CN114854237B - Method for inhibiting oxidation of MXene nano material and application of MXene nano material in anticorrosive paint - Google Patents
Method for inhibiting oxidation of MXene nano material and application of MXene nano material in anticorrosive paint Download PDFInfo
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- CN114854237B CN114854237B CN202210386187.8A CN202210386187A CN114854237B CN 114854237 B CN114854237 B CN 114854237B CN 202210386187 A CN202210386187 A CN 202210386187A CN 114854237 B CN114854237 B CN 114854237B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/10—Metal compounds
- C08K3/14—Carbides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
Abstract
The invention relates to an anti-corrosion nano filler, in particular to a method for inhibiting oxidation of an MXene nano material and application of a stable material obtained as the anti-corrosion nano filler in a polymer coating. And forming a protective layer on the surface of the MXene nano-sheet so as to keep the complete two-dimensional sheet structure of the MXene nano-material and inhibit oxidation. The resulting non-oxidized MXene nanoplatelets having a defect-free, platelet-like structure were used as corrosion-resistant nanofillers in polymeric coatings to develop long-term corrosion-resistant coatings on metallic structures. Thus, oxidation of the MXene nanoplatelets is inhibited by covalent functionalization with alkoxysilanes or hybridization with graphene-based nanomaterials, while improving the dispersion quality of the MXene nanoplatelets in the polymer matrix. The modified MXene-based nano-sheet is used as nano-filler in a polymer coating, and can exert long-acting corrosion resistance in a polymer matrix.
Description
Technical Field
The invention relates to an anti-corrosion nano filler, in particular to a method for inhibiting oxidation of an MXene nano material and application of a stable material obtained as the anti-corrosion nano filler in a polymer coating.
Background
MXene is a two-dimensional transition metal carbide, nitride or carbonitride of the formula M n+1 AX n (n=1, 2, 3), where M is a transition metal (e.g., titanium), a is a group IIIA or IV element (e.g., aluminum), and X is a carbon atom or a nitrogen atom. MXene can be synthesized by chemical etching of the "a" element in a compound of MAX phase crystal structure. As a result of this process, the MAX phase will recrystallize to 3D M n+1 X n The MXene was converted to a exfoliated two-dimensional platelet morphology and hexagonal crystallinity by vigorous stirring and centrifugation.
The MXene nano-sheet has the potential of developing an anti-corrosion nano-composite polymer coating and can effectively block the diffusion path of corrosive ions in a coating matrix. Meanwhile, the surface of the MXene has hydrophilic functional groups (such as-F, -OH and=O) so as to have high hydrophilicity, which is comparable with other two-dimensional hydrophobic materials such as graphene, and the aqueous dispersion of the MXene nano material can be uniformly dispersed in the polymer composite material. However, MXene is extremely susceptible to oxidative degradation due to exposure to air or water, making it the greatest challenge for widespread use.
In fact, MXene has excellent dispersibility in aqueous solutions because oxygen and water molecules in the solution readily react with hydroxyl groups on the surface of MXene, and oxidative degradation occurs. Due to the oxidation problem of MXene, MXene is converted into metal oxide particles (TiO 2 ) And the flakes will break down from the edges into small pieces. However, the two-dimensional structure of MXene, having a large surface area, is an important feature in achieving high barrier properties in corrosion resistant nanocomposite polymer coatings, which can be greatly impaired by oxidation reactions.
Although oxidation of MXene nanoplatelets can be suppressed by removing dissolved oxygen as a main oxidation source, controlling the time of storing MXene in an inert atmosphere, or storing at a lower temperature, etc., MXene nanoplatelets still undergo rapid oxidative decomposition once put into use, thereby affecting the characteristics of the material thereof. Thus, the use of stable MXene nanomaterials in polymeric coatings still presents some challenges.
Disclosure of Invention
The invention aims at a method for inhibiting oxidation of MXene nano-materials and application of the stable materials as anti-corrosion nano-fillers in polymer coatings.
In order to achieve the above purpose, the invention adopts the technical scheme that:
a method for inhibiting the oxidation of an MXene nano material comprises the steps of forming a protective layer on the surface of an MXene nano sheet, and further keeping the complete two-dimensional sheet structure of the MXene nano material.
The method comprises the following steps: the MXene nano material is modified by a silane coupling agent, or is subjected to hybrid coating by adopting graphene-based nano sheets, and the modified MXene nano material is modified by the silane coupling agent after the coating.
The hybrid coating is to carry out covalent bond combination on the MXene nano material and the graphene nano material to obtain the graphene/MXene nano hybrid material.
Further, the weight ratio of the silane coupling agent to the MXene nanomaterial is 0.1-100, preferably 1-50, more preferably 10-20; carrying out covalent silane functionalization on the material; wherein the silane coupling agent is one or more of 3- (2-amino ethyl amino) propyl trimethoxy silane, 3-chlorpropyl trimethoxy silane, 3-mercapto propyl trimethoxy silane, 3-glycidol ether oxygen propyl triethoxy silane, 3-amino propyl triethoxy silane, 3-iodophenyl trimethoxy silane, 3-bromopropyl trimethoxy silane, 3-trifluoro acetyl oxygen propyl trimethoxy silane, heptadecafluoro decyl triethoxy silane or 1H, 2H-perfluoro decyl triethoxy silane.
The covalent silane functionalization is performed at 60-100 ℃ for 6-24 hours, and is selected to inhibit the oxidation of MXene, provide a protective layer for MXene nanoplatelets, and improve the dispersion quality of the nanoplatelets in the polymer coating. Both of these factors can enhance the properties of the polymer coating by increasing the barrier properties of the polymer coating and the crosslink density of the polymer coating. The weight ratio of the silane coupling agent to the MXene-based nanomaterial can be selected to be within the range of 0.1-100.
The MXene nano material and the graphene-based nano material are mixed according to the weight ratio of 1:0.1-1:10 (preferably in the range of 1:0.1-1:5, more preferably in the range of 1:0.1-1:2) and carrying out the hydrothermal/solvothermal method to carry out covalent bonding, so as to obtain the graphene-based/MXene nano hybrid material, and then mixing the graphene-based/MXene nano hybrid material with a silane coupling agent according to the weight ratio of 1:0.5-1:5, carrying out covalent silane functionalization on the material; wherein the graphene-based nanomaterial is graphene or graphene oxide.
The hydrothermal/solvothermal reaction is carried out by heat-treating in stainless steel autoclave lined with polytetrafluoroethylene at 80-200 ℃ for 4-24 hours, preferably at 100-180 ℃ for 6-18 hours, and most preferably at 120-160 ℃ for 8-16 hours, washing the obtained product with deionized water and ethanol, and drying at 40-70 ℃.
Covalent hybrids of MXene nanoplatelets and graphene-based nanomaterials, the graphene nanoplatelets act as spacers between the MXene nanoplatelets to prevent their aggregation in the nanocomposite polymer matrix. In addition, graphene-based nanoplatelets can encapsulate the surface of the MXene nanoplatelets to reduce exposure to humidity/air and improve the chemical stability of MXene, the hybrids being further functionalized with an alkoxysilane.
The application of the stable MXene nano material prepared by the method is that the stable material is used as an anti-corrosion nano filler in a polymer coating.
A polymeric coating material, the stabilizing material prepared by the method being added to a polymeric matrix, wherein the stabilizing material comprises 0.005-5wt.%, preferably in the range of 0.05-2.5wt.%, more preferably in the range of 0.1-1wt.%, based on the mass of the polymeric matrix.
The polymer matrix consists of polymer resin, a curing agent, a filler and a solvent; the nano anti-corrosion filler is the stable material;
all materials added in the polymer matrix are commercially available, and the specific composition is added according to the recommended proportioning ratio of the product.
The MXene-based nanomaterial can be used as a corrosion-resistant nanofiller in a polymer coating to increase the useful life of the metal structure.
The stabilizing material is added into the polymer matrix by a solution mixing method to realize uniform dispersion of the nanofiller in the polymer matrix.
The solution mixing method is to add the materials into the medium solvent (water) to be uniformly dispersed into the solution, then to mix the solutions mutually, and to add the solution into the polymer matrix by a mechanical mixing method during mixing so as to realize the uniform dispersion of the nano filler in the coating matrix. The polymer matrix of the nanocomposite polymer coating may be selected from an aqueous or solvent-based polymer matrix of an epoxy coating system or an epoxy modified polydimethylsiloxane coating system.
The polymer coating material is directly applied to a metal structure to form a nano composite coating to carry out corrosion protection on the metal structure.
However, the optimal amount of MXene-based nanoplatelets can be selected according to the desired characteristics, polymer matrix, modifier, and other optional components of the coating. The composition may also include dispersants, defoamers, stabilizers, bactericides, and other fillers or pigments. The nanocomposite composition can be applied to a surface by brushing, spraying, dipping, spin coating, or powder coating to form a uniform coating.
The resulting coating described above has a nanocomposite polymer coating that enhances corrosion protection of the metal structure, consisting of polymer (resin and its hardener) and MXene-based nanofillers and other desired pigments.
In nanocomposite coating embodiments, MXene nanoplatelets are selected as corrosion-resistant two-dimensional nanofillers. In these embodiments, the MXene nanoplatelets should be protected from oxidation and degradation by exposure to moisture or water, thereby enhancing corrosion of the polymer coating using MXene nanoplatelets having a defect-free two-dimensional platelet morphology and no significant oxidation.
The invention has the advantages that:
the invention improves the oxidation condition of MXene and maintains the chemical stability thereof by a chemical modification method so as to promote the application of the MXene in nano composite polymer coating. The resulting nanocomposite polymer coating incorporates a stable MXene nanomaterial obtained by coating the surface and edges of MXene with an appropriate chemical agent that prevents oxidation of MXene and promotes dispersibility of MXene in the polymer coating, preventing oxidation and degradation of MXene nanoplatelets due to exposure to moisture or water.
The obtained stable MXene nano material is modified by a silane coupling agent, so that the MXene is oxidized, and the dispersion quality of the nano sheet in the polymer coating is improved. It is used to enhance the barrier properties of the polymer coating and the crosslink density of the polymer coating to enhance the properties of the polymer coating.
Meanwhile, the MXene nanometer is further hybridized before being modified by a silane coupling agent, namely the hybrid of the MXene nanometer sheet and the graphene-based nanometer material. The graphene nanoplatelets act as spacers between the MXene nanoplatelets to prevent their aggregation in the nanocomposite polymer matrix. In addition, graphene-based nanoplatelets can encapsulate the surface of the MXene nanoplatelets to reduce exposure to humidity/air and improve the chemical stability of the MXene, the hybrids are further functionalized modified with an alkoxysilane to inhibit oxidation and self-stacking of the MXene nanoplatelets, thereby obtaining a stable MXene nanomaterial that also improves the barrier properties of the polymer coating and the crosslinking density of the polymer coating to enhance the properties of the polymer coating.
Drawings
FIG. 1 (a) is a transmission electron microscope image of a fresh MXene nanoplatelet;
FIG. 1 (b) is a transmission electron microscope image of the modified MXene nanoplatelets.
FIG. 2 is a Bode plot of an example of the present invention showing the immersion of a pure epoxy coating and a F-MXene nanomaterial loaded composite resin coating in a 3.5wt.% sodium chloride solution for various times.
FIG. 3 is a transmission electron microscope image before and after modification of GO@MXene nano-hybrids provided by an embodiment of the invention, wherein FIG. (a) is a transmission electron microscope image before modification of GO@MXene nano-hybrids; and (b) is a transmission electron microscope image after GO@MXene nano hybrid modification.
Fig. 4 is a Bode plot of an example of the present invention provided with a pure epoxy coating and a F-go@mxene nanomaterial loaded composite resin coating immersed in a 3.5wt.% sodium chloride solution for different times.
FIG. 5 shows the corrosion resistance of a pure epoxy coating and a composite resin coating loaded with F-GO@MXene nanomaterial after 30 days in an accelerated salt spray test chamber provided by an embodiment of the invention.
FIG. 6 is a test of adhesion of a pure epoxy coating and a composite resin coating loaded with F-GO@MXene nanomaterial provided by an embodiment of the present invention.
Detailed Description
The following description of the embodiments of the present invention is further provided in connection with the accompanying examples, and it should be noted that the embodiments described herein are for the purpose of illustration and explanation only, and are not limiting of the invention.
The stable MXene nano material obtained by the invention can prevent the oxidation of MXene and the dispersibility of MXene in the polymer coating in different ways, so that the barrier property and corrosion resistance of the polymer coating are enhanced, and the long-term corrosion protection of a metal structure is realized.
In particular, the modification thereof with silane coupling agents, in particular the-OH and-O functional groups of the MXene surface, are reaction sites that form bonds on the surface and edges of MXene by reaction with chemical reagents, while alkoxysilanes are suitable candidates for covalent surface functionalization of MXene nanoplatelets. The alkoxy groups are converted to silanol (Si-OH) groups under hydrolysis, which can form chemical bonds with hydroxyl groups on the surface of the MXene nanoplatelets, forming an organic-inorganic hybrid material that can inhibit oxidation of fresh MXene nanoplatelets and increase adhesion of MXene to organic polymers. At the same time, the condensation reaction between silanol groups results in the formation of crosslinked Si-O-Si bonds.
In addition, the MXene nano-sheets and graphene-based nano-materials (such as graphene and graphene oxide) are subjected to covalent hybridization and then subjected to alkoxysilane functionalization, wherein the chemical stability of the MXene nano-sheets is obviously improved due to the existence of the graphene-based materials, and the stacking of the MXene nano-sheets is prevented by the existence of the graphene-based nano-materials.
Example 1
Fresh MXene nanoplatelets (transmission electron microscopy image as shown in FIG. 1 (a)) were prepared by dispersing 0.5g MXene in 95mL:5mL toluene: and (3) continuously stirring the solution of the 3-aminopropyl triethoxysilane for 12 hours at 80 ℃ under a reflux system to obtain the silane functionalized MXene nano material (F-MXene), as shown in the figure 1 (b).
0.1g of the silane functionalized MXene nano-sheet is added into 40g of Epoxy resin (MU-618) and is mixed with 20g of curing agent (CU-600) after being vigorously stirred at room temperature for 30min for full dispersion in a solution mixing mode, so that uniformly dispersed nano-composite coating (Epoxy/F-MXene) is obtained.
The epoxy resin is epoxy resin (MU-618) and curing agent (CU-600) which are purchased from Shanghai run carbon New Material technology Co.
The nanocomposite coating obtained above was applied on a Q235 steel substrate with a paint brush, cured at room temperature for 72 hours, then cured in an oven at 80 ℃ for 90 minutes, and then left for 7 days for electrochemical testing. The corrosion resistance of the coating was evaluated by the electrochemical workstation paramt4000+. Before the experiment, the sample is subjected to open circuit potential test in 3.5% NaCl solution, and after the open circuit potential is stabilized, the sample is subjected to electrochemical impedance spectrum test, wherein the frequency range is 105 Hz-0.01 Hz, and the amplitude of the alternating current sinusoidal disturbance signal is 20mV.
Meanwhile, a Pure Epoxy (PE) (epoxy (MU-618)) was used, and an electrochemical test was performed on a Q235 steel substrate as described above, as a control. (see FIG. 2).
As can be seen from fig. 2, it is shown that the composite coating loaded with fresh MXene nanoplatelets has a more excellent corrosion resistance compared to the pure epoxy sample.
Example 2
50mL of Graphene Oxide (GO) (10 mg/mL) was mixed with 20mL of ethanol, and after mixing and sonicated in a water bath for 60 minutes. Then, 50mL of a fresh aqueous MXene solution (10 mg/mL) was added to the mixture, and the mixture was magnetically stirred at room temperature for 1h. The resulting mixture was transferred to a 200mL polytetrafluoroethylene-lined autoclave and heated at 120 ℃ for 4 hours. Finally, the resulting solution was centrifuged and washed several times with water and ethanol, and freeze-dried to give the nanohybrids (go@mxene), as shown in fig. 3 (a).
Silane functionalization was performed by refluxing 0.5g of the nanohybrids in a mixture of 3-aminopropyl triethoxysilane (5 mL) and deionized water (95 mL) at 80 ℃ for 12 h. The reflux product was washed several times with absolute ethanol and deionized water and finally freeze-dried to obtain the modified nanohybrid (F-go@mxene) as shown in fig. 3.
As shown in fig. 3 (a), GO and MXene are tightly connected together, so that the fold structure of GO and the complete nanosheet structure of MXene can be clearly seen, and GO and MXene as two-dimensional nanomaterial have similar structural characteristics, and are easy to match and fuse with each other to form a strong interaction; panel (b) is a transmission electron microscopy image of F-GO@MXene, showing that silane functionalization does not alter the main morphology of GO@MXene, while the wrinkled structure of GO becomes less pronounced, the appearance of the nanohybrids darkens, which can be attributed to the modification of the surface silane agent.
Then, after 0.1wt.% of the modified nano-hybrid is mixed with 40g of Epoxy resin (MU-618) by means of solution, and vigorously stirred at room temperature for 30min to be fully dispersed, 20g of curing agent (CU-600) is added and mixed, and then the uniformly mixed nano-composite coating material (Epoxy/F-GO@MXene) is obtained.
The nanocomposite coating material obtained above was coated on a Q235 steel substrate with a paint brush, cured at room temperature for 72 hours, then cured in an oven at 80 ℃ for 90 minutes, and then subjected to electrochemical test after standing at room temperature for 7 days (see fig. 4).
Meanwhile, a Pure Epoxy (PE) (epoxy (MU-618)) was used, and an electrochemical test was performed on a Q235 steel substrate as described above, as a control.
As can be seen from fig. 4, the F-go@mxene nanohybrid loaded composite coating can provide superior corrosion resistance compared to the pure epoxy samples.
To further confirm the corrosion resistance, the nanocomposite coating formed by the nanocomposite coating material of example 2 described above and the coating formed by the pure epoxy resin were placed in an accelerated salt spray tank for 30 days, and the surface corrosion was observed (see fig. 5). As can be seen from fig. 5, the pure epoxy coating (PE) showed severe corrosion diffusion at day 30 on the coating surface, indicating failure of the coating; while the nanocomposite coating (Epoxy/F-GO@MXene) has no obvious corrosion diffusion condition, and still shows good corrosion resistance.
Finally, the adhesion strength of the coating on the steel substrate was tested by a drawing test for the two coatings, and the result is shown in fig. 6, which shows that the adhesion strength of the pure Epoxy coating (PE) to the steel plate is the lowest (3.7±0.2 MPa), while the adhesion strength of the nanocomposite coating (Epoxy/F-go@mxene) to the steel plate is 7.5±0.6MPa, indicating that adding silane functionalized nanomaterial into the polymer matrix is an effective method for improving the adhesion strength of the coating to the metal substrate.
Claims (6)
1. A method for inhibiting oxidation of an MXene nano material is characterized in that: forming a protective layer on the surface of the MXene nano material, so as to keep the complete two-dimensional lamellar structure of the MXene nano material and inhibit oxidation;
the preparation method comprises the steps of carrying out hybrid coating on an MXene nano material by adopting a graphene-based nano material, and modifying the MXene nano material by adopting a silane coupling agent after coating;
the hybrid coating is to carry out covalent bond combination on the MXene nano material and the graphene nano material to obtain a graphene/MXene nano hybrid material;
the MXene nano material and the graphene-based nano material are mixed according to the weight ratio of 1:0.1-1:10, carrying out covalent bond combination by a hydrothermal or solvothermal method to obtain the graphene-based/MXene nano hybrid material, and then mixing the graphene-based/MXene nano hybrid material with a silane coupling agent according to the weight ratio of 1:0.5-1:5, carrying out covalent silane functionalization on the material; wherein the graphene-based nanomaterial is graphene or graphene oxide;
the covalent silane is functionalized to reflux at 60-100 ℃ for 6-24 hours;
the hydrothermal or solvothermal reaction is to heat treat in a stainless steel autoclave lined with polytetrafluoroethylene at 80-200 ℃ for 4-24 hours.
2. The method of claim 1, wherein: the silane coupling agent and the MXene nano material are subjected to covalent silane functionalization according to the weight ratio of 0.1-100; wherein the silane coupling agent is one or more of 3- (2-amino ethyl amino) propyl trimethoxy silane, 3-chlorpropyl trimethoxy silane, 3-mercapto propyl trimethoxy silane, 3-glycidol ether oxygen propyl triethoxy silane, 3-amino propyl triethoxy silane, 3-iodophenyl trimethoxy silane, 3-bromopropyl trimethoxy silane, 3-trifluoro acetyl oxygen propyl trimethoxy silane, heptadecafluoro decyl triethoxy silane or 1H, 2H-perfluoro decyl triethoxy silane.
3. An application of the graphene-based/MXene nano hybrid material prepared by the method of claim 1, which is characterized in that: application of graphene-based/MXene nano hybrid material as anti-corrosion nano filler in polymer coating.
4. A polymeric coating material characterized by: the graphene-based/MXene nano-hybrid material prepared by the method of claim 1 is added to a polymer matrix, wherein the graphene-based/MXene nano-hybrid material occupies 0.005-5 wt% of the mass of the polymer matrix.
5. The polymeric coating material of claim 4, wherein: the graphene-based/MXene nano hybrid material is added into a polymer matrix through a solution mixing method so as to realize uniform dispersion of nano fillers in the polymer matrix.
6. The polymeric coating material of claim 4, wherein: the polymer coating material is directly applied to a metal structure to form a nano composite coating to carry out corrosion protection on the metal structure.
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