CN106374116A - High-entropy alloy composite coating on metal bipolar plate of fuel cell and process - Google Patents
High-entropy alloy composite coating on metal bipolar plate of fuel cell and process Download PDFInfo
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- CN106374116A CN106374116A CN201611087311.1A CN201611087311A CN106374116A CN 106374116 A CN106374116 A CN 106374116A CN 201611087311 A CN201611087311 A CN 201611087311A CN 106374116 A CN106374116 A CN 106374116A
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- entropy alloy
- composite coating
- double polar
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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
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
- H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
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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
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8892—Impregnation or coating of the catalyst layer, e.g. by an ionomer
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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 high-entropy alloy composite coating on a metal bipolar plate of a fuel cell and a preparation method of the high-entropy alloy composite coating. The high-entropy alloy composite coating is prepared on the surface of the metal bipolar plate through adopting a closed-field unbalanced magnetron sputtering technology. The composite coating on the surface of a substrate of the metal bipolar plate is composed of a high-entropy alloy layer, a multi-component alloy-carbon transition layer and an amorphous carbon layer located on the outermost surface. Compared with the prior art, multi-component compounding is carried out by adopting a step-by-step transition method through sufficiently utilizing a high-entropy effect, a delaying diffusing effect and a cocktail party effect of a high-entropy alloy, and electrical conductivity and corrosion resistance of an amorphous carbon film. The modified metal bipolar plate provided by the invention has high film-substrate bonding force, corrosion resistance and electrical conductivity, so that utilization requirements of the metal bipolar plate of the fuel cell are met.
Description
Technical field
The present invention relates to field of fuel cell technology, specifically, it is related specifically to a kind of fuel battery metal double polar plate
On high-entropy alloy composite coating and preparation method thereof.
Background technology
Proton Exchange Membrane Fuel Cells (pemfc) is increasingly subject to the concern of various countries as a kind of clean energy resource, and puts into huge
Money is researched and developed.Chemical energy in hydrogen directly can be changed into electric energy without burning by pemfc, and unique product is
Water, very friendly to environment, cell stack efficiency is up to more than 50%.Pemfc also has that operating temperature is low, toggle speed is fast
The advantages of, it is preferable portable power source and independent power supply device, in the vehicles, electronic product, national defense and military and stationary electric power plant
It is with a wide range of applications in field.
Bipolar plates are one of critical components of Proton Exchange Membrane Fuel Cells.It accounts for the 80% of battery pile volume, quality
70% and the 29% of cost, its major function is to play collection conduction, radiating, dispersed reaction medium and coolant in the battery
Effect, has support membrane electrode, prevents the multi-functionals such as reaction medium internal hemorrhage due to trauma and leakage.Therefore, preferable bipolar plate material should
There is high electrical conductivity and good corrosion resistance, there is high mechanical properties, high-air-tightness, chemical stability is good and easy processing becomes
The features such as type.At present, pemfc bipolar plate material mainly has three classes: graphite material, composite and metal material.Graphite bi-polar
Plate well conducting, easy processing, but material fragility is big, bad mechanical property, working (machining) efficiency are low it is difficult to it is raw to realize commercialization high-volume
Produce.Composite material double pole plate with carbon dust and resin as primary raw material, through molding etc. mode be prepared from, it is with low cost, but
Composite material double pole plate also haves such problems as that electric conductivity and gas permeate.Metal double polar plates have high intensity and conductive, heat conduction
Performance, can be produced using the mass production method such as sheet metal punching press, rolling, the head of the commercializing fuel cells being well recognized as
Choosing.
The working environment of pemfc is in faintly acid, and contains cl-、f-、so4 2-Plasma, to metal double polar plates (as rustless steel)
There is stronger corrosiveness, accordingly, it would be desirable to carry out surface modification treatment to improve its corrosion resistance and fall to metal double polar plates
Low contact resistance.As a example using stainless sheet steel as the material of bipolar plates, disclosed technology has in bipolar plate surfaces coating
Noble metal, nitride, oxide, carbide, carbon-base film etc..
Although noble coatings can meet fuel cell use requirement, fuel cell pole is not suitable for due to its high cost
The low-cost, high-volume production of plate.The method of Chinese Patent Application No. 200810086373.x arc ion plating is in stainless base steel
The crn thin film of 0.1～5 μm of material plated surface.Chinese Patent Application No. 02155187.1 proton exchange membrane fuel cell metal dual-polarity
Plate, prepares 0.1～50 μm of coating of metal oxides using methods such as vapour deposition, spray pyrolysis in metal base surface.China
Number of patent application 200810010110.0 is prepared for tic using high-energy micro-arc alloying technology in stainless steel double polar plate surface
Ceramic coating.However, though said method can make corrosion potential shuffle, corrosion current reduces, and improves decay resistance,
It is that its electric conductivity, hydrophobicity etc. need to improve further.
In recent years, carbon-base film receives the pass of more and more research worker due to its excellent corrosion resistance, electric conductivity
Note.Mori et al. [moyi y, ueda m, hashimoto m, aoi y, tanase s, sakai
Adopt electron cyclotron resonace (ecr) plasma sputtering technology t.surf.coat.technol.2008 (202): 4094-4101]
It is prepared for amorphous carbon-film, fu et al. [yu fu, guoqiang lin, ming hou.international journal
Ofhydrogen energy.2009,34 (1): 405-409] cr-c carbon-base film is prepared for using arc ions electroplating method, in
State's number of patent application 201110235087.7 is prepared for high sp2 using non-balance magnetically controlled sputter ion electroplating method in stainless steel surfaces
Hydridization dense carbon coating, decay resistance and electric conductivity are all significantly improved, but said method, because technique is inherently special
, can more or less there is the defects such as the pin-hole phenomena being difficult to avoid that in the coating, under fuel cell environment, when long in the restriction of point
Between operation can cause coating spot corrosion, and then cause coating shedding lost efficacy.
Content of the invention
Present invention aims to deficiency of the prior art, provide the height on a kind of fuel battery metal double polar plate
Entropy Alloy Composite Coating and preparation method thereof, to solve problems of the prior art.
Technical problem solved by the invention can employ the following technical solutions to realize:
A kind of high-entropy alloy composite coating on fuel battery metal double polar plate, is provided with metal double polar plates substrate surface
High-entropy alloy layer, the transition zone of multicomponent alloy-carbon and outermost amorphous carbon layer, therefore it is by three layers of compound painting being formed
Layer.
Further, the gross thickness of described composite coating is 0.1～5 μm.
Further, described high-entropy alloy layer is made up of 5 to 7 kinds of alloying elements, each element atomic percentage conc 5%～
Between 35%, its alloying element can be al, ti, ta, zr, w, cr, ru, nb, mn, fe, mo, ni etc..
Further, the target sputtering described high-entropy alloy layer can adopt high-entropy alloy target, it would however also be possible to employ several
Single element metal targets, 2 yuan of alloy target materials, 3 yuan of alloy target materials are applied in combination, and prepare high-entropy alloy bottom by adjusting sputtering parameter
Layer, shielding power supply is DC source or is radio-frequency power supply.
A kind of preparation method of the high-entropy alloy composite coating on fuel battery metal double polar plate, comprises the steps:
1) ion sputtering cleaning metal basal board；
2) prepare high-entropy alloy prime coat；
3) prepare high-entropy alloy-carbon mixed transition layer；
4) deposit outermost amorphous carbon layer.
Further, described step 1) concrete technology as follows:
By described metal double polar plates substrate after being cleaned by ultrasonic, put in non-balance magnetically controlled sputter equipment vacuum cavity,
It is evacuated to furnace chamber vacuum and be less than 2.5 × 10- 5Torr, is passed through argon, biasing -300～-700v on matrix, with high energy from
Son bombardment substrate surface, to remove the passivating film on its surface.
Further, described step 2) concrete technology as follows:
The method preparing high-entropy alloy prime coat is DC sputtering or radio frequency sputtering method；According to DC sputtering, then
Its electric current is 0.1～10a；According to radio frequency sputtering method, then its power is 50～600w, and operating air pressure is maintained at 4.0 × 10- 4
～9.0 × 10- 4Torr, substrate bias are 0～-200v, and the high entropy depositing one layer of micro/nano level on the surface of metal double polar plates closes
Golden prime coat.
Further, described step 3) concrete technology as follows:
Metal target current is gradually reduced, or RF source power is gradually reduced, and graphite target current is progressively opened, and electric current maintains
0～10a, thus deposit high-entropy alloy-carbon mixed transition layer, to strengthen boundary between film layer on the basis of high-entropy alloy prime coat
Face bond strength.
Further, described step 4) concrete technology as follows:
Close metal target power supply, graphite target current maintains 0.1～10a, substrate bias, in 0～-200v, deposit outermost layer
Amorphous carbon layer.
Compared with existing other technology, the present invention utilizes non-balance magnetically controlled sputter technology to deposit in stainless steel double polar plate surface
High-entropy alloy composite coating, takes full advantage of high-entropy alloy prime coat and the synergism of amorphous carbon-film outer layer, by adjustment
Coating process parameter, can improve corrosion resistance and the electric conductivity of fuel battery metal double polar plate, extend fuel cell and use
In the life-span, provide technical support for fuel cell industrialization.
Brief description
Between high-entropy alloy composite coating that Fig. 1 is prepared for the present invention and carbon paper, contact resistance is with pressure history.
Corrosion current pole under analog fuel cell cathode environment for the high-entropy alloy composite coating that Fig. 2 is prepared for the present invention
Change curve.
Specific embodiment
Technological means, creation characteristic, reached purpose and effect for making the present invention realize are easy to understand, with reference to
Specific embodiment, is expanded on further the present invention.
Embodiment 1
Using non-balance magnetically controlled sputter equipment, this equipment is equipped with 4 DC sources, is respectively mounted 2 alcrtatizr height
Entropy alloys target and 2 graphite target.316 stainless steel substrate samples are put in vacuum chamber of film coating machine after over cleaning, drying, takes out true
Empty to 2.5 × 10- 5Torr, is passed through argon, is biased to -500v, carries out Ion Cleaning to substrate specimen surface, to remove not
The passivating film of rust base steel plate surface；Then adjustment is biased into -100v, high-entropy alloy target current 5a, first deposits on the surface of the substrate
High-entropy alloy bottom；Then it is gradually reduced high-entropy alloy target current, open graphite target current simultaneously, and be gradually increased to 6a, partially
Press as -80v, deposition multicomponent alloy-carbon mixed transition layer；Finally close high-entropy alloy target current, graphite target current keeps 6a, partially
Press as -60v, the outmost amorphous carbon layer of deposition.Through test, prepared high-entropy alloy composite deposite gross thickness is 3.2 μm；
When pressure is for 1.5mpa, the contact resistance between plated film corrosion resistant plate and carbon paper is 8.8m ω cm2；At 70 DEG C, 0.5m h2so4
+ 3ppm hf, is passed through in the analog fuel cell cathode environment of air, and electrochemistry dynamic potential scanning corrosion potential is 0.23v, rotten
Erosion electric current is 1.37 μ acm-2.
Embodiment 2
Using non-balance magnetically controlled sputter equipment, this equipment is equipped with 2 radio frequency sources, 2 DC sources, pacifies wherein on radio frequency source
Dress alcrfemnni high-entropy alloy target, DC source is installed 2 graphite target.By 316 stainless steel substrate samples through over cleaning, drying
After put in vacuum chamber of film coating machine, be evacuated to 2.5 × 10- 5Torr, is passed through argon, is biased to -450v, to specimen surface
Carry out Ion Cleaning, to remove the passivating film on stainless steel substrate surface；Then adjustment is biased into -120v, high-entropy alloy target power output
300w, first deposits high-entropy alloy bottom on the surface of the substrate；Then it is gradually reduced high-entropy alloy target power output, open graphite target simultaneously
Electric current, and be gradually increased to 3a, bias as -60v, deposition multicomponent alloy-carbon mixed transition layer；Finally close radio frequency source, graphite
Target current keeps 3a, biases as -60v, the outmost amorphous carbon layer of deposition.Through test, prepared high-entropy alloy Composite Coatings
Layer gross thickness is 1.3 μm；When pressure is for 1.5mpa, the contact resistance between plated film corrosion resistant plate and carbon paper is 3.5m ω cm2；
At 70 DEG C, 0.5m h2so4+ 3ppm hf, is passed through in the analog fuel cell cathode environment of air, and electrochemistry dynamic potential scanning is rotten
Erosion current potential is 0.20v, and corrosion current is 3.34 μ acm-2.
Embodiment 3
Using non-balance magnetically controlled sputter equipment, this equipment is equipped with 2 radio frequency sources, 2 DC sources, wherein 2 radio frequency sources
On be respectively mounted ta-nb target, ti-w target, 2 DC sources are respectively mounted zr target, graphite target.By 316 stainless steel substrate sample warps
Put in vacuum chamber of film coating machine after over cleaning, drying, be evacuated to 2.5 × 10- 5Torr, is passed through argon, is biased to -550v,
Ion Cleaning is carried out to substrate specimen surface, to remove the passivating film on stainless steel substrate surface；Then adjustment is biased into -80v,
Power 300w and 280w is added on ta-nb target, ti-w target, zr target current is 4a respectively, first deposit zrtanbtiw on the surface of the substrate
High-entropy alloy bottom；Then it is gradually reduced ta-nb target, ti-w target power output, reduces zr target current, open graphite target current simultaneously,
And be gradually increased to 5a, bias as -40v, deposition multicomponent alloy-carbon mixed transition layer；Finally close ta-nb target, ti-w target, zr
Target, graphite target current keeps 5a, biases as -40v, the outmost amorphous carbon layer of deposition.Through test, prepared high-entropy alloy
Composite deposite gross thickness is 2.3 μm；When pressure is for 1.5mpa, the contact resistance between plated film corrosion resistant plate and carbon paper is
11.0mωcm2；At 70 DEG C, 0.5m h2so4+ 3ppm hf, is passed through in the analog fuel cell cathode environment of air, and electrochemistry is moved
Electric potential scanning corrosion potential is 0.12v, and corrosion current is 4.34 μ acm-2.
Ultimate principle and principal character and the advantages of the present invention of the present invention have been shown and described above.The technology of the industry
, it should be appreciated that the present invention is not restricted to the described embodiments, the simply explanation described in above-described embodiment and description is originally for personnel
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and its
Equivalent thereof.
Claims (9)
1. the high-entropy alloy composite coating on a kind of fuel battery metal double polar plate is it is characterised in that in metal double polar plates substrate
Surface is provided with high-entropy alloy layer, the transition zone of multicomponent alloy-carbon and outermost amorphous carbon layer, therefore it is formed by three layers
Composite coating.
2. the high-entropy alloy composite coating on fuel battery metal double polar plate according to claim 1 is it is characterised in that institute
The gross thickness stating composite coating is 0.1～5 μm.
3. the high-entropy alloy composite coating on fuel battery metal double polar plate according to claim 1 is it is characterised in that institute
State high-entropy alloy layer to be made up of 5 to 7 kinds of alloying elements, each element atomic percentage conc between 5%～35%, its alloying element
Can be al, ti, ta, zr, w, cr, ru, nb, mn, fe, mo, ni etc..
4. the high-entropy alloy composite coating on fuel battery metal double polar plate according to claim 3 is it is characterised in that splash
The target penetrating described high-entropy alloy layer can adopt high-entropy alloy target, it would however also be possible to employ several single element metal targets, 2 yuan of conjunctions
Gold target material, 3 yuan of alloy target materials are applied in combination, and prepare high-entropy alloy bottom by adjusting sputtering parameter, and shielding power supply is unidirectional current
Source or be radio-frequency power supply.
5. the high-entropy alloy composite coating on a kind of fuel battery metal double polar plate preparation method it is characterised in that include as
Lower step:
1) ion sputtering cleaning metal basal board；
2) prepare high-entropy alloy prime coat；
3) prepare high-entropy alloy-carbon mixed transition layer；
4) deposit outermost amorphous carbon layer.
6. the preparation method of the high-entropy alloy composite coating on fuel battery metal double polar plate according to claim 5, its
Be characterised by, described step 1) concrete technology as follows:
By described metal double polar plates substrate after being cleaned by ultrasonic, put in non-balance magnetically controlled sputter equipment vacuum cavity, take out true
Sky is less than 2.5 × 10 to furnace chamber vacuum- 5Torr, is passed through argon, biasing -300～-700v on matrix, is banged with energetic ion
Hit substrate surface, to remove the passivating film on its surface.
7. the preparation method of the high-entropy alloy composite coating on fuel battery metal double polar plate according to claim 5, its
Be characterised by, described step 2) concrete technology as follows:
The method preparing high-entropy alloy prime coat is DC sputtering or radio frequency sputtering method；According to DC sputtering, then its electricity
Flow for 0.1～10a；According to radio frequency sputtering method, then its power is 50～600w, and operating air pressure is maintained at 4.0 × 10- 4～9.0
×10- 4Torr, substrate bias are 0～-200v, and the high-entropy alloy depositing one layer of micro/nano level on the surface of metal double polar plates is beaten
Bottom.
8. the preparation method of the high-entropy alloy composite coating on fuel battery metal double polar plate according to claim 5, its
Be characterised by, described step 3) concrete technology as follows:
Metal target current is gradually reduced, or RF source power is gradually reduced, and graphite target current is progressively opened, and electric current maintains 0～
10a, thus deposit high-entropy alloy-carbon mixed transition layer, to strengthen interface between film layer on the basis of high-entropy alloy prime coat
Bond strength.
9. the preparation method of the high-entropy alloy composite coating on fuel battery metal double polar plate according to claim 5, its
Be characterised by, described step 4) concrete technology as follows:
Close metal target power supply, graphite target current maintains 0.1～10a, substrate bias, in 0～-200v, deposit outermost non-
Brilliant carbon-coating.
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| CN108914060A (en) * | 2018-07-10 | 2018-11-30 | 深圳森丰真空镀膜有限公司 | A kind of preparation method of fuel battery double plates surface protection coating |
| CN109560290A (en) * | 2018-12-26 | 2019-04-02 | 浙江锋源氢能科技有限公司 | A kind of metal double polar plates and preparation method thereof and fuel cell |
| DE102017128058A1 (en) | 2017-11-28 | 2019-05-29 | RUHR-UNIVERSITäT BOCHUM | Electrochemical electrode with multinary metal alloy as reduction catalyst |
| CN110343930A (en) * | 2019-08-22 | 2019-10-18 | 西安工业大学 | A kind of Flouride-resistani acid phesphatase high-entropy alloy, cladding tubes and preparation method thereof |
| CN110970626A (en) * | 2018-09-28 | 2020-04-07 | 武汉众宇动力***科技有限公司 | Fuel cell bipolar plate and coating thereof |
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| CN112993293A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Metal bipolar plate of fuel cell and preparation method thereof |
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| CN110970626A (en) * | 2018-09-28 | 2020-04-07 | 武汉众宇动力***科技有限公司 | Fuel cell bipolar plate and coating thereof |
| CN110970626B (en) * | 2018-09-28 | 2021-05-25 | 武汉众宇动力***科技有限公司 | Fuel cell bipolar plate and coating thereof |
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