CN110416557B - Method for preparing fuel cell gas diffusion layer by roll-to-roll printing at low cost - Google Patents
Method for preparing fuel cell gas diffusion layer by roll-to-roll printing at low cost Download PDFInfo
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- CN110416557B CN110416557B CN201910628636.3A CN201910628636A CN110416557B CN 110416557 B CN110416557 B CN 110416557B CN 201910628636 A CN201910628636 A CN 201910628636A CN 110416557 B CN110416557 B CN 110416557B
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/12—Stencil printing; Silk-screen printing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/26—Printing on other surfaces than ordinary paper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M3/00—Printing processes to produce particular kinds of printed work, e.g. patterns
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8803—Supports for the deposition of the catalytic active composition
- H01M4/8807—Gas diffusion layers
-
- 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
- H01M8/023—Porous and characterised by the material
- H01M8/0234—Carbonaceous material
-
- 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
- H01M8/023—Porous and characterised by the material
- H01M8/0239—Organic resins; Organic polymers
-
- 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
- H01M8/023—Porous and characterised by the material
- H01M8/0241—Composites
- H01M8/0245—Composites in the form of layered or coated products
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Composite Materials (AREA)
- Inert Electrodes (AREA)
- Fuel Cell (AREA)
Abstract
The invention belongs to the technical field of fuel cell gas diffusion layer preparation, and particularly relates to a method for preparing a fuel cell gas diffusion layer by roll-to-roll printing at low cost. The invention uses the polytetrafluoroethylene non-woven fabric as the base film, and prints the printing ink on the two sides of the base film in a roll-to-roll manner through the silk screens, wherein the printing ink is different from the traditional carbon powder, but the printing ink adopts the short carbon fiber and assists the polysilazane to carry out macroporous silk screen printing, so that the short carbon fiber is not only dispersed uniformly, but also the polysilazane is firmly bonded with the short carbon fiber after being cured in an amine environment to form the fiber mesh which is attached to the base film, thereby overcoming the micropore blockage caused by directly coating and infiltrating the carbon powder slurry. Furthermore, the gas diffusion layer is prepared by roll-to-roll printing, can be continuously printed in a roll mode, greatly reduces the cost, is suitable for large-scale production, and is easy to prepare the membrane electrode by matching the rolled proton exchange membrane. The whole preparation method has the characteristics of continuity, stabilization, low energy consumption and low material consumption.
Description
Technical Field
The invention belongs to the technical field of fuel cell gas diffusion layer preparation, and particularly relates to a method for preparing a fuel cell gas diffusion layer by roll-to-roll printing at low cost.
Background
A proton exchange membrane fuel cell (proton exchange membrane fuel cell) is a fuel cell, and corresponds to a "reverse" device for water electrolysis in principle. As the next generation of battery technology, the fuel cell has two advantages of energy density and energy storage time, and meanwhile, the fuel cell only generates water in the use process and does not generate any other pollution, so the fuel cell is an optimal energy storage device and is a solution for the ultimate battery in the future.
The proton exchange membrane fuel cell mainly comprises a membrane electrode, a bipolar plate and a shell, wherein the membrane electrode is formed by integrating a proton exchange membrane, a catalyst and a gas diffusion layer into a whole. The fuel cell gas diffusion layer generally comprises a substrate layer and a microporous layer, wherein the substrate layer generally uses porous carbon fiber paper, carbon fiber woven fabric, carbon fiber non-woven material and carbon black paper, the thickness of the substrate layer is about 100-; mainly plays a role of supporting a catalytic layer of the microporous layer; the microporous layer is mainly a layer of carbon powder with the thickness of about 10-100 μm for improving the pore structure of the substrate layer, and aims to reduce the contact resistance between the catalytic layer and the substrate layer, prevent the loss of the catalyst, and make the gas in a flow channel and the generated water uniformly distributed.
The Chinese patent application No. 201810493251.6 discloses a durable super-hydrophobic gas diffusion layer for a fuel cell, which comprises a conductive porous substrate and a microporous layer, wherein the conductive porous substrate is one of carbon fiber paper, carbon fiber non-woven fabric, carbon felt, a foamed metal plate and a metal net which are subjected to hydrophobic treatment; the microporous layer contains hydrophobic microspheres. The hydrophobic treatment is a conventional treatment method such as a treatment of impregnating a conductive porous substrate with a fluororesin and then firing the impregnated substrate. The microporous layer is formed by coating a conductive coating on the surface of a conductive porous substrate through blade coating and further firing; the conductive coating is composed of a conductive agent, hydrophobic microspheres and an adhesive, wherein the hydrophobic microspheres are high-sphericity glass microspheres or polytetrafluoroethylene microspheres. According to the invention, the hydrophobic microspheres are added into the conductive coating, so that the hydrophobicity can be improved, and the durability of the gas diffusion layer of the fuel cell can be improved.
The Chinese patent application No. 201310504496.1 discloses a carbon paper and a preparation method thereof, and more specifically, the invention relates to a high-performance carbon paper special for a gas diffusion layer of a fuel cell and a preparation method thereof, wherein the carbon paper is prepared by taking short carbon fibers, plant fibers, thermal bonding fibers and carbon black as raw materials, defibering, pulping, preparing pulp, then papermaking by a wet papermaking process, and then coating by waterproof paint, wherein the mixture ratio of the raw materials in parts by weight is as follows: 65-75 parts of short carbon fibers, 10-15 parts of plant fibers, 10-15 parts of thermal bonding fibers and 0-10 parts of carbon black. The invention adopts a production process combining wet forming, hot pressing and coating, has the characteristics of simple process flow, easy control of product quality, environment-friendly production process and the like, can accurately produce the material ratio of each raw material, and is beneficial to controlling the product quality; the disadvantages are poor conductivity (50 m.OMEGA.. multidot.cm), poor strength, poor hydrophobicity, and easy clogging of micropores if the hydrophobic layer is directly applied.
Chinese patent application No. 201810835192.6 discloses a fuel cell gas diffusion layer and a preparation method thereof, wherein the gas diffusion layer comprises a conductive mesh structure serving as a carrier and a coating coated on one or two surfaces of the conductive mesh structure, the coating comprises carbon powder and a binder, the coating is a porous structure with characteristic porosity and hydrophobicity, and is prepared by dispersing carbon powder particles in water, dispersing slurry through a homogenizer, adding the binder, mechanically stirring, and adjusting the slurry mixture to proper viscosity; applying the slurry mixture to the surface of the conductive mesh; the sample is heat treated to remove the additives and form a uniform cohesive mixture of carbon and binder, i.e., the product is made. Compared with the prior art, the gas diffusion layer has good pore structure and hydrophobic property, and has excellent performance and water management capability when a hydrogen/oxygen or hydrogen/air or other fuel cells are operated; however, the carbon powder prepared by the method is not firmly bonded, and the micropores of the conductive mesh structure are easily blocked.
The gas diffusion layer plays multiple roles of supporting the catalyst layer, collecting current, conducting gas, discharging water and the like in the fuel cell, realizes redistribution of reaction gas and product water between the flow field and the catalyst layer, and is a key material influencing the performance of the electrode. The gas diffusion layer is generally required to have good electrical conductivity, hydrophobicity, gas permeability, and mechanical strength. At present, carbon paper is mainly used as a base layer of a gas diffusion layer of a fuel cell, carbon fibers, polymer fibers and an adhesive are compounded to prepare paper, and the paper is further carbonized at a high temperature of 1600 ℃ to obtain the carbon fiber paper. The defects of brittleness, poor flexibility, low scale degree, high production energy consumption and extremely high cost. Further, since it is not flexible, a post-coating resin treatment is required, so that microporosity is affected.
Disclosure of Invention
The invention provides a method for preparing a gas diffusion layer of a fuel cell at low cost by roll-to-roll printing, which has the defects that the gas diffusion layer of the existing fuel cell is fragile, high in cost and difficult to prepare and use in a roll, and micropores are easy to block by coating a hydrophobic layer and increasing a flexible resin.
A method for roll-to-roll printing low cost production of a fuel cell gas diffusion layer comprising the steps of:
(1) preparing a modified base film: dispersing conductive carbon powder in acrylic emulsion according to a solid-to-liquid ratio of 1-3 kg: 5-10L to obtain a conductive solution, soaking a base film in the conductive solution for 24-36 h, drying, and coiling to obtain a modified base film; the base film is a polytetrafluoroethylene non-woven fabric with the aperture of 50-200 mu m;
(2) printing the printing ink on the modified base film in a roll-to-roll mode, treating the modified base film in an amine atmosphere for 30-90 min, drying the modified base film, laminating the protective film, and rolling; the printing ink is obtained by mixing short carbon fibers, polysilazane and a viscosity regulator according to a weight ratio of 5:90:5 and then ultrasonically dispersing for 3-5 hours;
(3) and (3) repeating the step (2), carrying out roll-to-roll printing on the other side of the modified base film by using the printing ink, treating for 30-90 min in an amine atmosphere, drying, laminating a protective film, and rolling to obtain the gas diffusion layer of the fuel cell.
The method for preparing the fuel cell gas diffusion layer by roll-to-roll printing at low cost comprises the step (1), wherein the conductive carbon powder is at least one of graphene, natural graphite and spherical graphite with the particle size of less than 10 mu m.
The gas diffusion layer of the fuel cell plays roles of supporting the catalyst layer and stabilizing the electrode structure in the electrode, and also has various functions of providing a gas channel, an electron channel and a water drainage channel for electrode reaction. Therefore, the material capable of functioning as a gas diffusion layer must satisfy: 1. uniform porous structure and good air permeability; 2. the resistivity is low, and the electron conductivity is strong; 3. the structure is compact, the surface is smooth, the contact resistance is reduced, and the conductivity is improved; 4. the electrode has certain mechanical strength and proper rigidity and flexibility, is beneficial to the manufacture of the electrode, and provides the stability of the electrode structure under the long-term operation condition; 5. proper hydrophilic/hydrophobic balance is adopted, so that the gas permeability is prevented from being reduced due to the blockage of pores by excessive moisture; 6. has chemical stability and thermal stability; 7. low manufacturing cost and high performance/price ratio.
In order to overcome the defect that carbon fiber paper lacks flexibility and carbon fiber woven cloth lacks dimensional stability, the substrate of the gas diffusion layer can be made of non-woven fabrics, and the non-woven fabrics have the advantages of certain mechanical strength, high flexibility, dimensional stability and the like, so that the electrode is favorably manufactured. Suitable materials include non-woven fabrics made of carbon fibers, glass fibers or fibers containing organic polymers such as polypropylene, polyester (polyethylene terephthalate), polyphenylene sulfide, polytetrafluoroethylene or polyether ketones, and the like. The invention discloses a method for preparing a gas diffusion layer of a fuel cell by roll-to-roll printing at low cost, wherein a base film in the step (1) is non-woven fabric, and the non-woven fabric is preferably polytetrafluoroethylene non-woven fabric with the aperture of 50-200 mu m.
The method for preparing the fuel cell gas diffusion layer by roll-to-roll printing at low cost comprises the step (1) of drying for 1-3 hours by adopting strong hot nitrogen flow at 100 ℃. The purpose of hot air blow drying is to keep the micropores unblocked.
The method for preparing the fuel cell gas diffusion layer in a roll-to-roll printing mode at low cost is characterized in that the printing ink in the step (2) is obtained by mixing short carbon fibers, polysilazane and a viscosity regulator according to a weight ratio of 5:90:5 and then performing ultrasonic dispersion for 3-5 hours.
The method for preparing the gas diffusion layer of the fuel cell at low cost by roll-to-roll printing is characterized in that the length of the chopped carbon fiber is less than 0.2 mm.
In the invention, printing ink is printed on the modified base film, and the modified base film is treated in the steam atmosphere of amine compound for a certain time, and the steam of the amine can enable polysilazane to be rapidly cured on the base film to form a silicon film with adhesive effect. In addition, the steam of the amine compound is selected to prevent the liquid or solid amine compound from damaging the undried printing ink on the modified base film, thereby influencing the performance of the gas diffusion layer of the fuel cell; further, it is selected to cure the amine compound with steam after printing the printing ink on the modified base film because if the amine compound is brought into contact with polysilazane or the like in advance, it is cured in advance, and thus it is not possible to form a silicon thin film on the modified base film better. Therefore, the amine atmosphere in the invention is a gaseous atmosphere of an amine compound; the amine compound may be one or a combination of any amine compound that can be in a gaseous state and does not affect the polysilazane film formation, and for example, an aliphatic amine, an aromatic amine, or a heterocyclic amine may be preferably used, and the aliphatic amine or the aromatic amine may be any of a primary amine, a secondary amine, or a tertiary amine. In the present invention, the amine compound is preferably at least one of methylamine, dimethylamine, ethylamine, diethylamine, dipropylamine, diisopropylamine, tripropylamine, butylamine, dibutylamine, tributylamine, isobutylamine, diisobutylamine, tert-butylamine, pentylamine, and tripentylamine. And for the gaseous amine atmosphere, the amine compound can be obtained by heating liquid or solid amine compound to a certain temperature for evaporation.
The method for preparing the fuel cell gas diffusion layer in a roll-to-roll printing mode at low cost comprises the step of mixing the hydroxypropyl methyl cellulose, the sodium polyacrylate and the fumed silica according to the weight ratio of 1-10: 5-10: 1-5. By adjusting the proper viscosity, the gap of the printing layer is prevented from being influenced by the diffusion of printing ink while the silk-screen printing is ensured.
The method for preparing the fuel cell gas diffusion layer with low cost through roll-to-roll printing is characterized in that the printing is performed through screen printing by using a roll-to-roll screen printing machine. Through the screen printing of big rhombus mesh, will cut the even printing of carbon fiber at the base film, the big mesh in silk screen printing hole has moreover guaranteed good voidness after the printing.
The method for preparing the fuel cell gas diffusion layer by roll-to-roll printing at low cost comprises the steps of enabling screen printing silk meshes to be large rhombic holes, enabling the diagonal length of the rhombic holes to be 0.2-0.5 mm, enabling the pressure of a screen printing scraper to be 0.5-0.8 MPa, and controlling the printing quantity to be 50-100 g/m2。
Polyvinyl alcohol film (PVA for short) has high water absorption and can be dissolved when immersed in water. The method for preparing the gas diffusion layer of the fuel cell by roll-to-roll printing at low cost is characterized in that the protective film is a hydrophilic polyvinyl alcohol film; the protective film is used to protect the gas diffusion layer from contamination and to remove the protective film when the gas diffusion layer is in use.
The traditional gas diffusion layer is carbon fiber paper sintered at high temperature, is fragile and easy to break, can only be used in a single piece to be compounded with the catalyst layer and the proton exchange membrane, directly influences the large-scale production and use, and has extremely high cost. In addition, when the carbon fiber paper is subjected to hydrophobic treatment, the coated hydrophobic layer easily blocks micropores, and the gas diffusion performance is influenced.
The invention relates to a method for preparing a fuel cell gas diffusion layer with low cost by roll-to-roll printing, which takes polytetrafluoroethylene non-woven fabric as a base film, and prints ink on two sides of the base film in a roll-to-roll manner through silk screens, wherein the ink is different from traditional carbon powder, but short carbon fibers are adopted, polysilazane is assisted, and the short carbon fibers are uniformly dispersed through macroporous silk screen printing, and the polysilazane is firmly bonded with the short carbon fibers after being cured in an amine environment to form fiber meshes attached to the base film, so that the micropore blockage caused by directly coating and infiltrating carbon powder slurry is overcome. Furthermore, the gas diffusion layer is prepared by roll-to-roll printing, can be continuously printed in a roll mode, greatly reduces the cost, is suitable for large-scale production, and is easy to prepare the membrane electrode by matching the rolled proton exchange membrane. The whole preparation method has the characteristics of continuity, stabilization, low energy consumption and low material consumption.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
A method for roll-to-roll printing low cost production of a fuel cell gas diffusion layer comprising the steps of:
(1) preparing a modified base film: dispersing conductive carbon powder in an acrylic emulsion according to a solid-to-liquid ratio of 2kg to 7L to obtain a conductive liquid, soaking a base film in the conductive liquid for 30 hours, drying, and coiling to obtain a modified base film; the conductive carbon powder is graphene with the particle size of less than 10 mu m; the base film is non-woven fabric, and the non-woven fabric is polytetrafluoroethylene non-woven fabric with the aperture of 150 mu m; the drying is carried out by adopting strong hot nitrogen flow at 100 ℃ for 2 h;
(2) printing the printing ink on the modified base film, treating for 60min in the steam atmosphere of methylamine, drying, laminating the protective film, and rolling; the printing ink is prepared by mixing short carbon fibers, polysilazane and a viscosity regulator according to a weight ratio of 5:90:5 and then ultrasonically dispersing for 4 hours; the length of the chopped carbon fiber is less than 0.2 mm; the viscosity regulator is a mixture of hydroxypropyl methyl cellulose, sodium polyacrylate and fumed silica according to a weight ratio of 5:7: 4; the printing is performed by adopting a roll-to-roll screen printing machine for screen printing; the silk screen mesh of the silk screen printing is a large diamond-shaped hole, the diagonal length of the diamond-shaped hole is 0.4mm, the pressure of a silk screen scraper is 0.7MPa, and the printing quantity is controlled at 80g/m2The protective film is a hydrophilic polyvinyl alcohol film; the protective film is removed when the gas diffusion layer is used;
(3) and (3) repeating the step (2), printing the printing ink on the other side of the modified base film in a roll-to-roll manner, treating for 60min in the steam atmosphere of methylamine, pressing the protective film after drying, and continuously rolling to obtain the gas diffusion layer of the fuel cell.
The sample of the invention adopts the ink with the carbon fiber mass concentration of 5 percent, and the printing quantity is controlled to be 80g/m2The obtained gas diffusion layer was tested for porosity and hydrophobic effect as shown in table 1.
Example 2
A method for roll-to-roll printing low cost production of a fuel cell gas diffusion layer comprising the steps of:
(1) preparing a modified base film: dispersing conductive carbon powder in acrylic emulsion according to a solid-to-liquid ratio of 1kg to 5L to obtain a conductive liquid, soaking a base film in the conductive liquid for 32 hours, drying, and coiling to obtain a modified base film; the conductive carbon powder is natural graphite with the particle size of less than 10 mu m; the base film is non-woven fabric, and the non-woven fabric is polytetrafluoroethylene non-woven fabric with the aperture of 120 mu m; the drying is carried out by adopting strong hot nitrogen flow at 100 ℃ for 1 h;
(2) printing the printing ink on the modified base film, treating for 90min in the steam atmosphere of diethylamine, drying, laminating the protective film, and coiling; the printing ink is prepared from short carbon fibers, polysilazane and viscosityThe regulator is obtained by ultrasonic dispersion for 3 hours after being mixed according to the weight ratio of 5:90: 5; the length of the chopped carbon fiber is less than 0.2 mm; the viscosity regulator is a mixture of hydroxypropyl methyl cellulose, sodium polyacrylate and fumed silica according to the weight ratio of 2:5: 3; the printing is performed by adopting a roll-to-roll screen printing machine for screen printing; the silk screen mesh of the silk screen printing is a large diamond-shaped hole, the diagonal length of the diamond-shaped hole is 0.4mm, the pressure of a silk screen scraper is 0.7MPa, and the printing quantity is controlled at 80g/m2(ii) a The protective film is a hydrophilic polyvinyl alcohol film; the protective film is removed when the gas diffusion layer is used;
(3) and (3) repeating the step (2), printing the printing ink on the other surface of the modified base film in a roll-to-roll mode, treating for 90min in the steam atmosphere of diethylamine, pressing the protective film after drying, and continuously rolling to obtain the gas diffusion layer of the fuel cell.
The sample of the invention adopts the ink with the carbon fiber mass concentration of 5 percent, and the printing quantity is controlled to be 80g/m2The obtained gas diffusion layer was tested for porosity and hydrophobic effect as shown in table 1.
Example 3
A method for roll-to-roll printing low cost production of a fuel cell gas diffusion layer comprising the steps of:
(1) preparing a modified base film: dispersing conductive carbon powder in acrylic emulsion according to a solid-to-liquid ratio of 3kg to 8L to obtain a conductive liquid, soaking a base film in the conductive liquid for 35 hours, drying, and coiling to obtain a modified base film; the conductive carbon powder is spherical graphite with the particle size of less than 10 mu m; the base film is non-woven fabric, and the non-woven fabric is polytetrafluoroethylene non-woven fabric with the aperture of 180 mu m; the drying is carried out by adopting strong hot nitrogen flow at 100 ℃ for 1 h;
(2) printing the printing ink on the modified base film, treating for 50min in the steam atmosphere of diisobutylamine, pressing the protective film after drying, and coiling; the printing ink is prepared by mixing short carbon fibers, polysilazane and a viscosity regulator according to a weight ratio of 5:90:5 and then ultrasonically dispersing for 4 hours; the length of the chopped carbon fiber is less than 0.2 mm; the viscosity regulator is hydroxypropyl methylcellulose, sodium polyacrylate, and gas phase dioxideA mixture of silicon in a weight ratio of 8:9: 3; the printing is performed by adopting a roll-to-roll screen printing machine for screen printing; the silk screen mesh of the silk screen printing is a large diamond-shaped hole, the diagonal length of the diamond-shaped hole is 0.3mm, the pressure of a silk screen scraper is 0.6MPa, and the printing quantity is controlled at 90g/m2(ii) a The protective film is a hydrophilic polyvinyl alcohol film; the protective film is removed when the gas diffusion layer is used;
(3) and (3) repeating the step (2), printing the printing ink on the other side of the modified base film in a roll-to-roll manner, treating for 50min in the steam atmosphere of diisobutylamine, laminating the protective film after drying, and continuously rolling to obtain the gas diffusion layer of the fuel cell.
The sample of the invention adopts the ink with the carbon fiber mass concentration of 5 percent, and the printing quantity is controlled to be 90g/m2The obtained gas diffusion layer was tested for porosity and hydrophobic effect as shown in table 1.
Example 4
A method for roll-to-roll printing low cost production of a fuel cell gas diffusion layer comprising the steps of:
(1) preparing a modified base film: dispersing conductive carbon powder in acrylic emulsion according to a solid-to-liquid ratio of 3kg to 9L to obtain a conductive liquid, soaking a base film in the conductive liquid for 32 hours, drying, and coiling to obtain a modified base film; the conductive carbon powder is natural graphite with the particle size of less than 10 mu m; the base film is non-woven fabric, and the non-woven fabric is polytetrafluoroethylene non-woven fabric with the aperture of 80 mu m; the drying is drying by blowing for 3 hours by adopting strong hot nitrogen flow at 100 ℃;
(2) printing the printing ink on the modified base film, treating for 45min in the steam atmosphere of pentylamine, drying, laminating the protective film, and rolling; the printing ink is prepared by mixing short carbon fibers, polysilazane and a viscosity regulator according to a weight ratio of 5:90:5 and then ultrasonically dispersing for 4 hours; the length of the chopped carbon fiber is less than 0.2 mm; the viscosity regulator is a mixture of hydroxypropyl methyl cellulose, sodium polyacrylate and fumed silica according to a weight ratio of 7:7: 4; the printing is performed by adopting a roll-to-roll screen printing machine for screen printing; the silk screen mesh of the silk screen printing is a large diamond-shaped hole, the diagonal of the diamond-shaped hole is 0.3mm, and the pressure of a silk screen scraper0.6MPa, and the printing quality is controlled to be 90g/m2(ii) a The protective film is a hydrophilic polyvinyl alcohol film; the protective film is removed when the gas diffusion layer is used;
(3) and (3) repeating the step (2), printing the printing ink on the other surface of the modified base film in a roll-to-roll mode, treating for 45min in the steam atmosphere of pentylamine, drying, laminating the protective film, and continuously rolling to obtain the gas diffusion layer of the fuel cell.
The sample of the invention adopts the ink with the carbon fiber mass concentration of 5 percent, and the printing quantity is controlled to be 90g/m2The obtained gas diffusion layer was tested for porosity and hydrophobic effect as shown in table 1.
Example 5
A method for roll-to-roll printing low cost production of a fuel cell gas diffusion layer comprising the steps of:
(1) preparing a modified base film: dispersing conductive carbon powder in acrylic emulsion according to a solid-to-liquid ratio of 2kg:9L to obtain a conductive liquid, soaking a base film in the conductive liquid for 36 hours, drying, and coiling to obtain a modified base film; the conductive carbon powder is graphene with the particle size of less than 10 mu m; the base film is non-woven fabric, and the non-woven fabric is polytetrafluoroethylene non-woven fabric with the aperture of 200 mu m; the drying is drying by blowing for 3 hours by adopting strong hot nitrogen flow at 100 ℃;
(2) printing the printing ink on the modified base film, treating for 30min in the steam atmosphere of dibutylamine, pressing the protective film after drying, and coiling; the printing ink is prepared by mixing short carbon fibers, polysilazane and a viscosity regulator according to a weight ratio of 5:90:5 and then ultrasonically dispersing for 5 hours; the length of the chopped carbon fiber is less than 0.2 mm; the viscosity regulator is a mixture of hydroxypropyl methyl cellulose, sodium polyacrylate and fumed silica according to a weight ratio of 6:9: 2; the printing is performed by adopting a roll-to-roll screen printing machine for screen printing; the silk screen mesh of the silk screen printing is a large diamond-shaped hole, the diagonal length of the diamond-shaped hole is 0.2mm, the pressure of a silk screen scraper is 0.5MPa, and the printing quantity is controlled at 60g/m2(ii) a The protective film is a hydrophilic polyvinyl alcohol film; the protective film is removed when the gas diffusion layer is used;
(3) and (3) repeating the step (2), printing the printing ink on the other side of the modified base film in a roll-to-roll mode, treating for 30min in the steam atmosphere of dibutylamine, laminating a protective film after drying, and continuously rolling to obtain the gas diffusion layer of the fuel cell.
The sample of the invention adopts the ink with the carbon fiber mass concentration of 5 percent, and the printing quantity is controlled to be 60g/m2The obtained gas diffusion layer was tested for porosity and hydrophobic effect as shown in table 1.
Comparative example 1
Comparative example 1 a commercially available carbon fiber paper with porosity of 85% was used as a substrate, and then carbon powder was dispersed in a polytetrafluoroethylene solution to obtain an ink with a carbon powder mass concentration of 5%, and single-sheet screen printing was performed; testing the porosity and the hydrophobic effect of the obtained gas diffusion layer; as in table 1.
Porosity: and (4) calculating the porosity of the experimental sample by adopting a mercury intrusion method test.
And (3) hydrophobic property test: the hydrophobicity of the experimental sample is tested by a sessile drop method under the conditions of room temperature of 25 ℃ and humidity of 35 percent, and the contact angle of the sample is measured by a water contact angle measuring instrument.
TABLE 1
| Performance index | Porosity (%) | Hydrophobicity (contact Angle) |
| Example 1 | 79.3 | 132 |
| Example 2 | 76.7 | 130 |
| Example 3 | 78.5 | 131 |
| Example 4 | 79.2 | 128 |
| Example 5 | 79.0 | 133 |
| Comparative example 1 | 61.5 | 137 |
Through detection, the gas diffusion layer maintains better micropores and has higher porosity, and the traditional comparative example causes the blockage of the micropores due to carbon powder and polytetrafluoroethylene; meanwhile, polytetrafluoroethylene coating liquid is not adopted, and the hydrophobicity close to that of polytetrafluoroethylene coating is still kept; the invention adopts roll-to-roll printing to prepare the gas diffusion layer, can continuously print in a roll mode, greatly reduces the cost, is suitable for large-scale production, and the rolled gas diffusion layer is easy to be matched with the rolled proton exchange membrane to prepare the membrane electrode. The whole preparation method has the characteristics of continuity, stabilization, low energy consumption and low material consumption.
Claims (9)
1. A method for roll-to-roll printing low cost production of a fuel cell gas diffusion layer, comprising the steps of:
(1) preparing a modified base film: dispersing conductive carbon powder in acrylic emulsion according to a solid-to-liquid ratio of 1-3 kg: 5-10L to obtain a conductive solution, soaking a base film in the conductive solution for 24-36 h, drying, and coiling to obtain a modified base film; the base film is a polytetrafluoroethylene non-woven fabric with the aperture of 50-200 mu m;
(2) printing the printing ink on the modified base film in a roll-to-roll mode, treating the modified base film in an amine atmosphere for 30-90 min, drying the modified base film, laminating the protective film, and rolling; the printing ink is obtained by mixing short carbon fibers, polysilazane and a viscosity regulator according to a weight ratio of 5:90:5 and then ultrasonically dispersing for 3-5 hours;
(3) and (3) repeating the step (2), carrying out roll-to-roll printing on the other side of the modified base film by using the printing ink, treating for 30-90 min in an amine atmosphere, drying, laminating a protective film, and rolling to obtain the gas diffusion layer of the fuel cell.
2. The method for preparing the gas diffusion layer of the fuel cell with low cost by roll-to-roll printing according to claim 1, wherein the conductive carbon powder in the step (1) is at least one of graphene, natural graphite and spherical graphite with the particle size of less than 10 μm.
3. The method for preparing the gas diffusion layer of the fuel cell in a roll-to-roll printing mode at low cost according to claim 1, wherein the drying in the step (1) is drying for 1-3 hours by using strong hot nitrogen flow at 100 ℃.
4. The roll-to-roll printing low-cost method for preparing a gas diffusion layer of a fuel cell according to claim 1, wherein the length of the chopped carbon fibers in the step (2) is less than 0.2 mm.
5. The method for preparing the gas diffusion layer of the fuel cell in a roll-to-roll printing mode at low cost according to claim 1, wherein the viscosity regulator is a mixture of hydroxypropyl methyl cellulose, sodium polyacrylate and fumed silica according to a weight ratio of 1-10: 5-10: 1-5.
6. The roll-to-roll printing low-cost method for preparing the gas diffusion layer of the fuel cell according to claim 1, wherein the amine atmosphere is a gaseous atmosphere of an amine compound; the amine compound is at least one of methylamine, dimethylamine, ethylamine, diethylamine, dipropylamine, diisopropylamine, tripropylamine, butylamine, dibutylamine, tributylamine, isobutylamine, diisobutylamine, tert-butylamine, pentylamine, tripentylamine and hexylamine.
7. The method for roll-to-roll printing low-cost preparation of a fuel cell gas diffusion layer according to claim 1, wherein the printing is screen printed using a roll-to-roll screen printer.
8. The method for preparing the gas diffusion layer of the fuel cell with low cost through roll-to-roll printing according to claim 7, wherein the silk screen holes are large diamond-shaped holes, the diagonal length of the diamond-shaped holes is 0.2-0.5 mm, the pressure of a silk screen scraper is 0.5-0.8 MPa, and the printing quantity is controlled to be 50-100 g/m2。
9. The roll-to-roll printing low-cost method for preparing a gas diffusion layer of a fuel cell according to claim 1, wherein the protective film is a hydrophilic polyvinyl alcohol film; the protective film is removed when the gas diffusion layer is used.
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