CN112267137A - Graphene corrosion-resistant conductive coating for metal surface and preparation method thereof - Google Patents
Graphene corrosion-resistant conductive coating for metal surface and preparation method thereof Download PDFInfo
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- CN112267137A CN112267137A CN202010995552.6A CN202010995552A CN112267137A CN 112267137 A CN112267137 A CN 112267137A CN 202010995552 A CN202010995552 A CN 202010995552A CN 112267137 A CN112267137 A CN 112267137A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
Abstract
The invention discloses a graphene corrosion-resistant conductive coating for a metal surface and a preparation method thereof, wherein the preparation method comprises the following steps: the coating comprises a metal substrate, a coating framework parallel to the metal substrate, a chemical corrosion inhibitor arranged on the coating framework and a modifier for chemically modifying the coating framework, wherein the coating framework is graphene which is arranged in an orientation parallel to the metal substrate. According to the invention, the problem of agglomeration of the high-addition-amount graphene derivative in the coating is solved by combining co-deposition of the graphene with good water dispersibility and the soluble inorganic corrosion inhibitor, the oriented graphene coating parallel to the metal substrate is prepared, and the electric conduction and corrosion resistance of the coating are realized by utilizing the complementary effect of chemical corrosion inhibition and physical barrier.
Description
Technical Field
The invention relates to the technical field of chemical engineering technology, in particular to a graphene corrosion-resistant conductive coating for a metal surface and a preparation method thereof.
Background
Graphene materials are one of the excellent additives in corrosion protection coatings due to their impermeability and high specific surface area. The dispersion and orientation of graphene sheets in the coating are key to achieving the physical barrier effect, the graphene dispersion problem has been paid attention to by a great deal of research work, and the chemical modification of the graphene surface, especially the chemical modification capable of forming covalent bond with graphene sheet layers, is key to solving the graphene dispersion problem. CN108531045A proposes a method for modifying graphene oxide with sulfonic acid, which utilizes the hydrophilicity of sulfonic acid groups to make the modified graphene derivative have good water dispersibility. However, the related solutions to the graphene orientation problem are limited, and especially, the preparation method of the oriented graphene coating with low cost, high efficiency and high quality has not been a breakthrough and is yet to be further solved.
CN106784915A proposes a preparation method of a graphene anticorrosive coating on a stainless steel surface, which uses a chemical vapor deposition technology, and consumes much energy when the temperature is 600-800 ℃. The electrodeposition method is a coating film forming method which has low cost, environmental protection, high efficiency and easy industrialization, and can be used for preparing a coating on a metal substrate. By adopting the method, the oriented graphene coating with good parallelism can be prepared by combining the preparation of graphene with good water dispersibility and further combining the co-deposition of the graphene and the soluble corrosion inhibitor, wherein a certain amount of corrosion inhibitor is loaded. The structural design of the coating material can realize the conductive performance and the corrosion resistance of the coating at the same time, so that the graphene coating product can meet the basic corrosion resistance requirement and simultaneously play roles of static resistance, electromagnetic shielding, electric conduction, heat conduction and the like. Potential applications include high value-added occasions such as bipolar plates of hydrogen energy automobile fuel cells, petroleum storage tanks, heat exchangers and the like. CN106283150A proposes a method for preparing an electrodeposited graphene conductive corrosion-resistant material, in which graphene coatings are electroplated on different metal substrates, but the problem that the graphene is not uniformly oriented in the metal substrates and agglomerated in the coatings is still not solved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the graphene corrosion-resistant conductive coating for the metal surface and the preparation method thereof, which are combined with the co-deposition of graphene with good water dispersibility and a soluble inorganic corrosion inhibitor, solve the problem of agglomeration of a high-addition amount of graphene derivative in the coating, prepare an oriented graphene coating parallel to a metal substrate, and simultaneously realize the conductivity and corrosion resistance of the coating by utilizing the complementary effect of chemical corrosion inhibition and physical barrier. To achieve the above objects and other advantages and in accordance with the purpose of the invention, there is provided a graphene corrosion-resistant conductive coating for a metal surface and a method for preparing the same, comprising:
the coating comprises a metal substrate, a coating framework parallel to the metal substrate, a chemical corrosion inhibitor arranged on the coating framework and a modifier for chemically modifying the coating framework, wherein the coating framework is graphene which is arranged in an orientation parallel to the metal substrate.
Preferably, the chemical corrosion inhibitor is a soluble salt, and comprises one or more of ammonium fluorozirconate, ammonium zirconium carbonate, ammonium phosphate, ammonium fluorotitanate and ammonium metavanadate.
Preferably, the modifier comprises silane coupling agent modification, titanate coupling agent modification, benzenesulfonic acid modification and polyether ammonia modification.
Preferably, the metal substrate includes stainless steel, carbon steel, galvanized steel, titanium alloy, and copper alloy.
A preparation method of a graphene corrosion-resistant conductive coating for a metal surface comprises the following steps:
s1, chemically modifying the graphene oxide serving as a precursor to improve the water dispersibility of the graphene;
s2, mixing the obtained modified graphene aqueous dispersion with a corrosion inhibitor according to a mass ratio of 2: 1-8: 1 mixing, ultrasonic dispersing for 10-20 minutes, and preparing the mixture with the concentration of 0.1-0.5 mol.L-1The deposition solution of (4);
s3, taking the metal substrate as an anode and the platinum sheet as a cathode, and depositing the modified graphene and the soluble corrosion inhibitor in the electrolyte on the surface of the metal substrate together after 5-15 min under the action of an electric field of 20-40V;
s4, drying the metal substrate in the step S3 to form the graphene corrosion-resistant conductive coating in the orientation arrangement.
Compared with the prior art, the invention has the beneficial effects that: the problem of agglomeration of graphene sheets in the coating under the condition of relatively high content of graphene is avoided, the content of the graphene derivative in the coating is improved to 88%, and the graphene derivative is uniformly distributed on the substrate instead of agglomeration. The water resistance and the chemical corrosion inhibition of ammonium zirconium carbonate, the combination of the ammonium zirconium carbonate with hydroxyl and carboxyl in sulfonated graphene oxide and the physical barrier effect of the graphene derivative are utilized, so that the corrosion resistance of the coating is improved, and the conductivity of the coating is improved. The invention is suitable for corrosion resistance and static electricity prevention of the inner wall of the oil tank and prolongs the service life of the oil tank.
In the preparation of the oriented graphene corrosion-resistant conductive coating, compared with chemical vapor deposition, the electrodeposition process has the advantage that the working temperature of electrodeposition only needs room temperature, and the chemical vapor deposition technology needs a high-temperature environment. Secondly, the electrodeposition can promote the charged particles to directionally move towards the substrate under the action of constant electric field force due to constant voltage, thereby achieving the effect of directional arrangement.
Drawings
FIG. 1 is an SEM image of the surface of a sulfonated graphene oxide/ammonium zirconium carbonate composite coating for a graphene corrosion-resistant conductive coating on a metal surface and a preparation method thereof according to the invention;
fig. 2 is an SEM image of a cross section of a sulfonated graphene oxide/ammonium zirconium carbonate composite coating for a graphene corrosion-resistant conductive coating on a metal surface and a method for preparing the same according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-2, a graphene corrosion-resistant conductive coating for a metal surface and a method for preparing the same includes:
the coating comprises a metal substrate, a coating framework parallel to the metal substrate, a chemical corrosion inhibitor arranged on the coating framework and a modifier used for chemically modifying the coating framework, wherein the coating framework is graphene which is arranged in parallel to the metal substrate in an oriented mode and can provide an electronic path and a barrier effect on corrosive media.
Furthermore, the chemical corrosion inhibitor is soluble salt, and comprises one or more of ammonium fluorozirconate, ammonium zirconium carbonate, ammonium phosphate, ammonium fluorotitanate and ammonium metavanadate, so that the corrosion resistance of the coating can be further enhanced.
Further, the modifier comprises silane coupling agent modification, titanate coupling agent modification, benzenesulfonic acid modification and polyether ammonia modification, the modifier can form a covalent bond structure with a graphene oxide precursor, and the aims of chemical modification comprise improving water dispersibility of graphene, improving film forming property of a coating and enhancing substrate adhesion of the coating.
Further, the metal substrate includes stainless steel, carbon steel, galvanized steel sheet, titanium alloy, and copper alloy.
A preparation method of a graphene corrosion-resistant conductive coating for a metal surface comprises the following steps:
s1, chemically modifying the graphene oxide serving as a precursor to improve the water dispersibility of the graphene;
s2, mixing the obtained modified graphene aqueous dispersion with a corrosion inhibitor according to a mass ratio of 2: 1-8: 1 mixing, ultrasonic dispersing for 10-20 minutes, and preparing the mixture with the concentration of 0.1-0.5 mol.L-1The deposition solution of (4);
s3, taking the metal substrate as an anode and the platinum sheet as a cathode, and depositing the modified graphene and the soluble corrosion inhibitor in the electrolyte on the surface of the metal substrate together after 5-15 min under the action of an electric field of 20-40V;
s4, drying the metal substrate in the step S3 to form the graphene corrosion-resistant conductive coating in the orientation arrangement.
Example 1
Step 1: introducing 184mg of sulfanilic acid into 500mg of graphene oxide serving as a precursor for sulfonation modification, so as to improve the water dispersibility of the graphene, and finally obtaining 4mg/mL sulfonated graphene oxide water dispersion;
step 2: mixing the obtained modified graphene aqueous dispersion with an inorganic corrosion inhibitor ammonium zirconium carbonate according to a mass ratio of 2: 1 mixing, ultrasonic dispersing for 10 minutes, and preparing the solution with the concentration of 0.1 mol.L-1The deposition solution of (4). The metal substrate is used as an anode, a platinum sheet is used as a cathode, after the action of an electric field of 20V for 5min, modified graphene and a soluble corrosion inhibitor in the electrolyte are jointly deposited on the surface of the metal substrate, and the oriented graphene corrosion-resistant conductive coating is formed after drying. The corrosion current density of the prepared graphene corrosion-resistant conductive coating in the oriented arrangement is 2.77 multiplied by 10-7A·cm-2The electrical conductivity is 2.22X 10-4S·cm-1。
The surface appearance of the graphene corrosion-resistant conductive coating in the oriented arrangement can be seen in the attached drawing 1, and the obtained graphene corrosion-resistant conductive coating is uniform in surface and free of particle aggregation.
Fig. 2 is a cross-sectional profile of the graphene anti-corrosion conductive coating in an aligned manner, and it can be seen that the thickness of the obtained graphene anti-corrosion conductive coating is about 2 microns.
Example 2
Step 1: introducing 184mg of sulfanilic acid into 500mg of graphene oxide serving as a precursor for sulfonation modification, so as to improve the water dispersibility of the graphene, and finally obtaining 4mg/mL sulfonated graphene oxide water dispersion;
step 2: mixing the obtained modified graphene aqueous dispersion with an inorganic corrosion inhibitor ammonium zirconium carbonate according to a mass ratio of 4: 1 mixing, ultrasonic dispersing for 10 minutes, and preparing the solution with the concentration of 0.5 mol.L-1The deposition solution of (4). Taking a metal substrate as an anode and a platinum sheet as a cathode, depositing modified graphene and a soluble corrosion inhibitor in electrolyte on the surface of the metal substrate together after 15min under the action of an electric field of 20V, and drying to form oriented grapheneAnd (3) corrosion-resistant conductive coating. The corrosion current density of the prepared graphene corrosion-resistant conductive coating in the oriented arrangement is 5.30 multiplied by 10-7A·cm-2The electrical conductivity was 4.22X 10-4S·cm-1。
Example 3
Step 1: introducing 184mg of sulfanilic acid into 500mg of graphene oxide serving as a precursor for sulfonation modification, so as to improve the water dispersibility of the graphene, and finally obtaining 4mg/mL sulfonated graphene oxide water dispersion;
step 2: mixing the obtained modified graphene aqueous dispersion with an inorganic corrosion inhibitor ammonium zirconium carbonate according to a mass ratio of 6: 1 mixing, ultrasonic dispersing for 20 minutes, and preparing the solution with the concentration of 0.1 mol.L-1The deposition solution of (4). The metal substrate is used as an anode, a platinum sheet is used as a cathode, after 5min under the action of an electric field of 40V, modified graphene and a soluble corrosion inhibitor in the electrolyte are jointly deposited on the surface of the metal substrate, and the oriented graphene corrosion-resistant conductive coating is formed after drying. The corrosion current density of the prepared graphene corrosion-resistant conductive coating in the oriented arrangement is 4.64 multiplied by 10-7A·cm-2The electrical conductivity is 6.03X 10-4S·cm-1。
Example 4
Step 1: introducing 184mg of sulfanilic acid into 500mg of graphene oxide serving as a precursor for sulfonation modification, so as to improve the water dispersibility of the graphene, and finally obtaining 4mg/mL sulfonated graphene oxide water dispersion;
step 2: mixing the obtained modified graphene aqueous dispersion with an inorganic corrosion inhibitor ammonium zirconium carbonate according to a mass ratio of 8: 1 mixing, ultrasonic dispersing for 20 minutes, and preparing the solution with the concentration of 0.5 mol.L-1The deposition solution of (4). The metal substrate is used as an anode, a platinum sheet is used as a cathode, after 15min under the action of an electric field of 40V, modified graphene and a soluble corrosion inhibitor in the electrolyte are jointly deposited on the surface of the metal substrate, and the oriented graphene corrosion-resistant conductive coating is formed after drying. The corrosion current density of the prepared graphene corrosion-resistant conductive coating in the oriented arrangement is 3.48 multiplied by 10-7A·cm-2The electrical conductivity is 1.90X 10-3S·cm-1。
The corrosion resistance and the conductivity of the coating obtained by co-deposition of the sulfonated graphene oxide and the ammonium zirconium carbonate in the above embodiment are tested, and the test results are shown in the following table:
as can be seen from the above table, the coating obtained by co-deposition of sulfonated graphene oxide and ammonium zirconium carbonate has good corrosion resistance, and the higher the ratio of sulfonated graphene oxide, the more positive the corrosion potential of the coating is, which indicates that the higher the ratio of sulfonated graphene oxide, the more difficult the coating is to corrode. Meanwhile, the conductivity of the coating also reaches 10-8S·cm-1Above, the requirements of antistatic coatings have been met.
The number of devices and the scale of the processes described herein are intended to simplify the description of the invention, and applications, modifications and variations of the invention will be apparent to those skilled in the art.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (5)
1. A graphene corrosion-resistant conductive coating for a metal surface, comprising:
the coating comprises a metal substrate, a coating framework parallel to the metal substrate, a chemical corrosion inhibitor arranged on the coating framework and a modifier for chemically modifying the coating framework, wherein the coating framework is graphene which is arranged in an orientation parallel to the metal substrate.
2. The graphene corrosion-resistant conductive coating for the metal surface according to claim 1, wherein the chemical corrosion inhibitor is a soluble salt comprising one or more of ammonium fluorozirconate, ammonium zirconium carbonate, ammonium phosphate, ammonium fluorotitanate and ammonium metavanadate.
3. The graphene corrosion-resistant conductive coating for the metal surface according to claim 1, wherein the modifier comprises silane coupling agent modification, titanate coupling agent modification, benzenesulfonic acid modification and polyether ammonia modification.
4. The graphene corrosion-resistant conductive coating for a metal surface of claim 1, wherein the metal substrate comprises stainless steel, carbon steel, galvanized steel, titanium alloy, and copper alloy.
5. The method for preparing the graphene corrosion-resistant conductive coating for the metal surface according to claim 1, comprising the following steps:
s1, chemically modifying the graphene oxide serving as a precursor to improve the water dispersibility of the graphene;
s2, mixing the obtained modified graphene aqueous dispersion with a corrosion inhibitor according to a mass ratio of 2: 1-8: 1 mixing, ultrasonic dispersing for 10-20 minutes, and preparing the mixture with the concentration of 0.1-0.5 mol.L-1The deposition solution of (4);
s3, taking the metal substrate as an anode and the platinum sheet as a cathode, and depositing the modified graphene and the soluble corrosion inhibitor in the electrolyte on the surface of the metal substrate together after 5-15 min under the action of an electric field of 20-40V;
s4, drying the metal substrate in the step S3 to form the graphene corrosion-resistant conductive coating in the orientation arrangement.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113106512A (en) * | 2021-04-26 | 2021-07-13 | 上海电气集团股份有限公司 | Surface modification method of titanium substrate for fuel cell |
| CN114773959A (en) * | 2022-05-31 | 2022-07-22 | 复旦大学 | High-performance transparent anticorrosive coating material and preparation method thereof |
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2020
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| QI LIU: "Improved anti-corrosion behaviour of an inorganic passive film on hot-dip galvanised steel by modified graphene oxide incorporation", 《CORROSION SCIENCE》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113106512A (en) * | 2021-04-26 | 2021-07-13 | 上海电气集团股份有限公司 | Surface modification method of titanium substrate for fuel cell |
| CN114773959A (en) * | 2022-05-31 | 2022-07-22 | 复旦大学 | High-performance transparent anticorrosive coating material and preparation method thereof |
| CN114773959B (en) * | 2022-05-31 | 2023-03-03 | 复旦大学 | High-performance transparent anticorrosive coating material and preparation method thereof |
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