Degree reaches maximum.
Embodiment 2
Test group 1 to experiment 7：40g/L silver nitrates, 200g/L sodium thiosulfate, 40g/L potassium metabisulfites, 1g/L oxidations
Graphene, 0.5g/LCTAB, polyethyleneimine 0.8g/L, thiosemicarbazide 0.8g/L, ultrasound 1h after being sufficiently stirred for are made compound
Silver-colored plating liquor.
The copper sheet substrate and silver strip that carry out oil removing, polishing, ultrasonic wave cleaning, alkali cleaning and pickling are placed in above-mentioned test group 1
After the composite silver plating liquor of~test group 7, carry out composite electrodeposition and prepare silver-graphene composite deposite.
The parameter of composite electrodeposition is set to：
Test group 1：Current density：0.1A/dm2；Mixing speed：1000r/min；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5；
Test group 2：Current density：0.2A/dm2；Mixing speed：1000r/min；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5；
Test group 3：Current density：0.3A/dm2；Mixing speed：1000r/min；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5；
Test group 4：Current density：0.4A/dm2；Mixing speed：1000r/min；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5；
Test group 5：Current density：0.5A/dm2；Mixing speed：1000r/min；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5；
Test group 6：Current density：0.6A/dm2；Mixing speed：1000r/min；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5；
Test group 7：Current density：0.7A/dm2；Mixing speed：1000r/min；Plating temperature：25℃；Electrodeposition time
30min；Bath pH value 5.
The thickness and hardness of the silver-graphene composite deposite of test group 1~7 are detected, as a result as shown in Fig. 2 current density
Hardness influence on silver-graphene composite deposite is larger, in 0.5A/dm2Current density under, silver-graphene composite deposite
Hardness reaches maximum；Likewise, current density is larger to the thickness effect of silver-graphene composite deposite, with current density
Constantly increase, its thickness also constantly increases.
Embodiment 3
Test group 1 to experiment 6：40g/L silver nitrates, 200g/L sodium thiosulfate, 40g/L potassium metabisulfites, 1g/L oxidations
Graphene, 0.5g/LCTAB, polyethyleneimine 0.8g/L, thiosemicarbazide 0.8g/L, ultrasound 1h after being sufficiently stirred for are made compound
Silver-colored plating liquor.
The copper sheet substrate and silver strip that carry out oil removing, polishing, ultrasonic wave cleaning, alkali cleaning and pickling are placed in above-mentioned test group 1
After the composite silver plating liquor of~test group 6, carry out composite electrodeposition and prepare silver-graphene composite deposite.
The parameter of composite electrodeposition is set to：
Test group 1：Plating temperature：20℃；Current density：0.5A/dm2；Mixing speed：1000r/min；Electrodeposition time
30min；Bath pH value 5；
Test group 2：Plating temperature：25℃；Current density：0.5A/dm2；Mixing speed：1000r/min；Electrodeposition time
30min；Bath pH value 5；
Test group 3：Plating temperature：30℃；Current density：0.5A/dm2；Mixing speed：1000r/min；Electrodeposition time
30min；Bath pH value 5；
Test group 4：Plating temperature：35℃；Current density：0.5A/dm2；Mixing speed：1000r/min；Electrodeposition time
30min；Bath pH value 5；
Test group 5：Plating temperature：40℃；Current density：0.5A/dm2；Mixing speed：1000r/min；Electrodeposition time
30min；Bath pH value 5；
Test group 6：Plating temperature：45℃；Current density：0.5A/dm2；Mixing speed：1000r/min；Electrodeposition time
30min；Bath pH value 5.
The thickness and hardness of the silver-graphene composite deposite of test group 1~6 are detected, as a result as shown in figure 3, plating temperature
Hardness influence on silver-graphene composite deposite is larger, under 25 DEG C of plating temperature, the hardness of silver-graphene composite deposite
Reach maximum；Likewise, plating temperature is larger to the thickness effect of silver-graphene composite deposite, when plating temperature is 20 DEG C
When, the thickness of silver-graphene composite deposite is minimum, but as plating temperature is improved constantly, its thickness also constantly increases.
Embodiment 4
Test group 1 to experiment 6：40g/L silver nitrates, 200g/L sodium thiosulfate, 40g/L potassium metabisulfites, 1g/L oxidations
Graphene, 0.5g/LCTAB, polyethyleneimine 0.8g/L, thiosemicarbazide 0.8g/L, ultrasound 1h after being sufficiently stirred for are made compound
Silver-colored plating liquor.
The copper sheet substrate and silver strip that carry out oil removing, polishing, ultrasonic wave cleaning, alkali cleaning and pickling are placed in above-mentioned test group 1
After the composite silver plating liquor of~test group 6, carry out composite electrodeposition and prepare silver-graphene composite deposite.
The parameter of composite electrodeposition is set to：
Test group 1：Bath pH value 4；Plating temperature：25℃；Current density：0.5A/dm2；Mixing speed：1000r/min；
Electrodeposition time 30min；
Test group 2：Bath pH value 4.5；Plating temperature：25℃；Current density：0.5A/dm2；Mixing speed：1000r/
min；Electrodeposition time 30min；
Test group 3：Bath pH value 5；Plating temperature：25℃；Current density：0.5A/dm2；Mixing speed：1000r/min；
Electrodeposition time 30min；
Test group 4：Bath pH value 5.5；Plating temperature：25℃；Current density：0.5A/dm2；Mixing speed：1000r/
min；Electrodeposition time 30min；
Test group 5：Bath pH value 6；Plating temperature：25℃；Current density：0.5A/dm2；Mixing speed：1000r/min；
Electrodeposition time 30min；
Test group 6：Bath pH value 6.5；Plating temperature：25℃；Current density：0.5A/dm2；Mixing speed：1000r/
min；Electrodeposition time 30min.
The thickness and hardness of the silver-graphene composite deposite of test group 1~6 are detected, as a result as shown in figure 4, bath pH value
Hardness influence on silver-graphene composite deposite is larger.With the increase of bath pH value, the hardness of coating is also in increase, in plating
When liquid pH value is 6, the hardness of silver-graphene composite deposite reaches maximum；Likewise, bath pH value is compound to silver-graphene
The thickness effect of coating is larger, and with the increase of bath pH value, the thickness of coating is also in increase, when bath pH value is 6, and silver-
The thickness of graphene composite deposite reaches maximum.
Embodiment 5
Test group：40g/L silver nitrates, 200g/L sodium thiosulfate, 40g/L potassium metabisulfites, 1g/L graphene oxides,
It is molten that composite silver plating is made in 0.5g/LCTAB, polyethyleneimine 0.8g/L, thiosemicarbazide 0.8g/L, ultrasound 1h after being sufficiently stirred for
Liquid.
The copper sheet substrate and silver strip that carry out oil removing, polishing, ultrasonic wave cleaning, alkali cleaning and pickling are placed in above-mentioned test group
After composite silver plating liquor, carry out composite electrodeposition and prepare silver-graphene composite deposite, the parameter of composite electrodeposition is set to
Current density：0.5A/dm2；Mixing speed：1200r/min；Plating temperature：25℃；Bath pH value 5.5；Electrodeposition time：
30min；Process conditions under prepare silver-graphene composite deposite.
As a result as shown in figure 5, left figure, which is silver-graphene composite deposite, amplifies 200 times of electron microscopes, right figure is 6000 times of amplification
Electron microscope, therefrom can be clearly seen that graphene sheet layer is buried and overlays among coating.
Claims (10)
1. a kind of composite silver plating liquor, it is characterised in that including following component：
2. composite silver plating liquor according to claim 1, it is characterised in that including following component：
3. a kind of preparation method of composite silver plating liquor, it is characterised in that including：
Step 1) water miscible Ag-containing compound, sodium thiosulfate, potassium metabisulfite, polyethyleneimine and thiosemicarbazide are mixed
Close, obtain mixed solution；
Step 2) by step 1) mixed solution mixed with graphene oxide and cetyl trimethylammonium bromide, in ultrasound condition
Under dissolve graphene oxide, obtain composite silver plating liquor.
4. preparation method according to claim 3, it is characterised in that step 1) PH of the mixed solution is 5-6.
5. a kind of electrodeposition technology, it is characterised in that including：
1) composite silver plating liquor) is prepared；
2)) copper sheet and silver plate are set；
3)) by step 2)) copper sheet and silver plate be placed in step 1)) composite silver plating liquor in carry out electro-deposition, obtain silver-graphitic
Alkene composite deposite.
6. electrodeposition technology according to claim 5, it is characterised in that the current density of the electro-deposition is 0.3-
0.6A/dm2。
7. electrodeposition technology according to claim 5, it is characterised in that the mixing speed of the electro-deposition is 1000-
1200r/min。
8. electrodeposition technology according to claim 5, it is characterised in that the plating temperature of the electro-deposition is 20-50 DEG C.
9. electrodeposition technology according to claim 5, it is characterised in that the parameter of the electro-deposition is：Current density is
0.5A/dm2；Mixing speed is 1200r/min；Plating temperature is 25 DEG C.
10. the system of the composite silver plating liquor described in composite silver plating liquor and/or claim 3 or 4 described in claim 1 or 2
Electrodeposition technology answering in silver-graphene composite deposite is prepared described in Preparation Method and/or claim 5 to 9 any one
With.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710487117.0A CN107217292A (en) | 2017-06-23 | 2017-06-23 | Composite silver plating liquor and preparation method thereof, electrodeposition technology and application |
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|---|---|---|---|
| CN201710487117.0A CN107217292A (en) | 2017-06-23 | 2017-06-23 | Composite silver plating liquor and preparation method thereof, electrodeposition technology and application |
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ID=59950204
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108221011A (en) * | 2018-01-05 | 2018-06-29 | 广西师范大学 | One kind prepares silver/redox graphene composite material and preparation method thereof based on graphene oxide |
| EP3636804A1 (en) * | 2018-10-11 | 2020-04-15 | ABB Schweiz AG | Silver-graphene composite coating for sliding contact and electroplating method thereof |
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| CN103590089A (en) * | 2013-11-20 | 2014-02-19 | 上海应用技术学院 | Preparation method of graphene/silver composite material |
| CN105821465A (en) * | 2016-05-09 | 2016-08-03 | 南昌航空大学 | Preparation method for silver and graphene composite coating of cyanide-free system |
| CN106048672A (en) * | 2016-08-17 | 2016-10-26 | 国家电网公司 | Neutral cyanide-free brush electroplating silver plating solution and preparation process and use method thereof |
| CN106283150A (en) * | 2015-05-11 | 2017-01-04 | 深圳中宇昭日科技有限公司 | A kind of electro-deposition graphene conductive corrosion-resistant material preparation method for material |
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| CN102051651A (en) * | 2011-01-11 | 2011-05-11 | 湖南大学 | Preparation method of graphene film |
| CN103590089A (en) * | 2013-11-20 | 2014-02-19 | 上海应用技术学院 | Preparation method of graphene/silver composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108221011A (en) * | 2018-01-05 | 2018-06-29 | 广西师范大学 | One kind prepares silver/redox graphene composite material and preparation method thereof based on graphene oxide |
| EP3636804A1 (en) * | 2018-10-11 | 2020-04-15 | ABB Schweiz AG | Silver-graphene composite coating for sliding contact and electroplating method thereof |
| WO2020074552A1 (en) * | 2018-10-11 | 2020-04-16 | Abb Schweiz Ag | Silver-graphene composite coating for sliding contact 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 |
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Application publication date: 20170929 |