CN204361172U - A kind of nitrogenize strengthens the bipolar plate for fuel cell on surface - Google Patents
A kind of nitrogenize strengthens the bipolar plate for fuel cell on surface Download PDFInfo
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- CN204361172U CN204361172U CN201520057173.7U CN201520057173U CN204361172U CN 204361172 U CN204361172 U CN 204361172U CN 201520057173 U CN201520057173 U CN 201520057173U CN 204361172 U CN204361172 U CN 204361172U
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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
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- 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
Nitrogenize strengthens the fuel battery double plates on surface, belongs to field of fuel cell technology.This bipolar plates is prepared successively on corrosion resistant plate or titanium alloy sheet matrix both side surface nitration case, chromium nitride film and carbon-based nano composite conductive thin film.The thickness of nitration case is 0.1 μm ~ 20 μm, and the thickness of chromium nitride film is 0.1 μm ~ 20 μm, and the thickness of described carbon-based nano composite conductive thin film is 0.1 μm ~ 20 μm.Carbon in chromium nitride film and carbon-based nano composite conductive thin film, nitrogen element content along perpendicular to corrosion resistant plate or titanium alloy sheet matrix direction in gradient continuous distribution the utility model in fuel cell battery double-polar plate surface modifying field, introduce ionic nitriding technology, prepare nitration case on surface and can avoid matrix passivation, effectively prevent from corroding and cause the situation of coating failure to occur, adopt ladder transition method by chromium nitride and nano combined conductive film multiple elements design, prevent in coating use procedure because internal stress is excessive, adhesion is too small and peel off.
Description
Technical field
The invention belongs to field of fuel cell technology, particularly strengthen the fuel battery double plates on surface and preparation method thereof.
Background technology
Fuel cell has the advantages such as energy conversion efficiency, high power density, safety and environmental protection because of it and enjoys the attention of national governments and research institution, and it is considered to a kind of high efficient energy sources device alleviating the day by day exhausted and environmental pollution of resource.Wherein, Proton Exchange Membrane Fuel Cells (PEMFC) has energy conversion efficiency high (40% ~ 60%), zero discharge, fast startup and specific power advantages of higher, is considered to for vehicle power, distributed power generation station and the ideal device that can carry power supply.Along with the application of pem cell in the vehicles such as automobile, it is as the energy technology of a new generation, can penetrate into social all trades and professions and even average family gradually.Therefore, the development of development to whole technical field of new energies of Proton Exchange Membrane Fuel Cells has very important effect.But the serviceability of fuel cell and Cost Problems hinder pem cell greatly and commercially produce widely.
Bipolar plates is the multi-functional critical component in pem cell, account for 80% of pem cell total weight, pem cell total cost 40% ~ 50%, its effect is separated reacting gas, collected current, to be got up by each cells in series and by flow field for the eliminating of reaction gas turnover electrode and water provides passage etc.In order to meet these functions, bipolar plates should have the characteristics such as very high conductivity, corrosion resistance, low-density, high mechanical properties, high-gas resistance ability, low cost and easy processing.The bipolar plate material of pem cell mainly contains three classes: graphite bi-polar plate, metal double polar plates, composite material double pole plate.Graphite is good conductivity after high-temperature process, corrosion-resistant, is used widely in the pem cell early stage of development, but such materials processing high cost, and be limited to mechanical strength and cannot realize sheet, cause the volume and weight of graphite bi-polar plate comparatively large, thus limit its practical application.Composite material double pole plate is that cost is lower, but still has much room for improvement in conductivity and choke ability with carbon dust and resin for major ingredient is prepared from through methods such as mold pressings.
Metal is the bipolar plate material of desirable Proton Exchange Membrane Fuel Cells, and it has conduction, the heat conductivility that good intensity is become reconciled, and rich reserves, easy processing, be easy to batch production, and improve power density by reducing thickness, there is the great potential reducing bipolar plates cost; In addition, metal can also to prevent in water cavity cooling agent to the diffusion of battery the two poles of the earth, and being particularly useful for can the fuel cell system of cold-starting.So metal double polar plates is considered to the inevitable choice that Proton Exchange Membrane Fuel Cells realizes industrialization, but, the subject matter of metal double polar plates is easily corroded under pem cell environment, its consequence is not only and is made bipolar plates disabler, but also proton exchange membrane can be caused " to poison ", its electric conductivity also declines due to surface corrosion simultaneously, and power output is reduced.Adopt alloying mode can improve the corrosion resistance of metal, but often bring the decline of its conductivity; Use some noble metals (such as Au, Ag) that corrosion resisting property and conductivity can be taken into account, but directly use noble metal can bring the significantly lifting of material cost.This is the bottleneck of restriction metal double polar plates extensive use to contradiction how to solve decay resistance and electric conductivity.In addition, common metal surface all has natural hydrophily, causes the blocking of bipolar plate flow field to be also one of subject matter causing bipolar plates operation stability to decline therefrom.
For the many difficult problems in metal double polar plates application, what prior art generally adopted is, in the common metal performance basis had metal reservation base material, to its modifying surface process, in recent years, using sheet metal as basis material, the method such as vapour deposition, ion implantation of employing prepares the study hotspot that the corrosion-resistant and heterogeneous coating that is conduction of one deck becomes this area in substrate.The surface modified coat carried out for metallic matrix at present is mainly divided into carbon-base coating and the large class of metal based coating two, the technique related to improves the surface property of metallic plate more or less, but these techniques are mostly still immature at present, can not be used in the middle of actual production, and wherein, the application prospect of Direct precipitation carbon chromium thin film is extensively had an optimistic view of on metal base.
For the technique of Direct precipitation carbon chromium thin film, due to the defect of vacuum technique itself, the general concrete dynamic modulus of film, this problem caused in application is exactly:
If film thickness is blocked up, although reduce porosity, this first aspect result in the rising of manufacturing cost, also increases the contact resistance of bipolar plates on the other hand.Inadvisable in the fuel battery double plates commercial application.
If film thickness is excessively thin, the oxygen of negative electrode distribution spreads by hole the bipolar plates matrix that can go directly, make its passivation, overall contact resistance is made to become large, directly cause the internal resistance of battery to improve, the output voltage of battery reduces and impact uses, and the contact resistance of bipolar plates is larger, ohm heat produced in cell operation is also more, and the battery temperature that this causes raises the activity that also can affect catalyst in battery; In addition, the porosity defects of vacuum coating can cause base material to be exposed in outer room environment, its electrochemical corrosion as anode occurs, causes coating premature failure.
In addition, prior art is direct carbon coating chromium thin film on metallic matrix, and such processing mode can cause the coating binding force between carbon chromium thin film and matrix less, causes the phenomenon in use occurring that film is peeled off.
Therefore the subject matter faced at present is, when preparing fuel battery double plates carbon chromium thin film, how to ensure, under the prerequisite that film thickness is thinner, to strengthen the resistance to corrosion of fuel battery double plates surface film.
Utility model content
In order to solve the problems referred to above that prior art exists, the invention provides a kind of corrosion-resistant, conduct electricity very well, the bipolar plate for fuel cell of surface coating that adhesion is high.Be characterized in introducing ionic nitriding technology on conventional arc ion plating technique, prepared nitration case, chromium nitride film and carbon-based nano composite conductive thin film successively in metal double polar plates both side surface.
The technical scheme that the present invention is adopted for achieving the above object is: a kind of nitrogenize strengthens the bipolar plate for fuel cell on surface, comprise corrosion resistant plate or titanium alloy sheet matrix, it is characterized in that: in described corrosion resistant plate or titanium alloy sheet matrix both side surface, preparation has nitration case, chromium nitride film and carbon-based nano composite conductive thin film successively.
The thickness of described nitration case is 0.1 μm ~ 20 μm, and the thickness of described chromium nitride film is 0.1 μm ~ 20 μm, and the thickness of described carbon-based nano composite conductive thin film is 0.1 μm ~ 20 μm.
Carbon in described chromium nitride film and carbon-based nano composite conductive thin film, nitrogen element content are along perpendicular to corrosion resistant plate or titanium alloy sheet matrix direction continuous distribution in gradient.
The beneficial effect that a kind of bipolar plate for fuel cell of the present invention and nitrogenize enhancing surface modifying method thereof can bring is:
(1) on traditional arc ion plating (aip) basis, ionic nitriding technology is introduced, namely in advance the element nitrogen elements such as chromium, iron, titanium within the scope of bipolar plates matrix surface certain depth are cured, define at substrate surface that porosity is extremely low, the nitration case of stable chemical nature, the oxygen around bipolar plates matrix and negative electrode can be isolated, reach the effect avoiding matrix passivation;
(2) by plasma nitrided technology, form nitride at matrix surface, its corrosion potential is higher, little with film difference, therefore can effectively avoid corroding causing the situation of coating failure to occur;
(3) in preparation process, the flow of nitrogen is passed into during Linear Control plated film, reach carbon in chromium nitride film and carbon-based nano composite conductive thin film, nitrogen element content along the effect perpendicular to corrosion resistant plate or titanium alloy sheet matrix direction continuous distribution in gradient, effectively can reduce coating internal stress, promote coating binding force, to prevent in use procedure the therefore coating stripping caused, extend the useful life of coating; Also can reduce the potential difference between coating and matrix simultaneously, reduce corrosion tendency.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the cross sectional profile views of bipolar plates of the present invention.
In figure, 1. corrosion resistant plate or titanium alloy sheet matrix, 2. nitration case, 3. chromium nitride film, 4. carbon-based nano composite conductive thin film.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment, but the present invention is not limited to specific embodiment.
Embodiment 1
Described bipolar plate for fuel cell nitrogenize strengthens surface modifying method, and it is characterized in that, the method comprises following processing step:
The present embodiment is in following implementation condition and technical requirement, implements in accordance with the following steps:
(1) nitration case preparation
Corrosion resistant plate or titanium alloy sheet matrix 1 are put into ultrasonic cleaning device clean, and carry out drying in vacuum drying oven after, install with special jig and put into pulsed bias arc ion plating equipment vacuum indoor, after vacuum house vacuum is evacuated to 0.5Pa by vacuum system, vacuum chamber is heated to 400 DEG C, the nitrogen of 3000SCCM is passed into by control flow check gauge, the hydrogen of 1500SCCM, vacuum chamber internal gas pressure is made to maintain 3pa, and in bipolar plates, apply the pulsed bias of-500V, duty ratio is 90%, operating frequency is 5KHz, open heated filament, heated filament two ends electric current is set to 20A, voltage is 60V, keep this state 10mins, carry out the preparation of nitration case 2, after close nitrogen and hydrogen.
(2) ion sputtering cleaning
Close heated filament, after vacuum house vacuum is evacuated to 0.001Pa, the argon gas of 3000SCCM is passed into by control flow check gauge, pressure in vacuum chamber is made to maintain 3pa, and in bipolar plates, applying the pulsed bias of-500V, duty ratio is 90%, and operating frequency is 40KHz, keep this state 10mins, carry out argon ion sputtering cleaning.
After argon ion sputtering has cleaned, the argon gas of 20SCCM is passed into by control flow check gauge, pressure in vacuum chamber is made to maintain 1Pa, and in bipolar plates, applying the pulsed bias of-500V, duty ratio is 90%, and operating frequency is 40KHz, arranging chromium target current is 120A, open chromium target, keep this state 5min, carry out chromium ion sputter clean.
(3) cvd nitride chromium thin film and carbon-based nano composite conductive thin film
After chromium ion sputter clean completes, 750SCCM nitrogen is passed into by control flow check gauge, pass into appropriate argon gas simultaneously, pressure in vacuum chamber must be made to maintain 1Pa, and apply the pulsed bias of-500V in bipolar plates, duty ratio is 90%, operating frequency is 5KHz, chromium target arc current is 120A, keeps this state 90mins, carries out the preparation of chromium nitride film 3.
After chromium nitride film 3 has deposited, arranging carbon target arc current is 50A, chromium target/carbon target arc current ratio is 2, and in bipolar plates, apply the pulsed bias of-500V, duty ratio is 10%, operating frequency is 5KHz, open carbon target one by one, by carbon target, chromium target arc stream is adjusted to set point, reduce gradually to pass into nitrogen flow by control flow check gauge, decreasing gradient is 50SCCM/min, continue 10mins, nitrogen flow is finally made to be 0, argon flow amount is 20SCCM, pressure in vacuum chamber is made to maintain 0.1Pa, process total time is 5mins, prepare carbon-based nano composite conductive thin film 4 under these conditions.
So melt at bipolar plate surfaces and cover the film that a layer thickness is the via nitride enhancing of 0.1 micron, record bipolar plates contact resistance≤15m Ω cm2 (under 0.8MPa thrust), corrosion current icor≤1.0 × 10-6A/cm2 under simulation PEMFC corrosive environment, water contact angle >=90 °, surface microhardness Hk >=6GPa, film/base adhesion >=70N.
Embodiment 2
Described bipolar plate for fuel cell nitrogenize strengthens surface modifying method, and it is characterized in that, the method comprises following processing step:
The present embodiment is in following implementation condition and technical requirement, implements in accordance with the following steps:
(1) nitration case preparation
Corrosion resistant plate or titanium alloy sheet matrix 1 are put into ultrasonic cleaning device clean, and carry out drying in vacuum drying oven after, install with special jig and put into pulsed bias arc ion plating equipment vacuum indoor, after vacuum house vacuum is evacuated to 0.3Pa by vacuum system, vacuum chamber is heated to 250 DEG C, the nitrogen of 3000SCCM is passed into by control flow check gauge, the hydrogen of 800SCCM, vacuum chamber internal gas pressure is made to maintain 1.5pa, and in bipolar plates, apply the pulsed bias of-750V, duty ratio is 50%, operating frequency is 25KHz, open heated filament, heated filament two ends electric current is set to 60A, voltage is 100V, keep this state 80mins, carry out the preparation of nitration case 2, after close nitrogen and hydrogen.
(2) ion sputtering cleaning
Close heated filament, after vacuum house vacuum is evacuated to 0.02Pa, the argon gas of 1500SCCM is passed into by control flow check gauge, pressure in vacuum chamber is made to maintain 1.5pa, and in bipolar plates, applying the pulsed bias of-1000V, duty ratio is 50%, and operating frequency is 25KHz, keep this state 20min, carry out argon ion sputtering cleaning.
(3) cvd nitride chromium thin film and carbon-based nano composite conductive thin film
After argon ion has cleaned, 1500SCCM nitrogen is passed into by control flow check gauge, pass into appropriate argon gas simultaneously, pressure in vacuum chamber must be made to maintain 0.5Pa, and apply the pulsed bias of-250V in bipolar plates, duty ratio is 50%, operating frequency is 25KHz, chromium target arc current is 90A, keeps this state 90mins, carries out the preparation of chromium nitride film 3.
After chromium nitride film 3 has deposited, arranging carbon target arc current is 65A, chromium target/carbon target arc current ratio is 1.2, and in bipolar plates, apply the pulsed bias of-250V, duty ratio is 50%, operating frequency is 25KHz, open carbon target one by one, by carbon target, chromium target arc stream is adjusted to set point, reduce gradually to pass into nitrogen flow by control flow check gauge, decreasing gradient is 120SCCM/min, continue 7mins, nitrogen flow is finally made to be 0, argon flow amount is 500SCCM, pressure in vacuum chamber is made to maintain 0.5Pa, process total time is 60mins, prepare carbon-based nano composite conductive thin film 4 under these conditions.
So melt at bipolar plate surfaces and cover the film that a layer thickness is the via nitride enhancing of 0.15 micron, record bipolar plates contact resistance≤15m Ω cm2 (under 0.8MPa thrust), corrosion current icor≤1.0 × 10-6A/cm2 under simulation PEMFC corrosive environment, water contact angle >=90 °, surface microhardness Hk >=6GPa, film/base adhesion >=70N.
Embodiment 3
Described bipolar plate for fuel cell nitrogenize strengthens surface modifying method, and it is characterized in that, the method comprises following processing step:
The present embodiment is in following implementation condition and technical requirement, implements in accordance with the following steps:
(1) nitration case preparation
Corrosion resistant plate or titanium alloy sheet matrix 1 are put into ultrasonic cleaning device clean, and carry out drying in vacuum drying oven after, install with special jig and put into pulsed bias arc ion plating equipment vacuum indoor, after vacuum house vacuum is evacuated to 0.001Pa by vacuum system, vacuum chamber is heated to 100 DEG C, the nitrogen of 20SCCM is passed into by control flow check gauge, the hydrogen of 10SCCM, vacuum chamber internal gas pressure is made to maintain 0.1Pa, and in bipolar plates, apply the pulsed bias of-1000V, duty ratio is 10%, operating frequency is 40KHz, open heated filament, heated filament two ends electric current is set to 100A, voltage is 30V, keep this state 180mins, carry out the preparation of nitration case 2, after close nitrogen and hydrogen.
(2) ion sputtering cleaning
Close heated filament, after vacuum house vacuum is evacuated to 0.05Pa, passed into the argon gas of 500SCCM by control flow check gauge, make pressure in vacuum chamber maintain 0.5Pa, and apply the pulsed bias of-1000V in bipolar plates, duty ratio is 50%, operating frequency is 5KHz, and arranging chromium target current is 60A, opens chromium target, keep this state 2.5mins, carry out chromium ion sputter clean.
(3) cvd nitride chromium thin film and carbon-based nano composite conductive thin film
After chromium ion sputter clean completes, pass into appropriate argon gas and make pressure in vacuum chamber maintain 0.5Pa, and apply the pulsed bias of-500V in bipolar plates, duty ratio is 10%, and operating frequency is 40KHz, and chromium target arc current is 60A, keep this state 10min, carry out the preparation of chromium nitride film 3.
After chromium nitride film 3 has deposited, arranging carbon target arc current is 80A, chromium target/carbon target arc current ratio is 0.25, and in bipolar plates, apply the pulsed bias of 0V, duty ratio is 90%, operating frequency is 40KHz, open carbon target one by one, by carbon target, chromium target arc stream is adjusted to set point, reduce gradually to pass into nitrogen flow by control flow check gauge, decreasing gradient is 200SCCM/min, continue 5mins, nitrogen flow is finally made to be 0, argon flow amount is 1000SCCM, pressure in vacuum chamber is made to maintain 1Pa, process total time is 120mins, prepare carbon-based nano composite conductive thin film 4 under these conditions.
So melt at bipolar plate surfaces and cover the film that a layer thickness is the via nitride enhancing of 0.12 micron, record bipolar plates contact resistance≤15m Ω cm2 (under 0.8MPa thrust), corrosion current icor≤1.0 × 10-6A/cm2 under simulation PEMFC corrosive environment, water contact angle >=90 °, surface microhardness Hk >=6GPa, film/base adhesion >=70N.
Claims (3)
1. a nitrogenize strengthens surperficial bipolar plate for fuel cell, comprise corrosion resistant plate or titanium alloy sheet matrix (1), it is characterized in that: in described corrosion resistant plate or titanium alloy sheet matrix (1) both side surface, preparation has nitration case (2), chromium nitride film (3) and carbon-based nano composite conductive thin film (4) successively.
2. a kind of nitrogenize according to claim 1 strengthens the bipolar plate for fuel cell on surface, it is characterized in that: the thickness of described nitration case (2) is 0.1 μm ~ 20 μm, the thickness of described chromium nitride film (3) is 0.1 μm ~ 20 μm, and the thickness of described carbon-based nano composite conductive thin film (4) is 0.1 μm ~ 20 μm.
3. a kind of nitrogenize according to claim 1 strengthens the bipolar plate for fuel cell on surface, it is characterized in that: carbon in described chromium nitride film (3) and carbon-based nano composite conductive thin film (4), nitrogen element content are along perpendicular to corrosion resistant plate or titanium alloy sheet matrix (1) direction continuous distribution in gradient.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104577144A (en) * | 2015-01-27 | 2015-04-29 | 大连理工常州研究院有限公司 | Fuel-cell bipolar plate with nitrified and enhanced surface and preparation method thereof |
| CN107171003A (en) * | 2017-06-15 | 2017-09-15 | 常州翊迈新材料科技有限公司 | Conductive super anti-corrosion functional coating material |
| CN109560289A (en) * | 2018-12-26 | 2019-04-02 | 浙江锋源氢能科技有限公司 | A kind of metal double polar plates and preparation method thereof and fuel cell |
-
2015
- 2015-01-27 CN CN201520057173.7U patent/CN204361172U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104577144A (en) * | 2015-01-27 | 2015-04-29 | 大连理工常州研究院有限公司 | Fuel-cell bipolar plate with nitrified and enhanced surface and preparation method thereof |
| CN107171003A (en) * | 2017-06-15 | 2017-09-15 | 常州翊迈新材料科技有限公司 | Conductive super anti-corrosion functional coating material |
| CN107171003B (en) * | 2017-06-15 | 2020-05-05 | 常州翊迈新材料科技有限公司 | Conductive super-corrosion-resistant functional coating material |
| CN109560289A (en) * | 2018-12-26 | 2019-04-02 | 浙江锋源氢能科技有限公司 | A kind of metal double polar plates and preparation method thereof and fuel cell |
| CN109560289B (en) * | 2018-12-26 | 2023-11-28 | 浙江锋源氢能科技有限公司 | Metal bipolar plate, preparation method thereof and fuel cell |
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