CN110565081A - chemical composite nickel-phosphorus-graphene plating solution and preparation method and application thereof - Google Patents
chemical composite nickel-phosphorus-graphene plating solution and preparation method and application thereof Download PDFInfo
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- CN110565081A CN110565081A CN201910860539.7A CN201910860539A CN110565081A CN 110565081 A CN110565081 A CN 110565081A CN 201910860539 A CN201910860539 A CN 201910860539A CN 110565081 A CN110565081 A CN 110565081A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1655—Process features
- C23C18/1662—Use of incorporated material in the solution or dispersion, e.g. particles, whiskers, wires
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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Abstract
The invention provides a chemical composite nickel-phosphorus-graphene plating solution, which comprises nickel sulfate, sodium hypophosphite, citric acid, lactic acid, sodium acetate, a first stabilizer, a second stabilizer, sodium dodecyl benzene sulfonate, graphene, distilled water and ammonia water; the components of the solution are dissolved in distilled water in a certain order, the solution is uniformly stirred, and the pH value of the solution is adjusted to 4.4-5.0, so that the composite chemical nickel-phosphorus-graphene plating solution is obtained. According to the chemical composite nickel-phosphorus-graphene plating solution prepared by the invention, the graphene is uniformly dispersed in the composite plating solution, the chemical composite nickel-phosphorus-graphene plating solution is used in the field of aluminum alloy electroplating, the processing efficiency is obvious, and the plating layer is fine in crystallization; the appearance and the binding force of the plating layer are good, and meanwhile, the composite plating layer has high hardness and good salt spray resistance; the preparation method of the plating solution is simple, the composite plating solution is stable and convenient to maintain, the complexing ability of the used complexing agent is moderate, the complex can be broken well in sewage treatment, and the production cost and the sewage treatment cost can be reduced.
Description
Technical Field
The invention belongs to the technical field of aluminum alloy electroplating, and particularly relates to a chemical composite nickel-phosphorus-graphene plating solution, and a preparation method and application thereof.
Background
The chemical nickel plating of the aluminum alloy is widely applied to the fields of aviation, aerospace and the like, and a good plating layer can be prepared on a metal material and a non-metal material by adopting a chemical plating method so as to obtain good performances such as corrosion resistance, wear resistance, self-lubrication, conductivity, decoration and the like. Under the more severe environment condition, the existing nickel plating layer can not meet the requirement, and the composite plating layer with graphene doped in the nickel-phosphorus-based plating layer appears, so that the composite plating layer has other excellent performances, and the performances of a single plating layer can be improved.
According to the research progress of the nickel-phosphorus-graphene composite coating for the aluminum alloy at home and abroad, in the prior art, the fusion degree of graphene and the nickel-phosphorus coating is poor, the graphene is mainly distributed on the surface of the coating and cannot be well fused with the nickel-phosphorus coating, and in an environment with severe conditions, the coating has thick crystallization, and the binding force, hardness and salt spray resistance of the coating cannot meet the requirements; meanwhile, in consideration of economic and environment-friendly development guidelines, the complexing agent used in the prior art has strong complexing ability, difficult complex breaking during sewage treatment and high sewage treatment cost.
Disclosure of Invention
In order to solve the technical problems, the invention provides a chemical composite nickel-phosphorus-graphene plating solution and a preparation method thereof, and the chemical composite nickel-phosphorus-graphene plating solution is provided with a double coordination agent, a double stabilizing agent and a surfactant, so that the degree of fusion of graphene and a nickel-phosphorus plating layer is improved, a smooth and uniform nickel-phosphorus-graphene composite plating layer is obtained, and the composite plating layer is enabled to obtain higher hardness and better salt spray resistance.
the invention is realized by the following technical scheme.
A chemical composite nickel-phosphorus-graphene plating solution comprises the following raw materials per liter:
The chemical composite nickel-phosphorus-graphene plating solution comprises the following raw materials per liter:
the first stabilizer is potassium iodate.
The second stabilizer is rare earth cerium.
a preparation method of a chemical composite nickel-phosphorus-graphene plating solution comprises the following steps:
S1: firstly, dissolving nickel sulfate in distilled water, adding sodium hypophosphite, stirring until the nickel sulfate is completely dissolved, adding sodium acetate, stirring until the sodium hypophosphite is completely dissolved, and obtaining solution A;
S2: dissolving citric acid in distilled water, adding lactic acid, halving to completely dissolve, and adding a first stabilizer and a second stabilizer to obtain a solution B;
S3: adding the solution B into the solution A, and uniformly stirring to obtain a solution C;
s4: adding graphene into distilled water, stirring, adding a surfactant sodium dodecyl benzene sulfonate, and performing ultrasonic oscillation to obtain a solution D, and adopting a surfactant (chemical method) and adding ultrasonic waves (physical method) to prepare a dispersion solution, so that the graphene can be more uniformly dispersed in a plating solution, the graphene in a composite plating layer is more dispersed, a better plating solution is obtained, and a better plating layer is obtained;
s5: adding the solution D into the solution C, and uniformly stirring to obtain a solution E;
S6: and adjusting the pH value of the solution E to 4.4-5.0 to obtain the composite chemical nickel-phosphorus-graphene plating solution.
the pH adjusting reagent in the step S6 is an ammonia solution.
the pH was adjusted to 4.6 in step S6.
The chemical composite nickel-phosphorus-graphene plating solution is used for forming a nickel-phosphorus-graphene composite plating layer on the surface of an aluminum alloy part through chemical plating, and the plating temperature is 84-88 ℃.
The chemical composite nickel-phosphorus-graphene plating solution is used for forming a nickel-phosphorus-graphene composite plating layer on the surface of an aluminum alloy part through chemical plating, and the plating temperature is 88 ℃.
the invention has the beneficial effects that:
compared with the prior art, the method selects the main citric acid complexing agent, the lactic acid as the auxiliary complexing agent, the first stabilizer and the second stabilizer as the bistable agents, and the sodium dodecyl benzene sulfonate as the surfactant, so that the composite plating solution with uniformly dispersed graphene can be obtained, the aluminum alloy is plated within the temperature range of 84-88 ℃, the obtained nickel-phosphorus-graphene composite plating layer has fine crystallization, the graphene can be better fused into the nickel-phosphorus plating layer, the distribution is uniform, and the processing efficiency is obvious; and the appearance and the binding force of the plating layer are better, and simultaneously, the composite plating layer has high hardness and good salt spray resistance. The plating solution of the invention has simple preparation method, stable composite plating solution and convenient maintenance, the complexing ability of the used complexing agent is moderate, the complex can be broken well in sewage treatment, and the performance of the composite plating layer is superior to that of a chemical nickel plating layer under the condition of the same thickness, so that the production cost and the sewage treatment cost can be reduced.
Drawings
FIG. 1 is a scanning electron microscope image of a prior art chemically compounded nickel-phosphorus-graphene layer;
FIG. 2 is a scanning electron micrograph of a chemically compounded nickel-phosphorus-graphene layer according to example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of the chemically compounded nickel-phosphorus-graphene layer of example 2 of the present invention;
fig. 4 is an EDS energy spectrum of the chemically compounded nickel-phosphorus-graphene layer of example 3 of the present invention;
FIG. 5 is a chemical element ratio of FIG. 4;
FIG. 6 is a distribution diagram of elements C of the scanning electron microscope of example 3 of the present invention;
FIG. 7 is a distribution diagram of P elements of a scanning electron microscope in example 3 of the present invention;
FIG. 8 is a distribution diagram of Ni elements in a scanning electron microscope of example 3 of the present invention;
Fig. 9 is a metallographic analysis diagram of a chemically compounded nickel-phosphorus-graphene layer according to example 3 of the present invention.
Detailed Description
the technical solution of the present invention is further described below, but the scope of the claimed invention is not limited to the described.
as shown in fig. 1, a 500-fold photograph under a scanning electron microscope shows that a large number of isolated particles exist on the surface of a plating layer obtained by adding graphene into chemical nickel plating liquid medicine in the prior art, the surface of the plating layer is loose, and graphene and a bottom plating layer are not well fused, so that the bonding force of the plating layer is poor.
Example 1
A chemical composite nickel-phosphorus-graphene plating solution comprises the following raw materials per liter:
The first stabilizer is potassium iodate.
the second stabilizer is rare earth cerium.
A preparation method of a chemical composite nickel-phosphorus-graphene plating solution comprises the following steps:
S1: firstly, dissolving nickel sulfate in distilled water, adding sodium hypophosphite, stirring until the nickel sulfate is completely dissolved, adding sodium acetate, stirring until the sodium hypophosphite is completely dissolved, and obtaining solution A;
S2: dissolving citric acid in distilled water, adding lactic acid, halving to completely dissolve, and adding a first stabilizer and a second stabilizer to obtain a solution B;
s3: adding the solution B into the solution A, and uniformly stirring to obtain a solution C;
s4: adding graphene into distilled water, stirring, adding a surfactant sodium dodecyl benzene sulfonate, and performing ultrasonic oscillation to obtain a solution D, and adopting a surfactant (chemical method) and adding ultrasonic waves (physical method) to prepare a dispersion solution, so that the graphene can be more uniformly dispersed in a plating solution, the graphene in a composite plating layer is more dispersed, a better plating solution is obtained, and a better plating layer is obtained;
S5: adding the solution D into the solution C, and uniformly stirring to obtain a solution E;
S6: and adjusting the pH value of the solution E to 4.4 by ammonia water to obtain the composite chemical nickel-phosphorus-graphene plating solution.
the chemical composite nickel-phosphorus-graphene plating solution is used for forming a nickel-phosphorus-graphene composite plating layer on the surface of an aluminum alloy part through chemical plating, and the plating temperature is 84 ℃.
as shown in fig. 2, scanning electron microscope characterization of the nickel-phosphorus-graphene composite coating obtained by the formulation, method and process conditions in example 1 shows that the coating obtained by the electroless composite nickel-phosphorus-graphene plating solution prepared by the present invention has smooth surface, good fusion of nickel-phosphorus-graphene, fine crystallization of the coating, and good coating bonding force, and thus a composite coating with high hardness and good salt spray resistance can be obtained.
Example 2
a chemical composite nickel-phosphorus-graphene plating solution comprises the following raw materials per liter:
the first stabilizer is potassium iodate.
The second stabilizer is rare earth cerium.
A preparation method of a chemical composite nickel-phosphorus-graphene plating solution comprises the following steps:
s1: firstly, dissolving nickel sulfate in distilled water, adding sodium hypophosphite, stirring until the nickel sulfate is completely dissolved, adding sodium acetate, stirring until the sodium hypophosphite is completely dissolved, and obtaining solution A;
S2: dissolving citric acid in distilled water, adding lactic acid, halving to completely dissolve, and adding a first stabilizer and a second stabilizer to obtain a solution B;
s3: adding the solution B into the solution A, and uniformly stirring to obtain a solution C;
S4: adding graphene into distilled water, stirring, adding a surfactant sodium dodecyl benzene sulfonate, and performing ultrasonic oscillation to obtain a solution D, and adopting a surfactant (chemical method) and adding ultrasonic waves (physical method) to prepare a dispersion solution, so that the graphene can be more uniformly dispersed in a plating solution, the graphene in a composite plating layer is more dispersed, a better plating solution is obtained, and a better plating layer is obtained;
S5: adding the solution D into the solution C, and uniformly stirring to obtain a solution E;
S6: and adjusting the pH value of the solution E to 5.0 by ammonia water to obtain the composite chemical nickel-phosphorus-graphene plating solution.
The chemical composite nickel-phosphorus-graphene plating solution is used for forming a nickel-phosphorus-graphene composite plating layer on the surface of an aluminum alloy part through chemical plating, and the plating temperature is 88 ℃.
as shown in fig. 3, scanning electron microscope characterization of the nickel-phosphorus-graphene composite coating obtained by the formulation, method and process conditions in example 1 shows that the coating obtained by the electroless composite nickel-phosphorus-graphene plating solution prepared by the present invention has smooth surface, good fusion of nickel-phosphorus-graphene, fine crystallization of the coating, and good coating bonding force, and thus a composite coating with high hardness and good salt spray resistance can be obtained.
In order to obtain the best component proportion, method and process condition and verify the technical effect, the following experiments are carried out:
1. determination of basic formula of composite plating solution
Respectively selecting 25g/L-35g/L solution of main salt nickel sulfate and 26g/L-36g/L solution of reducing agent sodium hypophosphite to carry out nickel-phosphorus proportioning, carrying out single-factor experiment, determining that the content of nickel sulfate is 28g/L and the content of sodium hypophosphite is 32g/L, and obtaining a plating layer with the phosphorus content of more than 9 percent and a composite plating layer which is a high-phosphorus plating layer.
2. screening of stabilizers
A solution of 60-120 mg/L of a first stabilizer and a solution of 5-10 mg/L of a second stabilizer are respectively selected to perform a single-factor experiment to determine the optimal addition amount, and after a compounding experiment of the two stabilizers is performed, the obtained composite plating solution is stable and has good comprehensive performance, wherein the optimal addition amount of the first stabilizer is 80mg/L, and the optimal addition amount of the second stabilizer is 8 mg/L.
3. screening of complexing Agents
and sequentially carrying out single-factor experiments on several types of O-complexing agents and N-complexing agents to determine that the O-complexing agent citric acid is the main complexing agent of the composite plating solution, carrying out the single-factor experiments on other complexing agents to finally determine that the lactic acid is the auxiliary complexing agent, the optimal addition amount of the citric acid is 25g/L, and the optimal addition amount of the lactic acid is 15ml/L, so that the obtained composite plating solution and the plating layer have better comprehensive performance.
4. screening of surfactants
And selecting a surfactant sodium dodecyl benzene sulfonate for carrying out a single-factor experiment to obtain that the graphene is uniformly dispersed in the plating solution and the plating layer, wherein the optimal addition amount of the surfactant sodium dodecyl benzene sulfonate is 50 mg/L.
5. Determination of the Process conditions
(1) Influence of pH
The pH of the plating solution is 4.0-5.0, single factor experiment is carried out, and the optimal pH process range is 4.4-4.8 by investigating the comprehensive performance of the plating solution and the plating layer.
(2) Influence of temperature
The plating temperature is 80-90 ℃ to carry out single-factor experiments, and the optimal plating temperature process parameter range is 84-88 ℃ by investigating the comprehensive performance of the plating solution and the plating layer.
(3) Effect of graphene content
and performing a single-factor experiment on the graphene addition amount range of 40-140 mg/L, and observing the comprehensive performance of the plating solution and the plating layer to obtain the optimal graphene addition amount process parameter range of 80-120 mg/L.
(4) optimized plating process for orthogonal experiment
Performing an orthogonal experiment by using the process range obtained by the single-factor experiment, and determining the optimal process by the orthogonal experiment as follows: the addition amount of the graphene is 100mg/L, the plating temperature is 88 ℃ + the pH value of the composite plating solution is 4.6.
Example 3
a chemical composite nickel-phosphorus-graphene plating solution comprises the following raw materials per liter:
the first stabilizer is potassium iodate.
the second stabilizer is rare earth cerium.
The preparation method of the chemical composite nickel-phosphorus-graphene plating solution comprises the following steps:
s1: firstly, dissolving nickel sulfate in distilled water, adding sodium hypophosphite, stirring until the nickel sulfate is completely dissolved, adding sodium acetate, stirring until the sodium hypophosphite is completely dissolved, and obtaining solution A;
S2: dissolving citric acid in distilled water, adding lactic acid, halving to completely dissolve, and adding a first stabilizer and a second stabilizer to obtain a solution B;
S3: adding the solution B into the solution A, and uniformly stirring to obtain a solution C;
S4: adding graphene into distilled water, stirring, adding a surfactant sodium dodecyl benzene sulfonate, and performing ultrasonic oscillation to obtain a solution D, and adopting a surfactant (chemical method) and adding ultrasonic waves (physical method) to prepare a dispersion solution, so that the graphene can be more uniformly dispersed in a plating solution, the graphene in a composite plating layer is more dispersed, a better plating solution is obtained, and a better plating layer is obtained;
S5: adding the solution D into the solution C, and uniformly stirring to obtain a solution E;
S6: and adjusting the pH value of the solution E to 4.6 by ammonia water to obtain the composite chemical nickel-phosphorus-graphene plating solution.
The chemical composite nickel-phosphorus-graphene plating solution is used for forming a nickel-phosphorus-graphene composite plating layer on the surface of an aluminum alloy part through chemical plating, and the plating temperature is 88 ℃.
Example 3 according to the optimum composition formula, method and process conditions, the electroplating of the chemical composite nickel-phosphorus-graphene plating is completed on the aluminum alloy test block, and further detection is performed, and the detection results are as follows:
(1) EDS energy Spectrum characterization
As shown in fig. 4, the elements contained in the coating are carbon, phosphorus and nickel, and the coating has no impurity, so as to meet the control requirement of coating impurities, and the element ratio is shown in fig. 5.
(2) Characterization of scanning Electron microscope
as shown in fig. 6 to 8, the plating surface obtained by the chemical composite nickel-phosphorus-graphene plating solution prepared by the present invention has uniform distribution of carbon, phosphorus and nickel, and good plating consistency.
(3) Metallographic analysis
as shown in fig. 9, the plating surface obtained by the chemical composite nickel-phosphorus-graphene plating solution prepared by the invention has the small black spots of carbon and phosphorus, uniform distribution and good plating consistency.
In summary, according to the chemical composite nickel-phosphorus-graphene plating solution provided by the invention, a citric acid main coordination agent is selected, lactic acid is used as an auxiliary coordination agent, a first stabilizer and a second stabilizer are used as bistable agents, and sodium dodecyl benzene sulfonate is used as a surfactant, so that a composite plating solution with uniformly dispersed graphene can be obtained, aluminum alloy is plated within a temperature range of 84-88 ℃, and the obtained nickel-phosphorus-graphene composite plating layer has fine crystallization, the graphene can be better fused into a nickel-phosphorus plating layer, and is uniformly distributed and has obvious processing efficiency; and the appearance and the binding force of the plating layer are better, and simultaneously, the composite plating layer has high hardness and good salt spray resistance. The plating solution of the invention has simple preparation method, stable composite plating solution and convenient maintenance, the complexing ability of the used complexing agent is moderate, the complex can be broken well in sewage treatment, and the performance of the composite plating layer is superior to that of a chemical nickel plating layer under the condition of the same thickness, so that the production cost and the sewage treatment cost can be reduced.
Claims (9)
1. the chemical composite nickel-phosphorus-graphene plating solution is characterized by comprising the following raw materials per liter:
2. The electroless composite nickel-phosphorus-graphene plating solution according to claim 1, wherein each liter of the plating solution comprises the following raw materials in percentage by weight:
3. the electroless composite nickel-phosphorus-graphene plating solution of claim 1, wherein: the first stabilizer is potassium iodate.
4. The electroless composite nickel-phosphorus-graphene plating solution of claim 1, wherein: the second stabilizer is rare earth cerium.
5. a preparation method of a chemical composite nickel-phosphorus-graphene plating solution comprises the following steps:
S1: firstly, dissolving nickel sulfate in distilled water, adding sodium hypophosphite, stirring until the nickel sulfate is completely dissolved, adding sodium acetate, stirring until the sodium hypophosphite is completely dissolved, and obtaining solution A;
S2: dissolving citric acid in distilled water, adding lactic acid, halving to completely dissolve, and adding a first stabilizer and a second stabilizer to obtain a solution B;
S3: adding the solution B into the solution A, and uniformly stirring to obtain a solution C;
S4: adding graphene into distilled water, stirring, adding a surfactant sodium dodecyl benzene sulfonate, and performing ultrasonic oscillation to obtain a solution D;
S5: adding the solution D into the solution C, and uniformly stirring to obtain a solution E;
s6: and adjusting the pH value of the solution E to 4.4-5.0 to obtain the chemical composite nickel-phosphorus-graphene plating solution.
6. The method for preparing the electroless composite nickel-phosphorus-graphene plating solution according to claim 5, wherein the plating solution comprises the following steps: the pH adjusting reagent in the step S6 is an ammonia solution.
7. the method for preparing the electroless composite nickel-phosphorus-graphene plating solution according to claim 5, wherein the plating solution comprises the following steps: the pH was adjusted to 4.6 in step S6.
8. The chemical composite nickel-phosphorus-graphene plating solution as claimed in claim 1 is used for forming a nickel-phosphorus-graphene composite plating layer on the surface of an aluminum alloy part through chemical electroplating, and the plating temperature is 84-88 ℃.
9. The chemical composite nickel-phosphorus-graphene plating solution as defined in claim 1 is used for forming a nickel-phosphorus-graphene composite plating layer on the surface of an aluminum alloy part through chemical plating, and the plating temperature is 88 ℃.
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| CN111112881A (en) * | 2020-01-03 | 2020-05-08 | 苏州优诺电子材料科技有限公司 | Graphene modified low-temperature solder and preparation method thereof |
| CN116043291A (en) * | 2023-01-30 | 2023-05-02 | 东北电力大学 | Nickel-graphene composite coating taking 310S stainless steel as base material and preparation method thereof |
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| CN111112881B (en) * | 2020-01-03 | 2021-06-04 | 苏州优诺电子材料科技有限公司 | Graphene modified low-temperature solder and preparation method thereof |
| CN116043291A (en) * | 2023-01-30 | 2023-05-02 | 东北电力大学 | Nickel-graphene composite coating taking 310S stainless steel as base material and preparation method thereof |
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Application publication date: 20191213 |