CN115188982A - All-vanadium redox flow battery bipolar plate base material with acid resistance and electrolyte resistance, bipolar plate and preparation method - Google Patents
All-vanadium redox flow battery bipolar plate base material with acid resistance and electrolyte resistance, bipolar plate and preparation method Download PDFInfo
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- CN115188982A CN115188982A CN202210616870.6A CN202210616870A CN115188982A CN 115188982 A CN115188982 A CN 115188982A CN 202210616870 A CN202210616870 A CN 202210616870A CN 115188982 A CN115188982 A CN 115188982A
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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
- H01M8/0226—Composites in the form of mixtures
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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
- H01M8/0213—Gas-impermeable carbon-containing materials
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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
- H01M8/023—Porous and characterised by the material
- H01M8/0234—Carbonaceous material
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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
- H01M8/023—Porous and characterised by the material
- H01M8/0241—Composites
- H01M8/0243—Composites in the form of mixtures
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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
- H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
- H01M8/184—Regeneration by electrochemical means
- H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
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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
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Abstract
The invention discloses a base material of a bipolar plate of an all-vanadium redox flow battery, which comprises the following components in percentage by weight: 40-50% of composite carbon-based conductive filler, 20-40% of thermosetting powder resin, 10-25% of modified toughening agent, 10-25% of high-temperature toughening curing agent and 1-5% of powder dispersant, wherein the sum of the components is 100%. The invention adopts two composite base material thin plates, the metal thin plate is arranged in the middle, the graphite metal thin plate is processed by a rolling technology, the composite base material graphite metal bipolar plate is formed by a mould pressing technology, the composite base material graphite metal bipolar plate can enter an oven for curing in batch, and the all-vanadium redox flow battery composite graphite metal bipolar plate with acid and electrolyte resistance can be obtained.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a base material of an all-vanadium redox flow battery composite graphite metal bipolar plate which can be quickly rolled and cold-pressed to be formed and has acid resistance and electrolyte resistance, a bipolar plate containing the base material and a preparation method of the bipolar plate.
Background
An all-Vanadium redox flow battery (abbreviated as VFB) is a secondary battery technology in which active substances are in a circulating liquid state, and chemical energy and electric energy are converted back and forth through valence state change of Vanadium ions, so that electric energy storage and release are realized.
The bipolar plate is required to have good chemical stability, high mechanical strength, good water impermeability, low manufacturing cost and long service life. At present, most of all vanadium redox flow batteries adopt graphite plates and carbon plastic plates. The conductive plastic plate has the advantages of light weight, large size, low manufacturing cost, good chemical stability and easy sealing; however, the plastic plate has a large contact resistance with the carbon felt, and the electrical conductivity is lower than that of the graphite plate. The graphite plate has the advantages of high conductivity, good impermeability and certain mechanical strength; however, the graphite plate also has some disadvantages, such as poor sealing performance, vacuum impregnation, and limitation of process manufacturing, and is mainly produced by adopting a machining mode and a molded graphite plate, the machining mode does not need to open a mold, the modification can be strong, but the batch processing period is long, the molded graphite plate is not suitable for a batch processing mainstream production mode after determining the flow channel configuration, the raw material strength of the graphite bipolar plate is limited, the thickness of the prepared bipolar plate is too thick, the improvement of the volume ratio power of the battery is not facilitated, the integral comprehensive performance is insufficient, the large-size graphite plate is difficult to manufacture, the mechanical performance is poor, the weight is large, the cost is high, and the surface of the graphite plate is corroded under the long-term high current density use. The graphite plate and the composite material bipolar plate can be produced in batch by adopting a die pressing or injection molding process, so that the manufacturing cost of the bipolar plate is reduced, and the composite material bipolar plate has a wide application prospect.
Disclosure of Invention
The invention aims to provide a base material of a composite graphite metal bipolar plate of an all-vanadium redox flow battery, which can be rapidly rolled and cold-pressed to form and has acid resistance and electrolyte resistance, a preparation method of the base material and the bipolar plate containing the base material.
In order to solve the technical problems, the invention provides a base material of a bipolar plate of an all-vanadium redox flow battery, which comprises the following components in percentage by weight:
40-50% of composite carbon-based conductive filler,
20 to 40 percent of thermosetting powder resin,
10 to 25 percent of modified toughening agent,
10 to 25 percent of high-temperature toughening curing agent,
1 to 5 percent of powder dispersant, and the sum of the components is 100 percent.
Preferably, the composite carbon-based conductive filler is one or more of graphite powder, carbon fibers, carbon nanotubes, graphene and conductive carbon black, and the composite carbon-based conductive filler has better conductivity, no corrosivity to a metal mold and higher requirements on electrode materials.
The graphite powder is a carbonaceous element crystalline mineral, the shape of the graphite powder is similar to a fish scale, the crystalline grid is in a hexagonal layered structure, the distance between every two network layers is 340pm, the distance between carbon atoms in the same network layer is 142pm, the graphite powder belongs to a hexagonal crystal system, has complete layered cleavage, has good high temperature resistance, electric conduction, heat conduction, lubrication, plasticity, acid and alkali resistance and the like, and can improve the weather resistance and the electric conductivity of the bipolar plate.
The carbon fiber is a novel fiber material of high-strength and high-modulus fiber with the carbon content of more than 95 percent, is formed by piling up organic fibers such as flake graphite microcrystals along the axial direction of the fiber, and can improve the strength and the conductivity of the bipolar plate through a microcrystalline graphite material obtained by carbonization and graphitization treatment;
graphene (Graphene) is a new material with a monolayer sheet structure composed of carbon atoms. The composite bipolar plate is called as a magic material due to excellent properties such as high electrical conductivity, high thermal conductivity and high strength, and the electrical conductivity and the strength of the bipolar plate can be improved by adding the magic material into the composite bipolar plate.
Conductive carbon black has carbon black with low resistance or high resistance properties. Can impart conductive or antistatic action to the article. The bipolar plate has the characteristics of small particle size, large and rough specific surface area, high structure, clean surface (few compounds) and the like, and can enhance the conductivity of the bipolar plate.
The composite carbon-based conductive filler with different meshes (50-100 meshes of graphite powder, 50-100 meshes of carbon fiber, 5-10um of graphene and 20-30nm of conductive carbon black) is mixed, so that the graphite powder can be better and closely communicated after mould pressing, the conductivity of the bipolar plate is improved, the charging cycle test can be carried out in an electrolyte environment for a long time, and the acid resistance test can be carried out in a mixed acid system of hydrochloric acid and sulfuric acid for a long time.
Preferably, the thermosetting powder resin is one or more of phenolic resin, urea resin, melamine-formaldehyde resin, epoxy resin, unsaturated resin, polyurethane and polyimide.
Preferably, the modified toughening agent is one or more of MBS toughening agent, CSR core-shell rubber toughening agent and blocked isocyanate toughening agent; the diameters of the selected resin solid modified resin powders are between 5 and 15 mu m, the resin solid modified resin powders are suitable for powder spraying, the charging cycle test can be carried out in the electrolyte environment for a long time, the acid resistance test can be carried out in a mixed acid system of hydrochloric acid and sulfuric acid for a long time,
preferably, the high-temperature toughening curing agent is one or two of 2-phenylimidazoline and modified imidazole addition compound; the high-temperature toughening curing agent is formed by polymerizing various compounds, and has a high-temperature resistant characteristic due to various high-temperature resistant active groups such as phenyl groups, so that a cured product can work at the temperature of 200 ℃ for a long time, and the high-temperature toughening curing agent belongs to a high-performance environment-friendly curing agent. The mixture of the powder epoxy toughening agent and the high-temperature toughening curing agent can be completely cured after being cured at 130 ℃ for 30-60 minutes and baked and cured at 180 ℃ for 30-60 minutes according to a proper proportion, the cured performance can be tested in a charging cycle in an electrolyte environment for a long time, and the acid resistance can be tested in a mixed acid system of hydrochloric acid and sulfuric acid for a long time.
Preferably, the powder dispersant is one or a mixture of acrylic block copolymers. The acrylic block copolymer is an ultrahigh molecular weight dispersing agent containing acidic groups, has excellent anti-settling, anti-flocculation and anti-coarse-preventing capabilities, has excellent universality, and is applicable to both aqueous systems and oily systems. The dispersion efficiency is high, the surface tension of nano material particles can be reduced to a large extent, and the electrostatic adsorption and agglomeration of nano materials are reduced.
The invention also provides a method for preparing the bipolar plate substrate base material, which comprises the following steps: the method comprises the steps of firstly adding various required composite carbon-based conductive fillers into a 600-mesh granulator according to a ratio for grinding, repeatedly discharging materials through a 600-mesh screen until all powder materials pass through the 600-mesh screen, then vacuumizing the materials into a high-efficiency mixer for high-speed stirring, mixing and stirring uniformly to form a premix 1, mixing powdered thermosetting powder resin, a modified toughening agent and a high-temperature toughening curing agent into a premix 2 through the high-efficiency mixer according to the ratio, then performing powder spraying on the premix 1 in the stirring of the high-efficiency mixer through a powder spraying machine by using the premix 2, adding a powder dispersing agent into the mixed materials according to the ratio after the spraying is completed, and taking out all the powder materials after mixing for a period of time.
The double-plate electrode comprises the powder prepared by the method, the powder is rolled and formed into composite base material graphite plate thin plates through a roller press, then a layer of metal thin plate is stacked between the two composite base material graphite plate thin plates, the stacked semi-finished product is rolled and formed into a graphite metal thin plate through the roller press for the second time, the graphite metal thin plate is directly pressed and formed in a mold through a mold press, the forming time is less than or equal to 1 minute, the forming thickness is less than or equal to 0.8mm, and the molded composite graphite metal plate is cured in an oven to obtain the double-plate.
Preferably, the metal sheet is one of stainless steel, copper, aluminum and titanium alloy.
The invention provides a base material formula and a manufacturing process of a composite graphite metal bipolar plate of an all vanadium redox flow battery with acid and electrolyte resistance, which is formed by rapid rolling and cold press molding.
The formula and the manufacturing process of the all-vanadium redox flow battery composite graphite metal bipolar plate with acid resistance and electrolyte resistance, which are formed by rapid rolling and cold pressing, can form a required composite graphite metal pre-formed plate through pre-rolling by a double-roller machine, and then carry out cold pressing forming on the pre-formed plate through a servo hydraulic press with a flow channel, wherein the forming time is less than or equal to 1 minute, the forming thickness is less than or equal to 0.8mm, the cold-pressed composite plate has initial strength and is not easy to break, a powder dispersing agent is contained in a base material, and the base material has a demolding effect on a metal surface, so that a demolding agent is not needed and demolding can be easily carried out. The molded composite board can enter the tunnel furnace for deep curing according to the above, the base material contains thermosetting powder resin and high-temperature toughening curing agent, and is directly heated and cured in the tunnel furnace to form the adhesive property to the metal, so that the metal can be directly cured and bonded without dispensing or injection bonding between the graphite plate and the metal plate, and the cured composite board has high density>1.5g/cm3, conductivity>350S/m, tensile strength>30MPa, bending strength>35MPa, corrosion current<0.016mA/cm 2 Air permeability<2×10-6cm 3 /scm 2 The thickness of the formed bipolar plate is more than or equal to 1.0mm, the qualified bipolar plate can be formed by direct dispensing and curing without vacuum impregnation, the charging cycle test can be carried out in the electrolyte environment for a long time, and the acid resistance test can be carried out in a mixed acid system of hydrochloric acid and sulfuric acid for a long time. The ultra-thin composite stone is prepared by adopting a production process combining rolling and mould pressingThe ink metal bipolar plate improves the power density of the galvanic pile, is suitable for the production of bipolar plates in large batch and improves the production efficiency.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to specific embodiments.
The invention provides a base material formula and a manufacturing process of an all-vanadium redox flow battery composite graphite metal bipolar plate with acid resistance and electrolyte resistance, which is formed by rapid rolling and cold pressing, and comprises the following components in percentage by weight:
in this example, the base material of the present invention comprises:
the method comprises the steps of firstly adding various required composite carbon-based conductive fillers into a 600-mesh granulator according to a ratio for grinding, repeatedly discharging materials through a 600-mesh screen until all powder materials pass through the 600-mesh screen, then vacuumizing the materials into a high-efficiency mixer for high-speed stirring, mixing and stirring uniformly to form premix 1, carrying out thermosetting modified resin on the powder, modifying and toughening agents, mixing a high-temperature toughening curing agent into premix 2 through the high-efficiency mixer according to the ratio, carrying out powder spraying on the premix 1 in the high-speed stirring of the high-efficiency mixer through a powder spraying machine by using the premix 2, adding a powder dispersing agent into a mixed material according to the ratio after spraying is finished, and taking out all the powder materials after mixing for a period of time.
The method comprises the following steps of rolling and forming a semi-finished product raw material into a composite base material graphite plate thin plate through a first rolling machine, stacking a metal thin plate layer between two graphite thin plates, performing secondary rolling and forming on the stacked semi-finished product into a graphite metal thin plate through the rolling machine, directly pressing and forming the graphite metal thin plate in a mould through a mould pressing machine, wherein the forming time is less than or equal to 1 minute, the forming thickness is less than or equal to 0.8mm, the moulded composite graphite metal plate can enter an oven for curing in batches, the base material contained in the composite graphite metal plate can directly form curing and bonding to metal, glue dispensing or injection molding bonding is not needed between the graphite plate and the metal plate, and the qualified bipolar plate can be formed through direct glue dispensing and curing without vacuum impregnation.
The sheet with the formula of the bipolar plate can be directly subjected to cold press forming in a mold with a flow channel by a hydraulic machine, the forming time is 60-120 seconds, the forming pressure is 100-120 MPa, the forming thickness is less than or equal to 0.8mm, and the cold-pressed composite plate has initial strength, does not need a release agent and can be easily released.
The physical and chemical indexes of the base materials of the bipolar plate formulations of examples 1-3 after cold press molding and baking curing at 130 ℃,1 hour and 160 ℃ for 1 hour are shown in the following table:
therefore, the formula and the manufacturing process of the composite graphite metal bipolar plate of the all-vanadium redox flow battery with acid resistance and electrolyte resistance, which are quickly rolled and cold-pressed and formed, can better combine the advantages of the graphite plate and the metal plate, greatly reduce the cost, solve the problems of insufficient toughness of the graphite plate and high cost of the surface coating of the metal plate, and the manufactured bipolar plate has the characteristics of low density, corrosion resistance, easy forming, resistance to the electrolyte and the acidity of the all-vanadium redox flow battery, high production efficiency, good formability and the like, can greatly reduce the unit price of a bipolar plate stack, meets the requirement of mass production, and has great economic value and practical value.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (8)
1. The bipolar plate base material of the all-vanadium redox flow battery with acid resistance and electrolyte resistance is characterized by comprising the following components in percentage by weight:
40 to 50 percent of composite carbon-based conductive filler,
20 to 40 percent of thermosetting powder resin,
10 to 25 percent of modified toughening agent,
10 to 25 percent of high-temperature toughening curing agent,
1 to 5 percent of powder dispersant, and the sum of the components is 100 percent.
2. The base material for bipolar plates of all-vanadium flow batteries with acid and electrolyte resistance according to claim 1, wherein: the composite carbon-based conductive filler is one or more of graphite powder, carbon fiber, carbon nano tube, graphene and conductive carbon black.
3. The base material for bipolar plates of all-vanadium flow batteries with acid and electrolyte resistance according to claim 1, wherein: the thermosetting powder resin is one or more of phenolic resin, urea resin, melamine-formaldehyde resin, epoxy resin, unsaturated resin, polyurethane and polyimide.
4. The substrate for an all-vanadium flow battery bipolar plate having acid and electrolyte resistance as claimed in claim 1, wherein: the modified toughening agent is one or more of MBS toughening agent, CSR core-shell rubber toughening agent and closed isocyanate toughening agent.
5. The base material for bipolar plates of all-vanadium flow batteries with acid and electrolyte resistance according to claim 1, wherein: the high-temperature toughening curing agent is one or two of 2-phenylimidazoline and modified imidazole addition compound.
6. The apparatus of claim 1 having: the acid-resistant electrolyte-resistant base material for the bipolar plate substrate of the all-vanadium redox flow battery is characterized in that: the powder dispersing agent is one or a mixture of acrylic block copolymers.
7. A method of preparing the bipolar plate substrate as set forth in any one of claims 1 to 6, wherein: the preparation method comprises the steps of firstly adding various required composite carbon-based conductive fillers into a 600-mesh granulator according to the proportion for grinding, repeatedly discharging materials through a 600-mesh screen until all powder materials pass through the 600-mesh screen, vacuumizing the materials into a high-efficiency mixer for high-speed stirring and mixing, uniformly stirring the materials to form a premix 1, mixing powdery thermosetting powder resin, a modified toughening agent and a high-temperature toughening curing agent into a premix 2 through the high-efficiency mixer according to the proportion, then spraying the powder of the premix 1 in the stirring process of the high-efficiency mixer through a powder spraying machine by using the premix 2, adding a powder dispersing agent into the mixed materials according to the proportion after the spraying is finished, and taking out all the powder materials after mixing for a period of time.
8. A biplate, characterized by: the method comprises the steps of rolling and molding the powder material prepared by the method of claim 7 through a roller press to form composite base material graphite plate sheets, then stacking a layer of metal sheet between the two composite base material graphite plate sheets, rolling and molding the stacked semi-finished product for the second time through the roller press to form a graphite metal sheet, directly pressing and molding the graphite metal sheet in a mold through a molding press, wherein the molding time is less than or equal to 1 minute, the molding thickness is less than or equal to 0.8mm, and putting the molded composite graphite metal plate into an oven to be cured to obtain the bipolar plate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210616870.6A CN115188982A (en) | 2022-06-01 | 2022-06-01 | All-vanadium redox flow battery bipolar plate base material with acid resistance and electrolyte resistance, bipolar plate and preparation method |
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| CN202210616870.6A CN115188982A (en) | 2022-06-01 | 2022-06-01 | All-vanadium redox flow battery bipolar plate base material with acid resistance and electrolyte resistance, bipolar plate and preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118522909A (en) * | 2024-07-19 | 2024-08-20 | 杭州德海艾科能源科技有限公司 | Preparation method of composite bipolar plate for vanadium battery |
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2022
- 2022-06-01 CN CN202210616870.6A patent/CN115188982A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118522909A (en) * | 2024-07-19 | 2024-08-20 | 杭州德海艾科能源科技有限公司 | Preparation method of composite bipolar plate for vanadium battery |
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