CN103078121A - Preparation method of chromium-nitrogen composite pole plate material for fuel cell - Google Patents
Preparation method of chromium-nitrogen composite pole plate material for fuel cell Download PDFInfo
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- CN103078121A CN103078121A CN2012105216319A CN201210521631A CN103078121A CN 103078121 A CN103078121 A CN 103078121A CN 2012105216319 A CN2012105216319 A CN 2012105216319A CN 201210521631 A CN201210521631 A CN 201210521631A CN 103078121 A CN103078121 A CN 103078121A
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- based substrate
- iron
- plate material
- nitrogen
- chromium
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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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a chromium-nitrogen composite pole plate material for a fuel cell, and its preparation method. The preparation method comprises the following steps: melting C, Al, Zn, Ni, Cu, Pb and Fe to prepare an Fe-based substrate; polishing the Fe-based substrate, immersing in anhydrous glycol, and carrying out ultrasonic treatment; placing the surface treated Fe-based substrate in the vacuum chamber of a magnetron sputtering device, heating for making the temperature in the vacuum chamber to 300-400DEG C from room temperature, sputtering under a sputtering power of 250-300W, letting nitrogen in when the glow discharge phenomenon of a Cr target appears, and depositing to obtain the chromium-nitrogen composite Fe-based substrate pole plate material. The chromium-nitrogen composite pole plate material for the fuel cell prepared in the invention is obtained through forming a uniform and compact chromium-nitrogen cover layer on the surface of the Fe-based alloy substrate containing specific components through sputtering, and the fuel cell using the pole plate material has the advantages of good conductivity, good corrosion resistance, and service life increase.
Description
Technical field
The present invention relates to a kind of fuel cell electrode material preparation method, relate in particular to a kind of fuel cell chromium nitrogen compound polar plate material and preparation method thereof.
Background technology
Polymer electrolyte fuel cells not only has the characteristics such as energy conversion efficiency height, life-span length, environmental friendliness, and working temperature is low, it is fast to start, thereby becomes the power source that is applied to communications and transportation and builds the dispersion power station.As one of multifunctional module important in the polymer electrolyte fuel cells, bipolar plates not only has the reacting gas of separation, afflux conduction, support membrane electrode and conductive force, can also be combined into reacting gas with flow-field plate passage is provided, reacting gas is evenly distributed, and the water that generates is discharged.
Bipolar plates must be by conduction and satisfactory mechanical property, the preparation of chemically stable hyposmosis material, thereby reduces the energy loss of battery pack and increase the service life.As a kind of important multifunctional module, the performance of bipolar plates directly affects useful life and the power output of PEMFC.
Traditional graphite bi-polar plate, large because of fragility, intensity is low, is difficult to prepare the fuel cell unit lightweight, that volume is little, and also it is consuming time and expense is high to process the technique in various flow fields at its machining surface.
Stainless electrical and thermal conductivity performance is good, aboundresources, cost is low, intensity is high, is the ideal material of making fuel battery double plates.But bipolar plate material will face the etching problems such as dissolving or passivation under acid operational environment, therefore be necessary to form one deck conduction and corrosion resistant cover layer at stainless steel surfaces.
Adopt electro-plating method in stainless steel surfaces chromium plating on the traditional sense, there are the defectives such as more loose, perforation in coating, and electric conductivity and decay resistance are not improved significantly.Therefore, in the urgent need to the metal double polar plates of low cost, high surface conductivity and good corrosion resistance is provided by a kind of new surface modifying method.
Summary of the invention
The invention provides a kind of fuel cell with chromium nitrogen compound polar plate material preparation method, when the pole plate composite material that uses the method to prepare is used for membrane fuel cell, have good conductivity and corrosion resistance, and cost is relatively low.
To achieve these goals, a kind of fuel cell provided by the invention comprises the steps: with chromium nitrogen compound polar plate material preparation method
Step 1, preparation iron-based substrate
By following mass percent founding ferrous alloy: C=0.10-0.35%, Al=0.15-0.35%, Zn=0.45-0.70%, Ni=0.15-0.25%, Cu=0.05-0.25%, Pb=0.05-0.15%, surplus is Fe, and the alloy after the founding is made the iron-based substrate;
Step 2 is processed the iron-based substrate
Immerse without in the water glycol after the above-mentioned iron-based substrate polishing, and be ultrasonic processing 1-2h under the 25-40kHz in frequency, then air-dry under the room temperature, obtain surface-treated iron-based substrate;
Step 3, vacuum sputtering obtain the compound iron-based substrate of chromium nitrogen plate material
Surface-treated iron-based substrate is placed in the vacuum chamber of magnetron sputtering apparatus, and pressure keeps 3 * 10
-4Pa-5 * 10
-4Till the Pa;
Take gas flow as 10sccm-12sccm helium is passed into, and make the vacuum indoor temperature rise to 300-400 ℃ from room temperature;
The sputtering power of magnetron sputtering apparatus is transferred to 250-300W, when producing the glow discharge phenomenon on the Cr target, pass into nitrogen, obtain the compound iron-based substrate of chromium nitrogen plate material.
Wherein, the substrate thickness of iron-based described in the step 1 is preferably 0.5-2mm.
Wherein, in the step 3, the gas flow ratio of nitrogen and helium is preferably 1
:(10-15).
Wherein, in the step 3, pass into nitrogen after, (sputter) deposition 2-3h.
The present invention also provides a kind of fuel cell of said method preparation chromium nitrogen compound polar plate material.
The fuel cell of the present invention's preparation chromium nitrogen compound polar plate material, by on the ferrous alloy substrate of special component, adopt the mode of sputter, form in its surface the chromium nitrogen cover layer of even compact, this plate material is being used for fuel cell, have good conductivity and corrosion resistance, increased the useful life of fuel cell.
Embodiment
Embodiment one
Preparation iron-based substrate
By following mass percent founding ferrous alloy: C=0.10%, Al=0.15%, Zn=0.45%, Ni=0.15%, Cu=0.05%, Pb=0.05% makes the iron-based substrate that thickness is 0.5mm with the alloy after the founding.
Process the iron-based substrate
Immerse without in the water glycol after the above-mentioned iron-based substrate polishing, and be ultrasonic processing 2h under the 25kHz in frequency, then air-dry under the room temperature, obtain surface-treated iron-based substrate.
Vacuum sputtering obtains the compound iron-based substrate of chromium nitrogen plate material
Surface-treated iron-based substrate is placed in the vacuum chamber of magnetron sputtering apparatus, and the vacuum chamber of magnetron sputtering apparatus is vacuumized, to vacuum indoor pressure be 3 * 10
-4Till the Pa; Take gas flow as 10sccm helium is passed into pressure and be 3 * 10
-4In the vacuum chamber of Pa, then make the vacuum indoor temperature rise to 300 ℃ from room temperature by regulating heating current; The sputtering power of magnetron sputtering apparatus is transferred to 250W, pass into nitrogen when producing the glow discharge phenomenon on the Cr target, the gas flow ratio of nitrogen and helium is 1
:10, deposition 2h namely obtains the compound iron-based substrate of chromium nitrogen plate material.
Embodiment two
Preparation iron-based substrate
By following mass percent founding ferrous alloy: C=0.35%, Al=0.35%, Zn=0.70%, Ni=0.25%, Cu=0.25%, Pb=0.15%, surplus is Fe, and the alloy after the founding is made the iron-based substrate that thickness is 2mm.
Process the iron-based substrate
Immerse without in the water glycol after the above-mentioned iron-based substrate polishing, and be ultrasonic processing 1h under the 40kHz in frequency, then air-dry under the room temperature, obtain surface-treated iron-based substrate.
Vacuum sputtering obtains the compound iron-based substrate of chromium nitrogen plate material
Surface-treated iron-based substrate is placed in the vacuum chamber of magnetron sputtering apparatus, and the vacuum chamber of magnetron sputtering apparatus is vacuumized, to vacuum indoor pressure be 5 * 10
-4Till the Pa; Take gas flow as 12sccm helium is passed into pressure and be 5 * 10
-4In the vacuum chamber of Pa, then make the vacuum indoor temperature rise to 400 ℃ from room temperature by regulating heating current; The sputtering power of magnetron sputtering apparatus is transferred to 300W, pass into nitrogen when producing the glow discharge phenomenon on the Cr target, the gas flow ratio of nitrogen and helium is 1
:15, deposition 3h namely obtains the compound iron-based substrate of chromium nitrogen plate material.
Comparative example
Adopt reactive magnetron sputtering method preparation at the thick stainless steel substrates of 1mm, sputtering chamber is vacuumized until less than 0.5MPa, adopt crome metal as sputtering target by a turbomolecular pump and a mechanical pump.Reacting gas is nitrogen, and the gas pressure intensity in the deposit film process remains on 0.7 Pa.The power of shielding power supply is 40 watts, and the distance that keeps depositing between sheet and the target is 5 centimetres.Elder generation sputter half an hour is to remove the pollution on the target, then at stainless steel substrates and deposition on glass film.Substrate temperature is 150 ℃ of room temperatures, and sedimentation time is 2 hours.
With above-described embodiment one, two and the comparative example products therefrom, make the fuel cell of same size.Be to carry out electric performance test under 25 ℃ at probe temperature, after tested this embodiment one with two material compare with the product of comparative example, electric conductivity has improved 30-45%, improves useful life more than 1.5 times.
More than specific embodiments of the invention are described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, not breaking away from impartial conversion and the modification of doing under the spirit and scope of the present invention, all should contain within the scope of the invention.
Claims (5)
1. a fuel cell is characterized in that with chromium nitrogen compound polar plate material preparation method, comprises the steps:
Step 1, preparation iron-based substrate
By following mass percent founding ferrous alloy: C=0.10-0.35%, Al=0.15-0.35%, Zn=0.45-0.70%, Ni=0.15-0.25%, Cu=0.05-0.25%, Pb=0.05-0.15%, surplus is Fe, and the alloy after the founding is made the iron-based substrate;
Step 2 is processed the iron-based substrate
Immerse without in the water glycol after the above-mentioned iron-based substrate polishing, and be ultrasonic processing 1-2h under the 25-40kHz in frequency, then air-dry under the room temperature, obtain surface-treated iron-based substrate;
Step 3, vacuum sputtering obtain the compound iron-based substrate of chromium nitrogen plate material
Surface-treated iron-based substrate is placed in the vacuum chamber of magnetron sputtering apparatus, and pressure keeps 3 * 10
-4Pa-5 * 10
-4Till the Pa;
Take gas flow as 10sccm-12sccm helium is passed into, and make the vacuum indoor temperature rise to 300-400 ℃ from room temperature;
The sputtering power of magnetron sputtering apparatus is transferred to 250-300W, when producing the glow discharge phenomenon on the Cr target, pass into nitrogen, obtain the compound iron-based substrate of chromium nitrogen plate material.
2. method according to claim 1 is characterized in that, the substrate thickness of iron-based described in the step 1 is 0.5-2mm.
3. method according to claim 1 is characterized in that, in the step 3, the gas flow ratio of nitrogen and helium is 1
:(10-15).
4. according to claim 1 or 3 described methods, it is characterized in that, in the step 3, pass into nitrogen after, deposition 2-3h.
One kind as claimed in claim 1 the fuel cell of method preparation with chromium nitrogen compound polar plate material.
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| CN2012105216319A CN103078121A (en) | 2012-12-07 | 2012-12-07 | Preparation method of chromium-nitrogen composite pole plate material for fuel cell |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1957102A (en) * | 2004-05-19 | 2007-05-02 | 山特维克知识产权股份有限公司 | Heat-resistant steel |
| CN101092688A (en) * | 2007-05-28 | 2007-12-26 | 大连理工大学 | Ion plating modified method for bipolar plate of stainless steel for fuel cell in type of proton exchange membrane |
| CN101950807A (en) * | 2009-07-10 | 2011-01-19 | 通用汽车环球科技运作公司 | Low cost manganese stabilisation austenitic stainless steel alloy, comprise the bipolar plates of this alloy and comprise the fuel cell system of this bipolar plates |
| CN102376960A (en) * | 2010-08-26 | 2012-03-14 | 北京有色金属研究总院 | Surface-modified metal dual-pole plate of proton exchange membrane fuel cell and surface modifying method of surface-modified metal dual-pole plate |
| CN102628162A (en) * | 2012-04-19 | 2012-08-08 | 哈尔滨工业大学 | Method for preparing plasma chromium-plated nitriding iron-based fuel battery bipolar plate material |
-
2012
- 2012-12-07 CN CN2012105216319A patent/CN103078121A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1957102A (en) * | 2004-05-19 | 2007-05-02 | 山特维克知识产权股份有限公司 | Heat-resistant steel |
| CN101092688A (en) * | 2007-05-28 | 2007-12-26 | 大连理工大学 | Ion plating modified method for bipolar plate of stainless steel for fuel cell in type of proton exchange membrane |
| CN101950807A (en) * | 2009-07-10 | 2011-01-19 | 通用汽车环球科技运作公司 | Low cost manganese stabilisation austenitic stainless steel alloy, comprise the bipolar plates of this alloy and comprise the fuel cell system of this bipolar plates |
| CN102376960A (en) * | 2010-08-26 | 2012-03-14 | 北京有色金属研究总院 | Surface-modified metal dual-pole plate of proton exchange membrane fuel cell and surface modifying method of surface-modified metal dual-pole plate |
| CN102628162A (en) * | 2012-04-19 | 2012-08-08 | 哈尔滨工业大学 | Method for preparing plasma chromium-plated nitriding iron-based fuel battery bipolar plate material |
Non-Patent Citations (1)
| Title |
|---|
| （苏）包尔纳茨基: "《炼钢过程的物理化学基础》", 31 May 1981, 冶金工业出版社 * |
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