CN107681173A - A kind of point-like conduction composite coating for fuel battery metal pole plate - Google Patents
A kind of point-like conduction composite coating for fuel battery metal pole plate Download PDFInfo
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- CN107681173A CN107681173A CN201710654929.XA CN201710654929A CN107681173A CN 107681173 A CN107681173 A CN 107681173A CN 201710654929 A CN201710654929 A CN 201710654929A CN 107681173 A CN107681173 A CN 107681173A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0206—Metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8803—Supports for the deposition of the catalytic active composition
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0223—Composites
- H01M8/0228—Composites in the form of layered or coated products
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The present invention relates to a kind of point-like conduction composite coating for fuel battery metal pole plate, the point-like conduction composite coating is previously deposited metal level, metal oxide layer or conductive non-metals layer in metal polar plate upper surface first, then the redeposited point-like metal on the coating being previously deposited.Compared with prior art, the present invention has more excellent electric conductivity and decay resistance, especially resistance to high potential corrosive nature, significantly increases metal polar plate durability under fuel cell acidic environment.The point-like conductive coating that simultaneously prepared by the present invention can substantially reduce noble metal use, reduce coating cost.
Description
Technical field
The present invention relates to a kind of fuel battery metal polar board surface coating, is used for fuel battery metal more particularly, to one kind
The point-like conduction composite coating of pole plate, for reducing contact resistance between fuel battery metal pole plate and gas diffusion layers, is carried simultaneously
Durability of the high metal pole plate under sour environment.
Background technology
Metal double polar plates have the characteristics that good mechanical performance, cost are low, quality is small, are considered as gradually fuel cell
The first choice of industrialization.Fuel battery metal double polar plate working environment is pH 2-5,70-100 DEG C of hot and humid environment, metal material
Material surface can be passivated, and cause contact resistance to increase, and reduce cell output.Metal material is sent out in sour environment simultaneously
Raw corrosion, the metal ion pollution catalyst of precipitation, reduces membrane electrode electrical conductivity.Therefore the decay resistance of metal polar plate is improved
It is the commercialized main direction of studying of metal double polar plates with contact resistance is reduced.
One layer of conductive corrosion-resistant is prepared by modes such as PVD, CVD, ion plating, chemical plating, plating on metal polar plate surface
Functional coating be recent domestic research focus.Many scholars apply thin to metal nitride, metal carbides, amorphous carbon
Film, noble coatings etc. have done widely studied, and the decay resistance and electric conductivity of metal polar plate are obviously improved.It is but existing
It is thicker that some technologies prepare standby coating layer thickness, and cost is high, and mass production is difficult.Simultaneously the few patents delivered of aspect and
Paper did research in terms of Coating Durability.Under the hot and humid strong acidic environment long-play of fuel cell, coating
Failure mode be generally coating shedding and contact resistance increase.Coating shedding main cause is the coating compactness extent prepared
It is low and poor to strengthen the corrosion resistance for the transition zone that adhesion designs, cause primer to corrode, then cause to fall film
Phenomenon.The working condition of complexity is undergone in the operation of actual pile, such as starts parking, CYCLIC LOADING, low load idling, these behaviour
Make the potential environment that condition produces complexity inside pile.Such as starting moment of stopping, 1.6V is produced in cathode sideSHEHigh potential
Corrosion dissolution phenomenon inevitably occurs in such circumstances for environment, general primer.Simultaneously because the generation of corrosion phenomenon,
Cause coating surface that oxidative phenomena can occur, cause contact resistance to increase.
Metal polar plate Coating Durability is improved, electroplating gold on surface is a kind of common preparation technology, but it is required to electroplate gold
Gold thin film thickness is generally too high in more than 100nm, cost, it is difficult to meets that metal polar plate is commercialized demand.Therefore preparation high efficiency,
Low cost, the metal polar plate coating of excellent in durability become particularly important.In actually contacting, contact surface is all rugged
Rough surface, contact of the metal polar plate with gas diffusion layers are occurred only on a small number of and small spots, the reality of nominal interface
Border contact area greatly reduces.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind is used for fuel cell
The point-like conduction composite coating of metal polar plate, metal polar plate corrosion resistance can be strengthened, improve Coating Durability energy, carry simultaneously
High metal pole plate coating manufacture efficiency, reduce production cost.
Present invention basis is in fuel cell actual environment, the gas diffusion layers of fibre structure and connecing for metal polar plate surface
It is some microcosmic point-like contacts to touch, i.e. reachable after there is the coating with good conductivity for covering certain percentage amounts on metal polar plate surface
To the purpose for reducing contact resistance and a kind of fuel battery metal pole plate point-like coating for proposing.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of point-like conduction composite coating for fuel battery metal pole plate, the point-like conduction composite coating is first in gold
Category pole plate upper surface is previously deposited metal level, metal oxide layer or conductive non-metals layer, then on the coating being previously deposited
Redeposited point-like metal.
Described metal level is W, Ni, Zr, Ti, Nb or Ta metal level, thickness 5-100nm.On the one hand point-like is improved to lead
The adhesion of electric layer and matrix, the corrosion resistance of metal on the other hand deposited is strong, can strengthen overall resistance to corrosion.Especially
It is to the caused high potential in pile.
Described metal oxide layer is WO2, NiO, TiO2, Nb2O5, WO2, Ta2O5Deng thickness is 0-200nm but is not 0.
Described conductive non-metals layer is SiO2, graphite, class graphite, conducting polymer, metal nitride or metallic carbide
Thing, thickness 5-100nm.
Be additionally provided with intermediate metal between described conductive non-metals layer and metal polar plate, the intermediate metal be W, Ni,
Zr, Ti, Nb or Ta corrosion resistant metal, to strengthen physics adhesion.
Described point-like metal is Pt, Y, Ag, Au or Ru, and coverage rate is between 10%-100%, point-like metal level particle
Degree is in 1-500nm.
Described point-like damascene is between the metal oxide or conductive non-metals being previously deposited.
Point-like conductive coating proposed by the present invention is embedded between metal oxide, can be mutually right by increasing before sedimentary origin
The shutter answered is realized.Such as point-like metal coverage rate is 50%, then placement percent 50% is blocked before noble metal sputter
Plate, and other 50% shutter is placed before another depositing metal oxide, the position of opening of two pieces of shutters is mutual
Dislocation.If the coverage rate of noble metal 100%, does not need deposit metal oxide layers.
Metal oxide is deposited on around point-like conductive layer, can significantly increase coating entirety resistance to corrosion.Metal simultaneously
Oxide structure does not form galvanic corrosion with point-like conductive structure around, can effectively avoid the corrosion of point-like conductive layer from being lost in now
As.
Described metal polar plate upper surface can be set to multilayer alternating structure, and alternately the number of plies and alternate cycle are adjustable, point-like
Metal structure is deposited on outermost layer.
Fuel battery metal pole plate point-like coating and preparation technology specific embodiment are as follows:
The first step:Stainless steel metal bipolar plates are cleaned up into surface and oil contaminant impurity with deionized water, are put into plasma
In cleaning equipment, using plasma bombardment polar board surface caused by ion gun, to remove surface oxide layer, matrix surface is improved
Energy surface-active, strengthens coating binding force;
Second step:The metal levels such as W, Ni, Zr, Ti, Nb, Ta are previously deposited in metal polar plate upper surface, or are previously deposited
WO2, NiO, TiO2, Nb2O5, WO2, Ta2O5, SiO2Deng metal oxide layer, or conducting polymer is previously deposited, metallic carbide
The non-metallic layers such as thing, metal nitride, class graphite linings;
3rd step:On the basis of the coating being previously deposited, point-like conductive noble metal layer is deposited, is dispersed in metal double polar plates
Surface, surface coverage is between 10%-100%;
Fuel battery metal double polar plate point-like conductive coating preparation method proposed by the present invention can be magnetron sputtering, multi sphere
Ion plating, chemical meteorology deposition, sol-gel method etc.;To improve production efficiency, Multicarity continous way deposition process can be used,
A technical process is completed in a process cavity.
A kind of point-like conductive coating proposed by the present invention is for the corrosion test of resistance to high potential and durability test evaluation side
Method is using the sample of preparation as working electrode, and electrochemical corrosion test is carried out with the three-electrode system commonly used in electrochemistry.Survey
Test ring border is pH3H2SO4+ 0.1ppm HF, 80 DEG C of temperature, apply relative hydrogen electrode 1.6V in sample surfaces and carry out constant potential polarization
After different time, contact resistance test, test pressure 1.4Mpa are carried out.
In preferred embodiments of the present invention, a kind of described point-like conduction composite coating is under 1.4Mpa, metal polar plate and carbon
Initial contact resistance is reduced to 1.5-2.0m Ω cm between paper2, corrosion electric current density is less than 1.0 μ A/cm2, by 1.6VSHEConstant potential
Polarize 36h, and sample is still excellent, and contact resistance does not have increase phenomenon, and the point-like conduction composite coating prepared by surface has
Good performance, metal polar plate durability can be significantly increased.
Compared with prior art, one kind proposed by the present invention is used for fuel battery metal pole plate point-like conductive coating and preparation
Technique, there is stronger resistance to corrosion, can especially resist high potential corrosive power, suitable for various vehicle-mounted operating modes;Together
When the coating there is good electric conductivity, long-time corrode under, coating layer touch resistance will not occur increase phenomenon, have it is good
Good endurance quality.Compared with traditional plating gold or vapor phase deposition noble metal film, coating structure proposed by the present invention can be big
Width reduces noble metal and used, and reduces production cost.Coating process proposed by the present invention is applicable to the production of continuous batch metaplasia simultaneously,
Contribute to metal polar plate industrialization process.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention of embodiment 1;
Fig. 2 is the cross section structure diagram of the present invention of embodiment 1;
Fig. 3 is the structural representation of the present invention of embodiment 2;
Fig. 4 is the cross section structure diagram of the present invention of embodiment 2;
Fig. 5 is the structural representation of the present invention of embodiment 3;
Fig. 6 is the cross section structure diagram of the present invention of embodiment 3;
Fig. 7 is the structural representation of the present invention of embodiment 4;
Fig. 8 is the cross section structure diagram of the present invention of embodiment 4;
Fig. 9 is the SEM image of the nano-dotted Ag layers of embodiment 5;
Figure 10 is metal polar plate contact resistance data under 1.4MPa;
Figure 11 is the SEM image of the nano-dotted Pt layers of embodiment 6;
Figure 12 is metal polar plate contact resistance data under 1.4MPa;
Figure 13 is the nano-dotted gold of embodiment 7 and amorphous carbon coating performance comparision.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
A kind of point-like conduction composite coating for fuel battery metal pole plate, its structure as shown in Figure 1-2, lead by the point-like
Electric composite coating is previously deposited metal level 1-2 in metal polar plate 1-1 upper surface first, and what is deposited in the present embodiment is that thickness is
5nm metal W.Then the redeposited point-like metal 1-3 on the coating being previously deposited, what is deposited in the present embodiment is that thickness is
1nm precious metals pt.
Embodiment 2
A kind of point-like conduction composite coating for fuel battery metal pole plate, its structure as shown in Figure 3-4, lead by the point-like
Electric composite coating is previously deposited metal level 2-2 in metal polar plate 2-1 upper surface first, and deposit thickness is 10nm W metal.
Then the redeposited point-like metal 2-3 on the coating being previously deposited, deposition is noble metal Y of the thickness for 1nm, and coverage rate exists
10%, then proceed to the deposited metal layer 2-4 on point-like metal 2-3, deposition be thickness 10nm metal Nb, and in the metal
Redeposited point-like metal 2-5 on layer 2-4, deposition is precious metals ag of the thickness for 10nm.
Embodiment 3
A kind of point-like conduction composite coating for fuel battery metal pole plate, its structure as seen in figs. 5-6, lead by the point-like
Electric composite coating is previously deposited oxide skin(coating) 3-2 in metal polar plate 3-1 upper surface first, deposition be thickness 1nm WO2,
Then the redeposited point-like metal 3-3 on the coating being previously deposited, deposition is noble metal Au of the thickness for 10nm, is embedded in
Between oxide.
Embodiment 4
A kind of point-like conduction composite coating for fuel battery metal pole plate, its structure as Figure 7-8, lead by the point-like
Electric composite coating is previously deposited oxide skin(coating) 4-2 in metal polar plate 4-1 upper surface first, then in the coating being previously deposited
Upper redeposited point-like metal 4-3, the deposited oxide layer 4-4 on point-like metal 4-3 is then proceeded to, and in oxide skin(coating) 4-4
Upper redeposited point-like metal 4-5, is embedded between oxide.
Embodiment 5
A kind of point-like conduction composite coating for fuel battery metal pole plate, make to obtain using following methods:
The first step:Stainless steel metal bipolar plates are cleaned up into surface and oil contaminant impurity with deionized water in advance, be put into etc. from
In daughter cleaning equipment, using plasma bombardment polar board surface caused by ion gun, to remove surface oxide layer, matrix is improved
Surface energy surface activity, strengthens coating binding force.
Second step:One layer of Nb metal is deposited on the metal polar plate surface cleaned up, Nb metal layer thickness is 30nm;
3rd step:The nano-dotted silver layer that coverage rate is 50% or so is deposited on Nb metal levels;
4th step:The metal polar plate for having deposited coating is carried out into Analysis of Surface Topography to detect with contact resistance.Fig. 9 is shown
The SEM image of nano-dotted Ag layers, Figure 10 are metal polar plate contact resistance data under 1.4MPa.White point-like in wherein SEM
Material is silver nano-grain.Compared to amorphous carbon coating, metal polar plate Nano Silver point-like coating manufactured in the present embodiment significantly drops
Low contact resistance, plays an important role for metal polar plate performance boost.
Embodiment 6
A kind of point-like conduction composite coating for fuel battery metal pole plate, make to obtain using following methods:
The first step:Stainless steel metal bipolar plates are cleaned up into surface and oil contaminant impurity with deionized water in advance, be put into etc. from
In daughter cleaning equipment, using plasma bombardment polar board surface caused by ion gun, to remove surface oxide layer, matrix is improved
Surface energy surface activity, strengthens coating binding force;
Second step:One layer of Ta metal level is deposited in the metal bipolar plate surface cleaned up;Metal Ta thickness degree is 30nm;
3rd step:One layer of class equadag coating, coating layer thickness 100nm are deposited in metal Ta layer surfaces;
4th step:One layer of Pt nano particle, the wherein covering of point-like Pt particles are deposited on the class equadag coating deposited
Rate is 40% or so;
5th step:The metal polar plate for having deposited coating carries out Analysis of Surface Topography and contact resistance detection.Figure 11 is shown
The SEM image of nano-dotted Pt layers, Figure 12 are metal polar plate contact resistance data under 1.4MPa.Compared to amorphous carbon coating,
Metal polar plate Nano Silver point-like coating manufactured in the present embodiment significantly reduces contact resistance, has for metal polar plate performance boost
Important function.
Embodiment 7
A kind of point-like conduction composite coating for fuel battery metal pole plate, make to obtain using following methods:
The first step:Stainless steel metal bipolar plates are cleaned up into surface and oil contaminant impurity with deionized water in advance, be put into etc. from
In daughter cleaning equipment, using plasma bombardment polar board surface caused by ion gun, to remove surface oxide layer, matrix is improved
Surface energy surface activity, strengthens coating binding force;
Second step:One layer of 5-10nm TiO is deposited in the metal bipolar plate surface cleaned up2Film;
3rd step:The nano-dotted layer gold that coverage rate is 30% is deposited on thin film of titanium oxide;The particle diameter of point-like gold
In 10-20nm.Wherein nano-dotted gold is embedded in thin film of titanium oxide;
4th step:The coating deposited is made annealing treatment, goes residual stress in removing coating, annealing temperature is not higher than
300℃;
5th step:The nano-dotted gold plating of the metal double polar plates deposited is subjected to decay resistance analysis.Method of testing
For 1.6VSHEConstant potential polarization, etchant solution pH3H2SO4Solution;Contact resistance under 1.4MPa is tested afterwards.Point-like nanogold
It is as shown in figure 13 with amorphous carbon coating performance comparison concrete outcome, wherein that (a) expression is constant potential 1.6VSHEPolarization current is close
Write music line, the low 1-2 magnitudes of nano-dotted golden current density ratio tradition amorphous carbon layer current density, show described conductive nano gold
With more preferable corrosion resistance, that (b) is represented is constant potential 1.6VSHEContact resistance after polarization, it is rotten by long-time high potential
Nanogold point-like coating layer touch resistance is held essentially constant after erosion, and amorphous carbon layer is increased to 25m Ω in corrosion 1h contact resistances
cm2.Thus contrast is it can be seen that the nm Au of example 3 has good decay resistance and electric conductivity.
Embodiment 8
A kind of point-like conduction composite coating for fuel battery metal pole plate, make to obtain using following methods:
The first step:Stainless steel metal bipolar plates are cleaned up into surface and oil contaminant impurity with deionized water in advance, be put into etc. from
In daughter cleaning equipment, using plasma bombardment polar board surface caused by ion gun, to remove surface oxide layer, matrix is improved
Surface energy surface activity, strengthens coating binding force;
Second step:In metal bipolar plate surface one layer of conductive polymer coating, coating layer thickness are deposited using so-gel method
In 100nm or so;
3rd step:One layer of point-like Pt layer is sprayed in the conductive polymer surfaces deposited using the mode of spin coating, it is poly- to increase
The electrical conductivity of compound layer, improve metal double polar plates performance.
Embodiment 9
A kind of point-like conduction composite coating for fuel battery metal pole plate, the point-like conduction composite coating is first in gold
Category pole plate upper surface is previously deposited conductive non-metals layer, then redeposited point-like metal, this reality on the coating being previously deposited
Apply in example, conductive non-metals layer is the thick graphite linings of 5nm, and point-like metal is Pt, and coverage rate is 100%, point-like metal level particle
Degree is in 1nm.
Embodiment 10
A kind of point-like conduction composite coating for fuel battery metal pole plate, the point-like conduction composite coating is first in gold
Category pole plate upper surface is previously deposited conductive non-metals layer, then redeposited point-like metal, this reality on the coating being previously deposited
Apply in example, conductive non-metals layer is the thick metal carbides of 100nm, and point-like metal is Pt, and coverage rate is 10%, point-like metal level
Granularity in 500nm, and conductive non-metals layer and metal polar plate between be additionally provided with intermediate metal Ta.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (8)
- A kind of 1. point-like conduction composite coating for fuel battery metal pole plate, it is characterised in that the conductive compound painting of the point-like Layer is previously deposited metal level, metal oxide layer or conductive non-metals layer in metal polar plate upper surface first, is then being previously deposited Redeposited point-like metal on good coating.
- 2. the point-like conduction composite coating according to claim 1 for fuel battery metal pole plate, it is characterised in that institute The metal level stated is W, Ni, Zr, Ti, Nb or Ta metal level, thickness 5-100nm.
- 3. the point-like conduction composite coating according to claim 1 for fuel battery metal pole plate, it is characterised in that institute The metal oxide layer stated is WO2, NiO, TiO2, Nb2O5, WO2Or Ta2O5, thickness is 0-200nm but is not 0.
- 4. the point-like conduction composite coating according to claim 1 for fuel battery metal pole plate, it is characterised in that institute The conductive non-metals layer stated is SiO2, graphite, class graphite, conducting polymer, metal nitride or metal carbides, thickness 5- 100nm。
- 5. the point-like conduction composite coating according to claim 4 for fuel battery metal pole plate, it is characterised in that institute Be additionally provided with intermediate metal between the conductive non-metals layer and metal polar plate stated, the intermediate metal be W, Ni, Zr, Ti, Nb or Ta corrosion resistant metal.
- 6. the point-like conduction composite coating according to claim 1 for fuel battery metal pole plate, it is characterised in that institute The point-like metal stated is Pt, Y, Ag, Au or Ru, and coverage rate is between 10%-100%, and point-like metal level granularity is in 1- 500nm。
- 7. the point-like conduction composite coating for fuel battery metal pole plate according to claim 1 or 6, its feature exist In described point-like damascene is between the metal oxide or conductive non-metals being previously deposited.
- 8. the point-like conduction composite coating according to claim 1 for fuel battery metal pole plate, it is characterised in that institute The metal polar plate upper surface stated can be set to multilayer alternating structure, and alternately the number of plies and alternate cycle are adjustable, and point-like metal structure is sunk Product is in outermost layer.
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CN108598497A (en) * | 2018-04-28 | 2018-09-28 | 上海治臻新能源装备有限公司 | A kind of nano metal layer and preparation method for fuel battery metal pole plate |
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