CN112708919A - Method for preparing aluminum-based composite coating by nano inorganic molten salt composite electrodeposition - Google Patents
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Abstract
The invention relates to the technical field of metal coating preparation by fused salt electrodeposition, in particular to a method for preparing an aluminum-based composite coating by nano inorganic fused salt composite electrodeposition, which comprises the following two steps: preparing solid NaCl and KCl mixed salt containing nano particles uniformly distributed; preparing an aluminum-based composite coating by carrying out composite electrodeposition on the obtained nano inorganic molten salt; the method for preparing the aluminum-based composite coating by the nano inorganic molten salt composite electrodeposition has the advantages that the obtained aluminum-based composite coating has high density and good bonding force with a substrate material, and solves the problems of serious dendritic crystal growth of the electrodeposited pure aluminum coating in the inorganic molten salt and the like.
Description
Technical Field
The invention relates to the technical field of metal coating preparation by fused salt electrodeposition, in particular to a method for preparing an aluminum-based composite coating by nano inorganic fused salt composite electrodeposition.
Background
Aluminum metal coatings have good corrosion resistance and are a common protective coating. The aluminum metal coating comprises a pure aluminum coating and an aluminum alloy coating, and compared with the aluminum alloy coating, the corrosion potential of the pure aluminum coating is obviously higher than that of the aluminum alloy, so that the aluminum metal coating has stronger corrosion resistance, good self-repairing capability and more excellent corrosion resistance in application environments such as atmosphere and ocean.
The electrodeposition method is the best choice for preparing pure aluminum coatings. At present, an electrolyte system adopted for preparing a pure aluminum coating by electrodeposition mainly comprises three types of organic solvents, organic molten salt and inorganic molten salt. Although the organic solvent electrolyte has high toxicity, is inflammable and explosive, is very sensitive to oxygen and water, and has extremely strict requirements on the operating environment, the organic solvent electrolyte is still adopted for electrodepositing the pure aluminum coating in the production practice. The main reason is that, although the potential window of the electrolyte of the organic molten salt (room temperature ionic solution) is wide and the viscosity of the electrolyte is low, the problems of expensive raw materials of the electrolyte, harsh operating environment, poor binding force between the obtained pure aluminum coating and the substrate material and the like still exist; for inorganic molten salts (mainly AlCl)3Inorganic fused salt based), although the electrolyte raw material cost is low, the equipment is simple, the operation condition is relatively loose compared with the organic electrolyte electrodeposition process, and the operation is safer, the inorganic fused salt based electrolyte has not been applied in production practice so far. The main reason is that the pure aluminum coating obtained by the electrodeposition of the inorganic molten salt has very serious dendritic crystal, which directly causes low current efficiency, poor surface appearance of the coating, loose internal structure and low bonding force with a substrate material, thus being incapable of being applied to practice.
Around the AlCl3The problems of serious dendritic crystal growth, loose interior, poor binding force and the like in the pure aluminum coating electrodeposited by the base inorganic molten salt are mainly solved by three methods: 1) preparing an aluminum alloy coating;2) adding a surfactant; 3) electrodeposition was performed using a periodically pulsed current. The preparation of the aluminum alloy coating requires that the deposition potentials of two metal ions are equal, and various complexing agents are generally added for adjustment, so that the fused salt electrodeposition process is difficult to control. Meanwhile, the corrosion resistance of the aluminum alloy coating is lower than that of a pure aluminum coating; the quality of the pure aluminum coating can be improved to a certain extent by adding surfactants such as urea and tetramethyl-ammonium chloride (TMA) and adopting pulse current electrodeposition, but the two methods have limited adjusting capability on the pure aluminum coating structure and can only be used as auxiliary means.
Although the pure aluminum coating electrodeposited in the inorganic molten salt has the advantages of low raw material cost, simplicity in operation, high safety and the like, the problem that the pure aluminum coating cannot be applied due to the fact that the aluminum dendrite grows seriously in the electrodeposition process and the surface appearance, the internal density and the adhesion force with a substrate of the pure aluminum coating are poor is solved by providing a new optimization measure.
In view of the above-mentioned drawbacks, the inventors of the present invention have finally obtained the present invention through a long period of research and practice.
Disclosure of Invention
The invention aims to solve the problems of serious dendritic crystal growth and the like of an electrodeposited pure aluminum coating in inorganic molten salt, and provides a method for preparing an aluminum-based composite coating by nano inorganic molten salt composite electrodeposition.
In order to realize the aim, the invention discloses a method for preparing an aluminum-based composite coating by nano inorganic molten salt composite electrodeposition, which comprises the following steps:
s1: preparing solid inorganic mixed salt containing nano particles: fully mixing NaCl and KCl inorganic salt, ball-milling to micron level, adding nano particles into the ball-milled NaCl and KCl mixed salt, wherein the addition amount of the nano particles is 40-60% of the total weight of the NaCl and KCl mixed salt, adding acetone liquid, performing ultrasonic dispersion for 1-3 hours, vacuumizing and heating in a vacuum drying oven at the heating temperature of 100-160 ℃ and the vacuum degree of 20-150 Pa, and performing vacuum heating treatment for 1-2 hours to obtain solid NaCl and KCl mixed salt with uniformly distributed nano particles;
s2: preparation of aluminum-based composite by nano inorganic fused salt composite electrodepositionCoating: mixing NaCl, KCl and AlCl3And (3) uniformly mixing inorganic salt, adding the mixture into a crucible, putting the crucible into an oil bath pan with high-purity argon protection and at the temperature of 160-190 ℃ for melting, adding the solid NaCl and KCl mixed salt with uniformly distributed nano particles prepared in the step S1 into the crucible, starting stirring after the mixture is completely melted, inserting a pure aluminum anode and a cathode to be deposited, and performing composite electrodeposition to prepare the aluminum-based composite coating.
The molar ratio of NaCl to KCl is 1: 1.
NaCl, KCl and AlCl3In a molar ratio of 17:17: 66.
The nano particles are carbides, nitrides, borides and silicides with certain conductivity. The conductivity of the nano particles is 1000-100000S/cm, and the size of the nano particles is 20-200 nm.
AlCl for composite electrodeposition3The concentration of the nano particles in the inorganic molten salt is 10-40 g/L.
In the composite electrodeposition process, the electrodeposition voltage is 0.1-0.4V, and the electrodeposition time is 10-50 min.
The cathode to be deposited is made of carbon steel, stainless steel and magnesium alloy material.
The stirring speed is 200-600 r/min, and the stirring mode is mechanical stirring or magnetic stirring.
The mass percentage of the nano particles in the aluminum-based composite coating prepared by the method is 2-10%, the density is 98-99.5%, and the bonding force with the substrate material is 30-80N.
Compared with the prior art, the invention has the beneficial effects that:
1. while the inorganic molten salt medium is used for dispersing the nano particles, magnetic stirring or mechanical stirring is adopted, so that the uniform dispersion of the nano particles in the inorganic molten salt medium can be further ensured, and the nano particles and aluminum ions can be conveniently deposited on the surface of a cathode together;
2. the aluminum-based composite coating with high density and good bonding force with a substrate material is obtained by directly adopting a small amount of nano particles and aluminum ions for composite deposition without alloying or adding an organic surfactant. In addition, the nano particles in the coating can further improve the mechanical properties such as hardness of the pure aluminum coating, thereby expanding the application range of the pure aluminum coating.
3. The equipment for preparing the aluminum-based composite coating by adopting the nano inorganic molten salt composite electrodeposition is convenient to operate, simple in process flow and low in cost.
Drawings
FIG. 1 is a SEM image of the cross section of an aluminum-based nano titanium carbide (average particle size of 50nm) composite coating;
FIG. 2 is Mapping of aluminum element and titanium element in the cross section of the aluminum-based nano titanium carbide (average particle size 50nm) composite coating;
FIG. 3 is an XRD analysis of an aluminum-based nano titanium carbide (average particle size 50nm) composite coating;
FIG. 4 is a TEM image of nano-titanium carbide in the aluminum-based nano-titanium carbide (average particle size 50nm) composite coating.
FIG. 5 is an SEM image of the surface of the aluminum-based nano tungsten carbide (average particle size of 150nm) composite coating.
Detailed Description
The above and further features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
Example 1
Fully mixing NaCl and KCl according to the molar ratio of 1:1, and putting the mixture into a planetary ball mill for ball milling to micron level. Adding titanium carbide with the average particle size of 50nm into the ball-milled NaCl-KCl mixed salt, wherein the weight of the nano titanium carbide is 45% of the total weight of the NaCl-KCl mixed salt, then adding acetone liquid, carrying out ultrasonic dispersion for 2 hours, then putting the mixture into a vacuum drying oven for heating, wherein the heating temperature is 130 ℃, the vacuum degree is 70Pa, and after carrying out vacuum heating treatment for 1.5 hours, completely volatilizing the acetone to obtain solid NaCl-KCl mixed salt with uniformly distributed nano particles; uniformly mixing NaCl, KCl and AlCl3 inorganic salts in a molar ratio of 17:17:66, adding the inorganic salts into a quartz crucible, melting the inorganic salts in an oil bath at 180 ℃ under the protection of high-purity argon, and filling the mixed salt containing the nano particles NaCl and KCl prepared in the first step into the quartz crucible after the inorganic salts are completely melted to ensure that the AlCl prepared finally3The concentration of nano particles in the nano inorganic molten salt is 30 g/L; argon shut-off after complete melting and stabilizationAnd gas, magnetic stirring is simultaneously applied, the stirring speed is 400r/min, then a pure aluminum anode and a 304 stainless steel cathode are inserted, composite electrodeposition is started, the electrodeposition voltage is 0.3V, the 304 stainless steel cathode is taken out after the electrolysis is finished with the electrodeposition time of 30min, and the aluminum-based nano composite coating with the nano particle mass percentage content of 4% is obtained.
As shown in fig. 1 to 4, fig. 1 is a cross-sectional SEM image of the composite coating obtained in the present embodiment, and it can be seen that the obtained composite coating has a dense cross section, a flat surface, and a tight bond with the substrate material; FIG. 2 is a Mapping diagram of aluminum and titanium in the cross section of the composite coating obtained in the example, wherein the distribution of the aluminum and titanium in the composite coating is very uniform, which shows that titanium boride nanoparticles can be uniformly distributed in an aluminum substrate; fig. 3 is an XRD analysis result of the composite coating obtained in this example, from fig. 3, it can be known that the existence form of the titanium element in the composite coating is in the form of a titanium boride compound, and fig. 4 is a TEM image of the nano titanium carbide in the composite coating obtained in this example. As can be seen from FIG. 4, the titanium boride compound present in the composite coating layer still remains in the form of nanoparticles, the size of which is about 50 nm.
Example 2
Fully mixing NaCl and KCl according to the molar ratio of 1:1, and putting the mixture into a planetary ball mill for ball milling to micron level. Adding tungsten carbide with the average particle size of 150nm into ball-milled NaCl and KCl mixed salt, wherein the weight ratio of the nano tungsten carbide is 40% of the total weight of the NaCl and KCl mixed salt, then adding acetone liquid, carrying out ultrasonic dispersion for 2 hours, then putting the mixture into a vacuum drying oven for heating, wherein the heating temperature is 150 ℃, the vacuum degree is 100Pa, and after carrying out vacuum heating treatment for 1.8 hours, completely volatilizing the acetone to obtain solid NaCl and KCl mixed salt with uniformly distributed nano particles; NaCl, KCl and AlCl in a molar ratio of 17:17:663Inorganic salt is evenly mixed and added into a quartz crucible, the mixture is melted in an oil bath kettle at the temperature of 180 ℃ under the protection of high-purity argon, and after the mixture is completely melted, the mixed salt containing the nano particle NaCl and the KCl prepared in the first step is filled into the quartz crucible to ensure that the finally prepared AlCl3The concentration of nano particles in the nano inorganic molten salt is 25 g/L; after complete melting and stabilization, argon is turned off, and mechanical stirring and stirring are simultaneously appliedAnd (3) at the speed of 500r/min, inserting a pure aluminum anode and an AZ91D magnesium alloy cathode, starting composite electrodeposition, wherein the electrodeposition voltage is 0.35V, and taking out the AZ91D magnesium alloy cathode after the electrodeposition time is 30min, so as to obtain the aluminum-based nano composite coating with the nano particle mass percentage of 6%.
Fig. 5 is an SEM image of the surface of the composite coating obtained in this example, and it can be seen from fig. 5 that the carbide nanoparticles can be co-deposited with aluminum and uniformly distributed on the surface of the aluminum metal, and the surface of the obtained composite coating is flat and has no dendrite.
Example 3
Fully mixing NaCl and KCl according to the molar ratio of 1:1, and putting the mixture into a planetary ball mill for ball milling to micron level. Adding molybdenum silicide with the average particle size of 50nm into the ball-milled NaCl-KCl mixed salt, wherein the weight ratio of the molybdenum silicide is 55% of the total weight of the NaCl-KCl mixed salt, then adding acetone liquid, performing ultrasonic dispersion for 1.5h, then putting the mixture into a vacuum drying oven to be heated, wherein the heating temperature is 120 ℃, the vacuum degree is 120Pa, and after vacuum heating treatment is carried out for 2 hours, completely volatilizing the acetone to obtain solid NaCl-KCl mixed salt with uniformly distributed nano particles; NaCl, KCl and AlCl in a molar ratio of 17:17:663Inorganic salt is evenly mixed and added into a quartz crucible, the mixture is melted in an oil bath kettle at the temperature of 190 ℃ under the protection of high-purity argon, and after the mixture is completely melted, the mixed salt containing the nano particle NaCl and the KCl prepared in the first step is filled into the quartz crucible to ensure that the AlCl prepared finally3The concentration of nano particles in the nano inorganic molten salt is 38 g/L; and (3) closing argon after complete melting and stabilization, simultaneously applying magnetic stirring at the stirring speed of 450r/min, inserting a pure aluminum anode and a Q235 low-carbon steel cathode, starting composite electrodeposition, wherein the electrodeposition voltage is 0.3V, and taking out the Q235 low-carbon steel cathode after the electrodeposition time is 30min, and thus obtaining the aluminum-based nano composite coating with the nano particle mass percentage of 7%.
The foregoing is merely a preferred embodiment of the invention, which is intended to be illustrative and not limiting. It will be understood by those skilled in the art that various changes, modifications and equivalents may be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for preparing an aluminum-based composite coating by nano inorganic molten salt composite electrodeposition is characterized by comprising the following steps:
s1: preparing solid inorganic mixed salt containing nano particles: fully mixing NaCl and KCl inorganic salt, ball-milling to micron level, adding nano particles into the ball-milled NaCl and KCl mixed salt, wherein the addition amount of the nano particles is 40-60% of the total weight of the NaCl and KCl mixed salt, adding acetone liquid, performing ultrasonic dispersion for 1-3 hours, vacuumizing and heating in a vacuum drying oven at the heating temperature of 100-160 ℃ and the vacuum degree of 20-150 Pa, and performing vacuum heating treatment for 1-2 hours to obtain solid NaCl and KCl mixed salt with uniformly distributed nano particles;
s2: preparing the aluminum-based composite coating by nano inorganic molten salt composite electrodeposition: mixing NaCl, KCl and AlCl3And (3) uniformly mixing inorganic salt, adding the mixture into a crucible, putting the crucible into an oil bath pan with high-purity argon protection and at the temperature of 160-190 ℃ for melting, adding the solid NaCl and KCl mixed salt with uniformly distributed nano particles prepared in the step S1 into the crucible, starting stirring after the mixture is completely melted, inserting a pure aluminum anode and a cathode to be deposited, and performing composite electrodeposition to prepare the aluminum-based composite coating.
2. The method for preparing the aluminum-based composite coating by the nano inorganic molten salt composite electrodeposition as claimed in claim 1, wherein the molar ratio of NaCl to KCl in the step S1 is 1: 1.
3. The method for preparing the aluminum-based composite coating by the nano inorganic molten salt composite electrodeposition as claimed in claim 1, wherein NaCl, KCl and AlCl are adopted in the step S23In a molar ratio of 17:17: 66.
4. The method for preparing the aluminum-based composite coating by the nano inorganic molten salt composite electrodeposition as claimed in claim 1, wherein the nano particles in the step S1 are carbides, nitrides, borides and silicides with certain electrical conductivity. The conductivity of the nano particles is 1000-100000S/cm, and the size of the nano particles is 20-200 nm.
5. The method for preparing the aluminum-based composite coating by the nano inorganic molten salt composite electrodeposition as claimed in claim 1, wherein the AlCl adopted in the composite electrodeposition in the step S23The concentration of the nano particles in the inorganic molten salt is 10-40 g/L.
6. The method for preparing the aluminum-based composite coating by the composite electrodeposition of the nano inorganic molten salt according to claim 1, wherein the electrodeposition voltage in the composite electrodeposition process in the step S2 is 0.1-0.4V, and the electrodeposition time is 10-50 min.
7. The method for preparing the aluminum-based composite coating by the composite electrodeposition of the nano inorganic molten salt according to claim 1, wherein the cathode to be deposited in the step S2 is carbon steel, stainless steel or magnesium alloy material.
8. The method for preparing the aluminum-based composite coating by the nano inorganic molten salt composite electrodeposition as claimed in claim 1, wherein the stirring speed adopted in the step S2 is 200 to 600 r/min.
9. The method for preparing the aluminum-based composite coating by the nano inorganic molten salt composite electrodeposition as claimed in claim 6, wherein the stirring manner in the step S2 is mechanical stirring or magnetic stirring.
10. An aluminum-based composite coating, which is characterized by being prepared by the method for preparing the aluminum-based composite coating through the nano inorganic molten salt composite electrodeposition according to any one of claims 1 to 9, wherein the mass percentage of nano particles in the aluminum-based composite coating is 2-10%, the density of the nano particles is 98-99.5%, and the bonding force between the nano particles and a substrate material is 30-80N.
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| CN114934297A (en) * | 2022-05-23 | 2022-08-23 | 安徽工业大学 | Method for preparing aluminum-based composite material by composite electrodeposition in aluminum electrolyte containing nanoparticles |
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