CN113224339B - Flexible ultrathin graphite bipolar plate and preparation method thereof - Google Patents
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Abstract
The invention discloses a flexible ultrathin graphite bipolar plate and a preparation method thereof. The preparation method comprises the following steps: providing a graphite powder material, wherein the graphite powder material comprises expanded graphite, carbon fibers, carbon nanotubes and a low-viscosity liquid binder; providing a carbon nanotube film, and roughening the surface of the carbon nanotube film by adopting a physical or chemical method; and arranging graphite powder material layers formed by the graphite powder materials on the surfaces of two sides of the carbon nanotube film, and combining the two graphite powder material layers and the carbon nanotube film by adopting a hot pressing mode to form the flexible ultrathin graphite bipolar plate. The preparation method of the flexible ultrathin graphite bipolar plate provided by the embodiment of the invention uses the carbon nanotube film, thereby greatly reducing the hydrogen permeability of the bipolar plate and simultaneously ensuring that the bipolar plate has good flexibility and strength.
Description
Technical Field
The invention relates to a bipolar plate, in particular to a flexible ultrathin graphite bipolar plate and a preparation method thereof, belonging to the technical field of fuel cells.
Background
The fuel cell has wide development prospect and can be widely applied to the fields of distributed power generation systems, electric automobiles and the like. The fuel cell bipolar plate is composed of a polar plate and a flow field, mainly has the functions of gas distribution, current collection, heat conduction and sealing, the performance of the bipolar plate determines the volume specific power and the mass specific power of a fuel cell stack, the bipolar plate is a core component of a fuel cell, and the weight of the bipolar plate accounts for 70-80% of the whole fuel cell stack.
The current bipolar plates are mainly divided into two types, namely graphite bipolar plates and metal alloy bipolar plates, the graphite bipolar plates are mainly in the market of fuel cells due to excellent chemical stability and low price, and are mainly formed by heating and pressing graphite, resin and other binders, so that the bipolar plates have very wide market space. With the trend of fuel cell lightening, higher requirements are put on the production of bipolar plates, the thickness of the bipolar plates is reduced to below 1mm at present, and therefore, higher requirements are put on production raw materials and processes.
In the prior art, solid resin powder and graphite powder are mainly uniformly mixed and are subjected to hot pressing to prepare the graphite bipolar plate, wherein the resin powder mainly plays a role in binding graphite, and thermoplastic resin is mainly used.
Disclosure of Invention
The invention mainly aims to provide a flexible ultrathin graphite bipolar plate and a preparation method thereof, so as to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a preparation method of a flexible ultrathin graphite bipolar plate, which comprises the following steps:
providing a graphite powder material, wherein the graphite powder material comprises expanded graphite, carbon fibers, carbon nanotubes and a low-viscosity liquid binder;
providing a carbon nanotube film, and roughening the surface of the carbon nanotube film by adopting a physical or chemical method;
and arranging graphite powder material layers formed by the graphite powder materials on the surfaces of two sides of the carbon nanotube film, and combining the two graphite powder material layers and the carbon nanotube film by adopting a hot pressing mode to form the flexible ultrathin graphite bipolar plate.
The embodiment of the invention also provides the flexible ultrathin graphite bipolar plate prepared by the preparation method.
Compared with the prior art, the invention has the advantages that:
1) according to the preparation method of the flexible ultrathin graphite bipolar plate, the highly compact carbon nanotube film is used, and the carbon nanotube has the capability of storing hydrogen and avoiding hydrogen leakage according to a literature report, so that the hydrogen permeability of the bipolar plate is greatly reduced, and the bipolar plate has good flexibility and strength;
2) the invention uses hot pressing technology to solidify the liquid binder at high temperature, which is convenient for the demoulding and forming of the bipolar plate;
3) the bipolar plate prepared by the embodiment of the invention has a sandwich three-layer structure, wherein the middle layer is a carbon nanotube film, so that the tensile breaking strength is very high, and compared with a graphite bipolar plate, the conductivity of the bipolar plate provided by the embodiment of the invention can be improved by 2 orders of magnitude at most;
4) according to the preparation method of the flexible ultrathin graphite bipolar plate provided by the embodiment of the invention, the bipolar plate is calcined under the condition of inert gas, so that the liquid binder is graphitized, and the conductivity of the bipolar plate is increased.
Drawings
Fig. 1 is a schematic structural view of a flexible ultra-thin graphite bipolar plate provided in an exemplary embodiment of the present invention.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide technical solutions of the present invention. The technical solution, its implementation and principles, etc. will be further explained as follows.
The embodiment of the invention provides a preparation method of a flexible ultrathin graphite bipolar plate, which comprises the following steps:
providing a graphite powder material, wherein the graphite powder material comprises expanded graphite, carbon fibers, carbon nanotubes and a low-viscosity liquid binder;
providing a carbon nanotube film, and roughening the surface of the carbon nanotube film by adopting a physical or chemical method;
and arranging graphite powder material layers formed by the graphite powder materials on the surfaces of two sides of the carbon nanotube film, and combining the two graphite powder material layers and the carbon nanotube film by adopting a hot pressing mode to form the flexible ultrathin graphite bipolar plate.
Further, the hot pressing pressure is 5-22MPa, the temperature is 100-250 ℃, and the time is 1-30 min.
Furthermore, the preparation method of the flexible ultrathin graphite bipolar plate further comprises the following steps: and calcining the flexible ultrathin graphite bipolar plate under the inert gas atmosphere condition.
Furthermore, the calcining temperature is 800-2500 ℃, and the time is 1-20 h.
Further, the chemical method comprises hydroxylation treatment on the surface of the carbon nanotube film, and the physical method comprises processing a plurality of grooves or holes on the surface of the carbon nanotube film.
Furthermore, the preparation method of the flexible ultrathin graphite bipolar plate further comprises the following steps: and processing the surface of the flexible ultrathin graphite bipolar plate to form a flow channel structure, wherein the flow channel structure is a snake-shaped flow channel structure.
Further, the preparation method of the flexible ultrathin graphite bipolar plate specifically comprises the following steps:
the method comprises the steps of mixing expanded graphite, carbon fibers and carbon nanotubes to form a powder material, and mixing the graphite powder material with a low-viscosity liquid binder to form a wet graphite powder material.
Further, the graphite powder material comprises 70-90wt% of expanded graphite, 5-20wt% of carbon fiber and 5-10wt% of carbon nano tube, and the amount of the low-viscosity liquid binder is 5-20% of the total mass of the powder material.
Further, the low viscosity liquid binder has a viscosity of less than 10 mpa.s.
Further, the low-viscosity liquid binder includes any one or a combination of two or more of a special phenol resin, a special melamine resin, a special epoxy resin, a special furan resin and a special urea resin, but is not limited thereto.
Further, the preparation method of the flexible ultrathin graphite bipolar plate further comprises the following steps: drying the wet graphite powder material at 40-60 ℃ for 1-10h to control the water content of the graphite powder material within 1%
The embodiment of the invention also provides the flexible ultrathin graphite bipolar plate prepared by the preparation method.
Further, the flexible ultrathin graphite bipolar plate comprises a first graphite layer, a carbon nanotube film layer and a second graphite layer which are sequentially stacked, wherein the first graphite layer and the second graphite layer are formed by graphite powder materials; the thickness of the carbon nano tube film layer is 0.05-0.1mm, and the thickness of the first graphite layer and the second graphite layer is 0.1-0.8 mm.
Further, the flexible ultrathin graphite bipolar plate has the density of 100-185g/cc, the conductivity of 100-310S/cm and the tensile strength of 100-300MPa, and is airtight under the negative pressure condition of 0.3-1 MPa.
Furthermore, the thickness of the flexible ultrathin graphite bipolar plate is 0.5-2 mm.
In the following, the technical scheme, the implementation process and the principle thereof will be further explained with reference to the drawings, and the manufacturing raw materials, the calcination, the roughening treatment, the testing method and the like used in the embodiments of the present invention may be any existing raw materials known to those skilled in the art unless otherwise specified.
Referring to fig. 1, a flexible ultra-thin graphite bipolar plate includes a first graphite layer, a carbon nanotube film layer and a second graphite layer, which are sequentially stacked, wherein the carbon nanotube film layer includes a plurality of carbon nanotubes, the thickness of the carbon nanotube film layer is 0.05-0.1mm, and the thickness of the first graphite layer and the second graphite layer is 0.1-0.8 mm.
Specifically, the flexible ultrathin graphite bipolar plate has the density of 100-185g/cc, the conductivity of 100-310S/cm and the tensile strength of 100-300MPa, and is airtight under the negative pressure condition of 0.3-1 MPa.
Specifically, the thickness of the flexible ultrathin graphite bipolar plate is 0.5-2mm, and a snake-shaped flow channel structure is formed on the surface of the flexible ultrathin graphite bipolar plate.
In some more specific embodiments, a method for preparing a flexible ultra-thin graphite bipolar plate comprises the following steps:
1) mixing expanded graphite, carbon fibers and carbon nanotubes according to a certain proportion to form a powder material, adding a low-viscosity liquid binder, and mixing and stirring for 2-5 hours to form a wet graphite powder material; wherein, the mass ratios of the expanded graphite, the carbon fiber and the carbon nano tube in the graphite powder material are respectively 70-90%, 20-5% and 10-5%, the liquid binder is any one or the combination of more than two of special phenolic resin, special melamine resin, special epoxy resin, special furan resin and special urea resin, and the addition amount of the liquid binder is 5-20% of the total mass of the powder material;
2) baking the uniformly mixed wet graphite powder material at 40-60 ℃ for 1-10 hours to remove a small amount of liquid solvent and control the water content in the graphite powder material within 1%;
3) roughening the surface of the carbon nano-tube film by adopting a physical or chemical method so as to enhance the interface bonding force between the carbon nano-tube film and the graphite powder; the chemical method comprises the step of carrying out hydroxylation treatment on the surface of the carbon nano tube film by using a mixed solution of sulfuric acid and hydrogen peroxide, and the physical method comprises the step of punching holes on the surface of the carbon nano tube by using a laser marking machine and the like;
4) firstly, laying a layer of graphite powder material in the step 2) on the surface of a mould, lightly pressing and flattening, then laying a layer of roughened carbon nanotube film, then laying a layer of graphite powder material in the step 2) on the carbon nanotube film, and carrying out hot-press forming by using the mould, wherein a liquid binder is cured at high temperature in the hot-press process, thereby forming a bipolar plate material; wherein the hot pressing pressure is 10-25MPa, the hot pressing temperature is 100-250 ℃, and the hot pressing time is 2-20 minutes; specifically, a mold with a flow channel on the surface can be used, and a proper amount of organic silicon release agent is sprayed on the surface of the mold before use, so that the bipolar plate with the flow channel can be obtained, wherein the thickness of the bipolar plate is 0.5-2 mm;
4) calcining the bipolar plate obtained in the step 4) at high temperature under the protection of inert gas, wherein the calcining temperature is 800-2500 ℃ and the calcining time is 1-20 hours, and the inert gas can be nitrogen, argon and the like.
Example 1 preparation of flexible ultra-thin graphite bipolar plate
1) Mixing 70 parts of expanded graphite, 20 parts of carbon fiber and 10 parts of carbon nano tube, adding 10 parts of liquid special phenolic resin binder, and mixing and stirring for 3 hours to moisten the powder;
2) baking the uniformly mixed wet powder at 50 ℃ for 2 hours to remove a small amount of liquid solvent;
3) putting the carbon nano tube in a hydrogen peroxide-sulfuric acid solution at 90 ℃ for heating for 2 hours to hydroxylate the surface of the carbon nano tube, wherein the treatment can increase the binding force between the carbon nano tube and the surface of graphite powder;
4) placing a proper amount of the powder material in the step 2) on the surface of a mould, slightly pressing and flattening, then laying a layer of carbon nanotube film, then adding a proper amount of the powder material in the step 2) on the nanotube film, and hot-pressing and molding by using the mould, wherein the hot-pressing pressure is 20MPa, the hot-pressing temperature is 200 ℃, the hot-pressing time is 5 minutes, and the liquid special phenolic resin is cured at high temperature in the process; the bipolar plate with the flow channel can be obtained by using a mold with a flow channel structure on the surface and spraying a proper amount of organic silicon release agent on the surface of the mold, wherein the thickness of the bipolar plate is 1 mm; the bipolar plate has a sandwich three-layer structure, the middle layer is a carbon nanotube film, and the tensile breaking strength is high;
5) calcining the bipolar plate in the step 4) for 5 hours at 2000 ℃ under the condition of nitrogen atmosphere, thereby obtaining the finished product of the graphite bipolar plate.
The graphite bipolar plate prepared in this example was subjected to a performance test, and the graphite bipolar plate in this example had a thickness of 1mm, an electrical conductivity of 310S/cm, a density of 1.85g/cc, an air permeability coefficient: the negative pressure is 0.4MPa, the air tightness is realized, and the tensile strength is 205 MPa.
Example 2 preparation of Flexible ultra-thin graphite Bipolar plate
1) Mixing 80 parts of expanded graphite, 10 parts of carbon fiber and 10 parts of carbon nano tube, adding 10 parts of liquid special melamine resin binder, and mixing and stirring for 4 hours to moisten the powder.
2) And (3) baking the uniformly mixed wet powder at 60 ℃ for 1 hour to remove a small amount of liquid solvent.
3) And (3) punching the surface of the carbon nano tube by using a laser marking machine to roughen the surface of the carbon nano tube so as to increase the bonding force between the carbon nano tube and the surface of the graphite powder.
4) Placing a proper amount of the powder material obtained in the step 2) on the surface of a mould, slightly pressing and flattening, then laying a layer of carbon nanotube film, then adding a proper amount of the powder material obtained in the step 2) on the nanotube film, and carrying out hot-press molding by using the mould, wherein the hot-press pressure is 22MPa, the hot-press temperature is 250 ℃, the hot-press time is 3 minutes, and the liquid is cured at high temperature in the process; the bipolar plate with the flow channel can be obtained by using a mold with a flow channel structure on the surface and spraying a proper amount of organic silicon release agent on the surface of the mold; the bipolar plate has a sandwich three-layer structure, the middle layer is a carbon nanotube film, and the tensile breaking strength is high;
5) calcining the plate in the step 4) for 4 hours at 2100 ℃ under the condition of nitrogen atmosphere, thereby obtaining the finished product of the graphite bipolar plate.
The graphite bipolar plate prepared in this example was subjected to a performance test, and the graphite bipolar plate in this example had a thickness of 1mm, an electrical conductivity of 330S/cm, a density of 1.88g/cc, an air permeability coefficient: the negative pressure is 0.4MPa, the air tightness is realized, and the tensile strength is 195 MPa.
The inventor also uses any one or the combination of more than two of special phenolic resin, special melamine resin, special epoxy resin, special furan resin and special urea resin as the binder, adjusts the dosage proportion of the expanded graphite, the carbon fiber, the carbon nanotube and the binder, the pressure and the temperature condition of hot pressing, obtains other graphite bipolar plates, and tests the performance of the graphite bipolar plates, and the test result is basically consistent with that in the embodiments 1 and 2.
The embodiment of the invention provides a flexible, high-strength and ultrathin graphite bipolar plate and a preparation method thereof.
According to the preparation method of the flexible ultrathin graphite bipolar plate provided by the embodiment of the invention, the bipolar plate is prepared by the carbon nanotube material and the special liquid adhesive resin (namely the liquid adhesive), and the carbon nanotube material can greatly increase the tensile breaking strength of the bipolar plate; the invention mixes the expanded graphite, the carbon fiber, the carbon nano tube and the liquid binder and then carries out low-temperature baking pretreatment, can remove a small amount of solvent, reduces the porosity and is convenient for industrial production.
The preparation method of the flexible ultrathin graphite bipolar plate provided by the embodiment of the invention also performs roughening treatment on the surface of the carbon nano tube, can enhance the interface bonding force between the carbon nano tube film and the graphite powder material, and can control the air tightness of the bipolar plate through roughening treatment on the carbon nano tube film.
According to the preparation method of the flexible ultrathin graphite bipolar plate provided by the embodiment of the invention, the carbon nanotube film is used, so that the hydrogen permeability of the bipolar plate is greatly reduced, and the bipolar plate has good flexibility and strength; meanwhile, the invention uses hot pressing technology to solidify the liquid binder at high temperature, which is convenient for the demoulding and forming of the bipolar plate; the bipolar plate prepared by the embodiment of the invention has a sandwich three-layer structure, the middle layer is a carbon nanotube film, the tensile breaking strength is very high, and compared with a graphite bipolar plate, the conductivity of the bipolar plate provided by the embodiment of the invention can be improved by 2 orders of magnitude at most.
According to the preparation method of the flexible ultrathin graphite bipolar plate provided by the embodiment of the invention, the bipolar plate is calcined under the condition of inert gas, so that the liquid binder is graphitized, and the conductivity of the bipolar plate is increased.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (11)
1. A preparation method of a flexible ultrathin graphite bipolar plate is characterized by comprising the following steps:
providing a graphite powder material, wherein the graphite powder material comprises expanded graphite, carbon fibers, carbon nanotubes and a low-viscosity liquid binder;
providing a carbon nanotube film, and roughening the surface of the carbon nanotube film by a physical or chemical method, wherein the chemical method comprises hydroxylation treatment on the surface of the carbon nanotube film, and the physical method comprises processing a plurality of grooves or holes on the surface of the carbon nanotube film;
arranging graphite powder material layers formed by the graphite powder materials on the surfaces of two sides of a carbon nano tube film, and combining the two graphite powder material layers and the carbon nano tube film by adopting a hot pressing mode to form a flexible ultrathin graphite bipolar plate, wherein the hot pressing pressure is 5-22MPa, the temperature is 100-250 ℃, and the time is 1-30 min;
and calcining the flexible ultrathin graphite bipolar plate under the inert gas atmosphere condition, wherein the calcining temperature is 800-2500 ℃ and the calcining time is 1-20 h.
2. The method for preparing a flexible ultra-thin graphite bipolar plate as claimed in claim 1, further comprising: and processing the surface of the flexible ultrathin graphite bipolar plate to form a flow channel structure.
3. The method for preparing a flexible ultra-thin graphite bipolar plate according to claim 1, comprising:
the method comprises the steps of mixing expanded graphite, carbon fibers and carbon nanotubes to form a powder material, and mixing the graphite powder material with a low-viscosity liquid binder to form a wet graphite powder material.
4. The method for preparing a flexible ultra-thin graphite bipolar plate as claimed in claim 3, wherein the graphite powder material comprises 70-90wt% of expanded graphite, 5-20wt% of carbon fiber and 5-10wt% of carbon nanotube, and the amount of the low viscosity liquid binder is 5-20% of the total mass of the powder material.
5. The method of preparing a flexible ultra-thin graphite bipolar plate according to claim 3, wherein the viscosity of the low viscosity liquid binder is less than 10 mPa.s.
6. The method for preparing the flexible ultra-thin graphite bipolar plate as claimed in claim 3, wherein the low viscosity liquid binder comprises any one or a combination of more than two of special phenolic resin, special melamine resin, special epoxy resin, special furan resin and special urea resin.
7. The method for preparing a flexible ultra-thin graphite bipolar plate as claimed in claim 3, further comprising: drying the wet graphite powder material at 40-60 ℃ for 1-10 h.
8. A flexible ultra-thin graphite bipolar plate produced by the production method as set forth in any one of claims 1 to 7.
9. The flexible ultra-thin graphite bipolar plate of claim 8, comprising a first graphite layer, a carbon nanotube film layer and a second graphite layer sequentially stacked, wherein the first graphite layer and the second graphite layer are formed by the graphite powder material; the thickness of the carbon nano tube film layer is 0.05-0.1mm, and the thickness of the first graphite layer and the second graphite layer is 0.1-0.8 mm.
10. The flexible ultra-thin graphite bipolar plate of claim 8, wherein: the flexible ultrathin graphite bipolar plate has the density of 100-185g/cc, the conductivity of 100-310S/cm and the tensile strength of 100-300MPa, and is airtight under the negative pressure condition of 0.3-1 MPa.
11. The flexible ultra-thin graphite bipolar plate of claim 8, wherein: the thickness of the flexible ultrathin graphite bipolar plate is 0.5-2 mm.
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| CN113745559B (en) * | 2021-09-22 | 2023-06-30 | 宁波信远材料科技股份有限公司 | Ultrathin carbon/carbon composite bipolar plate and preparation method thereof |
| CN114976097B (en) * | 2022-04-22 | 2024-02-27 | 同济大学 | Layered composite graphite polar plate for fuel cell and preparation method thereof |
| CN115000442A (en) * | 2022-06-08 | 2022-09-02 | 深圳市氢瑞燃料电池科技有限公司 | Fuel cell bipolar plate and preparation method thereof |
| CN114759210B (en) * | 2022-06-13 | 2022-09-02 | 湖南耕驰新能源科技有限公司 | Preparation method of bipolar plate |
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| TWI374568B (en) * | 2008-11-27 | 2012-10-11 | Univ Yuan Ze | Fabrication of metal meshes/carbon nanotubes/polymer composite bipolar plates for fuel cell |
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| CN101101994A (en) * | 2007-07-17 | 2008-01-09 | 武汉理工大学 | Expansion graphite base compound material dual-pole board and its making method |
| CN110676479A (en) * | 2018-07-03 | 2020-01-10 | 河北金雕新材料科技有限公司 | Full-vanadium redox flow battery bipolar plate and preparation method thereof |
| CN110289428A (en) * | 2019-06-19 | 2019-09-27 | 北京科技大学 | A kind of preparation of fuel cell stainless steel bi-polar plate and surface modifying method |
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