CN114927713B - Flow field plate and preparation method and application thereof - Google Patents

Flow field plate and preparation method and application thereof Download PDF

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Publication number
CN114927713B
CN114927713B CN202210675043.4A CN202210675043A CN114927713B CN 114927713 B CN114927713 B CN 114927713B CN 202210675043 A CN202210675043 A CN 202210675043A CN 114927713 B CN114927713 B CN 114927713B
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field plate
flow field
coating
transition metal
plasma treatment
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CN114927713A (en
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杨敏
陈福平
万玲玉
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Shanghai Electric Group Corp
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Shanghai Electric Group Corp
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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
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • 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
    • C23C14/0641—Nitrides
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • 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
    • C23C14/325—Electric arc evaporation
    • 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
    • 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
    • H—ELECTRICITY
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    • 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
    • H—ELECTRICITY
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    • 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
    • H01M8/0215—Glass; Ceramic materials
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    • 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
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    • H01M8/0223—Composites
    • H01M8/0228—Composites in the form of layered or coated products
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
    • H01M8/1018—Polymeric electrolyte materials
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    • H01M8/10—Fuel cells with solid electrolytes
    • H01M2008/1095—Fuel cells with polymeric electrolytes
    • 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
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Abstract

The invention discloses a flow field plate and a preparation method and application thereof. The preparation method of the flow field plate comprises the steps of carrying out plasma treatment on the flow field plate base material; the flow field plate substrate comprises a basal layer, a transition metal nitride coating and a conductive metal coating which are sequentially arranged; the gas source for the plasma treatment comprises a dilution gas and CF 4, wherein the volume ratio of the dilution gas to the CF 4 is (10-20): 1, the flow rate of the air source is 1-100 sccm; the pressure during the plasma treatment is 0.005-0.02 Pa; the power of the plasma treatment is 800-1200W. According to the invention, through fumbling and experiments on the online treatment process of the plasmas, the hydrophobicity of the surface of the flow field plate is improved, and the contact angle of the flow field plate is kept unchanged after long-term storage.

Description

Flow field plate and preparation method and application thereof
Technical Field
The invention relates to a flow field plate, a preparation method and application thereof.
Background
There are many methods of preparing fuel cell flow field plate coatings, including physical vapor deposition as applied to common plates. An important function of the flow field plate is to enable water generated by electrochemical reaction to be discharged rapidly, so that reactant gas can reach a catalytic layer, and electrochemical reaction can be smoothly carried out. The hydrophilicity/water transport properties of the flow field plate directly affect the distribution of water on the surface of the flow field plate, which in turn affects the rate at which the electrochemical reaction proceeds. The hydrophilicity/hydrophobicity was determined by testing the surface contact angle of the flow field plate. After a period of operation, the state of the surface of the flow field plate can be changed, and how to keep the state of the surface of the flow field plate relatively stable is an important aspect of ensuring the performance and service life of the fuel cell.
In the current flow field plate PVD coating technology, there is basically little mention of online hydrophilic/hydrophobic treatment of the coating, and of the change in the surface state of the coating over time. Typically, the near-surface region of the flow field plate has different properties from the bulk material, including mechanical properties, electrical properties, etc., which are related to the atmosphere in which the flow field plate is placed in the vacuum chamber.
The hydrophilic/hydrophobic properties of the surface of the metal flow field plate of the fuel cell directly affect the distribution and discharge velocity of water in the flow channels of the fuel cell, thereby affecting the power and stability of the fuel cell. At the same time, the change in hydrophilicity/hydrophobicity of the surface of the flow field plate also directly affects the life of the cell. At present, the design and manufacture of hydrophobic surfaces by adjusting the chemical composition and morphology of the material surface has become a hotspot in the field of material science. The hydrophobic properties of the material surface are generally obtained by a filling or coating process using silicon or fluorine compounds. These conventional methods are not environment-friendly because a large amount of water and chemicals are used, and a large amount of energy is required for evaporating the surplus water. The main methods for enhancing the hydrophobic surface at present are a template method, a sol-gel method, an autonomous loading method, a chemical deposition method, an etching method and the like. Essentially all of these methods involve solutions that use large amounts of water and chemicals and require a large amount of energy to evaporate the excess water and solvent.
Most of the processes also fail to obtain excellent hydrophobic properties and ensure good hydrophobicity for a long time. For example, chinese patent document CN112359328a discloses a surface treatment method for a bipolar plate of a fuel cell, specifically, a nano-scale conductive hydrophobic layer is prepared on the surface of a dried bipolar plate by a vapor deposition method, and then the nano-scale conductive hydrophobic layer is roughened, so as to obtain a bipolar plate with excellent hydrophobic property. However, in this patent, for example, a surface structure of a titanium nitride layer is adopted, and since water is a polar molecule, in a microscopic state, the titanium nitride layer is likely to electrostatically adsorb to the surface of an object, which inevitably affects the water-draining effect of the bipolar plate, resulting in poorer long-term water-draining performance.
Disclosure of Invention
The invention mainly aims to overcome the defects that the hydrophobicity of a flow field plate of a fuel cell in the prior art is poor and the hydrophobicity of the surface of the flow field plate is obviously reduced along with the time extension, and provides a flow field plate and a preparation method and application thereof. According to the invention, through fumbling and experiments on the online treatment process of the plasmas, the hydrophobicity of the surface of the flow field plate is improved, and the contact angle of the flow field plate is kept unchanged after long-term storage.
The invention mainly solves the technical problems through the following technical scheme.
The invention provides a preparation method of a flow field plate, which comprises the following steps: performing plasma treatment on the flow field plate substrate;
the flow field plate substrate comprises a basal layer, a transition metal nitride coating and a conductive metal coating which are sequentially arranged;
the gas source for the plasma treatment comprises a dilution gas and CF 4, wherein the volume ratio of the dilution gas to the CF 4 is (10-20): 1, the flow rate of the air source is 1-100 sccm; the pressure during the plasma treatment is 0.005-0.02 Pa;
the power of the plasma treatment is 800-1200W.
The inventor finds that the surface contact angle of the flow field plate is obviously improved by carrying out the plasma treatment on the specific flow field plate substrate in the research and development process, and unexpectedly finds that the surface contact angle of the prepared flow field plate is unchanged even if the flow field plate is placed for a long time. This is probably because the present invention changes the surface morphology of the flow field plate substrate by the plasma treatment while reducing the surface energy, thereby increasing the hydrophobicity.
Specifically, the surface energy of the freshly prepared flow field plate substrate is very high, crystals in the transition metal nitride layer and the conductive metal coating grow epitaxially, the surface density is low, the irregular arrangement of formed particles on the film surface after the gas source treatment of the diluent gas and the CF 4 endows the surface of the flow field plate substrate with different grades of roughness, the surface density is improved, water drops can form high air capturing rate and smaller roughness factor when contacting with the surface of the conductive metal coating, meanwhile, the introduction of F particles also reduces the surface energy of the coating, and the effects jointly endow the surface of the flow field plate with superhydrophobicity.
In the present invention, the flow field plate substrate is preferably a base layer, a transition metal nitride plating layer, and a conductive metal plating layer, which are sequentially provided.
In the present invention, the sequential arrangement may be in the meaning conventionally understood in the art, and may be prepared according to the actual requirements of the flow field plate. Generally, the transition metal nitride plating layer and the conductive metal plating layer are sequentially provided on one side surface of the base layer.
In the present invention, the material of the base layer is generally stainless steel, as known to those skilled in the art. The term stainless steel is used in the sense conventionally understood in the art and generally refers to steel having stainless, corrosion resistance as the primary property and a chromium content of at least 10.5% and a carbon content of at most 1.2%.
In the present invention, the thickness of the base layer may be conventional in the art, typically 0.05 to 0.15mm, for example 0.1mm.
In the present invention, the transition metal nitride coating preferably includes TiN coating and/or CrN coating.
In the present invention, the thickness of the transition metal nitride coating may be conventional in the art, typically 80 to 120nm, for example 100nm.
In the present invention, the thickness ratio of the base layer to the transition metal nitride plating layer is preferably (800 to 1200): 1, for example 1000:1.
In the present invention, the method of forming the transition metal nitride plating layer on the surface of the base layer may be conventional in the art, and preferably includes the steps of: and forming a transition metal coating on the surface of the substrate layer, and reacting with nitrogen to obtain the transition metal nitride coating.
Wherein, the method for forming the transition metal coating is preferably multi-arc ion plating.
Wherein the nitrogen reacts with the transition metal coating in the form of reactive sputtering.
In the present invention, the conductive metal plating layer is preferably a gold plating layer.
In a preferred embodiment of the invention, the TiN plating layer and/or the CrN plating layer are/is matched with the nano-scale gold plating layer, and the plasma treatment is carried out to form the flow field plate with the surface contact angle stability as high as 1 month. If the gold plating is replaced with other conductive metal plating, the hydrophobicity of the finally manufactured flow field plate is reduced.
In the present invention, the thickness of the conductive metal plating layer may be conventional in the art, for example, 10 to 30nm, for example, 20nm.
In the present invention, the thicknesses of the transition metal nitride plating layer and the conductive metal plating layer are preferably (4 to 6): 1, for example 5:1.
In the present invention, the method of forming the conductive metal plating layer on the surface of the transition metal nitride plating layer may be conventional in the art, and the conductive metal plating layer is generally formed by means of magnetron sputtering which is conventional in the art.
In the present invention, the diluent gas generally refers to inert gas and/or nitrogen, preferably nitrogen.
In the present invention, the volume ratio of the diluent gas to the CF 4 is preferably (10 to 15): 1.
In the present invention, the flow rate of the gas source is preferably 10 to 30sccm, for example, 20sccm.
In the present invention, as will be appreciated by those skilled in the art based on the flow field plate substrate, the plasma treatment generally refers to the plasma treatment of the surface of the conductive metal plating.
In the present invention, the plasma treatment may be performed by a conventional treatment method in the art, typically, the flow field plate substrate is placed in a chamber, the gas source is introduced, and the bias discharge is performed to generate plasma from the gas source.
In the present invention, the pressure at the time of the plasma treatment is preferably 0.08 to 0.12Pa, for example, 0.01Pa. The pressure is typically achieved by controlling the density and flow rate of the gas source.
In the present invention, the power of the plasma treatment is preferably 900 to 1100W, for example 1000W.
In the present invention, the power of the plasma treatment may be in the meaning conventionally understood in the art generally referred to as the power of the bias discharge.
In the present invention, the plasma treatment time may be controlled according to the actual requirement, and is generally 8 to 20 minutes, for example, 15 minutes.
It was found in experiments that the flow rate of the gas source, the pressure and the power all had a significant effect on the modification rate and uniformity of the plasma treatment. And the hydrophobicity of the flow field plate is different at different positions when the flow rate of the air source is smaller. This is probably because CF 4 in the gas source has a lower cross section and a higher electron dissociation adhesion threshold energy (5-6 eV) and CF 4 molecules need to stay between the electrodes for a period of time before they can be activated by the discharge. With all of these effects taken into account, the concentration of the active particles is considered to be large only at a position farther from the air inlet, while there is only a very small amount of active particles at a position closer to the air inlet. Thus, a significant amount of processing time is required to reach a contact angle of 100 ° near the gas inlet, whereas plasma processing proceeds more rapidly farther from the gas inlet.
In the present invention, the volume ratio of CF 4 to the diluent gas in the gas source should be within the above specific range of the present invention, mainly because the plasma-treated surface may be etched to cause the damage of the plating layer when the volume of CF 4 is relatively high. Thus, the discharge chemistry after CF 4 addition in the present invention may be advantageous to produce F atomic species or fragments of F and C based molecules, which then produce different surface chemistries.
The invention also provides a flow field plate which is manufactured by the manufacturing method.
The invention also provides application of the flow field plate in a proton exchange membrane fuel cell.
On the basis of conforming to the common knowledge in the field, the above preferred conditions can be arbitrarily combined to obtain the preferred examples of the invention.
The reagents and materials used in the present invention are commercially available.
The invention has the positive progress effects that: the problems of hydrophobicity of the surface of the plating layer and stability of the plating layer in the flow field plate are solved by an on-line treatment mode, the quality of the plating layer is improved, and the performance and stability of the PEM fuel cell are improved. Is beneficial to mass popularization and application of the metal bipolar plates.
Detailed Description
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
Example 1
(1) Carrying out ultrasonic cleaning and drying on a flow field plate punched by stainless steel with the thickness of 0.1 mm;
(2) Transferring the cleaning solution into a furnace chamber through a customized tool for bias cleaning;
(3) Priming is carried out by using a Ti target material through multi-arc ion plating to obtain a Ti plating layer;
(4) Introducing N 2, and performing reactive sputtering to generate a TiN coating with the thickness of 100 nm;
(5) Preparing an Au plating layer with the uppermost layer thickness of 20nm nano-scale thickness by a magnetron sputtering mode;
(6) Introducing an air source N 2/CF4, generating plasma in a bias discharge mode, and performing hydrophobic treatment on the surface of the coating; the volume ratio of N 2 to CF 4 in the air source is 10:1, the flow of the air source is 20sccm, the pressure of the cavity is 0.01Pa, the time for introducing the air source is 15min, and the power of bias discharge is 1000W.
(7) Breaking vacuum, taking out the sample after plating, and measuring the contact angle.
Example 2
In the step (4), crN coating is generated, and other processes are the same as in example 1.
Comparative example 1
And (3) introducing no N 2/CF4 mixed gas source, generating plasma in a bias discharge mode, and carrying out hydrophobic treatment on the surface of the coating. The rest of the procedure is the same as in example 1.
Effect example 1
1. Surface roughness and stability test
The surfaces of the above examples 1 and 2 and comparative example 1 were subjected to roughness test using a surface roughness meter in an air atmosphere at normal temperature and normal pressure, 5 positions were taken for each sample to perform roughness test, each vertex and center point of the regular quadrangle were used as test points, and finally an average value was taken. The results are shown in Table 1 below.
TABLE 1
Contact angle at day 1 Contact angle at 7 days Contact angle at 30 days
Example 1 100° 100° 100°
Example 2 100° 100° 100°
Comparative example 1 70° 50° /
The results show that the hydrophilicity/hydrophobicity of the flow field plate surface is related to the process control parameters and the flow rate of CF 4;
In the examples, after the base layer, the transition metal nitride plating layer and the gold plating layer, which were sequentially disposed, were subjected to a specific plasma treatment, the flow field plate sample was stored in air at room temperature, the contact angle was not reduced with the increase of the storage time, and remained stable at 100 °, even after 20 days of storage in air, the contact angle was hardly changed. Thus, it can be concluded that N 2/CF4 is stable after plasma treatment. Whereas the surface contact angle of the untreated flow field plate (i.e., comparative example 1) was reduced within 1 week.

Claims (12)

1. A method of making a flow field plate comprising the steps of: performing plasma treatment on the flow field plate substrate;
the flow field plate substrate comprises a basal layer, a transition metal nitride coating and a conductive metal coating which are sequentially arranged; the conductive metal coating is a gold coating;
The gas source for the plasma treatment comprises a dilution gas and CF 4, wherein the volume ratio of the dilution gas to the CF 4 is (10-20): 1, the flow rate of the air source is 1-100 sccm; the pressure during the plasma treatment is 0.005-0.02 Pa;
the power of the plasma treatment is 800-1200W.
2. The method for preparing a flow field plate according to claim 1, wherein the flow field plate substrate is a base layer, a transition metal nitride coating and a conductive metal coating which are sequentially arranged.
3. The method for manufacturing a flow field plate according to claim 1, wherein the substrate layer is made of stainless steel;
and/or the thickness of the substrate layer is 0.05-0.15 mm;
and/or the transition metal nitride coating comprises a TiN coating and/or a CrN coating.
4. The method for manufacturing a flow field plate according to claim 1, wherein the thickness of the transition metal nitride coating is 80-120 nm;
and/or, the thickness ratio of the base layer to the transition metal nitride coating is (800-1200): 1.
5. A method of preparing a flow field plate according to claim 1, wherein the method of forming the transition metal nitride coating on the surface of the base layer comprises the steps of: and forming a transition metal coating on the surface of the substrate layer, and reacting with nitrogen to obtain the transition metal nitride coating.
6. The method of preparing a flow field plate as claimed in claim 5, wherein the method of forming the transition metal coating is multi-arc ion plating.
7. The method of preparing a flow field plate according to claim 5, wherein the nitrogen gas reacts with the transition metal coating by reactive sputtering.
8. The method for manufacturing a flow field plate according to any one of claims 1 to 4, wherein the thickness of the conductive metal plating layer is 10 to 30nm;
and/or the thickness ratio of the transition metal nitride coating to the conductive metal coating is (4-6): 1, a step of;
And/or the method for forming the conductive metal coating on the surface of the transition metal nitride coating is magnetron sputtering.
9. The method for manufacturing a flow field plate according to any one of claims 1 to 4, wherein the diluent gas is inert gas and/or nitrogen gas;
And/or the volume ratio of the diluent gas to the CF 4 is (10-15): 1, a step of;
and/or the flow rate of the air source is 10-30 sccm.
10. The method for producing a flow field plate according to any one of claims 1 to 4, wherein the pressure at the time of the plasma treatment is 0.08 to 0.12pa;
and/or the power of the plasma treatment is 900-1100W;
and/or the plasma treatment time is 8-20 min.
11. A flow field plate produced by the method of producing a flow field plate according to any one of claims 1 to 10.
12. Use of a flow field plate as claimed in claim 11 in a proton exchange membrane fuel cell.
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