CN112359328A - Surface treatment method for bipolar plate of fuel cell - Google Patents
Surface treatment method for bipolar plate of fuel cell Download PDFInfo
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- CN112359328A CN112359328A CN202011185570.4A CN202011185570A CN112359328A CN 112359328 A CN112359328 A CN 112359328A CN 202011185570 A CN202011185570 A CN 202011185570A CN 112359328 A CN112359328 A CN 112359328A
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- 238000000034 method Methods 0.000 title claims abstract description 46
- 239000000446 fuel Substances 0.000 title claims abstract description 29
- 238000004381 surface treatment Methods 0.000 title claims abstract description 19
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 89
- 238000004140 cleaning Methods 0.000 claims abstract description 34
- 238000007788 roughening Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 54
- 238000004544 sputter deposition Methods 0.000 claims description 33
- 229910052786 argon Inorganic materials 0.000 claims description 27
- 239000012528 membrane Substances 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000013077 target material Substances 0.000 claims description 19
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 12
- 238000007733 ion plating Methods 0.000 claims description 12
- 238000005240 physical vapour deposition Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 230000007704 transition Effects 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 31
- 150000002500 ions Chemical class 0.000 description 8
- 239000002184 metal Substances 0.000 description 7
- 238000005259 measurement Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000037351 starvation Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0635—Carbides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0223—Composites
- H01M8/0228—Composites in the form of layered or coated products
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- 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
- H01M8/0258—Collectors; Separators, e.g. bipolar separators; Interconnectors characterised by the configuration of channels, e.g. by the flow field of the reactant or coolant
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention provides a surface treatment method of a bipolar plate of a fuel cell, which comprises the following steps: s1, cleaning a bipolar plate; s2, drying the cleaned bipolar plate; s3, preparing a nanoscale conductive hydrophobic layer on the surface of the dried bipolar plate; s4, roughening the bipolar plate with the nanoscale conductive hydrophobic layer so as to improve the roughness of the nanoscale conductive hydrophobic layer; the method can effectively improve the hydrophobic property of the surface of the bipolar plate.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to a surface treatment method for a bipolar plate of a fuel cell.
Background
The fuel cell generates water (hereinafter referred to as product water) during operation, the bipolar plate surface of the current fuel cell has poor hydrophobic property, the water contact angle is mostly lower than 90 degrees, the water is hydrophilic, and the product water is easy to adhere to the bipolar plate surface. When the fuel cell is operated at a low power, less water is generated and thus adheres to the surfaces of the flow channels in the form of small water droplets, thereby maintaining smooth flow of gas in the flow channels. However, when the fuel cell is operated at rated power, a large amount of water is generated, the water exists in the flow channel in the form of water flow, the product water is difficult to timely drain out of the cell stack, so that the flow channel of the bipolar plate is blocked, a large pressure drop is caused, and the cell stack is subjected to water flooding and air starvation in severe cases, so that irreversible damage is caused to the cell stack. In addition, because the product water is slightly acidic, when the product water is attached to the surface of the metal bipolar plate for a long time, the corrosion of the metal bipolar plate can be accelerated under a high-temperature and humid environment, the resistance of the metal bipolar plate is increased, or a trace amount of metal ions are corroded from the surface of the metal bipolar plate, so that the catalyst is poisoned, and the performance of the galvanic pile is finally reduced. Moreover, when purging is performed, because the product water has a large adhesive force on the surfaces of the bipolar plate flow channels, the product water is difficult to rapidly blow out from the bipolar plate flow channels, so that the residual water on the surfaces of the bipolar plates can be frozen and even can damage the membrane electrode during low-temperature storage.
Therefore, if the hydrophobic property of the bipolar plate surface can be improved and the adhesion of the product water to the bipolar plate flow channel surface can be reduced, the above problems can be avoided.
Disclosure of Invention
In order to solve at least one of the above technical problems in the prior art, an object of the present invention is to provide a surface treatment method for a bipolar plate of a fuel cell, so as to improve the hydrophobic property of the surface of the bipolar plate.
In order to achieve the purpose, the invention adopts the following technical scheme:
a surface treatment method for a bipolar plate of a fuel cell comprises the following steps:
s1, cleaning a bipolar plate;
s2, drying the cleaned bipolar plate;
s3, preparing a nanoscale conductive hydrophobic layer on the surface of the dried bipolar plate;
and S4, roughening the bipolar plate with the nanoscale conductive hydrophobic layer so as to improve the roughness of the nanoscale conductive hydrophobic layer.
In the surface treatment method of the fuel cell bipolar plate, the roughness of the nanoscale conductive hydrophobic layer is 1 nm-100 nm.
In the surface treatment method of the fuel cell bipolar plate, the nanoscale conductive hydrophobic layer is an MAX phase hydrophobic layer, a TiN or TiC layer.
In the method for treating the surface of the bipolar plate of the fuel cell, the step S3 includes:
and preparing a nanoscale conductive hydrophobic layer on the surface of the bipolar plate by a physical vapor deposition method or a cathode discharge ion plating method.
In some embodiments, step S3 includes:
preparing an MAX phase hydrophobic membrane layer on the surface of the bipolar plate by using a physical vapor deposition method;
step S4 includes:
and carrying out vacuum heat treatment on the bipolar plate after the MAX phase hydrophobic membrane layer is prepared so as to improve the roughness of the MAX phase hydrophobic membrane layer.
Further, the process of preparing the MAX phase hydrophobic membrane layer on the surface of the bipolar plate by using a physical vapor deposition method comprises the following steps:
A1. at a temperature of 300 ℃ and 1X 10-3Cleaning the target material by using argon under the air pressure of below Pa; the target comprises a Ti target and a MAX phase composite target;
A2. at a temperature of 300 ℃ and 6.8X 10-2Cleaning the bipolar plate with argon under the air pressure of Pa or below;
A3. sputtering a Ti transition layer on the surface of the bipolar plate by using the Ti target at the temperature of 300 ℃ and under the pressure of 1.0 Pa;
A4. and sputtering a MAX phase hydrophobic layer on the surface of the bipolar plate by using a MAX phase composite target at the temperature of 300 ℃ and under the pressure of 1.0 Pa.
Further, the process of performing vacuum heat treatment on the bipolar plate after the preparation of the MAX phase hydrophobic membrane layer to improve the roughness of the MAX phase hydrophobic membrane layer comprises:
in a high vacuum heat treatment furnace at 1X 10-3 Heating to 500-1000 ℃ at the speed of 10 ℃/min under the air pressure below Pa, and then preserving heat for 1 h.
In some embodiments, step S3 includes:
and preparing a TiN or TiC layer on the bipolar plate by using a cathode discharge ion plating method.
Further, the process of preparing the TiN layer on the bipolar plate by using the cathode discharge ion plating method comprises the following steps:
B1. at a temperature of 300 ℃ and 1X 10-3Cleaning the Ti target material by using argon under the air pressure of below Pa;
B2. at a temperature of 300 ℃ and 6.8X 10-2Cleaning the bipolar plate by using argon under the pressure of Pa;
B3. and introducing nitrogen into the sputtering furnace at the temperature of 300 ℃ and under the pressure of 1.0 Pa, and sputtering the Ti target on the surface of the bipolar plate.
Further, the process of preparing the TiC layer on the bipolar plate by using the cathode discharge ion plating method comprises the following steps:
C1. at a temperature of 300 ℃ and 1X 10-3Cleaning the target material by using argon under the air pressure of below Pa; the target comprises a Ti target and a C target;
C2. at a temperature of 300 ℃ and 6.8X 10-2Cleaning the bipolar plate by using argon under the pressure of Pa;
C3. sputtering a Ti transition layer on the surface of the bipolar plate by using the Ti target at the temperature of 300 ℃ and under the pressure of 1.0 Pa;
C4. and performing superposition sputtering on the surface of the bipolar plate by using a C target and a Ti target at the same time at the temperature of 300 ℃ and under the pressure of 1.0 Pa.
Has the advantages that:
according to the method for processing the surface of the bipolar plate of the fuel cell, the nanoscale conductive hydrophobic layer is prepared on the surface of the bipolar plate so as to improve the hydrophobic property of the surface of the bipolar plate, and the roughening treatment is carried out on the bipolar plate so as to improve the roughness of the nanoscale conductive hydrophobic layer, so that the hydrophobic property of the surface of the bipolar plate is further improved; the method can effectively improve the hydrophobic property of the surface of the bipolar plate, thereby avoiding the product water from blocking the bipolar plate flow channel, reducing the probability of the metal bipolar plate being corroded by the product water, quickly discharging the residual water in the flow channel during purging, and being more beneficial to the low-temperature storage of the galvanic pile.
Drawings
Fig. 1 is a flowchart of a surface treatment method for a bipolar plate of a fuel cell according to an embodiment of the present invention.
Fig. 2 is a schematic illustration of the hydrophobic corners of the bipolar plate surface before an exemplary nanoscale conductive hydrophobic layer is prepared.
Fig. 3 is a schematic view of the hydrophobic angle of the surface of the bipolar plate after the preparation of the MAX phase hydrophobic membrane layer.
Fig. 4 is a schematic view of the hydrophobic angle of the surface of the bipolar plate after vacuum heat treatment of the bipolar plate after the MAX phase hydrophobic membrane layer is prepared.
Fig. 5 is a schematic view of the hydrophobic angle of the bipolar plate surface after the TiN layer is prepared.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, features defined as "first", "second", may explicitly or implicitly include one or more of the described features.
Referring to fig. 1, the present invention provides a surface treatment method for a bipolar plate of a fuel cell, including the steps of:
s1, cleaning a bipolar plate;
s2, drying the cleaned bipolar plate;
s3, preparing a nanoscale conductive hydrophobic layer on the surface of the dried bipolar plate;
and S4, roughening the bipolar plate with the nanoscale conductive hydrophobic layer so as to improve the roughness of the nanoscale conductive hydrophobic layer.
In the method, the nanoscale conductive hydrophobic layer is prepared on the surface of the bipolar plate to improve the hydrophobic property of the surface of the bipolar plate, and the roughening treatment is carried out on the bipolar plate to improve the roughness of the nanoscale conductive hydrophobic layer, so that the hydrophobic property of the surface of the bipolar plate is further improved; the method can effectively improve the hydrophobic property of the surface of the bipolar plate, thereby bringing the following advantages:
1. when the fuel cell works in a low-power state, a large amount of generated micro water drops can quickly take away water in a flow channel even with small gas flow due to the hydrophobic effect on the surface of the bipolar plate;
2. when the fuel cell works in a high-power state, the speed of generating micro water drops is greatly increased, and due to the hydrophobic effect on the surface of the bipolar plate, the gas flow is high, the speed is high, the water can be quickly taken away, and the micro water drops are prevented from being aggregated into water drops or water films to block the flow;
3. when the galvanic pile is purged, residual water in the flow channel can be quickly discharged, so that the galvanic pile is more favorable for low-temperature storage;
4. due to the hydrophobic effect of the surface of the bipolar plate, the contact area between water generated by reaction and the metal bipolar plate is greatly reduced, and the probability of corrosion of the metal bipolar plate is effectively reduced.
In some preferred embodiments, the nanoscale electrically conductive hydrophobic layer has a roughness in the range of 1 nm to 100 nm. The nanoscale electrically conductive hydrophobic layer in this range is preferably hydrophobic.
Wherein, the nanoscale conductive hydrophobic layer is an MAX phase hydrophobic layer, a TiN or TiC layer. The hydrophobic performance and the conductive performance of the bipolar plate are better, and the influence on the conductive performance of the bipolar plate is smaller. Preferably, the nanoscale electrically conductive hydrophobic layer has a thickness of less than 1 μm.
In some embodiments, the cleaning process for the bipolar plate in step S1 includes: washing with neutral detergent several times, washing with anhydrous ethanol several times, and washing with deionized water several times.
In some embodiments, step S3 includes:
the nano-scale conductive hydrophobic layer is prepared on the surface of the bipolar plate by a physical vapor deposition method or a cathode discharge ion plating method.
The method for preparing the nano-scale conductive hydrophobic layer on the surface of the bipolar plate is not limited thereto, and for example, electroplating, CVD, PLD, or the like may be used.
In some embodiments, step S3 includes:
preparing an MAX phase hydrophobic film layer on the surface of the bipolar plate by using a physical vapor deposition method;
step S4 includes:
and carrying out vacuum heat treatment (belonging to one type of roughening treatment) on the bipolar plate after the MAX phase hydrophobic film layer is prepared so as to improve the roughness of the MAX phase hydrophobic film layer.
Further, the process of preparing the MAX phase hydrophobic membrane layer on the surface of the bipolar plate by using a physical vapor deposition method comprises the following steps:
A1. at a temperature of 300 ℃ and 1X 10-3Cleaning the target material by using argon under the air pressure of below Pa; the target comprises a Ti target and a MAX phase composite target;
specifically, after the bipolar plate is placed in a sample holder of a sputtering furnace, the bipolar plate is covered by a baffle plate, and heating and vacuumizing are carried out to ensure that the temperature in the furnace reaches 300 ℃ and the air pressure reaches 1 multiplied by 10-3Less than Pa (pumped to less than 5 Pa by mechanical pump, and pumped to 1 × 10 by molecular pump-3Below Pa), introducing argon into the furnace to start cleaning the target material, wherein the flow rate is 35 sccm; turning on an ion source power supply during cleaning, and setting the current to be 2.0A and the power to be 70% of rated power; turning on a bias power supply, setting the voltage of the bias power supply to be 200V and the duty ratio to be 50%; and (4) connecting the target with a direct current power supply, setting the current of the target to be 6.0A, and turning off the target power supply after the sputtering cleaning time is 15 min.
A2. At a temperature of 300 ℃ and 1X 10-3 Cleaning the bipolar plate by using argon under the air pressure of below Pa;
specifically, the temperature in the furnace is maintained at 300 deg.C, and the temperature is adjustedThe air pressure in the throttle is 6.8 multiplied by 10-2Pa, removing the baffle, and introducing argon into the furnace to clean the surface of the bipolar plate, wherein the flow rate is 35 sccm; rotating the sample holder and rotating the sample holder at a constant speed of 2 rpm; turning on an ion source, setting the current of the ion source to be 0.5A and the power to be 70% of rated power; and starting a bias power supply, setting the voltage of the bias power supply to be 200V, setting the duty ratio to be 50%, and setting the sputtering cleaning time to be 15 min.
A3. Sputtering a Ti transition layer on the surface of the bipolar plate by using a Ti target at the temperature of 300 ℃ and under the pressure of 1.0 Pa;
specifically, the temperature in the furnace is kept at 300 ℃, and the air pressure in the furnace is adjusted to be 1.0 Pa; introducing argon into the furnace, wherein the flow rate is 75 sccm; and (3) turning on a Ti target power supply, setting a constant power mode, starting sputtering the Ti transition layer with the power of 2.5kw and the duty ratio of 60 percent for 15 min.
A4. Sputtering MAX phase hydrophobic layer on the surface of the bipolar plate by using MAX phase composite target material at the temperature of 300 ℃ and under the pressure of 1.0 Pa;
specifically, the temperature in the furnace is kept at 300 ℃, and the pressure in the furnace is kept at 1.0 Pa; introducing argon into the furnace, wherein the flow rate is 75 sccm; turning on a power supply of the MAX phase composite target, and sputtering in a constant power mode, wherein the power is 3kW, the duty ratio is 40%, and the sputtering time is 60-90 min
Further, the process of performing vacuum heat treatment on the bipolar plate after the preparation of the MAX phase hydrophobic membrane layer so as to improve the roughness of the MAX phase hydrophobic membrane layer comprises the following steps:
in a high vacuum heat treatment furnace at 1X 10-3Heating to 500-1000 ℃ at the speed of 10 ℃/min under the air pressure below Pa, and then preserving heat for 1 h.
Specifically, the bipolar plate is placed in a high vacuum heat treatment furnace, and the furnace is evacuated to 1 × 10-3Heating to 500-1000 ℃ at the speed of 10 ℃/min under Pa, preserving heat for 1h, cooling along with the furnace, and taking out.
In this embodiment, the measurement results of the surface hydrophobic angle of the bipolar plate before the preparation of the MAX phase hydrophobic membrane layer (in this example, the bipolar plate is a SS304 stainless steel plate) are shown in fig. 2, the hydrophobic angle is 59.6 °, and the hydrophobicity is poor; the measurement result of the surface hydrophobic angle of the bipolar plate after the MAX phase hydrophobic membrane layer is prepared is shown in figure 3, and the hydrophobic angle is 73.6 degrees at the moment; the measurement results of the surface hydrophobic angle of the bipolar plate after vacuum heat treatment are shown in fig. 4, where the hydrophobic angle is 101.3 °. It can be seen that the hydrophobic properties of the bipolar plate treated by the above steps are greatly improved. And after vacuum heat treatment, the bonding force between the MAX phase hydrophobic membrane layer and the bipolar plate is stronger.
In some embodiments, step S3 includes:
and preparing a TiN or TiC layer on the bipolar plate by using a cathode discharge ion plating method.
Further, the process of preparing the TiN layer on the bipolar plate by using the cathode discharge ion plating method comprises the following steps:
B1. at a temperature of 300 ℃ and 1X 10-3Cleaning the Ti target material by using argon under the air pressure of below Pa;
specifically, the bipolar plate is placed on a sample holder of a sputtering furnace, covered by a baffle plate, heated and vacuumized to reach a temperature of 300 ℃ and a pressure of 1 × 10-3Pa below; and then introducing argon into the furnace to start cleaning the target material, introducing a direct current power supply to the target material, controlling the current to be 6.0A, performing sputtering cleaning for 15 min, and closing the power supply of the target material.
B2. At a temperature of 300 ℃ and 6.8X 10-2Cleaning the bipolar plate by using argon under the pressure of Pa;
specifically, the sample surface baffle plate was removed, the temperature in the furnace was maintained at 300 ℃ and the pressure in the furnace was adjusted to 6.8X 10-2Pa, removing the baffle, and introducing argon into the furnace to clean the surface of the bipolar plate, wherein the flow rate is 35 sccm; rotating the sample holder and rotating the sample holder at a constant speed of 2 rpm; turning on an ion source, setting the current of the ion source to be 0.5A and the power to be 70% of rated power; and starting a bias power supply, setting the voltage of the bias power supply to be 200V, setting the duty ratio to be 50%, and setting the sputtering cleaning time to be 15 min.
B3. Introducing nitrogen into the sputtering furnace at the temperature of 300 ℃ and under the pressure of 1.0 Pa, and sputtering the surface of the bipolar plate by using a Ti target material.
Specifically, the temperature in the furnace is kept at 300 ℃, and the pressure in the furnace is kept at 1.0 Pa; and introducing nitrogen into the furnace at the flow rate of 100sccm, turning on a Ti target power supply, setting a constant power mode, wherein the power is 2.5kw, the duty ratio is 60%, and the sputtering time is 15 min.
In this embodiment, the measurement results of the surface hydrophobic angle of the bipolar plate before the TiN layer was prepared (the bipolar plate in this example was a SS304 stainless steel plate) are shown in fig. 2, the hydrophobic angle was 59.6 °, and the hydrophobicity was poor; the measurement result of the surface hydrophobic angle of the bipolar plate after the TiN layer was prepared is shown in fig. 5, where the hydrophobic angle was 89.4 °. It can be seen that the hydrophobic properties of the bipolar plate treated by the above steps are greatly improved.
Further, the process of preparing the TiC layer on the bipolar plate by using the cathode discharge ion plating method comprises the following steps:
C1. at a temperature of 300 ℃ and 1X 10-3Cleaning the target material by using argon under the air pressure of below Pa; the target material comprises a Ti target material and a C target material;
specifically, after the bipolar plate is placed in a sample holder of a sputtering furnace, the bipolar plate is covered by a baffle plate, and heating and vacuumizing are carried out to ensure that the temperature in the furnace reaches 300 ℃ and the air pressure reaches 1 multiplied by 10-3Introducing argon into the furnace to start cleaning the target material with the flow of 35 sccm below Pa; turning on an ion source power supply during cleaning, and setting the current to be 2.0A and the power to be 70% of rated power; turning on a bias power supply, setting the voltage of the bias power supply to be 200V and the duty ratio to be 50%; and (4) connecting the target with a direct current power supply, setting the current of the target to be 6.0A, and turning off the target power supply after the sputtering cleaning time is 15 min.
C2. At a temperature of 300 ℃ and 6.8X 10-2Cleaning the bipolar plate by using argon under the pressure of Pa;
specifically, the temperature in the furnace is maintained at 300 ℃ and the pressure in the furnace is adjusted to 6.8X 10-2Pa, removing the baffle, and introducing argon into the furnace to clean the surface of the bipolar plate, wherein the flow rate is 35 sccm; rotating the sample holder and rotating the sample holder at a constant speed of 2 rpm; turning on an ion source, setting the current of the ion source to be 0.5A and the power to be 70% of rated power; and starting a bias power supply, setting the voltage of the bias power supply to be 200V, setting the duty ratio to be 50%, and setting the sputtering cleaning time to be 15 min.
C3. Sputtering a Ti transition layer on the surface of the bipolar plate by using a Ti target at the temperature of 300 ℃ and under the pressure of 1.0 Pa;
specifically, the temperature in the furnace is kept at 300 ℃, and the air pressure in the furnace is adjusted to be 1.0 Pa; introducing argon into the furnace, wherein the flow rate is 75 sccm; and (3) turning on a Ti target power supply, setting a constant power mode, starting sputtering the Ti transition layer with the power of 2.5kw and the duty ratio of 60 percent for 15 min.
C4. Performing superposition sputtering on the surface of the bipolar plate by using a C target and a Ti target at the temperature of 300 ℃ and under the pressure of 1.0 Pa;
specifically, the temperature in the furnace is kept at 300 ℃, and the pressure in the furnace is kept at 1.0 Pa; and (3) turning on a C target power supply, setting a constant power mode, setting the power to be 3kw and the duty ratio to be 40%, and keeping the Ti target power supply in the constant power mode, setting the power to be 2.5kw and the duty ratio to be 60%, and keeping the sputtering time to be 15 min.
In summary, although the present invention has been described with reference to the preferred embodiments, the above-described preferred embodiments are not intended to limit the present invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention, which are substantially the same as the present invention.
Claims (10)
1. A surface treatment method for a bipolar plate of a fuel cell, comprising the steps of:
s1, cleaning a bipolar plate;
s2, drying the cleaned bipolar plate;
s3, preparing a nanoscale conductive hydrophobic layer on the surface of the dried bipolar plate;
and S4, roughening the bipolar plate with the nanoscale conductive hydrophobic layer so as to improve the roughness of the nanoscale conductive hydrophobic layer.
2. The fuel cell bipolar plate surface treatment method according to claim 1, wherein the nanoscale electrically conductive hydrophobic layer has a roughness of 1 nm to 100 nm.
3. The surface treatment method for the bipolar plate of the fuel cell according to claim 1, wherein the nanoscale conductive hydrophobic layer is a MAX phase hydrophobic layer, a TiN layer or a TiC layer.
4. The fuel cell bipolar plate surface treatment method according to claim 1, wherein step S3 includes:
and preparing a nanoscale conductive hydrophobic layer on the surface of the bipolar plate by a physical vapor deposition method or a cathode discharge ion plating method.
5. The fuel cell bipolar plate surface treatment method according to claim 1, wherein step S3 includes:
preparing an MAX phase hydrophobic membrane layer on the surface of the bipolar plate by using a physical vapor deposition method;
step S4 includes:
and carrying out vacuum heat treatment on the bipolar plate after the MAX phase hydrophobic membrane layer is prepared so as to improve the roughness of the MAX phase hydrophobic membrane layer.
6. The surface treatment method of the bipolar plate of the fuel cell according to claim 5, wherein the process of preparing the MAX phase hydrophobic membrane layer on the surface of the bipolar plate by using the physical vapor deposition method comprises the following steps:
A1. at a temperature of 300 ℃ and 1X 10-3Cleaning the target material by using argon under the air pressure of below Pa; the target comprises a Ti target and a MAX phase composite target;
A2. at a temperature of 300 ℃ and 6.8X 10-2Cleaning the bipolar plate by using argon under the pressure of Pa;
A3. sputtering a Ti transition layer on the surface of the bipolar plate by using the Ti target at the temperature of 300 ℃ and under the pressure of 1.0 Pa;
A4. and sputtering a MAX phase hydrophobic layer on the surface of the bipolar plate by using a MAX phase composite target at the temperature of 300 ℃ and under the pressure of 1.0 Pa.
7. The method for processing the surface of the bipolar plate of the fuel cell according to claim 5, wherein the step of performing vacuum heat treatment on the bipolar plate after the MAX phase hydrophobic membrane layer is prepared so as to improve the roughness of the MAX phase hydrophobic membrane layer comprises the following steps:
in a high vacuum heat treatment furnace at 1X 10-3Heating to 500-1000 ℃ at the speed of 10 ℃/min under the air pressure below Pa, and then preserving heat for 1 h.
8. The fuel cell bipolar plate surface treatment method according to claim 1, wherein step S3 includes:
and preparing a TiN or TiC layer on the bipolar plate by using a cathode discharge ion plating method.
9. The surface treatment method of a fuel cell bipolar plate according to claim 8, wherein the preparing of the TiN layer on the bipolar plate using a cathode discharge ion plating method comprises:
B1. at a temperature of 300 ℃ and 1X 10-3Cleaning the Ti target material by using argon under the air pressure of below Pa;
B2. at a temperature of 300 ℃ and 6.8X 10-2Cleaning the bipolar plate by using argon under the pressure of Pa;
B3. and introducing nitrogen into the sputtering furnace at the temperature of 300 ℃ and under the pressure of 1.0 Pa, and sputtering the Ti target on the surface of the bipolar plate.
10. The surface treatment method for the bipolar plate of the fuel cell according to claim 8, wherein the step of preparing the TiC layer on the bipolar plate by using a cathode discharge ion plating method comprises:
C1. at a temperature of 300 ℃ and 1X 10-3 Cleaning the target material by using argon under the air pressure of below Pa; the target comprises a Ti target and a C target;
C2. at a temperature of 300 ℃ and 6.8X 10-2Cleaning the bipolar plate by using argon under the pressure of Pa;
C3. sputtering a Ti transition layer on the surface of the bipolar plate by using the Ti target at the temperature of 300 ℃ and under the pressure of 1.0 Pa;
C4. and performing superposition sputtering on the surface of the bipolar plate by using a C target and a Ti target at the same time at the temperature of 300 ℃ and under the pressure of 1.0 Pa.
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