CN113445014A - Surface functional coating process for hydrogen fuel cell titanium bipolar plate - Google Patents
Surface functional coating process for hydrogen fuel cell titanium bipolar plate Download PDFInfo
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- CN113445014A CN113445014A CN202110748542.7A CN202110748542A CN113445014A CN 113445014 A CN113445014 A CN 113445014A CN 202110748542 A CN202110748542 A CN 202110748542A CN 113445014 A CN113445014 A CN 113445014A
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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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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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
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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
- C23C14/48—Ion implantation
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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
- H01M8/0206—Metals or alloys
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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
- H01M8/0206—Metals or alloys
- H01M8/0208—Alloys
- H01M8/021—Alloys based on iron
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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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- 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
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Abstract
The invention discloses a surface functional coating process of a hydrogen fuel cell titanium bipolar plate, which is completed according to the following steps: the method comprises the following steps: putting the workpiece into ultrasonic cleaning equipment to sequentially carry out ultrasonic oil removal cleaning, pure water ultrasonic cleaning, pure water rinsing, dewatering and hydrocarbon solvent vacuum ultrasonic cleaning; then heating and drying in vacuum; step two: preparing a modified layer on the surface of one side or two sides of a workpiece to obtain a modified stainless steel bipolar plate, wherein the modified layer can be made of one or more of titanium, vanadium, niobium, nickel, chromium and zirconium, the step is completed in a vacuum environment, and then a surface coating material is formed on the modified layer in an ion plating mode; one or more of titanium, vanadium, niobium, nickel, chromium and zirconium are covered on the carbon paper, so that the contact resistance and corrosion current between the stainless steel and the carbon paper are reduced, in addition, the thickness of the modified layer is obviously reduced compared with that of the stainless steel, the thickness of the modified layer is reduced, the method is easy to obtain, the mass production is convenient, and the cost is reduced.
Description
Technical Field
The invention relates to the technical field of bipolar plate coating, in particular to a surface functional coating process of a hydrogen fuel cell titanium bipolar plate.
Background
Bipolar plates, also known as collector plates, are one of the important components of fuel cells. The bipolar plate needs to be subjected to appropriate surface treatment (protective layer) to ensure its high efficiency and long-term use stability, thereby improving the electric power density of the fuel cell bipolar plate.
At present, the weight problem of the bipolar plate is effectively improved, but the base material of the bipolar plate adopting the lightweight design is mostly stainless steel or titanium alloy which is easy to passivate on the surface, and due to long-time use, the surface of the bipolar plate can cause serious loss and low strength, so that the surface resistance of the bipolar plate is easily and rapidly improved in the battery environment, and the standard of the battery use cannot be reached, and therefore, a large amount of coatings and modification technologies aiming at the surface modification of the metal polar plate appear.
Disclosure of Invention
In order to overcome the defects that the surface of a bipolar plate is likely to cause serious loss and low strength due to long-time use in the prior art, so that the surface resistance of the bipolar plate is easily and rapidly improved in a battery environment, the invention provides a surface functional coating process of a hydrogen fuel battery titanium bipolar plate, a base layer of a stainless steel material is firstly modified and prepared on one side or two sides of the base layer, and one or more of titanium, vanadium, niobium, nickel, chromium and zirconium is covered on the base layer, so that the contact resistance and corrosion current between stainless steel and carbon paper are reduced, in addition, the thickness of a modified layer is obviously reduced compared with the thickness of the stainless steel plate, the thickness of the modified layer is reduced, the method is easy to obtain, the mass production is convenient, the cost is reduced, the carbon ions or the titanium ions are covered on the modified layer by a PVD surface forming process method on the surface of the base layer, so that the corrosion resistance of the structure surface is improved, compared with the method of adding noble metal in the prior art, the method achieves lower contact resistance and corrosion current density than the prior art.
In order to solve the technical problems, the invention provides the following technical scheme: the surface functional coating process of the hydrogen fuel cell titanium bipolar plate is completed according to the following steps:
the method comprises the following steps: putting the workpiece into ultrasonic cleaning equipment to sequentially carry out ultrasonic oil removal cleaning, pure water ultrasonic cleaning, pure water rinsing, dewatering and hydrocarbon solvent vacuum ultrasonic cleaning; then heating and drying in vacuum;
step two: preparing a modified layer on the surface of one side or two sides of a workpiece to obtain a modified stainless steel bipolar plate, wherein the modified layer can be made of one or more of titanium, vanadium, niobium, nickel, chromium and zirconium, the step is completed in a vacuum environment, and then a surface coating material is formed on the modified layer in an ion plating mode;
step three; performing ion etching on the surface of one side or two sides of the workpiece by using a PVD magnetron sputtering coating machine;
step four: forming a transition layer containing the ions and the free-state ions on the surface of the etched modified layer by ion implantation, and completing the process in an argon atmosphere; the workpiece is sequentially provided with a base layer, a modified layer and a transition layer from the middle part to the outside;
step five: and forming a corrosion-resistant protective layer on the transition layer obtained in the fourth step by a PVD (physical vapor deposition) method, and forming a surface forming process by the PVD method.
As a preferred technical scheme of the invention, the vacuum cleaning degree in the step one is 100-200 Pa, the heating temperature is kept at 100 ℃ for 20 minutes, and the finally obtained workpiece has the dryness of 50-75 Pa.
As a preferred technical scheme of the invention, the thickness of the modified layer obtained in the second step is 10-50 nm, and the vacuum degree of ion plating is 0.001-0.01 Pa.
As a preferred embodiment of the present invention, the ion etching performed in the third step and the fourth step may use carbon ions, tungsten ions, and titanium ions.
As a preferred technical scheme of the invention, the PVD forming process adopts a high-purity tungsten target (not less than 99.5%), a high-purity titanium target (not less than 99.5%) and a high-purity graphite target (not less than 99.5%).
As a preferred technical scheme of the invention, the deposition time of the ion plating is 15-100 minutes, and the current intensity is 20-150 amperes.
As a preferable technical scheme of the invention, the workpiece is made of stainless steel materials.
Compared with the prior art, the invention can achieve the following beneficial effects:
1. according to the invention, the base layer of the stainless steel material is modified on one side or two sides of the base layer, and one or more of titanium, vanadium, niobium, nickel, chromium and zirconium is covered on the base layer, so that the contact resistance and corrosion current between the stainless steel and the carbon paper are reduced.
2. According to the invention, the modified layer is covered by carbon ions or titanium ions through a PVD surface forming process on the surface of the base layer, so that the corrosion resistance strength of the structure surface is improved, and compared with the existing method for adding precious metal, the method achieves lower contact resistance and corrosion current density than the prior art.
Drawings
FIG. 1 is a schematic flow chart of the process steps of the present invention.
Detailed Description
The present invention will be further described with reference to specific embodiments for the purpose of facilitating an understanding of technical means, characteristics of creation, objectives and functions realized by the present invention, but the following embodiments are only preferred embodiments of the present invention, and are not intended to be exhaustive. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention. The experimental methods in the following examples are conventional methods unless otherwise specified, and materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example (b):
the invention provides a surface functional coating process of a hydrogen fuel cell titanium bipolar plate, which is completed according to the following steps:
the method comprises the following steps: putting the workpiece into ultrasonic cleaning equipment to sequentially carry out ultrasonic oil removal cleaning, pure water ultrasonic cleaning, pure water rinsing, dewatering and hydrocarbon solvent vacuum ultrasonic cleaning; then heating and drying in vacuum;
step two: preparing a modified layer on the surface of one side or two sides of a workpiece to obtain a modified stainless steel bipolar plate, wherein the modified layer can be made of one or more of titanium, vanadium, niobium, nickel, chromium and zirconium, the step is completed in a vacuum environment, and then a surface coating material is formed on the modified layer in an ion plating mode;
step three; performing ion etching on the surface of one side or two sides of the workpiece by using a PVD magnetron sputtering coating machine;
step four: forming a transition layer containing the ions and the free-state ions on the surface of the etched modified layer by ion implantation, and completing the process in an argon atmosphere; the workpiece is sequentially provided with a base layer, a modified layer and a transition layer from the middle part to the outside;
step five: and forming a corrosion-resistant protective layer on the transition layer obtained in the fourth step by a PVD (physical vapor deposition) method, and forming a surface forming process by the PVD method.
In other embodiments, the vacuum cleaning degree in the first step is 100-.
In other embodiments, the thickness of the modified layer obtained in step two is 10 nm to 50 nm, and the vacuum degree of ion plating is 0.001 Pa to 0.01 Pa.
In other embodiments, the ion etching performed in step three and step four may use carbon ions or titanium ions.
In other embodiments, a high-purity tungsten target (not less than 99.5%), a high-purity titanium target (not less than 99.5%) and a high-purity graphite target (not less than 99.5%) are used in the PVD forming process.
In other embodiments, the deposition time of the ion plating is 15-100 minutes and the current intensity is 20-150 amperes.
In other embodiments, the workpiece is a stainless steel material.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. The surface functional coating process of the hydrogen fuel cell titanium bipolar plate is characterized in that: the process is completed according to the following steps:
the method comprises the following steps: putting the workpiece into ultrasonic cleaning equipment to sequentially carry out ultrasonic oil removal cleaning, pure water ultrasonic cleaning, pure water rinsing, dewatering and hydrocarbon solvent vacuum ultrasonic cleaning; then heating and drying in vacuum;
step two: preparing a modified layer on the surface of one side or two sides of a workpiece to obtain a modified stainless steel bipolar plate, wherein the modified layer can be made of one or more of titanium, vanadium, niobium, nickel, chromium and zirconium, the step is completed in a vacuum environment, and then a surface coating material is formed on the modified layer in an ion plating mode;
step three; performing ion etching on the surface of one side or two sides of the workpiece by using a PVD magnetron sputtering coating machine;
step four: forming a transition layer containing the ions and the free-state ions on the surface of the etched modified layer by ion implantation, and completing the process in an argon atmosphere; the workpiece is sequentially provided with a base layer, a modified layer and a transition layer from the middle part to the outside;
step five: and forming a corrosion-resistant protective layer on the transition layer obtained in the fourth step by a PVD (physical vapor deposition) method, and forming a surface forming process by the PVD method.
2. The surface functional coating process of the hydrogen fuel cell titanium bipolar plate as claimed in claim 1, wherein: the vacuum cleaning degree in the step one is 100-.
3. The surface functional coating process of the hydrogen fuel cell titanium bipolar plate as claimed in claim 1, wherein: the thickness of the modified layer obtained in the second step is 10-50 nanometers, and the vacuum degree of ion plating is 0.001-0.01 Pa.
4. The surface functional coating process of the hydrogen fuel cell titanium bipolar plate as claimed in claim 1, wherein: the ion etching performed in the third step and the fourth step may use carbon ions, tungsten ions, and titanium ions.
5. The surface functional coating process of the hydrogen fuel cell titanium bipolar plate as claimed in claim 1, wherein: the PVD forming process adopts a high-purity tungsten target material (not less than 99.5%), a high-purity titanium target material (not less than 99.5%) and a high-purity graphite target material (not less than 99.5%).
6. The surface functional coating process of the hydrogen fuel cell titanium bipolar plate as claimed in claim 1, wherein: the deposition time of the ion plating is 15-100 minutes, and the current intensity is 20-150 amperes.
7. The surface functional coating process of the hydrogen fuel cell titanium bipolar plate as claimed in claim 1, wherein: the workpiece is made of stainless steel materials.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110748542.7A CN113445014A (en) | 2021-07-02 | 2021-07-02 | Surface functional coating process for hydrogen fuel cell titanium bipolar plate |
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| CN202110748542.7A CN113445014A (en) | 2021-07-02 | 2021-07-02 | Surface functional coating process for hydrogen fuel cell titanium bipolar plate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114464818A (en) * | 2022-01-18 | 2022-05-10 | 哈尔滨工业大学 | Low-cost surface treatment method for improving surface performance of titanium and titanium alloy for proton exchange membrane fuel cell polar plate |
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| CN107302094A (en) * | 2017-06-15 | 2017-10-27 | 常州翊迈新材料科技有限公司 | Superconductive super-corrosion-resistant functional coating of fuel cell metal bipolar plate and preparation method thereof |
| CN108574107A (en) * | 2018-03-16 | 2018-09-25 | 上海交通大学 | Improve fuel battery double plates carbide coating conduction and corrosion proof method |
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| CN112111716A (en) * | 2020-08-14 | 2020-12-22 | 昆山市恒鼎新材料有限公司 | Preparation process of ultralow-resistance corrosion-resistant coating for metal bipolar plate of hydrogen fuel cell |
| CN112993298A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Double-functional coating of fuel cell metal bipolar plate |
| CN112993300A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Transition layer for fuel cell metal bipolar plate coating |
-
2021
- 2021-07-02 CN CN202110748542.7A patent/CN113445014A/en active Pending
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| US20090269649A1 (en) * | 2008-04-23 | 2009-10-29 | Hyundai Hysco | Stainless separator for fuel cell and method of manufacturing the same |
| CN102201582A (en) * | 2010-03-22 | 2011-09-28 | 现代Hysco株式会社 | Metal separator for fuel cell and method of manufacturing the same |
| CN107302094A (en) * | 2017-06-15 | 2017-10-27 | 常州翊迈新材料科技有限公司 | Superconductive super-corrosion-resistant functional coating of fuel cell metal bipolar plate and preparation method thereof |
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| CN112993300A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Transition layer for fuel cell metal bipolar plate coating |
| CN112111716A (en) * | 2020-08-14 | 2020-12-22 | 昆山市恒鼎新材料有限公司 | Preparation process of ultralow-resistance corrosion-resistant coating for metal bipolar plate of hydrogen fuel cell |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114464818A (en) * | 2022-01-18 | 2022-05-10 | 哈尔滨工业大学 | Low-cost surface treatment method for improving surface performance of titanium and titanium alloy for proton exchange membrane fuel cell polar plate |
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