CN109183132A - A kind of preparation process of Sn-Ni- graphene/fluorinated graphene composite deposite - Google Patents
A kind of preparation process of Sn-Ni- graphene/fluorinated graphene composite deposite Download PDFInfo
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- CN109183132A CN109183132A CN201811420661.4A CN201811420661A CN109183132A CN 109183132 A CN109183132 A CN 109183132A CN 201811420661 A CN201811420661 A CN 201811420661A CN 109183132 A CN109183132 A CN 109183132A
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- graphene
- plating
- composite deposite
- fluorinated
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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
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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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
Abstract
The present invention relates to a kind of preparation processes of Sn-Ni- graphene/fluorinated graphene composite deposite, comprising the following steps: first by natural graphite/fluorographite and ammonium carbonate ball milling 60h, aqueous solution is made in obtained graphene product;Ultrasound 1h after graphene aqueous solution is mixed with basic bath again, adjusting solution ph is 8~10, mechanical stirring 1h, obtains coating Sn-Ni- graphene composite plating bath;Then using pretreated copper sheet as cathode, cathode-current density is 0.3~5A/dm2, 30~60 DEG C of plating temperature, time 10min, plating solution is stirred with constant speed with magnetic stirring apparatus in electroplating process, washed samples in deionized water after the completion of plating, and cold wind dries up;The present invention effectively increases the corrosion resistance and wearability of Sn-Ni coating, and graphene/fluorinated graphene of use has certain hydrophily, does not need that dispersing agent is added, just can preferably disperse in the plating solution.
Description
[technical field]
The invention belongs to electroplating technology, specifically a kind of Sn-Ni- graphene/fluorinated graphene composite deposite
Preparation process.
[background technique]
Sn-Ni alloy layer replaces coating as traditional nickel coating and chrome plating, can reduce preparation process
Pollution to environment and the damage to staff's health, and good wearability and corrosion resistance can be provided, therefore conduct
Protective coating is widely used in each field.However, for the field of certain current Special uses, tin-nickel alloy coating it is comprehensive
It can still need to further increase.
In recent years, composite deposition is increasingly becoming the effective method of another kind for improving coating corrosion resistance.Composite deposite
Preparation is that certain solid particle is added in the plating solution, coats solids particles precipitate in coating while metal ion reduction,
To obtain composite deposite.So far, has the composite deposite that related work person has developed variable grain, such as SiC, Al2O3、
SiO2, diamond, carbon nanotube etc..
Graphene, as a kind of SP2The original for the two-dimension periodic honeycomb structure that the connected carbon atom of hybridized orbit is combined into
Sub- crystal, main unit are the extremely stable benzene hexatomic rings of a length of 0.141nm of chain.In addition, σ key and pi bond in graphene
Conjugated structure makes active force with super strength between adjacent carbon atom, shows as excellent electric conductivity, thermal conductivity and mechanicalness
Energy.Currently, graphene is widely used in the fields such as pressure sensor, supercapacitor, electronic device.Fluorinated graphene is as stone
The new derivatives of black alkene are a kind of two-dimension plane structures, and wherein carbon atom and fluorine atom are combined in the form of covalent bond,
With surface can low, the excellent physical and chemical performance such as hydrophobicity is strong and band gap is wide, also there is high temperature resistant, corrosion resistance, antifriction
Wiping property, chemical property be stable and excellent lubricity, therefore can be widely used for high temperature coating, anti-wear lubricating coating and corrosion-resistant
Coating, while there is potential application prospect in fields such as nano electron device, opto-electronic device and thermoelectric devices.
Currently, existing related personnel is prepared for Ni base-graphite alkene composite deposite using electro-deposition techniques, and heavy by electricity
Product technology is prepared for Ni-Mn- graphene composite deposite, and discovery graphene is to the significant effect for improving corrosion resistance of coating and hardness
Fruit.Accordingly, it if graphene/fluorinated graphene is introduced into Sn-Ni alloy layer, is expected to directly improve the resistance to of Sn-Ni coating
Corrosion and hardness.And it is had not been reported about copper surface Sn-Ni- graphene/fluorinated graphene composite electroplated plating research.
[summary of the invention]
Present invention aim to solve above-mentioned deficiency and to provide a kind of Sn-Ni- graphene/fluorinated graphene compound
The preparation process of coating, can electro-deposition provide Sn-Ni- graphene/fluorine of excellent corrosion resistance and higher hardness
Graphene/fluorinated graphene of graphite alkene composite deposite, use has certain hydrophily, does not need that dispersing agent is added, just
Can preferably it disperse in the plating solution.
A kind of preparation process of Sn-Ni- graphene/fluorinated graphene composite deposite is designed to achieve the above object, including
Following steps:
1) plating Sn-Ni- graphene/fluorographite composite deposite electroplate liquid is prepared: first by natural graphite/fluorographite
With ammonium carbonate ball milling 60h, aqueous solution is made in obtained graphene/fluorinated graphene;It is again that graphene/fluorinated graphene is water-soluble
Ultrasound 1h after liquid is mixed with basic bath, adjusting solution ph is 8~10, and it is compound to obtain Sn-Ni- graphene by mechanical stirring 1h
Plating solution;Wherein, basic bath is the electrotinning nickel being configured to by pyrophosphate, pink salt, nickel salt, auxiliary complex-former, saccharin sodium
Basic bath, in the basic bath, P2O7 4-Molar concentration and Sn2+With Ni2+Total mol concentration ratio be 4:5~4:1,
Sn2+And Ni2+Molar concentration rate be 1:10~12:5, Sn2+And Ni2+0.1~0.6moL/L of total mol concentration, auxiliary complexing
The mass-volume concentration of agent is 5~50g/L, and the mass-volume concentration of saccharin sodium is 0.1~5g/L;
2) copper sheet successively matrix and processing: is passed through to the pretreatment of oil removing, pickling, polishing and activation step;
3) composite plating: using pretreated copper sheet as cathode, cathode-current density is 0.3~5A/dm2, plating temperature
30~60 DEG C, time 10min are spent, plating solution is stirred with constant speed with magnetic stirring apparatus in electroplating process, plating is completed
Washed samples in deionized water afterwards, and cold wind drying is to get Sn-Ni- graphene/fluorinated graphene composite deposite.
Further, in step 1), the auxiliary complex-former is the mixture that ammonium citrate and triethanolamine are formed, described
The mass ratio of ammonium citrate and triethanolamine is 2:1~4:1.
Further, in step 2), oil removing is that 2min is impregnated in 40 DEG C of degreaser, and composition of raw materials is as follows: NaOH
Mass fraction be 15%, Na2CO3The mass fraction of 1g/L, OP-10 are 2%, remaining is distilled water.Pickling is at 35 DEG C
30s is impregnated in pickling solution, composition of raw materials is as follows: H2SO4 40mL/L、HNO328mL/L, remaining is distilled water.Polishing be
50s is impregnated in 35 DEG C of polishing fluid, composition of raw materials is as follows: oxalic acid 40g/L, NaOH 18g/L, hydrogen peroxide 120mL/L, remaining
For distilled water.Activation is the H for being 5% in mass percent concentration2SO41min is activated in aqueous solution.
The present invention compared with the existing technology, can electro-deposition provide excellent corrosion resistance and higher hardness
Sn-Ni- graphene/fluorinated graphene composite deposite, the graphene obtained using graphite/fluorographite and ammonium carbonate ball milling 60h/
Fluorinated graphene has certain hydrophily, does not need that dispersing agent is added, just can preferably disperse in the plating solution, and graphene
The corrosion resistance and wearability for effectively increasing Sn-Ni coating is added.In addition, the present invention can mention to improve Sn-Ni alloy corrosion resistance
For a kind of new method.
[Detailed description of the invention]
Fig. 1 is the scanning electron microscope diagram for the Sn-Ni- graphene composite deposite that the embodiment of the present invention 1 obtains;
Fig. 2 is the EDS map for the Sn-Ni- graphene composite deposite that the embodiment of the present invention 1 obtains;
Fig. 3 is that graphite is not added under the Sn-Ni- graphene composite deposite and the same terms that the embodiment of the present invention 1,2 and 3 obtains
The corrosion weight loss figure for the Sn-Ni alloy layer that alkene obtains;
Fig. 4 is the scanning electron microscope diagram for the Sn-Ni- fluorinated graphene composite deposite that the embodiment of the present invention 4 obtains;
Fig. 5 is the EDS map for the Sn-Ni- fluorinated graphene composite deposite that the embodiment of the present invention 4 obtains;
Fig. 6 is not added under the Sn-Ni- fluorinated graphene composite deposite and the same terms that the embodiment of the present invention 4,5 and 6 obtains
The corrosion weight loss figure for the Sn-Ni alloy layer that fluorinated graphene obtains.
[specific embodiment]
The present invention provides a kind of preparation process of Sn-Ni- graphene/fluorinated graphene composite deposite, specifically include as
Lower step:
1) plating Sn-Ni- graphene/fluorographite composite deposite electroplate liquid is prepared
First by natural graphite/fluorographite and ammonium carbonate ball milling 60h, obtained graphene/fluorinated graphene is made water-soluble
Liquid, the aqueous solution have good hydrophily, and it is not stratified that solution places a couple of days.
Again by P2O7 4-Molar concentration and Sn2+With Ni2+Total mol concentration ratio be 4:5~4:1;Sn2+And Ni2+'s
Molar concentration rate is 1:10~12:5;Sn2+And Ni2+0.1~0.6moL/L of total mol concentration;The mass body of auxiliary complex-former
Product concentration is 5~50g/L, and auxiliary complex-former is the mixture that ammonium citrate and triethanolamine are formed, ammonium citrate and three ethyl alcohol
The mass ratio of amine is 2:1~4:1;The mass-volume concentration of saccharin sodium is 0.1-5g/L, is configured to the basic bath of electrotinning nickel.
Later, ultrasound 1h after graphene aqueous solution being mixed with basic bath, adjusting solution ph is 8~10, and mechanical stirring 1h is obtained
Coating Sn-Ni- graphene composite plating bath.
2) matrix and processing
Copper sheet is successively carried out to the pretreatment of oil removing, pickling, polishing and activation step, the pretreated specific steps are such as
Under,
Oil removing: impregnating 2min in 40 DEG C of degreaser, and composition of raw materials is following (mass fraction): NaOH 15%,
Na2CO31g/L, OP-10 2%, remaining is distilled water.
Pickling: impregnating 30s in 35 DEG C of pickling solution, and composition of raw materials is as follows: H2SO4 40mL/L、HNO328mL/L,
Remaining is distilled water.
Polishing: 50s is impregnated in 35 DEG C of polishing fluid, composition of raw materials is as follows: oxalic acid 40g/L, NaOH 18g/L, dioxygen
Water 120mL/L, remaining is distilled water.
Activation: the H for being 5% in mass percent concentration2SO41min is activated in aqueous solution.
3) composite plating
Using pretreated copper sheet as cathode, cathode-current density is 0.3~5A/dm2, 30~60 DEG C of plating temperature,
Time 10min is stirred plating solution with constant speed with magnetic stirring apparatus in electroplating process, in deionized water after the completion of plating
Middle washed samples, and cold wind dries up, i.e., obtains one layer of Sn-Ni- graphene/fluorinated graphene composite deposite on copper surface.
The present invention is made combined with specific embodiments below further explained below:
Embodiment 1
A kind of Sn-Ni- graphene composite deposite and preparation process, composite plating bath composition are as follows:
Electroplating technical conditions: pH 8.5,40 DEG C of temperature, DK 3A/dm2, plating time 10min.
Under this condition, silvery white coating has been obtained, successfully has been detected in coating and contains by elemental analysis (EDS technology)
Carbon shows successfully to have obtained the composite deposite containing graphene (see Fig. 1).Scanning electron microscope (SEM) photograph test discovery, what is obtained answers
It is careful (Fig. 2) to close coating light, is combined with matrix, coating is without any peeling and peeling.Under the identical testing time, contain stone
The wt-lossing rates of the composite deposite of black alkene show that the presence of graphene makes composite deposite much smaller than the composite deposite of not containing graphene
Corrosion resistance be better than Sn-Ni alloy layer (Fig. 3).
Embodiment 2
A kind of Sn-Ni- graphene composite deposite and preparation process, composite plating bath composition are as follows:
Electroplating technical conditions: pH 9,30 DEG C of temperature, DK 0.3A/dm2, plating time 100min.
Under this condition, the silvery white composite deposite light obtained is careful, is combined with matrix, coating without it is any peeling and
Peeling, under the identical testing time, the wt-lossing rates of the composite deposite of containing graphene are much smaller than the Composite Coatings of not containing graphene
Layer shows that the presence of graphene makes the corrosion resistance of composite deposite better than Sn-Ni alloy layer (see Fig. 3).
Embodiment 3
A kind of Sn-Ni- graphene composite deposite and preparation process, composite plating bath composition are as follows:
Electroplating technical conditions: pH 10,40 DEG C of temperature, DK 2A/dm2, plating time 15min.
Under this condition, the silvery white composite deposite light obtained is careful, is combined with matrix, coating without it is any peeling and
Peeling, under the identical testing time, the wt-lossing rates of the composite deposite of containing graphene are much smaller than the Composite Coatings of not containing graphene
Layer shows that the presence of graphene makes the corrosion resistance of composite deposite better than Sn-Ni alloy layer (see Fig. 3).
Embodiment 4
A kind of Sn-Ni- fluorinated graphene composite deposite and preparation process, composite plating bath composition are as follows:
Electroplating technical conditions: pH 8.5,40 DEG C of temperature, DK 3A/dm2, plating time 10min.
Under this condition, silvery white coating has been obtained, successfully has been detected in coating and contains by elemental analysis (EDS technology)
Carbon and fluorine element show successfully to have obtained the composite deposite containing fluorinated graphene (see Fig. 4).Scanning electron microscope (SEM) photograph test hair
Existing, obtained composite deposite light is careful (Fig. 5), is combined with matrix, and coating is without any peeling and peeling.In identical test
Under time, the wt-lossing rates of the composite deposite containing fluorinated graphene are much smaller than the composite deposite without fluorinated graphene, show fluorine
The presence of graphite alkene makes the corrosion resistance of composite deposite better than Sn-Ni alloy layer (Fig. 6).
Embodiment 5
A kind of Sn-Ni- fluorinated graphene composite deposite and preparation process, composite plating bath composition are as follows:
Electroplating technical conditions: pH 9,30 DEG C of temperature, DK 0.3A/dm2, plating time 100min.
Under this condition, the silvery white composite deposite light obtained is careful, is combined with matrix, coating without it is any peeling and
Peeling, under the identical testing time, the wt-lossing rates of the composite deposite containing fluorinated graphene, which are much smaller than, is free of fluorinated graphene
Composite deposite, show that the presence of fluorinated graphene makes the corrosion resistance of composite deposite better than Sn-Ni alloy layer (see figure
6)。
Embodiment 6
A kind of Sn-Ni- fluorinated graphene composite deposite and preparation process, composite plating bath composition are as follows:
Electroplating technical conditions: pH 10,40 DEG C of temperature, DK 2A/dm2, plating time 10min.
Under this condition, the silvery white composite deposite light obtained is careful, is combined with matrix, coating without it is any peeling and
Peeling, under the identical testing time, the wt-lossing rates of the composite deposite containing fluorinated graphene, which are much smaller than, is free of fluorinated graphene
Composite deposite, show that the presence of fluorinated graphene makes the corrosion resistance of composite deposite better than Sn-Ni alloy layer (see figure
6)。
Embodiment 7
A kind of Sn-Ni- fluorinated graphene composite deposite and preparation process, composite plating bath composition are as follows:
Electroplating technical conditions: pH 8,40 DEG C of temperature, DK 5A/dm2, plating time 10min.
Under this condition, the silvery white composite deposite light obtained is careful, is combined with matrix, coating without it is any peeling and
Peeling.
The present invention is simultaneously not limited to the embodiments described above, other any without departing from spiritual essence and principle of the invention
Changes, modifications, substitutions, combinations, simplifications made by lower, should be equivalent substitute mode, are included in protection model of the invention
Within enclosing.
Claims (6)
1. a kind of preparation process of Sn-Ni- graphene/fluorinated graphene composite deposite, which comprises the following steps:
1) plating Sn-Ni- graphene/fluorographite composite deposite electroplate liquid is prepared
First by natural graphite/fluorographite and ammonium carbonate ball milling 60h, aqueous solution is made in obtained graphene/fluorinated graphene;Again
Ultrasound 1h after graphene/fluorinated graphene aqueous solution is mixed with basic bath, adjusting solution ph is 8~10, and machinery stirs
1h is mixed, coating Sn-Ni- graphene composite plating bath is obtained;Wherein, basic bath is by pyrophosphate, pink salt, nickel salt, auxiliary network
The basic bath for the electrotinning nickel that mixture, saccharin sodium are configured to, in the basic bath, P2O7 4-Molar concentration and Sn2+With Ni2+
Total mol concentration ratio be 4:5~4:1, Sn2+And Ni2+Molar concentration rate be 1:10~12:5, Sn2+And Ni2+Always rub
You are 0.1~0.6moL/L of concentration, and the mass-volume concentration of auxiliary complex-former is 5~50g/L, and the mass-volume concentration of saccharin sodium is
0.1~5g/L;
2) matrix and processing
Copper sheet is successively passed through to the pretreatment of oil removing, pickling, polishing and activation step;
3) composite plating
Using pretreated copper sheet as cathode, cathode-current density is 0.3~5A/dm2, 30~60 DEG C of plating temperature, the time
10min is stirred plating solution with constant speed with magnetic stirring apparatus in electroplating process, clear in deionized water after the completion of plating
Sample is washed, and cold wind drying is to get Sn-Ni- graphene/fluorinated graphene composite deposite.
2. the preparation process of Sn-Ni- graphene/fluorinated graphene composite deposite as described in claim 1, it is characterised in that:
In step 1), the auxiliary complex-former is the mixture that ammonium citrate and triethanolamine are formed, the ammonium citrate and three ethyl alcohol
The mass ratio of amine is 2:1~4:1.
3. the preparation process of Sn-Ni- graphene/fluorinated graphene composite deposite as described in claim 1, which is characterized in that
In step 2), oil removing is that 2min is impregnated in 40 DEG C of degreaser, and composition of raw materials is as follows: the mass fraction of NaOH be 15%,
Na2CO3The mass fraction of 1g/L, OP-10 are 2%, remaining is distilled water.
4. the preparation process of Sn-Ni- graphene/fluorinated graphene composite deposite as described in claim 1, which is characterized in that
In step 2), pickling is that 30s is impregnated in 35 DEG C of pickling solution, and composition of raw materials is as follows: H2SO4 40mL/L、HNO3 28mL/
L, remaining is distilled water.
5. the preparation process of Sn-Ni- graphene/fluorinated graphene composite deposite as described in claim 1, which is characterized in that
In step 2), polishing is that 50s is impregnated in 35 DEG C of polishing fluid, and composition of raw materials is as follows: oxalic acid 40g/L, NaOH 18g/L, double
Oxygen water 120mL/L, remaining is distilled water.
6. the preparation process of Sn-Ni- graphene/fluorinated graphene composite deposite as described in claim 1, which is characterized in that
In step 2), activation is the H for being 5% in mass percent concentration2SO41min is activated in aqueous solution.
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Cited By (2)
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CN117587476A (en) * | 2024-01-18 | 2024-02-23 | 深圳华烯新材料有限公司 | Fluorinated graphene composite coating |
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