CN104716339B - Fuel battery metal pole plate carbide and metal oxide composite coating and preparation - Google Patents
Fuel battery metal pole plate carbide and metal oxide composite coating and preparation Download PDFInfo
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- CN104716339B CN104716339B CN201510057049.5A CN201510057049A CN104716339B CN 104716339 B CN104716339 B CN 104716339B CN 201510057049 A CN201510057049 A CN 201510057049A CN 104716339 B CN104716339 B CN 104716339B
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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 present invention relates to a kind of fuel battery metal polar board surface carbide and metal oxide composite coating and preparation method thereof, conductive nano metal oxide layer, carbide lamella which is set gradually upwards by metal polar plate surface form.Preparation process mainly includes：A, matrix surface pre-processes；B, deposit metal oxide layers；C, depositing silicon nitride layer.Compared with prior art, this method cooperates with the characteristic by the use of metal oxide as ion barrier and carbide as conductive layer, form the defects of dense coating avoids perforation, crackle, with higher film-substrate cohesion, good electric conductivity and corrosion resistance can meet the requirement of fuel battery metal pole plate.
Description
Technical field
The present invention relates to a kind of preparation method of field of fuel cell technology, specifically a kind of fuel battery metal pole plate is used
Carbide and metal oxide method for composite coating.
Background technology
Fuel cell is the power generator that a kind of startup rate is fast, energy conversion efficiency is high, environmental-friendly, in traffic, electricity
The fields such as son, national defence have wide application prospect, have become research hotspot in recent years.Pole plate be fuel cell key component it
One, account for about the 80% of entire pile total volume, the 70% of quality and the 30%~40% of cost.Pole plate mainly plays support membrane
Electrode, collected current, separates Oxidizing and Reducing Agents, conduction heat, the effect for discharging product water at distribution reaction gas.Fuel
Battery is run under strong acidic environment, and pH value contains 0.1~1M H between 0~3.52SO4, 1~5ppm F-It is and few
Other ions of amount.Therefore it is required that pole plate has certain intensity, good electric conductivity, corrosion resistance, gas impermeability.
Mainly include graphite, metal and C-base composte material currently used for plate material.Graphite electrode plate has good lead
Electrically, thermal conductivity, corrosion resistance, but graphite is more crisp, and processing difficulties, gas permeation rate is big, these shortcomings limit graphite electrode plate
Extensive use in a fuel cell.C-base composte material electrical and thermal conductivity performance is poor, and high processing costs are degradable.Metal material
There is good electrical and thermal conductivity, higher mechanical strength, anti-vibration, easily shape, is at low cost.Wherein stainless hardness of steel
Height, rotproofness performance are good, stamping suitable for high-volume, are one of optional materials for making fuel battery pole board.But metal pole
Plate is run under fuel cell highly acid, high humidity, hot conditions, is easily corroded, and metal ion degradation causes in catalyst
Poison seriously affects the service life of fuel cell；For metal polar plate under acidic environment, surface forms one layer of passivating film simultaneously, increases
Big contact resistance reduces fuel cell output performance.Therefore, it is corrosion-resistant need to further improve its for the extensive use of metal polar plate
Property and electric conductivity.
In existing public technology, improving metal polar plate corrosion resistance and electric conductivity, there are mainly three types of approach：(1) change metal
Pole plate morphological element；(2) metal polar plate surface is modified；(3) metal polar plate surface prepares one or more layers protective film.It improves stainless
Steel Polar plate matrix Cr, Mo constituent content can significantly improve pole plate corrosion resistance.Metal can be improved by way of alloying
The corrosion resistance of pole plate, but often increase contact resistance, reduce fuel cell output performance.Patent publication No.
CN100495779 is disclosed using the light metal pole plate for oozing expanding method in titanium and its alloy surface acquisition titanium nitride.Patent discloses
Number CN100382367C is disclosed penetrates into the elements such as nitrogen carbon in stainless steel surface, and nitride, carbide, nitrogen are obtained in polar board surface
Carbide is to improve corrosion resistance and electric conductivity.Patent publication No. CN102800871A is disclosed using closed field unbalanced
Magnetron sputtering technique stainless steel polar plate surface deposit carbon chromium ladder coating, by adjust Cr targets, C target currents, argon flow amount and
The technological parameters such as substrate bias adjust ladder Coating composition, the corrosion resistance of metal polar plate greatly improved, reduce and connect
It gets an electric shock and hinders.Patent publication No. CN101752575A discloses the tin oxide that F or Sb doping is prepared on metal polar plate surface, indium oxide
Tin or cadmium tin effectively increase the conductive anti-corrosion capability of metal polar plate as protective film.Patent publication No.
CN101496193A discloses a kind of fuel battery flow field plates, it includes the metal oxide layer for making the plate hydrophilic, to improve
Channel water transports, and improves the anti-corrosion capability of metal polar plate.However in the prior art, it is difficult to needle pore defect be avoided to cause resistance to
Corrosive nature reduces, and the smooth consistency of film surface is relatively low while physical difference increases contact electricity of the pole plate with gas diffusion layers
Resistance.It is therefore proposed that a kind of smooth fine and close film for avoiding needle pore defect simultaneously again, to improve metal polar plate rotproofness performance and lead
Electrical property meets the business requirement of fuel cell.
Invention content
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide.
The purpose of the present invention can be achieved through the following technical solutions：A kind of fuel battery metal pole plate carbide and
Metal oxide composite coating, which is characterized in that the conductive nano that the composite coating is set gradually upwards by metal polar plate surface
Metal oxide layer, carbide lamella composition.
Conductive nano metal oxide layer reduces matrix (i.e. metal polar plate) chemical mobility of the surface, improves matrix and is situated between in environment
Stability in matter, while compact film avoids hole defect, good Corrosion Protection is played in blocking acid ion diffusion.
Carbide lamella is nanostructured layers, smooth densification, good with gas diffusion layers physical property compatibility, can significantly reduce contact resistance.
The conductive nano metal oxide layer is conductive nano layer, and as metal layer and metal oxide layer period is handed over
For coating, to avoid film defects, while the electric conductivity of nano-metal-oxide layer is improved.Wherein, the thickness of metal layer is 0
~50nm, the thickness of metal oxide layer is 1nm~100nm.
Metal oxide in the metal oxide layer includes common metal oxide Al2O3、In2O3、SnO2Deng；It crosses
Cross metal oxide TiO2、ZrO2、Nb2O5、IrO2、MoO2、HfO2Or Ta2O5Deng；The metal oxide layer further includes non-gold
Belong to element doping metal oxide layer (nonmetalloid of doping includes nitrogen, fluorine, boron etc.), non-metering metal oxide, two kinds
And Yi Shang metal oxide mixed layer.
The carbide lamella is the nanostructured layers of carbide, wherein, carbide is class graphite, doped metallic elements
Two kinds in class graphite, metal carbides and two or more mixtures.
The class graphite of the doped metallic elements is formed in carbon network structure for metallic atom disperse, according to metal with
The power of carbide binding ability is divided into strong carbide, middle carbide and weak carbide, the metal packet in the strong carbide
Include Ti, Co or W, the metal in the middle carbide includes Cr, Ni or Mo, the metal in the weak carbide include Al,
Cu, Au or Ag.
Increase flexible metal transition zone, the flexible metal between the metal polar plate and conductive nano metal oxide layer
Transition zone is metal polar plate and multicomponent metallic mixed layer in conductive nano metal oxide layer, to reduce physical property difference, is increased
Strong film-substrate cohesion；
Increase intermediate metal between the conductive nano metal oxide layer and carbide lamella, in the intermediate metal
Metal be oxide and carbide composition metal mixed, to enhance the compatibility of metal oxide and carbide.
A kind of fuel battery metal pole plate carbide and metal oxide composite coating, which is characterized in that this method packet
Include following steps：
(1) metal polar plate surface preparation；
(2) conductive nano metal oxide layer is deposited；
(3) depositing silicon nitride layer；
Metal polar plate surface described in step (1) forms fluid channel by stamping, as the channel for being passed through reaction gas；
Metal polar plate material is stainless steel, aluminium alloy, magnesium alloy or titanium alloy, and metal polar plate thickness is 0.05-2mm, and pretreatment includes
Metal polar plate is cleaned using one or both of ultrasonic cleaning, magnetron sputtering method, multi-arc ion coating method；
Used by step (2) and step (3) sedimentation include magnetron sputtering method, multi-arc ion coating, electron-beam vapor deposition method,
The chemical vapor deposition that sol-gal process, plasma are strengthened.
Composite coating overall thickness is 0.5-5 μm, and flexible metal transition zone is deposited between step (1) and step (2), and thickness is
5-50nm, step (2) deposit conductive nano layer thickness as 10-500nm, deposited metal transition between step (2) and step (3)
Layer, thickness 5-50nm, step (3) precipitated carbide layer thickness are 500nm-5 μm.
Compared with prior art, the present invention is compound in fuel battery metal polar board surface precipitated carbide and metal oxide
Coating, matrix is strong with coating binding force, increases flexible metal transition zone, and carbide lamella is made to increase with metal oxide layer compatibility
By force.Conductive nano metal oxide layer avoids hole defect, it is resistance to can to effectively improve pole plate as corrosive ions barrier diffusion
Corrosive power, carbide lamella have preferable conductive anti-corrosion capability.It is adjusted by adjusting the technological parameter of different process method
Whole Coating composition greatly improves the corrosion resistance of metal polar plate, contact resistance is reduced, so as to improve fuel battery performance.It adopts
The metal polar plate prepared with the present invention can meet fuel cell requirement, have weight to accelerating fuel cell industrialized development
Want meaning.
Description of the drawings
Fig. 1 is one schematic diagram of fuel battery metal pole plate carbide and metal oxide composite coating scheme of the present invention；
Wherein：1- metal polar plate matrixes, 2- intermediate metals, 3- nano-metal-oxide layers, 4- intermediate metals, 5- gold
Belong to carbide lamella；
Fig. 2 is two schematic diagram of fuel battery metal pole plate carbide and metal oxide composite coating scheme of the present invention；
Wherein：1- metal polar plate matrixes, 2 '-intermediate metal, 3 '-metal oxide layer, 4 '-nanometer alternating layer, 5 '-class
Graphite linings；
Fig. 3 is three schematic diagram of fuel battery metal pole plate carbide and metal oxide composite coating scheme of the present invention；
Wherein：1- metal polar plate matrixes, 2 "-intermediate metal, 3 "-nano-metal-oxide layer, 4 "-nanometer alternating layer,
5 "-metal-doped amorphous carbon layer.
Specific embodiment
Below using stainless steel metal pole plate as matrix, with reference to example, the present invention is further explained, but the guarantor of the present invention
Shield range is not limited to following embodiments.
Embodiment 1
Using unbalanced magnetron sputter ion plating technique SnO2:F+GIC:Sn membrane systems
(1) 1 surface of metal polar plate substrate is cleaned by ultrasonic with acetone and absolute ethyl alcohol successively；
(2) metal polar plate after ultrasonic cleaning is put into non-balance magnetically controlled sputter ion plating furnace chamber, vacuumize better than 3 ×
10-5Torr, is filled with argon gas, and operating air pressure is maintained at 4 × 10-4Torr, substrate bias are -500V, carry out ion bombardment removal base
Body passivation layer, ion plating sputter clean process time are 30min, and sample is hung on runing rest, carrier velocity 4r/min；
(3) substrate bias holding -60V opens Sn target currents, and electric current progressively increases to 6A from 0, in metal polar plate matrix 1
Surface deposited metal transition zone 2, sedimentation time 5min；
(4) substrate bias holding -60V, Sn target current are gradually decreased as 0, open SnO2:F targets, electric current are gradually increased by 0
To 6A and then keep, SnO2:F targets are by SnO2With SnF4By atomic ratio F:O=0.025 is mixed, on 1 surface of metal polar plate matrix
The nano-metal-oxide layer 3 of the stannic oxide of Fluorin doped, sedimentation time 20min are deposited on intermediate metal 2.
(5) substrate bias holding -60V, SnO2:F targets are gradually decreased as 0, Sn target currents and gradually increase to 4A, sedimentation time
5min, the deposited metal transition zone 4 on nano-metal-oxide layer 3；
(6) substrate bias holding -60V, Sn target current are gradually decrease to 0.75A, gradually increase C target currents to 6A and then protect
It holds, in class equadag coating, that is, metal carbide layer 5 of 4 surface deposited metal Sn of intermediate metal doping, sedimentation time 60min.
Embodiment 2
TiO is prepared using pulse arc ion plate technology2+GIC:Ag membrane systems
(1) metal polar plate matrix surface is cleaned by ultrasonic with acetone and absolute ethyl alcohol successively；
(2) the metal polar plate matrix hair-dryer drying after ultrasonic cleaning is put on more family ion plating furnace chamber inner supports,
It is evacuated to 8 × 10-3Pa, is passed through Ar gas, and application -700V back bias voltages cause glow discharge and carry out the cleaning of Ar ions aura, time
10min；
(3) metal polar plate substrate bias is down to -500V, opens Ti target current 70A, be passed through O2, deposited in polar board surface
TiO2Obtain metal oxide layer, sedimentation time 10min；
(4) substrate bias is kept, closes oxygen flow, keeps Ti target currents, deposited metal Ti transition zones, sedimentation time
5min；
(5) substrate bias is kept, opens C target current 80A, opens Ag target current 30A, in polar board surface deposition Ag doping classes
Equadag coating, sedimentation time 60min.
Embodiment 3
ZrO is prepared using chemical vapour deposition technique2+ ZrC membrane systems
(1) metal polar plate matrix surface is cleaned by ultrasonic with acetone and absolute ethyl alcohol successively；
(2) by after ultrasonic cleaning metal polar plate matrix hair-dryer drying be put into furnace chamber, be elected to be Ar as carrier gas with
Diluent gas, H2As reducing gas, CO2As carbon-source gas, ZnCl4As Zr sources, deposited in metal polar plate matrix surface
ZrO2Layer, sedimentation time 5min.Total chemical equation is as follows：
H2+CO2=CO+H2O
ZrCl4+2H2O=ZrO2+4HCl
(3) CO is closed2Air source is passed through CH4As carbon source, while Ar is passed through as carrier gas and diluent gas, H2As reduction
Gas, ZnCl4As Zr sources, ZrC layers are deposited on metal polar plate surface.Total chemical equation is as follows：
ZrCl4+CH4=ZrC+4HCl.
Embodiment 4
As shown in Fig. 2, fuel battery metal pole plate carbide and metal oxide composite coating are made by the following method
Into：
(1) metal polar plate matrix surface is cleaned by ultrasonic with acetone and absolute ethyl alcohol successively；
(2) the metal polar plate matrix hair-dryer drying after ultrasonic cleaning is put on more family ion plating furnace chamber inner supports,
It is evacuated to 8 × 10-3Pa, is passed through Ar gas, and application -700V back bias voltages cause glow discharge and carry out the cleaning of Ar ions aura, time
10min；
(3) metal polar plate substrate bias is down to -500V, opens Ti target current 70A, deposited in metal polar plate matrix surface
Ti obtains metal layer, sedimentation time 10min；
(4) substrate bias is kept, is passed through oxygen, keeps Ti target currents, deposit metal oxide layers, sedimentation time 5min；
(5) substrate bias is kept, opens C target current 80A, class graphite linings, sedimentation time 60min are deposited in polar board surface.
The metal polar plate thickness is 0.05mm.The overall thickness of the metal polar plate surface composite coating is 3 μm；Institute
The thickness of conductive nano metal oxide layer stated is 100nm, the metal polar plate and conductive nano metal oxide layer it
Between metal layer thickness be 50nm.
Embodiment 5
As shown in figure 3, fuel battery metal pole plate carbide and metal oxide composite coating are made by the following method
Into：
(1) metal polar plate matrix surface is cleaned by ultrasonic with acetone and absolute ethyl alcohol successively；
(2) metal polar plate after ultrasonic cleaning is put into non-balance magnetically controlled sputter ion plating furnace chamber, vacuumize better than 3 ×
10-5Torr, is filled with argon gas, and operating air pressure is maintained at 4 × 10-4Torr, substrate bias are -500V, carry out ion bombardment removal base
Body passivation layer, ion plating sputter clean process time are 30min, and sample is hung on runing rest, carrier velocity 4r/min；
(3) metal polar plate substrate bias is down to -60V, opens Ni target current 7A, be passed through O2, NiO is deposited in polar board surface2
Obtain nano-metal-oxide layer, sedimentation time 10min；
(4) O is closed2Air source opens Ni target current 7A, and intermediate metal is obtained in metal polar plate matrix surface deposition Ni,
Sedimentation time 10min；
(4) substrate bias is kept, opens C target current 8A, opens Ag target current 3A, in polar board surface deposition Ag doping class stones
Black coating, that is, metal-doped amorphous carbon layer, sedimentation time 60min.
The metal polar plate thickness is 2mm.The overall thickness of the metal polar plate surface composite coating is 2 μm；It is described
Conductive nano metal oxide layer thickness for 500nm, between the metal polar plate and conductive nano metal oxide layer
Metal layer thickness be 50nm.
Foregoing provide some embodiments and the preferred embodiments of the present invention are described in detail to be best understood from this
Invention content, but the range that the present invention is protected is not limited merely to examples detailed above, and technical staff any in the art exists
Intention according to the present invention is conceived by logic on the basis of existing, analyzes obtained technical solution, should all be protected in right
In the range of shield.
Claims (5)
1. a kind of fuel battery metal pole plate carbide and metal oxide composite coating, which is characterized in that the composite coating
Conductive nano metal oxide layer, the carbide lamella set gradually upwards by metal polar plate surface forms；Conductive nano metal oxygen
Compound layer reduces metal polar plate chemical mobility of the surface, improves stability of the metal polar plate in surrounding medium, while conductive nano
Metal oxide layer avoids hole defect, and good Corrosion Protection, the smooth cause of carbide lamella are played in blocking acid ion diffusion
Close, good conductivity is good with gas diffusion layers physical property compatibility, can significantly reduce contact resistance；
The conductive nano metal oxide layer be metal layer and metal oxide layer period alternate coatings, the metal oxygen
Metal oxide in compound layer includes TiO2、ZrO2、Nb2O5、IrO2、MoO2、HfO2Or Ta2O5；The metal oxide layer
Further include nonmetal doping metal oxide layer or non-metering metal oxide layer, the nonmetalloid include nitrogen,
Fluorine or boron；
The carbide lamella is the nanostructured layers of carbide, wherein, carbide is class graphite, the class stone of doped metallic elements
Two or more mixtures in ink, metal carbides.
2. a kind of fuel battery metal pole plate carbide according to claim 1 and metal oxide composite coating,
It is characterized in that, the class graphite of the doped metallic elements is formed for metallic atom disperse in carbon network structure, according to metal
It is divided into strong carbide, middle carbide and weak carbide with the power of carbide binding ability, the metal in the strong carbide
Including Ti, Co or W, metal in the middle carbide includes Cr, Ni or Mo, and the metal in the weak carbide includes
Al, Cu, Au or Ag.
3. a kind of fuel battery metal pole plate carbide according to claim 1 and metal oxide composite coating,
It is characterized in that, increases flexible metal transition zone, flexibility gold between the metal polar plate and conductive nano metal oxide layer
Belong to transition zone for metal polar plate and multicomponent metallic mixed layer in conductive nano metal oxide layer, to reduce physical property difference,
Enhance the binding force of metal polar plate and conductive nano metal oxide layer；
Increase intermediate metal between the conductive nano metal oxide layer and carbide lamella, which is nanometer
Conductive metal oxide layer is mixed with carbide lamella multicomponent metallic, to enhance the compatibility of metal oxide and carbide.
4. a kind of preparation of fuel battery metal pole plate carbide as described in claim 1 and metal oxide composite coating
Method, which is characterized in that this method includes the following steps：
(1) metal polar plate surface preparation；
(2) conductive nano metal oxide layer is deposited；
(3) depositing silicon nitride layer；
Metal polar plate surface described in step (1) forms fluid channel by stamping, as the channel for being passed through reaction gas；Metal
Plate material is stainless steel, aluminium alloy, magnesium alloy or titanium alloy, and metal polar plate thickness is 0.05-2mm, and pretreatment includes will be golden
Belong to pole plate to be cleaned using one or both of ultrasonic cleaning, magnetron sputtering method, multi-arc ion coating method；
Sedimentation includes magnetron sputtering method, multi-arc ion coating, electron-beam vapor deposition method, colloidal sol used by step (2) and step (3)
The chemical vapor deposition that gel method, plasma are strengthened.
5. the system of a kind of fuel battery metal pole plate carbide according to claim 4 and metal oxide composite coating
Preparation Method, which is characterized in that composite coating overall thickness is 0.5-5 μm, and flexible metal mistake is deposited between step (1) and step (2)
Layer is crossed, thickness 5-50nm, step (2) deposition conductive nano layer thickness is 10-500nm, is sunk between step (2) and step (3)
Product intermediate metal, thickness 5-50nm, step (3) precipitated carbide layer thickness are 500nm-5 μm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106129422B (en) * | 2016-08-09 | 2018-09-11 | 上海交通大学 | Improve the densification of fuel battery metal double polar plate overlay coating and corrosion resistant method |
| CN107186352A (en) * | 2017-07-19 | 2017-09-22 | 成都新柯力化工科技有限公司 | A kind of laser color marking method for stainless steel |
| CN108060398A (en) * | 2017-11-01 | 2018-05-22 | 上海交通大学 | A kind of fuel cell composite Nano coating and its plating method |
| 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 |
| CN108598497B (en) * | 2018-04-28 | 2023-12-19 | 上海治臻新能源股份有限公司 | Nano metal layer for fuel cell metal polar plate and preparation method |
| CN110061257A (en) * | 2018-06-28 | 2019-07-26 | 南方科技大学 | Metal Substrate bipolar plates and preparation method thereof for PEMFC |
| CN109037723B (en) | 2018-07-23 | 2022-05-27 | 上海交通大学 | Graphite microcrystalline carbon coating for fuel cell metal bipolar plate and application |
| CN109560290B (en) * | 2018-12-26 | 2023-10-27 | 浙江锋源氢能科技有限公司 | Metal bipolar plate, preparation method thereof and 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 |
| CN111029606B (en) * | 2019-12-20 | 2022-02-25 | 佛山国防科技工业技术成果产业化应用推广中心 | Metal boride-based composite coating for fuel cell bipolar plate and preparation method thereof |
| CN112609165B (en) * | 2020-12-15 | 2022-11-29 | 辽宁科技大学 | Composite coating on surface of bipolar plate of stainless steel-based fuel cell and preparation method thereof |
| CN113584441B (en) * | 2021-08-02 | 2023-11-07 | 杭州兴态环保科技有限公司 | Metal bipolar plate coating and preparation method thereof |
| CN115354297B (en) * | 2022-08-05 | 2024-04-05 | 深圳市氢瑞燃料电池科技有限公司 | Titanium-based coating fuel cell metal polar plate and preparation method thereof |
| CN115332552B (en) * | 2022-10-14 | 2022-12-20 | 上海治臻新能源股份有限公司 | Conductive precoat for fuel cell titanium polar plate and preparation method thereof |
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