CN113659165A - Carbon-based composite conductive slurry, graphite plate and preparation method of graphite plate - Google Patents
Carbon-based composite conductive slurry, graphite plate and preparation method of graphite plate Download PDFInfo
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- CN113659165A CN113659165A CN202110897973.XA CN202110897973A CN113659165A CN 113659165 A CN113659165 A CN 113659165A CN 202110897973 A CN202110897973 A CN 202110897973A CN 113659165 A CN113659165 A CN 113659165A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 48
- 239000010439 graphite Substances 0.000 title claims abstract description 48
- 239000002002 slurry Substances 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims description 4
- 229920005989 resin Polymers 0.000 claims abstract description 18
- 239000011347 resin Substances 0.000 claims abstract description 18
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 16
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 12
- 238000001723 curing Methods 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 8
- 239000002109 single walled nanotube Substances 0.000 claims abstract description 8
- 238000007598 dipping method Methods 0.000 claims abstract description 6
- 238000005520 cutting process Methods 0.000 claims abstract description 4
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- 239000002245 particle Substances 0.000 claims abstract description 3
- -1 acrylate compound Chemical class 0.000 claims abstract 3
- 238000000034 method Methods 0.000 claims description 12
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 6
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- 238000000465 moulding Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- FSDNTQSJGHSJBG-UHFFFAOYSA-N piperidine-4-carbonitrile Chemical compound N#CC1CCNCC1 FSDNTQSJGHSJBG-UHFFFAOYSA-N 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims 1
- 230000004888 barrier function Effects 0.000 abstract description 3
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- 230000002708 enhancing effect Effects 0.000 abstract 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
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- 238000007731 hot pressing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
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Images
Classifications
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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
-
- 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
- H01M8/0243—Composites in the form of mixtures
-
- 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
- H01M8/0247—Collectors; Separators, e.g. bipolar separators; Interconnectors characterised by the form
-
- 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
Abstract
A carbon-based composite conductive composite slurry comprises a conductive carbon material, a resin binder and a catalyst. The conductive carbon material is mainly one or a mixture of acetylene black, graphene oxide, graphene and single-walled carbon nanotubes. The main component of the resin binder is acrylate compound, and the content of the acrylate compound is 85.0-99.5%; the content of the conductive carbon material is 3-10%. Cutting and compression molding the graphite felt and the expanded graphite sheet, dipping, curing and washing the conductive slurry to obtain the graphite bipolar plate. According to the invention, the conductive carbon material is dispersed in the impregnant, and the graphite bipolar plate has abundant conductive networks, so that the conductive and heat-conducting properties are further improved; in addition, the control of the carbon materials with different particle size ranges is beneficial to forming a curing center in the graphite plate, enhancing the gas and liquid barrier property of the polar plate and improving the yield of products.
Description
Technical Field
The invention relates to the field of fuel cells, in particular to carbon-based composite conductive slurry, a graphite plate and a preparation method thereof.
Background
The fuel cell can convert chemical energy of fuel and oxidant into electric energy, the energy conversion efficiency is not limited by the cycle theoretical efficiency of the Carnot heat engine, and the fuel cell has the advantages of high efficiency, environmental friendliness, quietness, high reliability and the like, and has wide development prospect in various fields.
The proton exchange membrane fuel cell has high power density, quick start and quick response to load change, and becomes an important development direction of energy in the field of transportation. The core component of the fuel cell is a membrane electrode material, and is formed by compounding a proton exchange membrane, a catalyst and a gas diffusion layer through a hot pressing process. The reaction gas, the anode is hydrogen and the cathode is air or oxygen, which is guided by the flow guide polar plate and then diffused to the surface of the catalyst by the gas diffusion layer to react, and the water of the reaction product passes out of the diffusion layer from the surface of the membrane electrode and then joins in the gas flow to be discharged.
Bipolar plates are a key component of proton exchange membrane fuel cells, accounting for 45% of the cost and 80% of the mass of the cell. Therefore, the bipolar plate plays an important role in heat dissipation of the proton exchange membrane fuel cell, in addition to supporting the cell, transporting the gas, and acting as a current collector in an external circuit. Materials for bipolar plates include graphite, metal and graphite-polymer composites, and non-porous, electrically conductive graphite plates are desirable for bipolar plate materials due to the excellent electrical conductivity and chemical stability of graphite. The oriented thermal conductivity of the graphite single crystal reaches 2000W/(mK), and the graphite single crystal is considered to be a novel heat conduction material with great development potential. However, the graphite plate which is processed by CNC of the conventional artificial graphite has larger rigidity and stronger brittleness, and is not easy to be processed too thin. At present, a molded graphite plate developed based on flexible graphite in the market is the mainstream development direction due to simple processing technology, low cost and easy large-scale production. The mould pressing plate has higher porosity, irregular pore size distribution and no guarantee of leakage of the polar plate, and can improve the strength and gas barrier after resin impregnation treatment. However, the non-uniformity of the resin filling causes variation in the overall conductivity, and the overall operational uniformity of the battery is degraded.
The existing method for improving the conductivity is to start from a graphite plate base material and improve the conductivity of a body by a modified material. For example, patent CN112038654 provides a method for preparing a corresponding electrode plate by mixing graphite oxide, graphene and a carbon material to prepare a slurry, and then performing hot press molding. The method can change and improve the conductivity, but the density and other characteristics of the graphene, the graphite oxide and the resin high polymer material are obviously different, and the dispersion and final molding are difficult to realize. In addition, patent CN109921051 improves the gas barrier and conductivity by placing an ultra-thin flexible graphene film between two graphite electrode plates. The cost of graphene films and how to ensure uniform distribution into the plates is relatively difficult to control, limiting large-scale production and application. It can be seen that the existing technical means can not really realize the production of the graphite plate with large scale, high reliability, high electrical conductivity and heat conductivity, and the related process and method are urgently needed to be solved.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the carbon-based composite conductive slurry developed based on the requirements of the fuel cell polar plate.
The technical principle of the invention is as follows:
the primary functions of the fuel cell plates include providing support for the cell, gas transport, and electrical and thermal conduction. The expanded graphite based on the porous structure has the characteristics of good corrosion resistance, low cost, easy processing and the like, and becomes a main development direction of the fuel cell pole plate. The carbon-based material in the carbon-based conductive slurry can be in contact with the expanded graphite substrate, so that a continuous carbon-carbon contact interface is provided, and the heat conduction and electric conductivity of the polar plate are improved; the resin binder can meet the requirements of the pole plate on strength and bending resistance after being cured.
The purpose of the invention can be realized by the following technical scheme: a carbon-based composite conductive paste comprises a conductive carbon material, a resin binder and a resin curing agent.
Preferably, the conductive carbon material comprises one or a mixture of acetylene black, graphene oxide, graphene and single-walled carbon nanotubes, the particle diameter range is 1-30um, and the weight content is 0.5-10.0%.
Preferably, the resin binder comprises any one of dipropylene glycol diacrylate, phenolic resin or methacrylate, and the weight content is 85.0-99.5%.
Preferably, the resin curing agent comprises azo compounds, preferably azobisisobutyronitrile and azobisisoheptonitrile, and the weight content of the azo compounds is 0.1-1.0%.
According to a second aspect of the present invention, there is provided a method for preparing a graphite electrode plate, comprising the steps of:
cutting, vacuum molding, dipping, cleaning and curing an expanded graphite plate with a certain thickness to obtain a graphite polar plate; in the dipping treatment process, the polar plate after compression molding is placed in a high-pressure tank and is subjected to vacuum, injection of carbon-based composite conductive slurry and pressurization treatment in sequence;
preferably, the pressure of the vacuum die pressing is 100-200T, and the vacuum degree is-10 to-50 Pa.
The impregnation conditions are as follows: the vacuum degree is-10 to-100 Pa, and the pressure is 0.5 to 10 Mpa; in order to make the carbon-based composite conductive slurry completely enter the porous graphite substrate, the carbon-based composite conductive slurry needs to be vacuumized and then pressurized.
Preferably, the curing conditions of the curing agent are as follows: the temperature is 70-100 deg.C, and the time is 90 min.
Compared with the prior art, the invention has the following advantages:
1. the carbon material in the resin binder is beneficial to forming a continuous conduction network and improving the electrical conductivity and the heat conduction performance of the polar plate.
2. The carbon material and the resin completely enter the gap of the expanded graphite substrate under the action of vacuum, and gaps with different aperture ranges are filled, so that the air tightness of the polar plate is improved;
drawings
FIG. 1 is an SEM image of the surface of a substrate after being treated with the conductive paste of example 1;
FIG. 2 is a flow chart of the production of a graphite sheet for a fuel cell according to the present invention.
Detailed Description
Example 1
Preparing carbon-based composite conductive slurry: calculated by weight percentage, the composite conductive slurry is prepared by fully stirring, mixing and dispersing 3% of graphene oxide (wherein the thickness of 60% of sheet layers is 2-10um, the thickness of 20% of sheet layers is less than 1um, and the thickness of 20% of sheet layers is less than 0.5um), 0.5% of single-walled carbon nanotube (SWNTs), 3% of isopropanol, 1% of azodiisobutyronitrile and the balance of methacrylate.
Preparing a graphite plate: an expanded graphite plate (Qingdao Haishan carbon Material Co., Ltd.) with a thickness of 6mm is cut, placed in a vacuum press machine for mould pressing (pressure 200T, vacuum degree-10 Pa), dipped (the pole plate after mould pressing is placed in a high-pressure tank, kept for 60min under vacuum (-50 Pa), injected with mixed conductive slurry, pressurized (nitrogen is introduced to maintain 0.9MPa and 90min), cleaned (oscillation cleaning in deionized water at 20 ℃), cured (water bath at 90 ℃ and standing for 90min) to prepare the graphite plate.
The SEM image of the substrate surface of the graphite plate is shown in figure 1, and the result in the SEM image shows that the single-walled carbon nanotubes are uniformly distributed in the substrate to form a three-dimensional conduction network structure, so that the electric conduction and heat conduction performance of the polar plate is improved. The plate material has the characteristics of 20.5MPa of bending strength, 5.0MPa of compressive strength and 6.5m omega cm of surface resistance in performance test2Thermal conductivity of 50Wm-1k-1(ii) a Air tightness test, leakage value: 2X 10-7cm3.cm-2.sec-1@He，50kPa。
Example 2
Preparing carbon-based composite conductive slurry: according to the weight percentage, the composite conductive slurry is prepared by fully stirring, mixing and dispersing 0.4% of graphene oxide (wherein the thickness of 60% of sheet layers is 2-10um, the thickness of 20% of sheet layers is less than 1um, and the thickness of 20% of sheet layers is less than 0.5um), 0.1% of single-walled carbon nanotube (SWNTs), 3% of isopropanol, 1% of azodiisobutyronitrile and the balance of methacrylate.
Preparing a graphite plate: expanded graphite sheet (6 mm in thickness) ((Qingdao Haishan carbon Material Co., Ltd.), cutting, placing in a vacuum press for mould pressing (pressure 100T, vacuum degree-50 Pa), dipping (placing the plate after mould pressing in a high-pressure tank, vacuum (-50Pa, maintaining time 60min), injecting mixed conductive slurry, pressurizing (introducing nitrogen to maintain 4.0MPa, 90min)), cleaning (30 ℃ deionized water), curing (100 ℃ water bath, standing for 90min) to obtain the graphite plate. The plate material has the characteristics of 22.5MPa of bending strength, 4.9MPa of compressive strength and 6.8m omega cm of surface resistance in performance test2The thermal conductivity is 47Wm-1k-1(ii) a Air tightness test, leakage value: 1.1X 10-7cm3.cm-2.sec-1@He，50kPa。
Comparative example
Preparing resin filling slurry: the methacrylate and 1% of azobisisobutyronitrile are fully stirred, mixed and dispersed to prepare filling slurry.
Preparing a graphite plate: an expanded graphite plate (Qingdao Haishan carbon material Co., Ltd.) with the thickness of 6mm is cut, placed in a vacuum press machine for mould pressing (the pressure is 100T, the vacuum degree is-50 Pa), dipped (the plate after mould pressing is placed in a high-pressure tank, vacuum is carried out, the mixed conductive slurry is injected, the pressure is 4.0MPa, the plate is cleaned (deionized water at the temperature of 30 ℃) and solidified (water bath at the temperature of 100 ℃ and standing for 90 minutes) to prepare the graphite plate. The plate material has the characteristics of 20.5MPa of bending strength, 3.8MPa of compressive strength and 11.4m omega cm of surface resistance in performance test2Thermal conductivity of 12Wm-1k-1(ii) a Air tightness test, leakage value: 3X 10-6cm3.cm- 2.sec-1@He，50kPa。
The comparison shows that the polar plate prepared by the technical scheme has obvious improvement on electric conduction, heat conduction and air tightness. The main raw material of the expanded graphite is natural graphite, and the pore size and the distribution of the prepared base material are uncontrollable. The carbon-based material can physically fill the aperture with the size equivalent to that of the carbon-based material, the aperture size of the base material is reduced, and the carbon-based material is filled and cured by resin, so that the compactness of the polar plate can be improved, and the gas blocking capability is improved.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. A carbon-based composite conductive paste is characterized by comprising a conductive carbon material, a resin binder and a resin curing agent.
2. The carbon-based composite conductive paste according to claim 1, wherein the conductive carbon material comprises one or more of acetylene black, graphene oxide, graphene and single-walled carbon nanotubes, the particle diameter ranges from 1um to 30um, and the weight content is 0.5-10.0%.
3. The carbon-based composite conductive paste according to claim 1, wherein the resin binder comprises dipropylene glycol diacrylate, phenolic resin and methacrylate, and the weight content is 85.0-99.5%.
4. The carbon-based composite conductive paste according to claim 1, wherein the resin curing agent comprises an azo compound, preferably azobisisobutyronitrile, azobisisoheptonitrile, in an amount of 0.1-1.0% by weight.
5. The preparation method of the graphite polar plate is characterized by comprising the following steps:
cutting, vacuum molding, dipping, cleaning and curing an expanded graphite plate with a certain thickness to obtain a graphite polar plate; the filling agent in the dipping treatment process is the carbon-based composite conductive slurry as defined in any one of claims 1 to 4.
6. The method for preparing a graphite electrode plate according to claim 5, wherein the vacuum molding conditions are as follows: the pressure is 100-200T, and the vacuum degree is-10 to-50 Pa.
7. The method for preparing a graphite electrode plate according to claim 5, wherein the impregnation conditions are as follows: the vacuum degree is-10 to-100 Pa, and the pressure is 0.5 to 10 Mpa.
8. The method for preparing the graphite plate according to claim 5, wherein the curing agent is cured under the following conditions: the temperature is 70-100 deg.C, and the time is 90 min.
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Cited By (1)
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|---|---|---|---|---|
| CN114094120A (en) * | 2021-11-23 | 2022-02-25 | 成都先进金属材料产业技术研究院股份有限公司 | Integrated graphite electrode for vanadium cell and vanadium cell |
| CN114094120B (en) * | 2021-11-23 | 2023-10-27 | 成都先进金属材料产业技术研究院股份有限公司 | Integrated graphite electrode for vanadium battery and vanadium battery |
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