CN114456676B - Preparation method of metal electrode protective coating of hydrogen-oxygen fuel cell - Google Patents
Preparation method of metal electrode protective coating of hydrogen-oxygen fuel cell Download PDFInfo
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- CN114456676B CN114456676B CN202210025291.4A CN202210025291A CN114456676B CN 114456676 B CN114456676 B CN 114456676B CN 202210025291 A CN202210025291 A CN 202210025291A CN 114456676 B CN114456676 B CN 114456676B
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- mxene
- coating
- fuel cell
- deionized water
- epoxy resin
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0223—Composites
- H01M8/0228—Composites in the form of layered or coated products
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a preparation method of a protective coating of a metal electrode of an oxyhydrogen fuel cell. The method is characterized in that Dopamine (DA) is polymerized on the surface of titanium carbide (MXene) through a wet chemical method to form PDA-Mxene filler, and then the PDA-Mxene filler and epoxy resin are uniformly mixed to prepare the protective coating with the functions of conductivity and corrosion resistance. The coating obtained by the invention has good conductivity and corrosion resistance, and has good application prospect on the surface of the stainless steel bipolar plate of the hydrogen-oxygen fuel cell.
Description
Technical Field
The invention belongs to the technical field of protective coatings, and particularly relates to a preparation method of a protective coating of a metal electrode of an oxyhydrogen fuel cell.
Background
With the increasing consumption of traditional energy sources including coal, petroleum and the like, environmental protection and energy crisis have become common problems all over the world. The hydrogen-oxygen fuel cell is used as an energy conversion device mainly based on green energy, has high energy conversion rate, and is environment-friendly and pollution-free. However, the pem fuel cell may undergo complicated circulation processes of fuel supply, humidity, temperature, current, voltage, etc. with actual vehicle conditions, resulting in accelerated degradation of the electrodes of the fuel cell.
Although the conventional graphene bipolar plate of the hydrogen-oxygen fuel cell has the characteristics of high conductivity, good corrosion performance and the like, the following defects are not suitable for batch production: (1) The brittle substance causes assembly difficulty, and the thickness is not easy to be thinned; (2) sintering into porous plate, adding additive; (3) Long graphitization time, difficult mechanical processing and high price.
The metal bipolar plate of the hydrogen-oxygen fuel cell has good electric and thermal conductors; the mechanical property is good, and the strength is high; the gas barrier property is good; non-porous, etc., but is susceptible to corrosion and requires surface modification.
Disclosure of Invention
Aiming at the problem that the conventional oxyhydrogen fuel cell is extremely easy to wear, the invention provides a preparation method of a metal electrode protective coating of the oxyhydrogen fuel cell, dopamine (DA) is polymerized on the surface of titanium carbide (MXene) by a wet chemical method to form PDA-Mxene filler, and then the PDA-MXene is introduced into an epoxy resin coating, so that the corrosion resistance of the coating is improved.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
a method for preparing an electrode protective coating for a hydrogen-oxygen fuel cell, comprising the steps of:
step 1, adding 200-500 mg of MXene into 100 mL of deionized water, and performing ultrasonic dispersion;
step 2, adding 100-400 mg of dopamine hydrochloride into the mixed solution obtained in the step 1, stirring vigorously for 1 h, and adding a Tris-HCl solution to adjust the pH value of the solution to 8-9 during the period;
step 3, continuously stirring the system obtained in the step 2 under a dark condition for reacting for 24-48 h;
step 4, centrifugally separating the obtained suspension for 5min at the speed of 5000-8000 r/min, centrifugally washing away unreacted reagents by deionized water, and finally, drying the obtained solid for 24 h in vacuum;
and 5, mixing the epoxy resin, the N, N-dimethylformamide and the solid prepared in the step 4 according to the weight ratio of 100g:10mL of: 1g of the solid and N, N-dimethylformamide are mixed and then ultrasonically dispersed for 10 min, then epoxy resin is added into the system to continue to ultrasonically disperse for 10 min, then a rubber head dropper is used for sucking the system, 0.4-0.7 g of the system is dripped on a steel sheet, and a wire rod is used for uniformly roller-coating the steel sheet from the same direction to prepare a coating;
and 6, drying the prepared coating in a drying oven at the temperature of 80-100 ℃ for 20 min.
Aiming at the problem that the electricity of the existing oxyhydrogen fuel cell is easy to be lost, the invention provides an electrode protective coating of the oxyhydrogen fuel cell, which is prepared by taking epoxy resin base resin and PDA-MXene as filler. The invention self-polymerizes DA on the surface of MXene under the slightly alkaline condition to obtain MXene-PDA, and then coats the MXene-PDA as a filler on a 304 stainless steel bipolar plate in combination with epoxy resin.
The invention has the beneficial effects that: (1) The high specific surface area and wide adhesion of MXene allow PDA to adhere to the surface of MXene as much as possible, and the blocking effect of MXene is enhanced; (2) The secondary reactivity of PDA can be corroded instead of MXene, enhancing corrosion protection.
Detailed Description
The present invention is described in further detail below with reference to specific examples, but the present invention should not be construed as being limited thereto. Modifications or substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and scope of the invention. The experimental methods and reagents of the formulations not specified in the examples are in accordance with the conventional conditions in the art.
Example 1
(1) Adding 500 mg of MXene into 100 mL of deionized water, and ultrasonically dispersing for 0.5 h by using an ultrasonic machine;
(2) Adding 250 mg of dopamine hydrochloride into the solution, and stirring the solution vigorously for 1 h, wherein 25 mL of 50 mM Tris-HCl solution is added into the solution system dropwise during the period, and the pH is adjusted to 8.5;
(3) Continuously stirring the system in the step 2 under a dark condition for reaction for 24 hours;
(4) The obtained suspension is centrifuged at 5000 r/min for 5min, and deionized water is used for centrifuging to wash away unreacted reagents. Finally, drying the obtained solid in vacuum for 24 hours;
(5) Adding 0.01 g of MXene-PDA into 1.5 mL of DMF, performing ultrasonic dispersion for 10 min, adding 1g of epoxy resin into the system, continuing performing ultrasonic dispersion for 10 min, sucking the system by using a rubber head dropper, dropwise adding 6 drops of epoxy resin onto a steel sheet, and uniformly coating the mixture in the same direction by using a wire rod;
(6) The prepared coating is put into a drying oven to be dried for 20 min at the temperature of 100 ℃.
Example 2
(1) Adding 500 mg of MXene into 100 mL of deionized water, and ultrasonically dispersing for 0.5 h by using an ultrasonic machine;
(2) Adding 250 mg of dopamine hydrochloride into the solution, and stirring the solution vigorously for 1 h, wherein 25 mL of 50 mM Tris-HCl solution is added into the solution system dropwise, and the pH is adjusted to 8.5;
(3) Continuously stirring the system in the step 2 under a dark condition for reacting for 36 hours;
(4) The obtained suspension is centrifuged at 5000 r/min for 5min, and deionized water is used for centrifuging to wash away unreacted reagents. Finally, drying the obtained solid in vacuum for 24 hours;
(5) 0.01 g of MXene-PDA is taken, 1.5 mL of DMF is added, ultrasonic dispersion is carried out for 10 min, then 1g of epoxy resin is added into the system, ultrasonic dispersion is continued for 10 min, then 6 drops of epoxy resin are dripped on a steel sheet by the system which is sucked by a rubber head dropper, and a wire rod is used for uniformly coating the mixture in the same direction;
(6) The prepared coating is put into a drying oven to be dried for 20 min at 100 ℃.
Example 3
(1) Adding 500 mg of MXene into 100 mL of deionized water, and ultrasonically dispersing for 0.5 h by using an ultrasonic machine;
(2) Adding 250 mg of dopamine hydrochloride into the solution, and stirring the solution vigorously for 1 h, wherein 25 mL of 50 mM Tris-HCl solution is added into the solution system dropwise during the period, and the pH value is adjusted to 8;
(3) Continuously stirring the system in the step 2 under a dark condition for reacting for 48 hours;
(4) The resulting suspension was centrifuged at 5000 r/min for 5min and the unreacted reagents were washed off by centrifugation with deionized water. Finally, drying the obtained solid in vacuum for 24 hours;
(5) Adding 0.01 g of MXene-PDA into 1.5 mL of DMF, performing ultrasonic dispersion for 10 min, adding 1g of epoxy resin into the system, continuing performing ultrasonic dispersion for 10 min, sucking the system by using a rubber head dropper, dropwise adding 6 drops of epoxy resin onto a steel sheet, and uniformly coating the mixture in the same direction by using a wire rod;
(6) The prepared coating is put into a drying oven to be dried for 20 min at 100 ℃.
Example 4
(1) Adding 500 mg of MXene into 100 mL of deionized water, and ultrasonically dispersing for 0.5 h by using an ultrasonic machine;
(2) 300 mg of dopamine hydrochloride is put into the solution and stirred vigorously for 1 h, during which 25 mL of 50 mM Tris-HCl solution is added into the solution system dropwise, and the pH is adjusted to 9;
(3) Continuously stirring the system in the step 2 under a dark condition for reacting for 24 hours;
(4) The resulting suspension was centrifuged at 5000 r/min for 5min and the unreacted reagents were washed off by centrifugation with deionized water. Finally, drying the obtained solid in vacuum for 24 hours;
(5) Adding 0.01 g of MXene-PDA into 1.5 mL of DMF, performing ultrasonic dispersion for 10 min, adding 1g of epoxy resin into the system, continuing performing ultrasonic dispersion for 10 min, sucking the system by using a rubber head dropper, dropwise adding 6 drops of epoxy resin onto a steel sheet, and uniformly coating the mixture in the same direction by using a wire rod;
(6) The prepared coating is put into a drying oven to be dried for 20 min at 100 ℃.
Example 5
(1) Adding 500 mg of MXene into 100 mL of deionized water, and ultrasonically dispersing for 0.5 h by using an ultrasonic machine;
(2) 300 mg of dopamine hydrochloride is put into the solution and stirred vigorously for 1 h, during which 25 mL of 50 mM Tris-HCl solution is added into the solution system dropwise, and the pH is adjusted to 8.5;
(3) Continuously stirring the system in the step 2 under a dark condition for reaction for 24 hours;
(4) The resulting suspension was centrifuged at 5000 r/min for 5min and the unreacted reagents were washed off by centrifugation with deionized water. Finally, the obtained solid is dried for 24 hours in vacuum;
(5) Adding 0.01 g of MXene-PDA into 1.5 mL of DMF, performing ultrasonic dispersion for 10 min, adding 0.1 g of epoxy resin into the system, continuing the ultrasonic dispersion for 10 min, sucking the system by using a rubber head dropper, dropwise adding 6 drops of epoxy resin onto a steel sheet, and uniformly coating the mixture in the same direction by using a wire rod;
(6) The prepared coating is put into a drying oven to be dried for 20 min at 100 ℃.
Example 6
(1) Adding 400 mg of MXene into 100 mL of deionized water, and ultrasonically dispersing for 0.5 h by using an ultrasonic machine;
(2) Adding 250 mg of dopamine hydrochloride into the solution, and stirring the solution vigorously for 1 h, wherein 25 mL of 50 mM Tris-HCl solution is added into the solution system dropwise, and the pH is adjusted to 8.5;
(3) Continuously stirring the system in the step 2 under a dark condition for reaction for 24 hours;
(4) The obtained suspension is centrifuged at 5000 r/min for 5min, and deionized water is used for centrifuging to wash away unreacted reagents. Finally, the obtained solid is dried for 24 hours in vacuum;
(5) Adding 0.01 g of MXene-PDA into 1.5 mL of DMF, performing ultrasonic dispersion for 10 min, adding 1g of epoxy resin into the system, continuing performing ultrasonic dispersion for 10 min, sucking the system by using a rubber head dropper, dropwise adding 6 drops of epoxy resin onto a steel sheet, and uniformly coating the mixture in the same direction by using a wire rod;
(6) The prepared coating is put into a drying oven to be dried for 20 min at 100 ℃.
The samples from examples 1, 4, and 6 were tested with bare 304 stainless steel, conventional epoxy coating, and MXene coating in an electrochemical workstation for Tafel testing, and the corrosion resistance of the coating was observed, as shown in table 1.
TABLE 1 sample self-corrosion Voltage and self-corrosion Density from Tafel extrapolation for different samples
From the above results, the coating of the present invention has excellent corrosion resistance, and is suitable for the anti-corrosion coating of the hydrogen-oxygen fuel cell bipolar plate to resist electrochemical corrosion to protect the electrode and prolong the service life of the hydrogen-oxygen fuel cell.
Claims (1)
1. A preparation method of an electrode protective coating of an oxyhydrogen fuel cell is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding MXene into deionized water, wherein the dosage ratio of MXene to deionized water is 200-500 mg:100 mL, ultrasonic dispersion;
step 2, adding dopamine hydrochloride into the mixed solution obtained in the step 1, wherein the added dopamine hydrochloride is 100-400 mg, violently stirring for 1 h, and adding a Tris-HCl solution to adjust the pH value of the solution to 8-9;
step 3, continuously stirring the system obtained in the step 2 under a dark condition for reaction for 24-48 h;
step 4, centrifugally separating the obtained suspension, centrifugally washing away unreacted reagents by using deionized water under the centrifugal separation conditions of 5000-8000 r/min and 5min, and finally, drying the obtained solid for 24 h in vacuum;
and step 5, mixing the epoxy resin, the N, N-dimethylformamide and the solid prepared in the step 4 according to the proportion of 100g:10mL of: 1g of the solid and N, N-dimethylformamide are mixed and then ultrasonically dispersed, epoxy resin is added into the system for continuous ultrasonic dispersion, then the system is sucked by a rubber head dropper to be dripped on a steel sheet, and a coil bar is used for uniformly roller-coating in the same direction to prepare a coating;
and 6, drying the prepared coating for 20 min at the drying condition of 80-100 ℃.
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| CN114456676B true CN114456676B (en) | 2023-02-07 |
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| CN115621483B (en) * | 2022-09-26 | 2024-02-02 | 海卓动力(北京)能源科技有限公司 | MXene composite bipolar plate and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4436456A1 (en) * | 1994-10-12 | 1996-04-18 | Siemens Ag | Electrically conductive deformable coating for high temp. fuel cell electrode |
| CN108137955A (en) * | 2015-11-26 | 2018-06-08 | 米其林集团总公司 | It is particularly useful as the metal bonding of fuel battery double plates coating, hydrophobic and conductive coating |
| CN110117431A (en) * | 2019-05-16 | 2019-08-13 | 哈尔滨工业大学 | A kind of preparation method of MXene base electro-magnetic screen coating material |
| CN112552801A (en) * | 2020-12-25 | 2021-03-26 | 南京大学 | Ti-containing alloy3C2TX(MXene)/polyaniline water-based anticorrosive paint and preparation method thereof |
| CN113214738A (en) * | 2021-05-13 | 2021-08-06 | 青岛理工大学 | Polydopamine-modified graphene oxide-modified silane emulsion and preparation method and application thereof |
| CN215049815U (en) * | 2021-05-18 | 2021-12-07 | 江苏科辉环境科技有限公司 | Double-layer composite anticorrosive coating |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113801533B (en) * | 2021-02-05 | 2022-03-01 | 中国科学院兰州化学物理研究所 | Dry film lubricant based on dopamine modified pigment filler and application thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4436456A1 (en) * | 1994-10-12 | 1996-04-18 | Siemens Ag | Electrically conductive deformable coating for high temp. fuel cell electrode |
| CN108137955A (en) * | 2015-11-26 | 2018-06-08 | 米其林集团总公司 | It is particularly useful as the metal bonding of fuel battery double plates coating, hydrophobic and conductive coating |
| CN110117431A (en) * | 2019-05-16 | 2019-08-13 | 哈尔滨工业大学 | A kind of preparation method of MXene base electro-magnetic screen coating material |
| CN112552801A (en) * | 2020-12-25 | 2021-03-26 | 南京大学 | Ti-containing alloy3C2TX(MXene)/polyaniline water-based anticorrosive paint and preparation method thereof |
| CN113214738A (en) * | 2021-05-13 | 2021-08-06 | 青岛理工大学 | Polydopamine-modified graphene oxide-modified silane emulsion and preparation method and application thereof |
| CN215049815U (en) * | 2021-05-18 | 2021-12-07 | 江苏科辉环境科技有限公司 | Double-layer composite anticorrosive coating |
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