CN107254696A - Silver/graphite alkene composite silver plating liquor and preparation method thereof and electrodeposition technology - Google Patents
Silver/graphite alkene composite silver plating liquor and preparation method thereof and electrodeposition technology Download PDFInfo
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- CN107254696A CN107254696A CN201710428078.7A CN201710428078A CN107254696A CN 107254696 A CN107254696 A CN 107254696A CN 201710428078 A CN201710428078 A CN 201710428078A CN 107254696 A CN107254696 A CN 107254696A
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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
Abstract
The invention belongs to field of electroplating, more particularly to silver/graphite alkene composite silver plating liquor and preparation method thereof and electrodeposition technology.The invention provides silver/graphite alkene 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, ammonium acetate are that 20 30g/L, thiosemicarbazide are that 0.2 1g/L, graphene are that 5 10g/L, polyvinylpyrrolidone are 5mL/L.The invention also discloses a kind of electrodeposition technology.Silver/graphite alkene composite silver plating liquor disclosed by the invention and preparation method thereof and electrodeposition technology can effectively solve the technological deficiency that graphene in silver/graphite alkene composite deposite prepared by current composite silver plating liquor is not attached to composite deposite well.
Description
Technical field
The invention belongs to field of electroplating, more particularly to silver/graphite alkene composite silver plating liquor and preparation method thereof and electro-deposition
Technique.
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, there is scholar's proposition to prepare silver/graphite alkene composite and prepare new silver plating solution, but current silver/graphite alkene
Graphene is not attached to silver/graphite alkene composite deposite well in silver/graphite alkene composite deposite prepared by composite silver plating liquor
In, cause silver/graphite alkene composite deposite hydraulic performance decline.
The content of the invention
In view of this, silver/graphite alkene composite silver plating liquor disclosed by the invention and preparation method thereof can be solved effectively currently
Graphene is not attached to silver/graphite alkene well in silver/graphite alkene composite deposite prepared by silver/graphite alkene composite silver plating liquor
The technological deficiency of composite deposite.
Present invention also offers silver/graphite alkene composite silver plating liquor, including following component：
Preferably, the solvent of the silver/graphite alkene composite silver plating liquor is water.
More preferably, the solvent of the silver/graphite alkene composite silver plating liquor is deionized water.
Preferably, including following component：
Preferably, the solvent of shown silver/graphite alkene composite silver plating liquor is water.
More preferably, the solvent of the silver/graphite alkene composite silver plating liquor is deionized water.
The invention also discloses the preparation method of silver/graphite alkene composite silver plating liquor, including：
1) water miscible Ag-containing compound, sodium thiosulfate, potassium metabisulfite, ammonium acetate and thiosemicarbazide are mixed,
Obtain mixed solution；
2) by step 1) mixed solution mixed with graphene platelet and polyvinylpyrrolidone, make stone under ultrasound condition
Black alkene dissolving, obtains silver/graphite alkene composite silver plating liquor.
Preferably, graphene drying at 80 DEG C~120 DEG C is prepared for 1 hour.
Preferably, shown graphene is less than five layers, its two-dimentional yardstick is less than 10 μm.
Preferably, step 1) PH of the mixed solution is 5-6.
The invention also discloses a kind of electrodeposition technology, including：
1) silver/graphite alkene composite silver plating liquor) is prepared；
2)) copper sheet is set；
3)) by step 2)) copper sheet be placed in step 1)) silver/graphite alkene composite silver plating liquor in carry out electro-deposition, obtain
Silver/graphite alkene composite deposite.
Preferably, the step 2)) the method to set up of copper sheet be：Through 1000#Coated abrasive working, enters through alcohol, acetone
Activated after row cleaning through 10% dilute sulfuric acid.
Preferably, the current density of the electro-deposition is 1-5A/dm2。
More preferably, the current density of the electro-deposition is 2.5A/dm2。
Preferably, the plating temperature of the electro-deposition is 20-50 DEG C.
More preferably, the plating temperature of the electro-deposition is 25-45 DEG C.
Present invention also offers silver/graphite prepared by the preparation method of silver/graphite alkene composite silver plating liquor, the preparation method
Graphene dispersion is good in alkene composite silver plating liquor；Silver/graphite alkene prepared by the silver/graphite alkene composite silver plating liquor of the present invention is answered
Graphene in coating is closed to combine in coating well.
The invention also discloses a kind of electrodeposition technology, compared to traditional hot-working method, because hot-working method is needed
It could be carried out under more than 500 DEG C hot conditions, so expensive production equipment is needed, and the electrodeposition technology is utilized
Silver/graphite alkene composite silver plating liquor is processed, it is not necessary to hot conditions, and operation temperature can be carried out directly at room temperature, to life
Produce equipment requirement relatively low, therefore, the investment cost of the electrodeposition technology is few, required equipment is simple and easily controllable.
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 shape appearance figure of the silver/graphite alkene composite deposite of test group 1, test group 2 and test group 3；
Fig. 2 shows the shape appearance figure of the silver/graphite alkene composite deposite of test group 4, test group 5 and test group 6；
Fig. 3 shows the shape appearance figure of the silver/graphite alkene composite deposite of test group 7, test group 8 and test group 9；
Fig. 4 shows the shape appearance figure of the silver/graphite alkene composite deposite of test group 6, test group 9 and test group 10.
Embodiment
The invention provides silver/graphite alkene composite silver plating liquor and preparation method thereof, current silver/graphite alkene can be effectively solved
Graphene is not attached to silver/graphite alkene composite deposite well in silver/graphite alkene composite deposite prepared by composite silver plating liquor
Technological deficiency.
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 polyvinylpyrrolidone is referred to as PVP, the poly- second
Alkene pyrrolidone is bought from the hyper-dispersants of Lu Borun 27000, solsperse (TM) 27000.
Embodiment 1
Test group 1：40g/L silver nitrates, 250g/L sodium thiosulfate, 40g/L potassium metabisulfites, 25g/L ammonium acetates,
0.6g/L thiosemicarbazides, 5g/L graphenes, 5mL/L PVP, are made silver/graphite alkene composite silver plating liquor；By copper sheet be placed in silver/
Electro-deposition, current density are carried out in graphene composite silver plating liquor：2.5A/dm2；Mixing speed：1500r/min；Plating temperature：
25℃；PH is 5.4-5.8；Electrodeposition time 30min, obtains silver/graphite alkene composite deposite；
Test group 2：40g/L silver nitrates, 250g/L sodium thiosulfate, 40g/L potassium metabisulfites, 25g/L ammonium acetates,
0.6g/L thiosemicarbazides, 5g/L graphenes, 5mL/L PVP, are made silver/graphite alkene composite silver plating liquor；By copper sheet be placed in silver/
Electro-deposition, current density are carried out in graphene composite silver plating liquor：2.5A/dm2；Mixing speed：1500r/min；Plating temperature：
35℃；PH is 5.4-5.8；Electrodeposition time 30min, obtains silver/graphite alkene composite deposite；
Test group 3：40g/L silver nitrates, 250g/L sodium thiosulfate, 40g/L potassium metabisulfites, 25g/L ammonium acetates,
0.6g/L thiosemicarbazides, 5g/L graphenes, 5mL/L PVP, are made silver/graphite alkene composite silver plating liquor；By copper sheet be placed in silver/
Electro-deposition, current density are carried out in graphene composite silver plating liquor：2.5A/dm2；Mixing speed：1500r/min；Plating temperature：
45℃；PH is 5.4-5.8；Electrodeposition time 30min, obtains silver/graphite alkene composite deposite；
Test group 4：40g/L silver nitrates, 250g/L sodium thiosulfate, 40g/L potassium metabisulfites, 25g/L ammonium acetates,
0.6g/L thiosemicarbazides, 10g/L graphenes, 5mL/L PVP, are made silver/graphite alkene composite silver plating liquor；Copper sheet is placed in
Electro-deposition, current density are carried out in silver/graphite alkene composite silver plating liquor：2.5A/dm2；Mixing speed：1500r/min；Plating temperature
Degree：25℃；PH is 5.4-5.8；Electrodeposition time 30min, obtains silver/graphite alkene composite deposite；
Test group 5：40g/L silver nitrates, 250g/L sodium thiosulfate, 40g/L potassium metabisulfites, 25g/L ammonium acetates,
0.6g/L thiosemicarbazides, 10g/L graphenes, 5mL/L PVP, are made silver/graphite alkene composite silver plating liquor；Copper sheet is placed in
Electro-deposition, current density are carried out in silver/graphite alkene composite silver plating liquor：2.5A/dm2；Mixing speed：1500r/min；Plating temperature
Degree：35℃；PH is 5.4-5.8；Electrodeposition time 30min, obtains silver/graphite alkene composite deposite；
Test group 6：40g/L silver nitrates, 250g/L sodium thiosulfate, 40g/L potassium metabisulfites, 25g/L ammonium acetates,
0.6g/L thiosemicarbazides, 10g/L graphenes, 05mL/L PVP, are made silver/graphite alkene composite silver plating liquor；Copper sheet is placed in
Electro-deposition, current density are carried out in silver/graphite alkene composite silver plating liquor：2.5A/dm2；Mixing speed：1500r/min；Plating temperature
Degree：45℃；PH is 5.4-5.8；Electrodeposition time 30min, obtains silver/graphite alkene composite deposite；
Test group 7：40g/L silver nitrates, 250g/L sodium thiosulfate, 40g/L potassium metabisulfites, 25g/L ammonium acetates,
0.6g/L thiosemicarbazides, 10g/L graphenes, 5mL/L PVP, are made silver/graphite alkene composite silver plating liquor；Copper sheet is placed in
Electro-deposition, current density are carried out in silver/graphite alkene composite silver plating liquor：3.75A/dm2；Mixing speed：1500r/min；Plating
Temperature：25℃；PH is 5.4-5.8；Electrodeposition time 30min, obtains silver/graphite alkene composite deposite；
Test group 8：40g/L silver nitrates, 250g/L sodium thiosulfate, 40g/L potassium metabisulfites, 25g/L ammonium acetates,
0.6g/L thiosemicarbazides, 10g/L graphenes, 5mL/L PVP, are made silver/graphite alkene composite silver plating liquor；Copper sheet is placed in
Electro-deposition, current density are carried out in silver/graphite alkene composite silver plating liquor：3.75A/dm2；Mixing speed：1500r/min；Plating
Temperature：35℃；PH is 5.4-5.8；Electrodeposition time 30min, obtains silver/graphite alkene composite deposite；
Test group 9：40g/L silver nitrates, 250g/L sodium thiosulfate, 40g/L potassium metabisulfites, 25g/L ammonium acetates,
0.6g/L thiosemicarbazides, 10g/L graphenes, 5mL/L PVP, are made silver/graphite alkene composite silver plating liquor；Copper sheet is placed in
Electro-deposition, current density are carried out in silver/graphite alkene composite silver plating liquor：3.75A/dm2；Mixing speed：1500r/min；Plating
Temperature：45℃；PH is 5.4-5.8；Electrodeposition time 30min, obtains silver/graphite alkene composite deposite；
Test group 10：40g/L silver nitrates, 250g/L sodium thiosulfate, 40g/L potassium metabisulfites, 25g/L ammonium acetates,
0.6g/L thiosemicarbazides, 10g/L graphenes, 5mL/L PVP, are made silver/graphite alkene composite silver plating liquor；Copper sheet is placed in
Electro-deposition, current density are carried out in silver/graphite alkene composite silver plating liquor：5.0A/dm2；Mixing speed：1500r/min；Plating temperature
Degree：45℃；PH is 5.4-5.8；Electrodeposition time 30min, obtains silver/graphite alkene composite deposite.
Contrast groups 1：40g/L silver nitrates, 250g/L sodium thiosulfate, 40g/L potassium metabisulfites, 25g/L ammonium acetates,
0.6g/L thiosemicarbazides, are made silver plating liquor；Copper sheet is placed in silver-colored plating liquor and carries out electro-deposition, current density：2.5A/
dm2；Mixing speed：1500r/min；Plating temperature：25℃；PH is 5.4-5.8；Electrodeposition time 30min, obtains fine silver plating
Layer；
Contrast groups 2：Buy industrial fine copper.
The coating of test group 1~10 and contrast groups 1~2 is subjected to hardness determination, as a result as shown in table 1.
The test group 1~10 of table 1 and contrast groups 1~2 determine the hardness number of coating under different temperatures
As shown in Table 1, added in electroplate liquid after graphene, the hardness number of obtained silver coating changes without regular, examination
Group 1~10 is tested mostly in 120.0HV or so, and the coating of the fine silver of contrast groups 1 is 84.7HV, the fine copper of contrast groups 2 is
130.2HV.The coating that plating solution added with graphene is obtained improves 40HV or so than the coating that fine silver plating solution is obtained, and illustrates
The coating obtained in the plating solution for adding graphene may doped graphene.
Embodiment 2
The pattern of the silver/graphite alkene composite deposite of test group 1, test group 2 and test group 3 in embodiment 1 is analyzed,
As a result as shown in figure 1, Fig. 1-1, Fig. 1-2, Fig. 1-3, are that test group 1 photomacrograph, SEM scannings low power at 25 DEG C are micro- respectively
Photo, SEM scanning high magnification micrographs；Fig. 1-4, Fig. 1-5, Fig. 1-6, be respectively photomacrograph of the test group 2 at 35 DEG C,
SEM scannings low magnification micrographs, SEM scanning high magnification micrographs；Fig. 1-7, Fig. 1-8, Fig. 1-9 are test group 3 respectively at 45 DEG C
Under photomacrograph, SEM scanning low magnification micrographs, SEM scanning high magnification micrographs.
It is 2.5mA/cm in current density2When, when graphene addition is 5.0g/L, 1,4,7 in Fig. 1,25 DEG C, 35
DEG C, the silver/graphite alkene composite deposite under 45 DEG C of different temperatures is well combined, without occurring peeling off vestige；2,5,8 in Fig. 1,
Silver/graphite alkene composite deposite at different temperatures occurs without hole；3,6,9 in Fig. 1, it is brilliant with the increase of temperature
The no significant change of grain and silver/graphite alkene composite deposite flatness is become better and better.
Embodiment 3
To the surface composition table of the silver/graphite alkene composite deposite of test group 1, test group 2 and test group 3 in embodiment 1, knot
Fruit is as shown in table 2.
The test group 1~3 of table 2 determines the coating surface component list under different temperatures
| Project | Region spectrogram | C/ (at%) | Ag/ (at%) |
| Test group 1 | 1 | 0 | 100.00 |
| 2 | 25.23 | 74.77 | |
| 3 | 2.63 | 97.37 | |
| 4 | 0 | 100 | |
| Test group 2 | 1 | 26.11 | 73.89 |
| 2 | 22.24 | 77.76 | |
| 3 | 24.08 | 75.92 | |
| 4 | 21.54 | 78.46 | |
| Test group 3 | 1 | 16.74 | 83.26 |
| 2 | 26.41 | 73.59 | |
| 3 | 0 | 100.00 | |
| 4 | 0 | 100.00 |
As seen in Table 2, when test group 1 and test group 3 are at 25 DEG C, 45 DEG C, EDS power spectrums determine silver/graphite alkene Composite Coatings
During layer surface composition, sending out position existing contains carbon component, and some positions do not have carbon component, and spot scan is random selecting point, carbon containing
The low position of amount is fine silver, and the high position of phosphorus content is probably doped with graphene.And sector scanning phosphorus content be 0, be because
Cladding portion position has been doped into graphene, and overall phosphorus content is less, is shown as 0.Position in test group 2 containing carbon into
Point.
Embodiment 4
The pattern of the silver/graphite alkene composite deposite of test group 4, test group 5 and test group 6 in embodiment 1 is analyzed,
As a result as shown in Fig. 2 Fig. 2-1, Fig. 2-2, Fig. 2-3, are that test group 4 photomacrograph, SEM scannings low power at 25 DEG C are micro- respectively
Photo, SEM scanning high magnification micrographs；Fig. 2-4, Fig. 2-5, Fig. 2-6, be respectively photomacrograph of the test group 5 at 35 DEG C,
SEM scannings low magnification micrographs, SEM scanning high magnification micrographs；Fig. 2-7, Fig. 2-8, Fig. 2-9 are test group 6 respectively at 45 DEG C
Under photomacrograph, SEM scanning low magnification micrographs, SEM scanning high magnification micrographs.
It is 2.5mA/cm in current density2When, when graphene addition is 10.0g/L, Fig. 2-1, Fig. 2-4, figure in Fig. 2
2-7, the coating at 25 DEG C, 45 DEG C is well combined, without there is peeling off vestige, and the binding force of cladding material at 35 DEG C it is poor,
There is peeling phenomenon.Fig. 2-2, Fig. 2-5, Fig. 2-8 in Fig. 2, at 25 DEG C, coating locally occurs in that cavity；At 35 DEG C, plating
Layer occurs in that a large amount of holes, and hole diameter is larger；At 45 DEG C, coating does not find cavity.Fig. 2-3, Fig. 2-6 in Fig. 2,
Fig. 2-9, at 45 DEG C, coating crystal grain is comparatively fine.At 35 DEG C, coating crystal grain is more thick, and flatness be then 35 DEG C most
It is good.
Analyze embodiment 3 and embodiment 4 is understood, the pattern that the numbering in Fig. 1 and Fig. 2 is 2,5,8 is understood, in current density
For 2.5mA/cm2When, at a temperature of 25 DEG C, 35 DEG C, 45 DEG C of contrast (test group 1~6), different graphene additions are to coating microstructure
Influence.When graphene containing 5g/L in plating solution, coating does not find hole.When the graphene containing 10g/L in plating solution
When, at 25 DEG C, 35 DEG C, coating surface finds hole, and in 45 DEG C of higher temperature, coating does not find hole.
Embodiment 5
To the surface composition table of the silver/graphite alkene composite deposite of test group 4, test group 5 and test group 6 in embodiment 1, knot
Fruit is as shown in table 3.
The test group 4~6 of table 3 determines the coating surface component list under different temperatures
Table 3 understands that test group 4~6 is at 25 DEG C, 35 DEG C, 45 DEG C, and EDS power spectrum spot scan silver/graphite alkene composite deposite is surveyed
Go out to have carbon containing position, illustrate that coating surface may adulterate by graphene.Test group 6 is at 45 DEG C, portion, EDS power spectrums
The position of cupric is measured in spot scan, and illustrating that coating surface is exposed has Copper substrate.
In contrast table 2 and table 3, test group 2 and test group 5 are at 35 DEG C, the carbon contents that EDS power spectrums are determined, 10g/L
Carbon content be twice of 5g/L or so, illustrate that the carbon content that graphene addition is determined to coating surface has a certain impact.
Embodiment 6
The pattern of the silver/graphite alkene composite deposite of test group 7, test group 8 and test group 9 in embodiment 1 is analyzed,
As a result as shown in figure 3, Fig. 3-1, Fig. 3-2, Fig. 3-3, are that test group 7 photomacrograph, SEM scannings low power at 25 DEG C are micro- respectively
Photo, SEM scanning high magnification micrographs；Fig. 3-4, Fig. 3-5, Fig. 3-6, be respectively photomacrograph of the test group 8 at 35 DEG C,
SEM scannings low magnification micrographs, SEM scanning high magnification micrographs；Fig. 3-7, Fig. 3-8, Fig. 3-9 are test group 9 respectively at 45 DEG C
Under photomacrograph, SEM scanning low magnification micrographs, SEM scanning high magnification micrographs.
It is 3.75mA/cm in current density2, during 10.0g/L graphene additions, Fig. 3-1, Fig. 3-4, Fig. 3-7 in Fig. 3
When, the peeling conditions with the increase silver/graphite alkene composite deposite of temperature gradually mitigate.Fig. 3-2, Fig. 3-5, Fig. 3-8 in Fig. 3
When, the equal surface of silver/graphite alkene composite deposite occurs in that different degrees of hole and peeling phenomenon.Fig. 3-3, Fig. 3-6 in Fig. 3,
During Fig. 3-9, test group 7 and test group 8 are at 25 DEG C, 35 DEG C, and spherical loose row is presented in silver/graphite alkene composite deposite microstructure
Row, flatness is bad.Test group 9 is at 45 DEG C, and square close-packed arrays are presented in coating microstructure, and flatness is preferable.
Embodiment 7
To the surface composition table of the silver/graphite alkene composite deposite of test group 7, test group 8 and test group 9 in embodiment 1, knot
Fruit is as shown in table 4.
The test group 7~9 of table 4 determines the coating surface component list under different temperatures
| Project | Region spectrogram | C (at%) | Ag (at%) | Cu (at%) | S (at%) |
| Test group 7 | 1 | 0 | 92.28 | 5.72 | 1.99 |
| 2 | 0 | 93.78 | 4.48 | 1.74 | |
| 3 | 0 | 51.26 | 48.74 | 0 | |
| 4 | 35.86 | 0 | 64.14 | ||
| 5 | 51.41 | 48.59 | 0 | 0 | |
| Test group 8 | 1 | 0 | 97.31 | 2.69 | 0 |
| 2 | 37.15 | 61.85 | 1.01 | 0 | |
| 3 | 39.52 | 1.64 | 58.84 | ||
| 4 | 24.18 | 39.83 | 35.99 | 0 | |
| Test group 9 | 1 | 0 | 0 | 100.00 | |
| 2 | 0 | 95.72 | 4.28 | ||
| 3 | 0 | 6.55 | 93.45 | ||
| 4 | 0 | 100.00 | 0 | ||
| 5 | 0 | 95.63 | 4.37 |
As known from Table 4, test group 7 and test group 8 are at 25 DEG C, 35 DEG C, and EDS power spectrums determine silver/graphite alkene Composite Coatings
There is carbon content layer surface component portion position, illustrates that silver/graphite alkene composite deposite portion may adulterate by graphene, experiment
Group 9 is at 45 DEG C, and silver/graphite alkene composite deposite surface does not determine carbon content.
Embodiment 8
The pattern of the silver/graphite alkene composite deposite of test group 6, test group 9 and test group 10 in embodiment 1 is divided
Analysis, is test group 6 respectively in 2.5mA/cm as a result as shown in figure 4, Fig. 4-1, Fig. 4-2, Fig. 4-32Lower photomacrograph, SEM scannings
Low magnification micrographs, SEM scanning high magnification micrographs；Fig. 4-4, Fig. 4-5, Fig. 4-6 are test group 9 respectively in 3.75mA/cm2
Under photomacrograph, SEM scanning low magnification micrographs, SEM scanning high magnification micrographs；Fig. 4-7, Fig. 4-8, Fig. 4-9, be respectively
Test group 10 is in 5.0mA/cm2Under photomacrograph, SEM scanning low magnification micrographs, SEM scanning high magnification micrographs.
As shown in figure 4, test group 6 is 45 DEG C in temperature, when graphene addition is 10g/L, 1,4,7 in Fig. 4 understand,
With the increase of current density, binding force of cladding material is gradually reduced, and plating exfoliation is increasingly severe；Test group 9 is 45 DEG C in temperature,
When graphene addition is 10g/L, 2,5,8 in Fig. 4 understand, coating surface peels off increasingly severe, does not find cavity；Examination
Test group 10 and be 45 DEG C in temperature, when graphene addition is 10g/L, 3,6,9 in Fig. 4 understand that coating surface is peeled off increasingly
Seriously, cavity is not found.In addition, as shown in Figure 4, coating crystal grain is in 2.5mA/cm2When, coating crystal grain is smaller, is square tight
Solid matter is arranged, and flatness is preferable；In 3.75mA/cm2When, coating crystal grain becomes big, and be square close-packed arrays, and flatness is preferable；
5.0mA/cm2When, coating crystal grain arrangement spherical in shape, flatness is good.
Embodiment 9
To the surface composition table of the silver/graphite alkene composite deposite of test group 6, test group 9 and test group 10 in embodiment 1,
As a result it is as shown in table 5.
The test group 6 of table 5, test group 9, test group 10 determine the coating surface component list under different current densities
It was found from the data in table 5, test group 6 is in 2.5mA/cm2, EDS power spectrums measure silver/graphite alkene composite deposite surface
Portion has carbon content, illustrates that silver/graphite alkene composite deposite may adulterate by graphene；Test group 9 and test group 10 exist
3.75mA/cm2、5.0mA/cm2When, carbon content is not measured on silver/graphite alkene composite deposite surface.
Above example illustrates, effective using silver/graphite alkene composite silver plating liquor disclosed by the invention and preparation method thereof
Graphene in silver/graphite alkene composite deposite prepared by current silver/graphite alkene composite silver plating liquor is solved not to be attached to well
The technological deficiency of silver/graphite alkene composite deposite.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. silver/graphite alkene composite silver plating liquor, it is characterised in that including following component：
2. silver/graphite alkene composite silver plating liquor according to claim 1, it is characterised in that including following component：
3. the preparation method of silver/graphite alkene composite silver plating liquor, it is characterised in that including：
1) water miscible Ag-containing compound, sodium thiosulfate, potassium metabisulfite, ammonium acetate and thiosemicarbazide are mixed, obtained
Mixed solution；
2) by step 1) mixed solution mixed with graphene platelet and polyvinylpyrrolidone, make graphene under ultrasound condition
Dissolving, obtains silver/graphite alkene composite silver plating liquor.
4. preparation method according to claim 3, it is characterised in that it is small that the graphene dries 1 at 80 DEG C~120 DEG C
When prepare.
5. preparation method according to claim 3, it is characterised in that step 1) PH of the mixed solution is 5-6.
6. a kind of electrodeposition technology, it is characterised in that including：
1) silver/graphite alkene composite silver plating liquor) is prepared；
2)) copper sheet is set；
3)) by step 2) copper sheet be placed in step 1) silver/graphite alkene composite silver plating liquor in carry out electro-deposition, obtain silver/stone
Black alkene composite deposite.
7. electrodeposition technology according to claim 6, it is characterised in that the current density of the electro-deposition is 1-5A/dm2。
8. electrodeposition technology according to claim 7, it is characterised in that the current density of the electro-deposition is 2.5A/dm2。
9. electrodeposition technology according to claim 6, it is characterised in that the plating temperature of the electro-deposition is 20-50 DEG C.
10. electrodeposition technology according to claim 9, it is characterised in that the plating temperature of the electro-deposition is 25-45
℃。
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