CN114277422B - Preparation method of tin-graphene composite brush plating solution and aluminum substrate surface plating layer - Google Patents
Preparation method of tin-graphene composite brush plating solution and aluminum substrate surface plating layer Download PDFInfo
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- 238000007747 plating Methods 0.000 title claims abstract description 159
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 67
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- 125000002252 acyl group Chemical group 0.000 claims description 3
- JRBRVDCKNXZZGH-UHFFFAOYSA-N alumane;copper Chemical compound [AlH3].[Cu] JRBRVDCKNXZZGH-UHFFFAOYSA-N 0.000 claims description 3
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- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 3
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- Electroplating Methods And Accessories (AREA)
Abstract
The invention provides a tin-graphene composite brush plating solution and a preparation method of an aluminum substrate surface plating layer, and belongs to the technical field of metal surface treatment. The tin-graphene composite brush plating solution provided by the invention comprises the following components: 20-40 g/L of soluble stannous salt, 0.1-0.5 g/L of graphene, 50-80 g/L of sulfuric acid, 60-80 g/L of pH stabilizer, 2-8 g/L of chelating agent, 1-2 g/L of surfactant, 1-2 g/L of antioxidant, 2-4 g/L of polar solvent and water. The plating layer prepared by the brush plating solution provided by the invention is uniform and smooth, has high adhesive force and excellent conductivity and wear resistance, and can reduce friction heat.
Description
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to a tin-graphene composite brush plating solution and a preparation method of an aluminum substrate surface plating layer.
Background
Tribology is a scientific technology for researching the interaction surface of relative motion in friction and abrasion processes and related theories and practices, and with the rapid development of scientific technology, the use conditions of friction pairs are increasingly harsh and complicated. Among them, current-carrying friction is also of increasing interest. The current-carrying frictional wear refers to the frictional wear behavior of the pair of grinding pairs in relative motion under electrical contact. The current-carrying frictional wear is mainly reflected in power transmission systems, railway traffic systems (high-speed rails, tramways and the like), industrial generators, electromagnetic track guns, rocket launching rectifying systems and the like. The aluminum alloy has the characteristics of low cost, light weight, high conductivity and the like, and is often used as an armature material for a current-carrying friction working condition. However, under the current-carrying friction working condition, the aluminum alloy armature can be subjected to mechanical abrasion, electrical abrasion and arc abrasion, and can generate huge temperature rise, so that the phenomenon of 'sticking aluminum' on the guide rail is easy to generate, and the service life of the guide rail is reduced. Before, many scholars at home and abroad are researching from the angle of enhancing the performance of the guide rail, and influence of the armature as a friction pair on the temperature rise of the guide rail and the phenomenon of aluminum sticking in the friction process is ignored.
In order to effectively solve or alleviate the problems, an aluminum armature coating is designed in the prior art, and the current-carrying friction performance of the aluminum armature can be optimized on the basis of not sacrificing the original good conductivity of the aluminum armature. For example, du Chuantong (Du Chuantong, lei Bin, lv Qingao, xing Yanchang, zhang Qian. Influence of graphene coating on sliding electrical contact performance of electromagnetic rail cannon [ J ]. Inset firing and control theory, 2018,39 (02): 1-5+3; lei Bin, du Chuantong, lv Qingao, zhang Qian, xing Yanchang. Experimental study of graphene coating influence on electromagnetic rail cannon performance [ J ]. High voltage technology, 2019,45 (06): 1929-1935.). Et al prepared graphene coating on armature surface by drop coating method using excellent mechanical, electrical and thermal properties of graphene, and analyzed the application of graphene coating on pivot rail interface by theoretical analysis simulation study and firing test. The results show that: the graphene coating is beneficial to improving the electric contact state between pivot rail interfaces and has good current passing capability. The graphene coating has positive effects on improving the relative speed of the armature and reducing the generation of heat between interfaces, and has the effects of arc ablation resistance and lubrication. However, the pure graphene coating has low bonding force with the matrix, is not wear-resistant, and is not suitable for engineering application. Meanwhile, graphene has a serious agglomeration problem and is difficult to uniformly disperse into a system, so that when a coating containing graphene is prepared on the surface of an aluminum base, a uniform coating cannot be obtained, and therefore, the aluminum alloy is difficult to obtain a good lubricating effect and has poor wear resistance.
Therefore, how to improve the binding force between the plating layer and the aluminum substrate, improve the conductivity and the wear resistance, and reduce the friction heat generation of the plating layer and the aluminum substrate is a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to provide a tin-graphene composite brush plating solution and a preparation method of an aluminum-based surface plating layer.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a tin-graphene composite brush plating solution, which comprises the following components: 20-40 g/L of soluble stannous salt, 0.1-0.5 g/L of graphene, 50-80 g/L of sulfuric acid, 60-80 g/L of pH stabilizer, 2-8 g/L of chelating agent, 1-2 g/L of surfactant, 1-2 g/L of antioxidant, 2-4 g/L of polar solvent and water.
Preferably, the saidThe soluble tin salt comprises SnSO 4 、SnCl 2 And Sn (NO) 3 ) 2 One of them.
Preferably, the graphene is a monolayer graphene powder.
Preferably, the pH stabilizer comprises one of ammonium sulfate, ammonium nitrate and ammonium chloride.
Preferably, the chelating agent comprises one of ethylenediamine tetraacetic acid, aminotriacetic acid and sodium potassium tartrate.
Preferably, the surfactant comprises one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and sodium fatty alcohol acyl sulfate.
Preferably, the antioxidant comprises one of ascorbic acid, tea polyphenol and tocopherol.
The invention also provides a preparation method of the aluminum-based surface coating, which comprises the following steps:
(1) Performing brush plating on the surface of an aluminum base body by adopting copper plating liquid to obtain a copper-plated aluminum base body;
(2) Performing electric brush plating on the surface of the pre-plated copper aluminum substrate obtained in the step (1) by adopting a tin-graphene composite brush plating solution to obtain an aluminum-based tin-graphene composite plating material; the tin-graphene composite brush plating solution is prepared by the technical scheme.
Preferably, in the step (2), the power supply voltage of the brush plating is 8-12V, and the time of the brush plating is 8-12 min.
Preferably, the relative speed of the brush plating in the step (2) is 10-15 m/min.
The invention provides a tin-graphene composite brush plating solution, which comprises the following components: 20-40 g/L of soluble stannous salt, 0.1-0.5 g/L of graphene, 50-80 g/L of sulfuric acid, 60-80 g/L of pH stabilizer, 2-8 g/L of chelating agent, 1-2 g/L of surfactant, 1-2 g/L of antioxidant, 2-4 g/L of polar solvent and water. The graphene in the brush plating solution provided by the invention has excellent conductivity and lubricating property, so that the obtained composite plating layer has excellent conductivity and lubricating property, meanwhile, the graphene can also play a role of refining grains, so that the plating layer has a more compact structure, and thus, the brush plating solution has excellent wear resistance, and the graphene also has excellent thermal conductivity, so that heat generated by friction can be rapidly dissipated, and the friction heat can be effectively reduced; the soluble tin salt is reduced into tin during brush plating, has the characteristics of soft texture, low melting point and good conductivity, can improve the lubrication effect of a coating, and can be melted into liquid state when the temperature is increased to form a liquid lubrication film, so that the temperature rise of a contact surface can be effectively reduced, and the wear resistance can be improved; the sulfuric acid and the antioxidant can avoid the oxidation of stannous ions, and the polar solvent and the surfactant sodium dodecyl sulfate can enable graphene to be dispersed in the brush plating solution more stably, so that the aggregation of graphene is reduced, the plating layer is more uniform and smooth, the adhesive force is higher, and the wear resistance is better.
The results of the examples show that the conductivity of the aluminum-based tin-graphene composite material obtained by brush plating the surface of the aluminum-based tin-graphene composite brush plating solution provided by the invention is 43-47% IACS, the friction coefficient is 0.18-0.24, and the wear rate is 4.29 multiplied by 10 -14 ～5.94×10 -14 m 3 And (3) the binding force of the tin-graphene composite coating and the aluminum substrate can reach 15.6-18.0 MPa, the binding force is high, the tin-graphene composite coating has compact structure, and the tin-graphene composite coating is firmly bonded on the surface of the aluminum substrate.
Drawings
FIG. 1 is a schematic structural diagram of an aluminum-based tin-graphene composite material prepared according to an application example of the invention;
fig. 2 is an SEM image of the tin-graphene composite plating layer of application example 2 of the present invention.
Detailed Description
The invention provides a tin-graphene composite brush plating solution, which comprises the following components: 20-40 g/L of soluble stannous salt, 0.1-0.5 g/L of graphene, 50-80 g/L of sulfuric acid, 60-80 g/L of pH stabilizer, 2-8 g/L of chelating agent, 1-2 g/L of surfactant, 1-2 g/L of antioxidant, 2-4 g/L of polar solvent and water.
The tin-graphene composite brush plating solution provided by the invention comprises 20-40 g/L of soluble stannous salt, preferably 20-40 g/L, more preferably 25-35 g/L, and most preferably 30g/L. The invention can utilize the soluble tin salt to reduce into tin during the electric brush plating by adding the soluble tin salt and controlling the concentration thereof within the range, has the characteristics of soft texture, low melting point and good conductivity, can improve the lubrication effect of the coating, can melt into liquid state when the temperature is increased, forms a liquid lubrication film, and can effectively reduce the temperature rise of a contact surface and improve the wear resistance.
In the present invention, the soluble tin salt preferably comprises SnSO 4 、SnCl 2 And Sn (NO) 3 ) 2 One of more preferably SnSO 4 。
The tin-graphene composite brush plating solution provided by the invention comprises 0.1-0.5 g/L of graphene, preferably 0.15-0.45 g/L, more preferably 0.2-0.4 g/L, and most preferably 0.3g/L. According to the invention, by adding graphene and controlling the concentration of the graphene within the range, the graphene can be utilized to have excellent conductivity and lubricating property, so that the obtained composite coating has excellent conductivity and lubricating property, meanwhile, the graphene can also play a role of refining grains, so that the coating structure is more compact, and thus, the composite coating has excellent wear resistance, and the graphene also has excellent thermal conductivity, so that heat generated by friction can be rapidly dissipated, and the friction heat can be effectively reduced.
In the present invention, the graphene is preferably a single-layer graphene powder. The invention is more beneficial to improving the conductivity and the lubricating property of the tin-graphene composite coating by selecting the single-layer graphene powder.
The tin-graphene composite brush plating solution provided by the invention comprises 50-80 g/L sulfuric acid, preferably 55-75 g/L sulfuric acid, more preferably 60-70 g/L sulfuric acid, and most preferably 65g/L sulfuric acid. The concentration of the sulfuric acid is controlled within the range, so that the tin-graphene composite brush plating solution is more favorable for obtaining good conductivity in the process of brush plating, and meanwhile, the tin-graphene composite brush plating solution is maintained under an acidic condition, and the oxidation of stannous ions and the oxidation of tin and graphene in a plating layer formed in the process of brush plating are more favorable for being avoided.
The tin-graphene composite brush plating solution provided by the invention comprises 60-80 g/L of pH stabilizer, preferably 62-78 g/L, more preferably 65-75 g/L, and most preferably 70g/L. The invention is more favorable for the stable maintenance of the composite brush plating liquid system in an acidic condition by adding the pH stabilizer and controlling the content thereof in the range, thereby being more favorable for the discharge crystallization of stannous ions on the surface of a negative electrode (workpiece) to form a uniform plating layer.
In the present invention, the pH stabilizer preferably includes one of ammonium sulfate, ammonium nitrate and ammonium chloride, and more preferably ammonium sulfate.
The tin-graphene composite brush plating solution provided by the invention comprises 2-8 g/L of chelating agent, preferably 3-7 g/L, more preferably 4-6 g/L, and most preferably 5g/L. The chelating agent is added and the concentration is controlled in the range, so that ions of other components can be complexed, the ion concentration in a system is stabilized, the ion concentration is stably changed in the brush plating reduction process, and the formed plating layer is more uniform and compact, and is more beneficial to improving the conductivity, lubricity and wear resistance of the plating layer.
In the present invention, the chelating agent preferably includes one of ethylenediamine tetraacetic acid, aminotriacetic acid and potassium sodium tartrate, more preferably ethylenediamine tetraacetic acid.
The tin-graphene composite brush plating solution provided by the invention comprises 1-2 g/L of surfactant, preferably 1.2-1.8 g/L, more preferably 1.4-1.6 g/L, and most preferably 1.5g/L. According to the invention, the surfactant is added and the concentration of the surfactant is controlled within the range, so that each component in the composite plating solution system can be uniformly dispersed, the aggregation of graphene is avoided, the formed uniform plating layer is uniform and compact, and the conductivity, the lubricity and the wear resistance of the plating layer are improved.
In the present invention, the surfactant preferably includes one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and sodium fatty alcohol acyl sulfate, and more preferably sodium dodecyl sulfate.
The tin-graphene composite brush plating solution provided by the invention comprises 1-2 g/L of antioxidant, preferably 1.2-1.8 g/L, more preferably 1.4-1.6 g/L, and most preferably 1.5g/L. The invention can avoid the oxidation of stannous ions and the oxidation of tin and graphene in a plating layer formed in the brush plating process by adding the antioxidant and controlling the concentration of the antioxidant in the range.
In the present invention, the antioxidant preferably includes one of ascorbic acid, tea polyphenol and tocopherol, more preferably ascorbic acid.
The tin-graphene composite brush plating solution provided by the invention comprises 2-4 g/L of polar solvent, preferably 2.2-3.8 g/L, more preferably 2.5-3.5 g/L and most preferably 3g/L. According to the invention, the graphene can be more stably dispersed in the brush plating solution by adding the polar solvent and controlling the concentration of the polar solvent within the range, so that the aggregation of the graphene is reduced, the plating layer is more uniform and smooth, the adhesive force is higher, and the wear resistance is better.
In the present invention, the polar solvent preferably includes one of N-methylpyrrolidone, dimethyl sulfoxide and N, N-dimethylformamide, more preferably N-methylpyrrolidone.
The tin-graphene composite brush plating solution provided by the invention comprises water.
In the present invention, the water content is preferably determined according to the pH value of the tin-graphene composite brush plating solution.
In the invention, the pH value of the tin-graphene composite brush plating solution is preferably 4-5. The pH value of the tin-graphene composite brush plating solution is controlled within the range, so that the tin-graphene composite brush plating solution is more favorable for obtaining good conductivity in the process of electric brush plating, and meanwhile, the tin-graphene composite brush plating solution is maintained under an acidic condition, so that oxidation of stannous ions and oxidation of tin and graphene in a plating layer formed in the electric brush plating process are more favorable for being avoided.
In the invention, the preparation method of the tin-graphene composite brush plating solution preferably comprises the following steps: and mixing the soluble stannous salt, graphene, sulfuric acid, a pH stabilizer, a chelating agent, a surfactant, an antioxidant, a polar solvent and water, and performing ultrasonic dispersion to obtain the tin-graphene composite brush plating solution.
The invention is more beneficial to improving the bonding force between the tin-graphene composite and the matrix, and the conductivity and the wear resistance by controlling the types and the mass concentration of each component of the tin-graphene composite brush plating solution.
The operation of mixing and ultrasonic dispersion is not particularly limited, and the uniformly dispersed tin-graphene composite brush plating solution can be obtained by adopting the operation of mixing and ultrasonic dispersion which is well known to the person skilled in the art. In the present invention, the time of the ultrasonic dispersion is preferably 25 to 35 minutes, more preferably 30 minutes.
The invention also provides a preparation method of the aluminum-based surface coating, which comprises the following steps:
(1) Performing brush plating on the surface of an aluminum base body by adopting copper plating liquid to obtain a copper-plated aluminum base body;
(2) Performing electric brush plating on the surface of the pre-plated copper aluminum substrate obtained in the step (1) by adopting a tin-graphene composite brush plating solution to obtain an aluminum-based tin-graphene composite plating material; the tin-graphene composite brush plating solution is prepared by adopting the technical scheme.
The invention adopts copper plating solution to carry out brush plating on the surface of an aluminum base body to obtain a copper-plated aluminum base body. According to the invention, copper plating is firstly carried out on the surface of the aluminum base, so that the binding force between the tin-graphene composite coating and the aluminum base can be effectively improved, the stripping caused by stress in a friction pair is avoided, and the abrasion resistance of the composite coating is improved.
In the present invention, the aluminum substrate is preferably subjected to a cleaning treatment and an activation treatment in this order before the brush plating.
In the invention, the cleaning treatment preferably comprises polishing, alkali washing, acid washing, ultrasonic treatment, electric cleaning oil removal and water washing which are sequentially carried out, and the polishing is preferably carried out by sequentially adopting 800# abrasive paper, 1000# abrasive paper and 1500# abrasive paper; the alkaline washing solvent is preferably 10% NaOH solution with mass concentration; the pickling solvent is preferably nitric acid solution with the mass concentration of 5-10%; the time of the alkali washing and the acid washing is independently preferably 1 to 5 minutes, more preferably 3 minutes; the solvent for ultrasonic cleaning is preferably absolute ethyl alcohol; the time of the ultrasonic cleaning is preferably 10 to 20 minutes, more preferably 15 minutes. In the invention, the power supply voltage of the electric clean degreasing is preferably 8-12V, more preferably 10V; the time for the electric cleaning degreasing is preferably 1 to 5min, more preferably 3min. The invention has no special requirements on the electro-cleaning degreasing liquid and the water washing operation of the electro-cleaning degreasing, and the electro-cleaning degreasing liquid and the water washing operation which are well known in the art can ensure that the aluminum substrate has good cleaning effect.
In the present invention, the activation treatment preferably includes a strong activation treatment and a weak activation treatment which are sequentially performed. The invention can effectively improve the activity of the surface of the aluminum matrix by carrying out strong activation treatment and weak activation treatment, and is more beneficial to improving the binding force between the composite coating and the surface of the aluminum matrix, thereby being more beneficial to improving the wear resistance of the composite coating.
In the present invention, the power supply voltage of the strong activation treatment is preferably 8 to 12V, more preferably 9 to 11V, and most preferably 10V; the time of the strong activation treatment is preferably 0.5 to 1.5min, more preferably 0.8 to 1.2min, and most preferably 1min; the relative speed of the strong activation treatment is preferably 12 to 15m/min, more preferably 13 to 14m/min.
The reagent used in the strong activation treatment is not particularly limited, and a commercially available strong activation treatment known to those skilled in the art may be used. In the present invention, the reagent used for the strong activation treatment is preferably a 2# activation solution.
In the present invention, it is preferable to wash the treated material with water after the completion of the strong activation treatment. The invention has no special requirement on the water washing operation, and the water washing operation well known by the person skilled in the art can ensure that the reagent subjected to the strong activation treatment is cleaned.
In the present invention, the power supply voltage of the weak activation treatment is preferably 6 to 8V, more preferably 7 to 8V, and most preferably 8V; the weak activation treatment time is preferably 2 to 3min, more preferably 2 to 2.5min, and most preferably 2min; the relative speed of the weak activation treatment is preferably 8 to 10m/min, more preferably 9m/min.
In the present invention, the weak activation treatment agent is preferably an aluminum activation solution. The aluminum activation liquid is not particularly required in the invention, and commercially available aluminum activation liquid well known to those skilled in the art can be used.
In the present invention, it is preferable to wash the treated material with water after the weak activation treatment is completed. The invention has no special requirement on the water washing operation, and the water washing operation well known by the person skilled in the art can ensure that the reagent subjected to weak activation is cleaned.
In the present invention, the plating pen is preferably replaced before the brush plating is performed on the surface of the aluminum substrate by using the copper plating solution. The invention is more beneficial to improving the cleanliness of the plating layer by replacing the electroplating pen, and avoids introducing other impurities into the plating layer.
In the present invention, when brush plating is performed on the surface of an aluminum substrate using a copper plating solution, the power supply voltage of the brush plating is preferably 9 to 12V, more preferably 10 to 11V, and most preferably 10V; the brush plating time is preferably 1 to 3 minutes, more preferably 2 minutes; the relative speed of the brush plating is preferably 6 to 8m/min, more preferably 7m/min.
The source of the copper plating solution is not particularly required, and the copper plating solution can be used for ensuring that a copper plating layer is preformed on the surface of an aluminum substrate by using commercially available copper plating solutions which are well known to a person skilled in the art.
After a copper-plated aluminum substrate is obtained, the tin-graphene composite brush plating solution is adopted to carry out brush plating on the surface of the copper-plated aluminum substrate, so that the aluminum-based tin-graphene composite plating material is obtained.
In the invention, the tin-graphene composite brush plating solution is prepared by adopting the technical scheme.
In the invention, the plating pen is preferably replaced before the tin-graphene composite brush plating solution is adopted to brush the surface of the copper-plated aluminum substrate. The invention is more beneficial to improving the cleanliness of the plating layer by replacing the electroplating pen, and avoids introducing other impurities into the plating layer.
In the invention, when the tin-graphene composite brush plating solution is adopted to carry out brush plating on the surface of the copper-plated aluminum substrate, the power supply voltage of the brush plating is preferably 8-12V, more preferably 9-11V, and most preferably 10V; the brush plating time is preferably 8 to 12 minutes, more preferably 9 to 11 minutes, and most preferably 10 minutes. The invention is more beneficial to improving the deposition efficiency and the deposition uniformity of the plating layer by controlling the power supply voltage and the electroplating time of the brush plating.
In the invention, when the tin-graphene composite brush plating solution is adopted to carry out brush plating on the surface of the copper-plated aluminum substrate, the relative speed of the brush plating is preferably 10-15 m/min, more preferably 11-14 m/min, and most preferably 12-13 m/min. The invention is more favorable for the stable and uniform deposition of the plating layer by controlling the relative speed of the brush plating in the range, so that the plating layer is more uniform and compact, and the conductivity and the wear resistance of the plating layer are more favorable to be improved.
The preparation method of the aluminum-based surface coating provided by the invention is simple and feasible, safe and effective, and the prepared graphene composite coating is uniform and compact, has high binding force with a substrate and excellent conductivity and wear resistance.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples
The compositions of the tin-graphene composite brush plating solutions provided in examples 1 to 4 are shown in table 1.
Table 1 the compositions of the tin-graphene composite brush plating solutions provided in examples 1 to 4
| Component (A) | Example 1 | Example 2 | Example 3 | Example 4 |
| Soluble stannous salt (stannous sulfate) | 30g/L | 40g/L | 20g/L | 40g/L |
| Graphene (Single-layer graphene powder) | 0.1g/L | 0.2g/L | 0.3g/L | 0.5g/L |
| Sulfuric acid | 60g/L | 50g/L | 50g/L | 80g/L |
| PH stabilizer (ammonium sulfate) | 70g/L | 80g/L | 60g/L | 80g/L |
| Chelating agent (ethylenediamine tetraacetic acid) | 5g/L | 6g/L | 2g/L | 8g/L |
| Surfactant (sodium dodecyl sulfate) | 1g/L | 1.5g/L | 1.5g/L | 2g/L |
| Antioxidant (ascorbic acid) | 1.5g/L | 2g/L | 1g/L | 2g/L |
| Polar solvent (N-methylpyrrolidone) | 2g/L | 3g/L | 3g/L | 4g/L |
| Water and its preparation method | -- | -- | -- | -- |
The preparation methods of the tin-graphene composite brush plating solution provided in examples 1 to 4 are the same, and specifically comprise the following steps: the soluble stannous salt, graphene, sulfuric acid, a pH stabilizer, a chelating agent, a surfactant, an antioxidant and a polar solvent were mixed and then subjected to ultrasonic dispersion for 30min, to obtain a total of 4 groups of tin-graphene composite brush plating solutions (ph=4) of examples 1 to 4.
Application example
The 4 groups of tin-graphene composite brush plating solutions in the examples 1-4 are subjected to brush plating on the surface of an aluminum base to prepare an aluminum base tin-graphene composite material, and the specific preparation method is as follows:
(1) Cleaning treatment of aluminum alloy:
the 6061 aluminum alloy surface is polished by using No. 800, no. 1000 and No. 1500 sand paper, then is soaked in a 10 mass percent NaOH solution and a 10 mass percent nitric acid solution for 3 minutes respectively, and is then soaked in absolute ethyl alcohol for ultrasonic cleaning for 15 minutes.
Electric cleaning and degreasing: the pretreated aluminum alloy is connected with the negative electrode of a power supply, the plating pen is connected with the positive electrode, the voltage is 10V, the electro-hydraulic electro-cleaning oil is used for removing the oil for 3 minutes, the relative speed is 8m/min, and the cleaning water is used for flushing.
(2) Aluminum alloy activation treatment
Strong activation treatment: the aluminum alloy is connected with the positive electrode of a power supply, the plating pen is connected with the negative electrode, the voltage is 10V, the activation is carried out by using 2# activating solution for 1 minute, the relative speed is 12m/min, and the cleaning is carried out.
Weak activation treatment: the aluminum alloy is connected with the negative electrode of the power supply, the plating pen is connected with the positive electrode, the voltage is 8V, the aluminum activation liquid is used for weak activation for 2 minutes, the relative speed is 10m/min, and the aluminum alloy is cleaned by clean water.
(3) Copper plating: and (3) maintaining connection in the weak activation step, replacing brush plating copper liquid for a plating pen, and pre-plating copper for 2 minutes at the voltage of 10V and the relative speed of 8m/min.
(4) Brush tin plating-graphene composite plating layer: and (3) keeping weak activation wiring, replacing a plating pen, and respectively performing brush plating by using the tin-graphene composite brush plating prepared in the examples 1-4, wherein the voltage is 10V, the brush plating time is 10 minutes, and the relative speed is 15m/min, so that four groups of aluminum-based tin-graphene composite materials in the application examples 1-4 are respectively obtained.
Comparative example
6061 aluminum alloy subjected to cleaning treatment only.
1. Conductivity test
Four groups of aluminum-based tin-graphene composite materials prepared in the above-mentioned application examples 1 to 4 and the aluminum alloy of comparative example 1 were respectively subjected to conductivity tests, and the test results are shown in table 2.
Table 2 conductivity of aluminum-based tin-graphene composite materials and comparative aluminum alloys of application examples 1 to 4 in total
| Application example | Conductivity of electric conductivity |
| Application example 1 | 45％IACS |
| Application example 2 | 47％IACS |
| Application example 3 | 43％IACS |
| Application example 4 | 46％IACS |
| Comparative example | 43％IACS |
As shown in Table 2, the conductivity of the aluminum-based tin-graphene composite material prepared by the graphene composite brush plating solution provided by the invention is 43-47% IACS, and the aluminum-based tin-graphene composite material can achieve the same conductivity as the aluminum alloy or even higher conductivity.
2. Wear resistance test
The four groups of aluminum-based tin-graphene composite materials prepared in the above-mentioned application examples 1 to 4 and the aluminum alloy of comparative example 1 were subjected to wear resistance test, and the test results are shown in table 3.
Table 3 wear resistance of aluminum-based tin-graphene composites of four groups of application examples 1 to 4 and comparative aluminum alloys
As can be seen from Table 3, the tin-graphene composite brush plating solution provided by the invention is preparedThe friction coefficient of the aluminum-based tin-graphene composite material is 0.18-0.24, and the wear rate is 4.29 multiplied by 10 -14 ～5.94×10 -14 m 3 The friction coefficient and the wear rate of the surface of the aluminum alloy are obviously lower than those of the surface of the aluminum alloy, and therefore, the aluminum-based tin-graphene composite material prepared by the tin-graphene composite brush plating solution provided by the invention has excellent lubricity and wear resistance.
3. Coating binding force test
Table 4 application examples 1-4 four groups of aluminum-based tin-graphene composite coating bonds
| Application example | Coating binding force |
| Application example 1 | 17.7MPa |
| Application example 2 | 18.0MPa |
| Application example 3 | 15.6MPa |
| Application example 4 | 17.0MPa |
As can be seen from Table 4, the bonding force between the tin-graphene composite coating and the aluminum substrate provided by the invention can reach 15.6-18.0 MPa, and the bonding force is high.
Fig. 1 is a schematic structural diagram of an aluminum-based tin-graphene composite material prepared by application example of the invention. As can be seen from FIG. 1, the invention is characterized in that the copper layer is pre-plated on the surface of the substrate, and then the tin-graphene composite plating layer is plated on the surface of the copper layer, so that the bonding force between the plating layer and the substrate is higher under the composite structure, and the wear resistance is excellent.
Fig. 2 is an SEM image of the aluminum-based tin-graphene composite material of application example 2 of the present invention. As can be seen from fig. 2, the tin-graphene composite coating is uniform and compact as a whole, and is flat and continuous.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (8)
1. The preparation method of the aluminum-based surface coating comprises the following steps:
(1) Performing brush plating on the surface of an aluminum base body by adopting copper plating liquid to obtain a copper-plated aluminum base body;
(2) Performing electric brush plating on the surface of the pre-plated copper aluminum substrate obtained in the step (1) by adopting a tin-graphene composite brush plating solution to obtain an aluminum-based tin-graphene composite plating material;
the tin-graphene composite brush plating solution comprises the following components: 20-40 g/L of soluble stannous salt, 0.1-0.5 g/L of graphene, 50-80 g/L of sulfuric acid, 60-80 g/L of pH stabilizer, 2-8 g/L of chelating agent, 1-2 g/L of surfactant, 1-2 g/L of antioxidant, 2-4 g/L of polar solvent and water;
the graphene is single-layer graphene powder;
the pH value of the tin-graphene composite brush plating solution is 4-5;
the polar solvent is selected from one of N-methyl pyrrolidone, dimethyl sulfoxide and N, N-dimethylformamide.
2. The tin-graphene composite brush plating solution according to claim 1, wherein said soluble stannous salt is selected from one of SnSO4, snCl2 and Sn (NO 3) 2.
3. The tin-graphene composite brush plating solution according to claim 1, wherein the pH stabilizer is selected from one of ammonium sulfate, ammonium nitrate and ammonium chloride.
4. The tin-graphene composite brush plating solution according to claim 1, wherein the chelating agent is one selected from ethylenediamine tetraacetic acid, aminotriacetic acid and sodium potassium tartrate.
5. The tin-graphene composite brush plating solution according to claim 1, wherein the surfactant is selected from one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and sodium fatty alcohol acyl sulfate.
6. The tin-graphene composite brush plating solution according to claim 1, wherein said antioxidant is selected from one of ascorbic acid, tea polyphenol and tocopherol.
7. The method according to claim 1, wherein the power supply voltage of the brush plating in the step (2) is 8 to 12V, and the time of the brush plating is 8 to 12min.
8. The method according to claim 1, wherein the relative speed of brush plating in the step (2) is 10 to 15m/min.
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