CN112993276A - Metal bipolar plate for Nb-Cr-C coating modified fuel cell and preparation method thereof - Google Patents
Metal bipolar plate for Nb-Cr-C coating modified fuel cell and preparation method thereof Download PDFInfo
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- CN112993276A CN112993276A CN201911287549.2A CN201911287549A CN112993276A CN 112993276 A CN112993276 A CN 112993276A CN 201911287549 A CN201911287549 A CN 201911287549A CN 112993276 A CN112993276 A CN 112993276A
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8867—Vapour deposition
- H01M4/8871—Sputtering
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals or alloys
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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 relates to a metal bipolar plate for a fuel cell modified by an Nb-Cr-C coating and a preparation method thereof. The metal bipolar plate comprises a metal substrate and a niobium carbide and chromium carbide codeposition layer on the metal substrate. The niobium carbide and chromium carbide conductive ceramic material in the coating effectively reduces the contact resistance between the metal plate and the carbon paper, the high hardness characteristic of the niobium carbide and chromium carbide conductive ceramic material provides the coating with better wear resistance, in addition, the codeposition of the niobium carbide and the chromium carbide effectively avoids the problem of a large number of crystal grain boundaries existing in the single component deposition, the coating has better compactness and strong corrosion resistance.
Description
Technical Field
The invention belongs to the field of fuel cells, and particularly relates to a metal bipolar plate for a fuel cell modified by a Nb-Cr-C coating and a preparation method thereof.
Background
The proton exchange membrane fuel cell is a device capable of converting chemical energy in an active substance into electric energy through electrochemical reaction, theoretically, only an oxidant and fuel are continuously introduced into a cathode and an anode of the proton exchange membrane fuel cell, the electric energy can be continuously output without multiple energy conversion, Carnot cycle limitation exists, the energy conversion efficiency is far higher than that of an internal combustion engine, and products only contain heat and water, the working noise is low, and the proton exchange membrane fuel cell belongs to a clean environment-friendly power generation device, so that the proton exchange membrane fuel cell has wide application prospects in various fields.
As one of the key components of the pem fuel cell, the bipolar plate accounts for over 80% of the weight and 30% of the cost, and besides uniformly dispersing the reactant to the membrane electrode and providing mechanical support, the bipolar plate needs to realize the conductive connection between the adjacent unit cells, prevent the mixing of hydrogen and oxygen, and lead out the excessive heat and water, therefore, the bipolar plate material needs to have the following characteristics: high electric and thermal conductivity, high strength, corrosion resistance, good compactness, easy processing, low cost and the like. The traditional graphite bipolar plate has good electrical conductivity and strong corrosion resistance, but has general mechanical strength and compactness, so the bipolar plate has large volume and complex processing technology, and the improvement of the power density of a fuel cell and the reduction of the cost are limited. The metal plate is expected to replace the traditional graphite plate to become the mainstream material of the fuel cell bipolar plate due to the advantages of high strength, compactness, easy processing and the like. At present, the main problems faced by metal bipolar plates are corrosion and passivation problems in proton exchange membrane fuel cells, metal cations generated by corrosion can pollute membrane electrodes, and the formation of a metal surface passivation film can increase the contact resistance between the metal surface passivation film and diffusion layers, thereby reducing the performance of the cells. Therefore, the current research on metallic bipolar plates mainly focuses on depositing conductive and corrosion-resistant coatings on the surface of the metal plate by physical, chemical vapor deposition, etc., including noble metal materials, carbon materials, transition metal conductive ceramic materials, etc.
Chinese patent CN108574107A discloses a method for improving the conductivity and corrosion resistance of a carbide coating of a fuel cell bipolar plate, which comprises the steps of sequentially depositing a metal transition layer and a metal carbide coating on the surface of a metal bipolar plate, then carrying out etching treatment on the bipolar plate coated with the coating, changing the surface structure and the composition of the carbide coating, and further improving the conductivity and corrosion resistance of the niobium carbide coating. Chinese patent CN102637880A discloses a method for surface modification of iron-based alloy metal plate by depositing a chromium carbide coating through plasma carburization and thermal reaction deposition and diffusion composite surface modification technology, wherein the chromium carbide coating is metallurgically bonded to the substrate, so that the chromium carbide coating has high film-substrate bonding force, but the deposited coating is thicker, which increases the influence of internal stress, so the corrosion resistance of the material is not ideal.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the Nb-Cr-C coating modified metal bipolar plate for the fuel cell and the preparation method thereof, wherein the Nb-Cr-C coating modified metal bipolar plate has the advantages that the corrosion resistance is greatly improved, and the contact resistance is kept low.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a metal bipolar plate for a fuel cell modified by a Nb-Cr-C coating comprises a metal substrate, wherein niobium carbide and chromium carbide coatings are co-deposited on the metal substrate.
In the above technical scheme, further, the carbon atom proportion of the niobium carbide and chromium carbide coating is 20% -60%, the niobium atom proportion is 1% -67%, and the chromium atom proportion is 1% -80%.
In the above technical scheme, further, the thickness of the codeposition coating of niobium carbide and chromium carbide is 50nm to 3000 nm.
In the above technical solution, further, the niobium carbide includes NbC and Nb2C, the chromium carbide comprises CrC and Cr3C2、Cr7C3、Cr3C、Cr23C6One or more of (a).
In the above technical solution, further, the metal substrate is one of stainless steel, titanium alloy, aluminum, and aluminum alloy.
A method for preparing a metal bipolar plate for a fuel cell modified by a Nb-Cr-C coating comprises the following steps: firstly, cleaning and drying a metal substrate in deionized water, ethanol and acetone in sequence, and then depositing a niobium carbide and chromium carbide codeposition layer on the metal substrate.
In the above technical solution, further, the preparation method of the co-deposition layer of niobium carbide and chromium carbide is magnetron sputtering or arc ion plating.
In the above technical solution, further, the carbon in the co-deposition layer of niobium carbide and chromium carbide is derived from one of graphite target, methane, ethane, ethylene, and acetylene.
The invention has the beneficial effects that: niobium carbide and chromium carbide both belong to transition metal ceramic compounds, have conductivity similar to metal, can guarantee lower contact resistance between bipolar plate and carbon paper, and this kind of compound hardness is high, and the coating wearability that prepares is better, and in addition, the codeposition of niobium carbide and chromium carbide has effectively avoided the problem that preferred orientation produced grain boundary when single component deposits, and the coating compactness is better, and corrosion resistance is strong.
Drawings
Fig. 1 is a schematic structural diagram of a bipolar plate according to the present invention, in which 1, a metal plate substrate, 2, a co-deposition layer of niobium carbide and chromium carbide;
FIG. 2 is a scanning electron micrograph of a bipolar plate coating prepared in example 6;
FIG. 3 is a graph showing the proportions of the elements in the bipolar plate coatings prepared in the examples;
FIG. 4 is a graph showing the contact resistance between the bipolar plate and the carbon paper prepared in each example as a function of pressure;
fig. 5 is a graph showing the potentiostatic polarization of the bipolar plates prepared in each example under simulated fuel cell cathode conditions.
Detailed Description
The invention is further illustrated but is not in any way limited by the following specific examples.
Comparative example 1
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa below; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; using niobium target as evaporation source, controlling target current at 60A, substrate bias at-600V, sputteringCleaning for 5 min; then 15sccm of acetylene gas is introduced into the vacuum chamber, the target current is controlled to be 100A, the substrate bias voltage is-200V, and the niobium carbide layer is deposited for 30 min; and cooling and taking out to obtain the metal plate with the modified surface coating, wherein the thickness of the coating is about 600 nm.
As shown in the figure, the contact resistance between the bipolar plate and the carbon paper is 0.97m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4+5ppm F-After the material is corroded for 10 hours at a constant potential of 0.6V (vs. SCE) under the condition of air introduction, the corrosion current is 1.92 mu A/cm2。
Example 1
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; taking a niobium target as an evaporation source, controlling the target current to be 60A, controlling the substrate bias voltage to be-600V, and carrying out sputtering cleaning for 5 min; adjusting the flow of argon gas to 300sccm, and introducing 9sccm of acetylene gas into the vacuum chamber to keep the pressure of the vacuum chamber at 0.8 Pa; adjusting the niobium target current to 70A, introducing a chromium target evaporation source, controlling the target current to 80A, biasing the substrate to-100V, and depositing a niobium carbide and chromium carbide codeposition layer for 30 min; and cooling and taking out to obtain the metal plate with the modified surface coating, wherein the thickness of the coating is about 500 nm.
As shown in the figure, the contact resistance between the bipolar plate and the carbon paper is 2.14m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4+5ppm F-After the material is corroded for 10 hours at a constant potential of 0.6V (vs. SCE) under the condition of air introduction, the corrosion current is 0.57 mu A/cm2Compared with the coating prepared in the comparative example 1, the corrosion resistance of the coating is obviously improved.
Example 2
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; taking a niobium target as an evaporation source, controlling the target current to be 60A, controlling the substrate bias voltage to be-600V, and carrying out sputtering cleaning for 5 min; will be provided withAdjusting the flow of argon gas to 300sccm, and introducing 9sccm of acetylene gas into the vacuum chamber to keep the pressure of the vacuum chamber at 0.8 Pa; adjusting the niobium target current to 70A, introducing a chromium target evaporation source, controlling the target current to 90A, biasing the substrate to-100V, and depositing a niobium carbide and chromium carbide codeposition layer for 30 min; and cooling and taking out to obtain the metal plate with the modified surface coating, wherein the thickness of the coating is about 500 nm.
As shown in the figure, the contact resistance between the bipolar plate and the carbon paper is 1.26m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4+5ppm F-After the material is corroded for 10 hours at a constant potential of 0.6V (vs. SCE) under the condition of air introduction, the corrosion current is 0.70 mu A/cm2Compared with the coating prepared in the comparative example 1, the corrosion resistance of the coating is obviously improved.
Example 3
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; taking a niobium target as an evaporation source, controlling the target current to be 60A, controlling the substrate bias voltage to be-600V, and carrying out sputtering cleaning for 5 min; adjusting the flow of argon gas to 300sccm, and introducing 9sccm of acetylene gas into the vacuum chamber to keep the pressure of the vacuum chamber at 0.8 Pa; keeping the niobium target current unchanged, introducing a chromium target evaporation source, controlling the target current at 90A, biasing the substrate to 125V, and depositing a niobium carbide and chromium carbide codeposition layer for 60 min; and cooling and taking out to obtain the metal plate with the modified surface coating, wherein the thickness of the coating is about 600 nm.
As shown in the figure, the contact resistance between the bipolar plate and the carbon paper is 4.63m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4+5ppm F-After the material is corroded for 10 hours at a constant potential of 0.6V (vs. SCE) under the condition of air introduction, the corrosion current is 0.52 mu A/cm2Compared with the coating prepared in the comparative example 1, the corrosion resistance of the coating is obviously improved.
Example 4
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece holder of an arc ion plating machine, and pumpingVacuum to 3X 10-3Pa; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; taking a niobium target as an evaporation source, controlling the target current to be 60A, controlling the substrate bias voltage to be-600V, and carrying out sputtering cleaning for 5 min; adjusting the flow of argon gas to 300sccm, and introducing 9sccm of acetylene gas into the vacuum chamber to keep the pressure of the vacuum chamber at 0.8 Pa; keeping the current of the niobium target unchanged, introducing a chromium target evaporation source, controlling the target current to be 90A, biasing the substrate to be 150V, and depositing a niobium carbide and chromium carbide codeposition layer for 60 min; and cooling and taking out to obtain the metal plate with the modified surface coating, wherein the thickness of the coating is about 500 nm.
As shown in the figure, the contact resistance between the bipolar plate and the carbon paper is 3.12m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4+5ppm F-After the material is corroded for 10 hours at a constant potential of 0.6V (vs. SCE) under the condition of air introduction, the corrosion current is 0.47 mu A/cm2Compared with the coating prepared in the comparative example 1, the corrosion resistance of the coating is obviously improved.
Example 5
Taking TA1 type pure titanium as a substrate, and ultrasonically cleaning and drying in deionized water, ethanol and acetone in sequence; mounting the substrate on a workpiece rack of an arc ion plating machine, and vacuumizing to 3 x 10-3Pa; introducing argon of 200sccm into the vacuum chamber to keep the pressure at 0.5 Pa; taking a niobium target as an evaporation source, controlling the target current to be 60A, controlling the substrate bias voltage to be-600V, and carrying out sputtering cleaning for 5 min; adjusting the flow of argon gas to 300sccm, and introducing acetylene gas of 12sccm into the vacuum chamber to keep the pressure of the vacuum chamber at 0.8 Pa; keeping the current of the niobium target unchanged, introducing a chromium target evaporation source, controlling the target current at 100A, biasing the substrate to 200V, and depositing a niobium carbide and chromium carbide codeposition layer for 60 min; and cooling and taking out to obtain the surface modified metal plate.
As shown in the figure, the thickness of the coating is about 500nm, and the contact resistance between the bipolar plate and the carbon paper is 1.28m omega cm under 1.5MPa2At 80 ℃ 0.5M H2SO4+5ppm F-After the material is corroded for 10 hours at a constant potential of 0.6V (vs. SCE) under the condition of air introduction, the corrosion current is 0.47 mu A/cm2Compared with the coating prepared in the comparative example 1, the corrosion resistance of the coating is obviously improved.
It will be apparent to those skilled in the art from this disclosure that many changes and modifications can be made, or equivalents modified, in the embodiments of the invention without departing from the scope of the invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention shall still fall within the protection scope of the technical solution of the present invention, unless the contents of the technical solution of the present invention are departed.
Claims (8)
1. A metal bipolar plate for a fuel cell modified by a Nb-Cr-C coating comprises a metal substrate, and is characterized in that niobium carbide and chromium carbide coatings are co-deposited on the metal substrate.
2. The metal bipolar plate for a fuel cell modified by an Nb-Cr-C coating of claim 1, wherein the Nb-Cr-C coating has a carbon atom ratio of 20-60%, a Nb atom ratio of 1-67%, and a Cr atom ratio of 1-80%.
3. The Nb-Cr-C coating modified metal bipolar plate for fuel cells as in claim 1, wherein the co-deposited coating thickness of niobium carbide and chromium carbide is 50nm to 3000 nm.
4. The Nb-Cr-C coating modified metal bipolar plate for fuel cells as in claim 1, wherein the niobium carbide comprises NbC, Nb2C, the chromium carbide comprises CrC and Cr3C2、Cr7C3、Cr3C、Cr23C6One or more of (a).
5. The Nb-Cr-C coating modified metallic bipolar plate for fuel cells as in claim 1, wherein the metal substrate is one of stainless steel, titanium alloy, aluminum, and aluminum alloy.
6. The method for preparing the metal bipolar plate for the Nb-Cr-C coating modified fuel cell, which is described in claim 1, is characterized in that the method comprises the following steps: firstly, cleaning and drying a metal substrate in deionized water, ethanol and acetone in sequence, and then depositing a niobium carbide and chromium carbide codeposition layer on the metal substrate.
7. The method for preparing the metal bipolar plate for the Nb-Cr-C coating modified fuel cell according to claim 5, wherein the method for preparing the niobium carbide and chromium carbide co-deposition layer is magnetron sputtering or arc ion plating.
8. The method for preparing a metal bipolar plate for a fuel cell modified by an Nb-Cr-C coating according to claim 5, wherein the carbon in the co-deposited layer of niobium carbide and chromium carbide is derived from one of graphite target, methane, ethane, ethylene and acetylene.
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| CN201911287549.2A CN112993276A (en) | 2019-12-14 | 2019-12-14 | Metal bipolar plate for Nb-Cr-C coating modified fuel cell and preparation method thereof |
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2019
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