CN113773709A - Self-warning and self-repairing dual-functional coating based on natural polyphenol filler and preparation - Google Patents
Self-warning and self-repairing dual-functional coating based on natural polyphenol filler and preparation Download PDFInfo
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- CN113773709A CN113773709A CN202111033093.4A CN202111033093A CN113773709A CN 113773709 A CN113773709 A CN 113773709A CN 202111033093 A CN202111033093 A CN 202111033093A CN 113773709 A CN113773709 A CN 113773709A
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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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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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
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2202/00—Metallic substrate
- B05D2202/10—Metallic substrate based on Fe
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2502/00—Acrylic polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2503/00—Polyurethanes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2504/00—Epoxy polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2506/00—Halogenated polymers
- B05D2506/10—Fluorinated polymers
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Abstract
The invention discloses a self-warning and self-repairing dual-functional coating based on natural polyphenol fillers and a preparation method thereof. The method comprises the steps of firstly preparing the mesoporous silica nano-carrier loaded with natural polyphenols, then adding the mesoporous silica nano-carrier into resin according to a certain proportion, uniformly mixing the mesoporous silica nano-carrier with the resin, and finally constructing the intelligent coating with the double functions of self-warning and self-repairing on the surface of steel. When the coating is damaged, the natural polyphenols are released from the mesoporous silica carrier and undergo a complexing reaction with ferric ions generated when the substrate is corroded to generate macroscopic color change, so that the damage of the coating is indicated and the occurrence of metal corrosion is warned; at the same time, the complex is deposited on the metal surface, inhibiting further progress of the corrosion reaction. The intelligent coating has the double effects of self-warning and self-repairing, and has the advantages of simple preparation process and wide application prospect.
Description
Technical Field
The invention relates to a self-warning and self-repairing dual-functional coating based on natural polyphenol fillers and a preparation method thereof, belonging to the field of anticorrosive coating materials.
Background
The corrosion is an important factor causing serious degradation of the structure and the function of the metal material, seriously threatens the service safety of the metal structure and the facility and the smooth operation of the production and living order, and causes immeasurable economic loss to human society and natural environment. One of the most common corrosion protection strategies is corrosion protection coatings, however, in severe service environments, the coatings are highly susceptible to damage, even nano-or micro-cracks or micro-defects, which further cause local damage and even deterioration of the integrity of the coatings, resulting in corrosion. Therefore, early monitoring of the coating for damage and initiation of corrosion is essential. To address this problem, researchers have proposed the concept of self-warning coatings. A fluorescent compound or color-changing dye having a response characteristic to a corrosion-induced environmental change is introduced into the coating, and when the coating is damaged, local fluorescence or color change occurs at the damaged site, thereby identifying active corrosion sites before corrosion products are observed. In addition to early warning of coating damage, it is also important to repair coating damage. The self-repairing substance is added into the coating, so that the coating can realize the double functions of self-warning and self-repairing, and is favorable for timely sending out corrosion warning and effectively inhibiting the further development of corrosion activity before the damage is repaired manually.
The mesoporous silica nano-carrier loaded with natural polyphenols is prepared, is added into resin according to a certain proportion, is uniformly mixed, and finally, an intelligent coating with double functions of self-warning and self-repairing is constructed on the surface of steel. On one hand, when the coating is damaged, the natural polyphenol substances are released from the mesoporous silica nano-carrier and undergo a complexing reaction with ferric ions generated when the metal matrix is corroded to generate a macroscopic color change, so that the damage of the coating is indicated and the occurrence of metal corrosion is early warned; meanwhile, the complex is deposited on the surface of the metal substrate, so that the further progress of corrosion reaction is inhibited, and the service life of the metal is prolonged.
Disclosure of Invention
The invention aims to provide a self-warning and self-repairing dual-functional coating based on natural polyphenol fillers and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a self-warning and self-repairing dual-functional coating based on natural polyphenol packing is characterized in that a metal substrate is one of pig iron, cast iron, low-carbon steel, medium-carbon steel and high-carbon steel, and the coating is composed of a mesoporous silica nano carrier loading natural polyphenols and resin; the thickness of the coating is 50-150 μm.
Further, the natural polyphenols are one of tannic acid, ellagic acid, chlorogenic acid, caffeic acid, and gallic acid.
Further, the resin is one of polyurethane resin, epoxy resin, acrylic resin and fluorocarbon resin.
Furthermore, the natural polyphenols are loaded in mesoporous pores of the silicon dioxide nano-carrier, the diameter of the nano-carrier is 50nm-200nm, and the loading rate of the natural polyphenols is 5% -15%.
Furthermore, the mesoporous silica nano-carrier loaded with the polyphenol substances accounts for 2.5-15% of the mass of the coating.
The preparation method of the self-warning and self-repairing dual-functional coating based on the natural polyphenol filler is characterized by comprising the following steps of:
(1) dissolving 68-272 mg of natural polyphenols in 50mL of ethanol, adding 25-50 mL of concentrated ammonium hydroxide under vigorous stirring at room temperature, then adding 0.3-2.0 mL of tetraethoxysilane, continuously stirring for 1-3h, and then centrifuging at 3000-10000 rpm for 10-30 min to prepare the mesoporous silica nano carrier loaded with the natural polyphenols;
(2) and fully stirring and uniformly mixing the carrier and the resin, uniformly coating the mixture on the surface of the steel material in a blade coating, rotary coating or spraying manner, and curing at room temperature for 65-75h to obtain the intelligent coating with double functions of self-warning and self-repairing.
The self-warning and self-repairing dual-functional coating based on the natural polyphenol filler is characterized in that the self-warning and the self-repairing of the coating are carried out simultaneously: when the coating is damaged, the natural polyphenol substances are released from the mesoporous silica nano-carrier and undergo a complexing reaction with ferric ions generated when the substrate is corroded to generate macroscopic color change, so that the damage of the coating is indicated and the occurrence of metal corrosion is early warned; meanwhile, the complex is deposited on the surface of the metal substrate, so that the further progress of the corrosion reaction is inhibited, and the protective effect of the coating on the metal substrate is maintained.
The invention has the following advantages and prominent technical effects: the invention prepares a self-warning and self-repairing dual-functional coating based on natural polyphenol fillers. The coating has excellent anti-corrosion performance, when the coating is damaged, the polyphenol substances are released from the mesoporous silicon dioxide and perform a complexing reaction with ferric ions generated when the metal material is corroded to generate a macroscopic color change, so that the damage of the coating is indicated and the metal corrosion is early warned; meanwhile, the complex is deposited on the surface of the metal matrix, so that the further progress of corrosion reaction is inhibited, and the protective effect of the coating on the metal matrix is maintained. The intelligent coating has the double effects of self-warning and self-repairing, and has the advantages of simple preparation process, low production price and wide application prospect.
Drawings
Fig. 1a is a transmission electron microscope image (TEM) of the mesoporous silica nano-carrier prepared in example 1; FIG. 1b shows the color change of the solution containing natural polyphenols dissolved therein and ferric chloride solution of example 1 before and after mixing.
Fig. 2 shows the color change of the scratch damage on the surface of the coating before and after the salt spray test, in the epoxy resin coating and the pure epoxy resin coating with the double functions of self-warning and self-repairing prepared in example 2.
Fig. 3 is an electrochemical impedance spectrum of the scratches of the polyurethane resin coating with the self-warning and self-repairing functions and the pure polyurethane resin coating prepared in example 3.
Detailed Description
The invention is further illustrated by the following examples.
The invention discloses a self-warning and self-repairing dual-functional coating based on natural polyphenol fillers and a preparation method thereof. The method comprises the steps of firstly preparing the mesoporous silica nano-carrier loaded with natural polyphenols, then adding the mesoporous silica nano-carrier into resin according to a certain proportion, uniformly mixing the mesoporous silica nano-carrier with the resin, and finally constructing the intelligent coating with the double functions of self-warning and self-repairing on the surface of steel. When the coating is damaged, the natural polyphenols are released from the mesoporous silica carrier and undergo a complexing reaction with ferric ions generated when the substrate is corroded to generate macroscopic color change, so that the damage of the coating is indicated and the occurrence of metal corrosion is warned; at the same time, the complex is deposited on the metal surface, inhibiting further progress of the corrosion reaction. The intelligent coating has the double effects of self-warning and self-repairing, and has the advantages of simple preparation process and wide application prospect.
The present invention will be described in detail with reference to the accompanying drawings 1 to 3. The following examples are illustrative and not intended to be limiting, and are not intended to limit the scope of the invention.
Example 1
1. Dispersing 68mg of gallic acid into 50mL of ethanol, uniformly dissolving, pouring into a conical flask, and violently stirring;
2. adding 25mL of concentrated ammonium hydroxide under the condition of vigorous stirring, then adding 0.3mL of tetraethoxysilane, and leading the solution to be turbid, which indicates that a silicon dioxide carrier begins to be formed;
3. stirring for 2h, centrifuging the reacted suspension at 10000rpm for 10min, and drying in a 60 ℃ oven for 24h to obtain the gallic acid-loaded nano carrier;
4. polishing the medium carbon steel sheet by using sand paper, ultrasonically cleaning by using acetone and alcohol, and airing;
5. adding a nano carrier with the mass fraction of 2.5% into acrylic resin, stirring for 3 hours, and uniformly coating the surface of the treated low-carbon steel by using a blade coating rod;
6. the coating was cured at room temperature for 72h, after which the coating thickness was 50 μm.
Fig. 1a is a transmission electron micrograph of the gallic acid-loaded mesoporous silica nanocarrier prepared in example 1, and it can be seen that the nanocarrier has a spherical structure with a diameter of 150nm to 200nm and is uniform in size.
FIG. 1b shows the color change before and after mixing the aqueous solution containing gallic acid dissolved therein with the aqueous solution of ferric chloride in example 1. It can be seen that the gallic acid solution exhibited a nearly transparent color, and after mixing with the ferric chloride solution, exhibited a distinct bluish black color, due to the complexation of gallic acid with ferric ions, producing a macroscopic color change.
Example 2
1. Dispersing 120mg of tannic acid into 50mL of ethanol, uniformly dissolving, pouring into a conical flask, and violently stirring;
2. adding 50mL of concentrated ammonium hydroxide under the condition of vigorous stirring, then adding 0.6mL of tetraethoxysilane, and leading the solution to be turbid, which indicates that a silicon dioxide carrier begins to be formed;
3. stirring for 2h, centrifuging the reacted suspension for 20min at the speed of 5000rpm, and drying in an oven at the temperature of 60 ℃ for 24h to obtain the nano carrier loaded with the tannic acid;
4. polishing the low-carbon steel sheet by using sand paper, ultrasonically cleaning by using acetone and alcohol, and airing;
5. adding a nano carrier with the mass fraction of 5% into epoxy resin, stirring for 3 hours, and uniformly coating the surface of the treated low-carbon steel by using a blade coating rod;
6. curing at room temperature for 72h, wherein the thickness of the coating after curing is 100 mu m;
7. a notch defect with a width of 120 μm was made on the surfaces of the epoxy resin coating added with the nano-carrier and the pure epoxy resin coating using a scalpel, followed by a neutral salt spray test.
Fig. 2 is photographs of the surface scratches of the epoxy resin coating with the added nano-carrier and the pure epoxy resin coating of example 2 before and after the salt spray. After 5h of salt spray, the epoxy resin coating with the added nano-carrier shows macroscopic color change at the cut, because in the process of salt spray, tannic acid is released from the nano-carrier and is complexed with ferric ions generated by metal corrosion at the cut, so that the damage and the metal corrosion of the coating can be warned, and the color change at the cut of the pure epoxy resin coating is not obvious.
Example 3
1. Dispersing 272mg of ellagic acid into 50mL of ethanol, uniformly dissolving, pouring into a conical flask, and violently stirring;
2. adding 50mL of concentrated ammonium hydroxide under the condition of vigorous stirring, then adding 2.0mL of tetraethoxysilane, and leading the solution to be turbid, which indicates that a silicon dioxide carrier begins to be formed;
3. stirring for 2h, centrifuging the reacted suspension at 3000rpm for 30min, and drying in an oven at 60 ℃ for 24h to obtain the nano carrier loaded with ellagic acid;
4. polishing the low-carbon steel sheet by using sand paper, ultrasonically cleaning by using acetone and alcohol, and airing;
5. adding 7.5% by mass of nano-carrier into polyurethane resin, stirring for 3h, and uniformly coating the surface of the treated low-carbon steel by using a blade coating rod;
6. curing at room temperature for 72h, wherein the thickness of the coating after curing is 70 mu m;
7. manufacturing a cutting defect with the width of 120 mu m on the surfaces of the polyurethane coating added with the nano carrier and the pure polyurethane coating by adopting a scalpel;
8. electrochemical impedance spectra of the polyurethane coating with added nano-carriers and the pure polyurethane coating after notching were measured using an electrochemical workstation, and the test solution was 3.5 wt.% NaCl aqueous solution.
FIG. 3 is the surface of polyurethane resin coating and pure polyurethane coating with added nano-carrier in example 3Electrochemical impedance spectroscopy after bubble. It was found that the low frequency impedance modulus value of the pure polyurethane coating was 3.45X 10 at 1 day immersion4Ωcm2The low-frequency impedance modulus value of the polyurethane coating added with the nano carrier is 1.04 multiplied by 106Ωcm2A pure polyurethane coating which is obviously higher than the cut; when soaked for 7 days, the low-frequency impedance modulus of the pure polyurethane coating is reduced to 2.01 multiplied by 104Ωcm2While the low-frequency impedance modulus of the polyurethane coating added with the polyphenols is maintained to be 1.01 multiplied by 106Ωcm2The added nano carrier loaded ellagic acid and ferric ions are complexed, and the complex is deposited on a metal substrate, so that the corrosion reaction is inhibited, and the excellent self-repairing performance is shown.
Claims (7)
1. A self-warning and self-repairing dual-functional coating based on natural polyphenol packing is characterized in that a metal substrate is one of pig iron, cast iron, low-carbon steel, medium-carbon steel and high-carbon steel, and the coating is composed of a mesoporous silica nano carrier loading natural polyphenols and resin; the thickness of the coating is 50-150 μm.
2. The self-warning and self-repairing dual-functional coating based on the natural polyphenol filler as claimed in claim 1, wherein the natural polyphenol substances are one of tannic acid, ellagic acid, chlorogenic acid, caffeic acid and gallic acid.
3. The self-warning and self-repairing dual-functional coating based on the natural polyphenol filler as claimed in claim 1, wherein the resin is one of polyurethane resin, epoxy resin, acrylic resin and fluorocarbon resin.
4. The self-warning and self-repairing dual-functional coating based on the natural polyphenol filler as claimed in claim 1 or 2, wherein the natural polyphenol material is loaded in mesoporous pores of the silica nano-carrier, the diameter of the nano-carrier is 50nm-200nm, and the loading rate of the natural polyphenol material is 5% -15%.
5. The self-warning and self-repairing dual-functional coating based on the natural polyphenol filler as claimed in claim 1 or 3, wherein the mesoporous silica nano-carrier loaded with the polyphenol substances accounts for 2.5-15% of the coating by mass.
6. The preparation method of the self-warning and self-repairing dual-functional coating based on the natural polyphenol filler as claimed in claim 1, characterized by comprising the following steps:
(1) dissolving 68-272 mg of natural polyphenols in 50mL of ethanol, adding 25-50 mL of concentrated ammonium hydroxide under vigorous stirring at room temperature, then adding 0.3-2.0 mL of tetraethoxysilane, continuously stirring for 1-3h, and then centrifuging at 3000-10000 rpm for 10-30 min to prepare the mesoporous silica nano carrier loaded with the natural polyphenols;
(2) and fully stirring and uniformly mixing the carrier and the resin, uniformly coating the mixture on the surface of the steel material in a blade coating, rotary coating or spraying manner, and curing at room temperature for 65-75h to obtain the intelligent coating with double functions of self-warning and self-repairing.
7. The self-warning and self-repairing dual-functional coating based on the natural polyphenol filler, prepared by the method of claim 6, is characterized in that the self-warning and the self-repairing of the coating are carried out simultaneously: when the coating is damaged, the natural polyphenol substances are released from the mesoporous silica nano-carrier and undergo a complexing reaction with ferric ions generated when the substrate is corroded to generate macroscopic color change, so that the damage of the coating is indicated and the occurrence of metal corrosion is early warned; meanwhile, the complex is deposited on the surface of the metal substrate, so that the further progress of the corrosion reaction is inhibited, and the protective effect of the coating on the metal substrate is maintained.
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Cited By (7)
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CN114561516A (en) * | 2022-02-09 | 2022-05-31 | 浙江瑞强汽车部件有限公司 | High-strength guide locking bolt for driving axle and manufacturing method thereof |
CN114574977A (en) * | 2022-02-24 | 2022-06-03 | 中国海洋大学 | Self-early-warning coaxial electrostatic spinning fiber and preparation method and application thereof |
CN114716879A (en) * | 2022-03-10 | 2022-07-08 | 华中科技大学 | Intelligent coating material for early warning of damage perception corrosion and application thereof |
CN115028896A (en) * | 2022-06-24 | 2022-09-09 | 北京科技大学 | Natural antioxidant-coated silicon oxide composite anti-aging filler and preparation method thereof |
CN115895317A (en) * | 2022-11-25 | 2023-04-04 | 山东科技大学 | Hierarchical response self-warning anticorrosive coating and preparation method thereof |
CN116948506A (en) * | 2022-11-02 | 2023-10-27 | 中国科学院金属研究所 | Intelligent paint with dual functions of corrosion repair and early corrosion early warning, and preparation method and application thereof |
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Cited By (11)
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