CN108018529A - Aluminum-based fuel cell bipolar plate surface composite coating and preparation method thereof - Google Patents
Aluminum-based fuel cell bipolar plate surface composite coating and preparation method thereof Download PDFInfo
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- CN108018529A CN108018529A CN201711099972.0A CN201711099972A CN108018529A CN 108018529 A CN108018529 A CN 108018529A CN 201711099972 A CN201711099972 A CN 201711099972A CN 108018529 A CN108018529 A CN 108018529A
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- aluminum
- fuel cell
- preparation
- bipolar plate
- based fuel
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- 238000000576 coating method Methods 0.000 title claims abstract description 89
- 239000011248 coating agent Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 48
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 43
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000000446 fuel Substances 0.000 title claims abstract description 32
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 29
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 230000007704 transition Effects 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 40
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 36
- 239000007789 gas Substances 0.000 claims description 30
- 239000011159 matrix material Substances 0.000 claims description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- 229910052786 argon Inorganic materials 0.000 claims description 18
- 229910000838 Al alloy Inorganic materials 0.000 claims description 15
- 238000002203 pretreatment Methods 0.000 claims description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- 238000004062 sedimentation Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 238000007733 ion plating Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 4
- 230000002000 scavenging effect Effects 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000013527 degreasing agent Substances 0.000 claims description 2
- 238000010407 vacuum cleaning Methods 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 abstract description 19
- 239000004332 silver Substances 0.000 abstract description 19
- 238000004544 sputter deposition Methods 0.000 abstract description 17
- 238000000151 deposition Methods 0.000 abstract description 16
- 230000007797 corrosion Effects 0.000 abstract description 10
- 238000005260 corrosion Methods 0.000 abstract description 10
- 238000001465 metallisation Methods 0.000 abstract description 4
- 239000010936 titanium Substances 0.000 description 53
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 18
- 229910045601 alloy Inorganic materials 0.000 description 17
- 239000000956 alloy Substances 0.000 description 17
- 230000008021 deposition Effects 0.000 description 13
- 238000005137 deposition process Methods 0.000 description 12
- 238000000861 blow drying Methods 0.000 description 6
- 230000000717 retained effect Effects 0.000 description 6
- 230000002269 spontaneous effect Effects 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3435—Applying energy to the substrate during sputtering
- C23C14/345—Applying energy to the substrate during sputtering using substrate bias
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3464—Sputtering using more than one target
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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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
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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
-
- 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
- H01M2004/8678—Inert electrodes with catalytic activity, e.g. for fuel cells characterised by the polarity
- H01M2004/8694—Bipolar electrodes
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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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
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- Manufacturing & Machinery (AREA)
- Physical Vapour Deposition (AREA)
- Fuel Cell (AREA)
Abstract
The invention discloses a preparation method of a composite coating on the surface of a bipolar plate of an aluminum-based fuel cell, which comprises the following steps: (1) carrying out plasma cleaning on the substrate under a vacuum condition; (2) depositing a pure Ti coating on the cleaned substrate by ion sputtering; (3) depositing a TiN transition layer on the pure Ti coating by ion sputtering; (4) depositing a silver-doped TiN coating on the TiN transition layer; (5) keeping the vacuum condition unchanged, and carrying out heat treatment to ensure that the silver in the silver-doped TiN coating forms short silver wires at the interface of the TiN coating and the short silver wires are aggregated. Silver in the silver-doped TiN coating prepared by the method cannot spontaneously escape to the surface, and short silver lines are formed at the interface of the TiN coating, so that the conductivity of the TiN coating is improved, the surface contact resistance of the TiN coating is reduced, the corrosion resistance of the product is greatly improved, and a theoretical basis and an experimental basis are provided for metallization of a fuel cell pole plate.
Description
Technical field
The present invention relates to belong to field of metal surface treatment, and in particular to a kind of aluminum-based fuel Cell Bipolar plate surface is modified
Method, particularly a kind of method for preparing Ag doping nitridation titanium compound coating in aluminum-based fuel Cell Bipolar plate surface.
Background technology
Proton Exchange Membrane Fuel Cells (PEMFC) is considered because having the advantages that transformation efficiency is high, pollution-free, startup is fast
It is the terminal power of new-energy automobile.But since traditional PEMFC bipolar plates are mostly the graphite cake of veneer thickness 2mm, cause difficulty
To meet the small size of Vehicular battery group, high-energy-density requirement.Therefore, 2mm thickness is substituted with the metal polar plate of below 0.5mm thickness
Graphite cake be the effective way for realizing vehicle fuel battery reduction in bulk.But since the metallic surfaces such as stainless steel, aluminium are easily blunt
Change characteristic and cause its contact resistance to increase.Therefore prepare one layer of electrical conductivity and contact resistance and graphite electrode plate on metal polar plate surface
Quite, the conductive coating for being even less than graphite electrode plate becomes the difficulties solved for fuel battery pole board metallization needs.
Although metal polar plate surface, which prepares class equadag coating, can significantly reduce contact resistance, even in connecing for 1.5MPa
Under touch pressure, the big many of contact resistance of the still purer graphite electrode plate of its contact resistance value.And the resistivity (22 × 10 of titanium nitride-6
Ω cm) than the resistivity (8~13 × 10 of pure graphite-4Ω cm) low two orders of magnitude, therefore select titanium nitride membrane to change
The conductive corrosion resisting property on property aluminum substrate surface.
But since titanium nitride film prepared by sputtering method has defect and the difference of crystal form arrangement, cause contact electricity
Hinder higher, it is therefore necessary to which silver-doped improves its electrical conductivity in titanium nitride coating, reduces contact resistance.Mix metallic silver
The electrical conductivity of titanium nitride coating can be improved, but has a small amount of silver-colored spontaneous effusion, influences the corrosion resisting property of film layer.Therefore,
The method that research suppresses the spontaneous effusion of silver in Ag doping class titanium nitride coating, has important section to fuel battery pole board metallization
Meaning and engineering value are learned, providing theoretical and experiment for the exploitation of subsequent fuel cell pole plate supports.
The content of the invention
The technical problem to be solved in the present invention is overcome the deficiencies of the prior art and provide a kind of aluminum-based fuel cell bipolar plate
The preparation method of surface composite coating, spontaneous surface will not be escaped into using the silver in the Ag doping TiN coatings of this method preparation,
And short and small silver wire is formed in the interface of TiN coatings, the electric conductivity of TiN coatings is improved, reduces its surface contacted resistance, and
The corrosion resistance of product greatly improves, and provides fundamental basis and experimental basis for fuel battery pole board metallization.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of preparation method of aluminum-based fuel cell bipolar plate surface composite coating, comprises the following steps：
(1) matrix through pre-treatment is placed in the vacuum chamber equipped with Ti targets and Ag targets, carry out under vacuum etc. from
Daughter is cleaned；
(2) using Ti targets as evaporation source, using argon gas as working gas, under vacuum using ion plating through step
(1) the pure Ti coatings of one layer of substrate deposit after handling；
(3) using Ti targets as evaporation source, using argon gas and nitrogen as working gas, existed under vacuum using ion plating
One layer of TiN transition zone is deposited on pure Ti coatings obtained by step (2)；
(4) using Ti targets and Ag targets as evaporation source, using argon gas and nitrogen as working gas, under vacuum using ion plating
Technique deposits one layer of Ag doping TiN coating on the TiN transition zones obtained by step (3)；
(5) keep vacuum condition constant, the matrix after step (4) processing is heat-treated, makes Ag doping TiN coatings
In silver in the interface of TiN coatings form short and small silver wire, and reunite.
Preferably, the detailed process of the heat treatment is：200 DEG C~500 are risen to the heating rate of 10~20 DEG C/min
DEG C, insulation 1h~12h postcoolings to room temperature.
Preferably, in the step (1), the operating condition of plasma cleaning is：Vacuumize≤5.0 × 10-3Pa, Ti target electricity
It is -400~-200V to flow for 0.1~0.5A, sample bias, and scavenging period is 15~30min.
Preferably, in the step (2), air pressure is 0.5~0.6Pa in vacuum chamber, and work rest rotating speed is 5~10r/min,
Ti target currents 0.2A~5A, sample bias are -100~-90V, and sedimentation time is 5~10min.
Preferably, in the step (3), air pressure is 0.5~0.6Pa in vacuum chamber, and nitrogen flow increases in 15min from 0
15sccm is added to, is subsequently always maintained at 15sccm, work rest rotating speed is 5~10r/min, and Ti target currents are 2~5A, sample bias
For -90~-60V, sedimentation time is 10~20min.
Preferably, in the step (4), air pressure is 0.5~0.6Pa in vacuum chamber, and nitrogen flow maintains 15sccm, work
Part frame rotating speed is 5~10r/min, and Ti target currents are 2~5A, and Ag 0.01~2A of target current, substrate bias is -90V~-60V, is sunk
The product time is 60~120min.
Preferably, the aluminum-based fuel cell bipolar plate material is aluminium alloy or stainless steel.
Preferably, the pre-treatment includes：Matrix is put into the solution containing degreaser, ultrasonic oil removal processing 5~
10min；Again by ultrasonic cleaning 1~2 time in deionized water of the matrix after oil removing, 3~5min of scavenging period, then in anhydrous second
Ultrasonic cleaning 3~5 times in alcohol, clean 3~5min every time.
Preferably, the distance between matrix and each target are 60~120mm.
The inventive concept total as one, the present invention also provides a kind of aluminum-based fuel as made from above-mentioned preparation method electricity
Pond bipolar plate surfaces composite coating.
Compared with prior art, the advantage of the invention is that：
The present invention carries out hot place by the aluminum-based fuel cell bipolar plate surface composite coating deposited to vacuum ion sputtering
Reason, the effect of heat treatment：(1) silver in aluminum-based fuel cell bipolar plate surface composite coating is formed in the interface of TiN coatings
Short and small silver wire, increases the conductive channel of coating, reduces contact resistance；(2) in aluminum-based fuel cell bipolar plate surface composite coating
Silver reunite under heat treatment condition in coating, form big Silver Clusters, silver-colored spontaneous effusion in suppression coating.Therefore
The silver in Ag doping TiN coatings after this treatment spontaneous will not escape into surface, improve the electric conductivity of TiN coatings, reduce
Its surface contacted resistance.And the method for the present invention preparation process is simple, process stabilizing, reproducible.
Embodiment
Below in conjunction with specific preferred embodiment, the invention will be further described, but not thereby limiting the invention
Protection domain.
Embodiment 1：
Aluminium alloy is chosen as base material, in aluminium alloy matrix surface deposition of silver doped titanium nitride coating, is comprised the following steps that：
(1) sample pre-treatments：The ultrasonic cleaning in deionized water and absolute ethyl alcohol respectively by alloy matrix aluminum, and with heat
Air blow drying；
(2) coating deposition pre-preparation：Alloy matrix aluminum after cleaning is sent into the vacuum chamber equipped with Ti targets and Ag targets, target
Cardinal distance is constant；It is evacuated to 5 × 10-3After Pa, then in Ti target currents it is 0.2A, sample bias carries out under conditions of being -400V etc.
Gas ions clean 20min.
(3) preparation of Ti prime coats：Ti target currents 5A, sample bias -100V, the pure Ti that 8min is deposited under sputtering condition are applied
Layer, argon gas is persistently led in deposition process, ensures in vacuum chamber that air pressure is 0.5Pa, work rest rotating speed is 5r/ in sample preparation procedure
min。
(3) preparation of TiN transition zones：Ti target currents 5A, sample bias -90V, the TiN that 30min is deposited under sputtering condition are applied
Layer, argon gas and nitrogen are persistently led in deposition process, nitrogen flow is gradually increased to 15sccm from 0, ensures that air pressure is in vacuum chamber
0.5Pa, work rest rotating speed is 5r/min in sample preparation procedure.
(4) Ag doping TiN coatings deposit：Ti target currents 5A, Ag target current 0.05A is kept, substrate bias is -60V, deposition
Time 120min；
(5) heat treatment process：After sputter deposition craft, sample is retained in the vacuum chamber, open heating unit, rise
Warm speed is 10 DEG C/min, 400 DEG C of heat treatment temperature, heat treatment time 3h.
The surface contacted resistance for the Ag doping titanium nitride coating that the present embodiment is prepared in aluminum alloy surface is 5m Ω cm2,
Corrosion electric current density is 1.238 × 10-7A/cm2。
Embodiment 2：
Aluminium alloy is chosen as base material, deposition of silver doped titanium nitride coating, comprises the following steps that on alloy matrix aluminum：
(1) sample pre-treatments：The ultrasonic cleaning in deionized water and absolute ethyl alcohol respectively by alloy matrix aluminum, and with heat
Air blow drying；
(2) coating deposition pre-preparation：Alloy matrix aluminum after cleaning is sent into the vacuum chamber equipped with Ti targets and Ag targets, target
Cardinal distance is constant；It is evacuated to 5 × 10-3Be 0.2A in Ti target currents after Pa, sample bias carries out under conditions of being -400V etc. from
20min is cleaned in daughter.
(3) preparation of Ti prime coats：Deposited under conditions of Ti target current 0.2A gradual changes to 5A, sample bias -100V
The pure Ti coatings of 8min, argon gas is persistently led in deposition process, ensures in vacuum chamber that air pressure is 0.5Pa, work in sample preparation procedure
Part frame rotating speed is 5r/min.
(3) preparation of TiN transition zones：Ti target currents 5A, sample bias -90V sputtering condition under deposit 30min
TiN coatings, argon gas and nitrogen are persistently led in deposition process, and nitrogen flow is gradually increased to 15sccm from 0, ensures gas in vacuum chamber
Press as 0.5Pa, work rest rotating speed is 5r/min in sample preparation procedure.
(4) Ag doping TiN coatings deposit：In Ti target currents 2A, Ag target current 0.01A, substrate bias is the condition of -90V
Under, sedimentation time 120min, work rest rotating speed is 5r/min.
(5) heat treatment process：After sputter deposition craft, sample is retained in the vacuum chamber, open heating unit, rise
Warm speed is 20 DEG C/min, 500 DEG C of heat treatment temperature, heat treatment time 12h.
The surface contacted resistance for the Ag doping titanium nitride coating that the present embodiment is prepared in aluminum alloy surface is 8m Ω cm2,
Corrosion electric current density is 4.396 × 10-7A/cm2。
Embodiment 3：
Aluminium alloy is chosen as base material, deposition of silver doped titanium nitride coating, comprises the following steps that on alloy matrix aluminum：
(1) sample pre-treatments：The ultrasonic cleaning in deionized water and absolute ethyl alcohol respectively by alloy matrix aluminum, and with heat
Air blow drying；
(2) coating deposition pre-preparation：Alloy matrix aluminum after cleaning is sent into the vacuum chamber equipped with Ti targets and Ag targets, target
Cardinal distance is constant；It is evacuated to 5 × 10-3Be 0.2A in Ti target currents after Pa, sample bias carries out under conditions of being -400V etc. from
20min is cleaned in daughter.
(3) preparation of Ti prime coats：Deposited under conditions of Ti target current 0.2A gradual changes to 5A, sample bias -100V
The pure Ti coatings of 8min, argon gas is persistently led in deposition process, ensures in vacuum chamber that air pressure is 0.5Pa, work in sample preparation procedure
Part frame rotating speed is 5r/min.
(3) preparation of TiN transition zones：Ti target currents 5A, sample bias -90V sputtering condition under deposit 30min
TiN coatings, argon gas and nitrogen are persistently led in deposition process, and nitrogen flow is gradually increased to 15sccm from 0, ensures gas in vacuum chamber
Press as 0.5Pa, work rest rotating speed is 5r/min in sample preparation procedure.
(4) Ag doping TiN coatings deposit：In Ti target currents 4A, Ag target current 2A, under conditions of substrate bias is -60V,
Sedimentation time 120min, work rest rotating speed are 5r/min.
(5) heat treatment process：After sputter deposition craft, sample is retained in the vacuum chamber, open heating unit, rise
Warm speed is 20 DEG C/min, 500 DEG C of heat treatment temperature, heat treatment time 12h.
The surface contacted resistance for the Ag doping titanium nitride coating that the present embodiment is prepared in aluminum alloy surface is 4m Ω cm2,
Corrosion electric current density is 2.317 × 10-6A/cm2。
Embodiment 4：
Aluminium alloy is chosen as base material, deposition of silver doped titanium nitride coating, comprises the following steps that on alloy matrix aluminum：
(1) sample pre-treatments：The ultrasonic cleaning in deionized water and absolute ethyl alcohol respectively by alloy matrix aluminum, and with heat
Air blow drying；
(2) coating deposition pre-preparation：Alloy matrix aluminum after cleaning is sent into the vacuum chamber equipped with Ti targets and Ag targets, target
Cardinal distance is constant；It is evacuated to 5 × 10-3Be 0.2A in Ti target currents after Pa, sample bias carries out under conditions of being -400V etc. from
20min is cleaned in daughter.
(3) preparation of Ti prime coats：Deposited under conditions of Ti target current 0.2A gradual changes to 5A, sample bias -100V
The pure Ti coatings of 8min, argon gas is persistently led in deposition process, ensures in vacuum chamber that air pressure is 0.5Pa, work in sample preparation procedure
Part frame rotating speed is 5r/min.
(3) preparation of TiN transition zones：Ti target currents 5A, sample bias -90V sputtering condition under deposit 30min
TiN coatings, argon gas and nitrogen are persistently led in deposition process, and nitrogen flow is gradually increased to 15sccm from 0, ensures gas in vacuum chamber
Press as 0.5Pa, work rest rotating speed is 5r/min in sample preparation procedure.
(4) Ag doping TiN coatings deposit：In Ti target currents 5A, Ag target current 1.5A, substrate bias is the condition of -70V
Under, sedimentation time 120min, work rest rotating speed is 5r/min.
(5) heat treatment process：After sputter deposition craft, sample is retained in the vacuum chamber, open heating unit, rise
Warm speed is 20 DEG C/min, 500 DEG C of heat treatment temperature, heat treatment time 12h.
The surface contacted resistance for the Ag doping titanium nitride coating that the present embodiment is prepared in aluminum alloy surface is 5m Ω cm2,
Corrosion electric current density is 8.364 × 10-7A/cm2。
Embodiment 5：
Aluminium alloy is chosen as base material, deposition of silver doped titanium nitride coating, comprises the following steps that on alloy matrix aluminum：
(1) sample pre-treatments：The ultrasonic cleaning in deionized water and absolute ethyl alcohol respectively by alloy matrix aluminum, and with heat
Air blow drying；
(2) coating deposition pre-preparation：Alloy matrix aluminum after cleaning is sent into the vacuum chamber equipped with Ti targets and Ag targets, target
Cardinal distance is constant；It is evacuated to 5 × 10-3Be 0.2A in Ti target currents after Pa, sample bias carries out under conditions of being -400V etc. from
20min is cleaned in daughter.
(3) preparation of Ti prime coats：Deposited under conditions of Ti target current 0.2A gradual changes to 5A, sample bias -100V
The pure Ti coatings of 8min, argon gas is persistently led in deposition process, ensures in vacuum chamber that air pressure is 0.5Pa, work in sample preparation procedure
Part frame rotating speed is 5r/min.
(3) preparation of TiN transition zones：Ti target currents 5A, sample bias -90V sputtering condition under deposit 30min
TiN coatings, argon gas and nitrogen are persistently led in deposition process, and nitrogen flow is gradually increased to 15sccm from 0, ensures gas in vacuum chamber
Press as 0.5Pa, work rest rotating speed is 5r/min in sample preparation procedure.
(4) Ag doping TiN coatings deposit：In Ti target currents 4A, Ag target current 1A, under conditions of substrate bias is -80V,
Sedimentation time 120min, work rest rotating speed are 5r/min.
(5) heat treatment process：After sputter deposition craft, sample is retained in the vacuum chamber, open heating unit, rise
Warm speed is 20 DEG C/min, 500 DEG C of heat treatment temperature, heat treatment time 12h.
The surface contacted resistance for the Ag doping titanium nitride coating that the present embodiment is prepared in aluminum alloy surface is 6m Ω cm2,
Corrosion electric current density is 7.896 × 10-7A/cm2。
Embodiment 6：
Aluminium alloy is chosen as base material, deposition escapes into the Ag doping titanium nitride painting on surface without silver on alloy matrix aluminum
Layer, comprises the following steps that：
(1) sample pre-treatments：The ultrasonic cleaning in deionized water and absolute ethyl alcohol respectively by alloy matrix aluminum, and with heat
Air blow drying；
(2) coating deposition pre-preparation：Alloy matrix aluminum after cleaning is sent into the vacuum chamber equipped with Ti targets and Ag targets, target
Cardinal distance is constant；It is evacuated to 5 × 10-3Be 0.2A in Ti target currents after Pa, sample bias carries out under conditions of being -400V etc. from
20min is cleaned in daughter.
(3) preparation of Ti prime coats：Deposited under conditions of Ti target current 0.2A gradual changes to 5A, sample bias -100V
The pure Ti coatings of 8min, argon gas is persistently led in deposition process, ensures in vacuum chamber that air pressure is 0.5Pa, work in sample preparation procedure
Part frame rotating speed is 5r/min.
(3) preparation of TiN transition zones：Ti target currents 5A, sample bias -90V sputtering condition under deposit 30min
TiN coatings, argon gas and nitrogen are persistently led in deposition process, and nitrogen flow is gradually increased to 15sccm from 0, ensures gas in vacuum chamber
Press as 0.5Pa, work rest rotating speed is 5r/min in sample preparation procedure.
(4) Ag doping TiN coatings deposit：In Ti target currents 2A, Ag target current 0.01A, substrate bias is the condition of -90V
Under, sedimentation time 120min, work rest rotating speed is 5r/min.
(5) heat treatment process：After sputter deposition craft, sample is retained in the vacuum chamber, open heating unit, rise
Warm speed is 20 DEG C/min, 500 DEG C of heat treatment temperature, heat treatment time 12h.
The surface contacted resistance for the Ag doping titanium nitride coating that the present embodiment is prepared in aluminum alloy surface is 7m Ω cm2,
Corrosion electric current density is 9.546 × 10-7A/cm2。
The invention has the advantages that side of the method provided by the present invention for the spontaneous effusion of silver in suppression titanium nitride coating
Method, can realize the effect for improving coating electrical conductivity, reducing contact resistance, for fuel battery pole board exploitation provides experiment support with
Foundation.
The above, is only the preferred embodiment of the application, any type of limitation is not done to the application, although this Shen
Please with preferred embodiment disclose as above, but and be not used to limitation the application, any person skilled in the art, is not taking off
In the range of technical scheme, make a little variation using the technology contents of the disclosure above or modification is equal to
Case study on implementation is imitated, is belonged in the range of technical solution.
Claims (10)
1. a kind of preparation method of aluminum-based fuel cell bipolar plate surface composite coating, comprises the following steps：
(1) matrix through pre-treatment is placed in the vacuum chamber equipped with Ti targets and Ag targets, carries out plasma under vacuum
Cleaning；
(2) using Ti targets as evaporation source, using argon gas as working gas, under vacuum using ion plating through step (1)
The pure Ti coatings of one layer of substrate deposit after processing；
(3) using Ti targets as evaporation source, using argon gas and nitrogen as working gas, under vacuum using ion plating in step
(2) one layer of TiN transition zone is deposited on the pure Ti coatings obtained by；
(4) using Ti targets and Ag targets as evaporation source, using argon gas and nitrogen as working gas, under vacuum using ion plating
One layer of Ag doping TiN coating is deposited on the TiN transition zones obtained by step (3)；
(5) keep vacuum condition constant, the matrix after step (4) processing is heat-treated, is made in Ag doping TiN coatings
Silver forms short and small silver wire in the interface of TiN coatings, and reunites.
2. the preparation method of aluminum-based fuel cell bipolar plate surface composite coating according to claim 1, it is characterised in that
The detailed process of the heat treatment is：200 DEG C~500 DEG C are risen to the heating rate of 10~20 DEG C/min, after keeping the temperature 1h~12h
It is cooled to room temperature.
3. the preparation method of aluminum-based fuel cell bipolar plate surface composite coating according to claim 1 or 2, its feature exist
In in the step (1), the operating condition of plasma cleaning is：Vacuumize≤5.0 × 10-3Pa, Ti target current for 0.1~
0.5A, sample bias are -400~-200V, and scavenging period is 15~30min.
4. the preparation method of aluminum-based fuel cell bipolar plate surface composite coating according to claim 3, it is characterised in that
In the step (2), air pressure is 0.5~0.6Pa in vacuum chamber, and work rest rotating speed is 5~10r/min, Ti target currents 0.2A~
5A, sample bias are -100~-90V, and sedimentation time is 5~10min.
5. the preparation method of aluminum-based fuel cell bipolar plate surface composite coating according to claim 4, it is characterised in that
In the step (3), air pressure is 0.5~0.6Pa in vacuum chamber, and nitrogen flow increases to 15sccm in 15min from 0, subsequently
15sccm is always maintained at, work rest rotating speed is 5~10r/min, and Ti target currents are 2~5A, sample bias is -90~-60V, is sunk
The product time is 10~20min.
6. the preparation method of aluminum-based fuel cell bipolar plate surface composite coating according to claim 5, it is characterised in that
In the step (4), air pressure is 0.5~0.6Pa in vacuum chamber, and nitrogen flow maintains 15sccm, work rest rotating speed for 5~
10r/min, Ti target current are 2~5A, Ag 0.01~2A of target current, and substrate bias is -90V~-60V, sedimentation time for 60~
120min。
7. the preparation method of aluminum-based fuel cell bipolar plate surface composite coating according to any one of claim 4 to 6, its
It is characterized in that, the aluminum-based fuel cell bipolar plate material is aluminium alloy or stainless steel.
8. the preparation method of aluminum-based fuel cell bipolar plate surface composite coating according to claim 7, it is characterised in that
The pre-treatment includes：Matrix is put into the solution containing degreaser, ultrasonic oil removal handles 5~10min；Again by after oil removing
Matrix ultrasonic cleaning 1~2 time in deionized water, 3~5min of scavenging period, then ultrasonic cleaning 3 in absolute ethyl alcohol
~5 times, 3~5min is cleaned every time.
9. the preparation method of aluminum-based fuel cell bipolar plate surface composite coating according to claim 8, it is characterised in that
The distance between matrix and each target are 60~120mm.
A kind of 10. aluminum-based fuel cell bipolar plate surface composite coating, it is characterised in that the aluminum-based fuel cell bipolar plate table
Surface composite coating is made by claim 1~9 any one of them preparation method.
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Application publication date: 20180511 |