CN101609898B - Preparation method for metal base fuel battery bipolar plate with hydrophobicity - Google Patents
Preparation method for metal base fuel battery bipolar plate with hydrophobicity Download PDFInfo
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- CN101609898B CN101609898B CN2009100633215A CN200910063321A CN101609898B CN 101609898 B CN101609898 B CN 101609898B CN 2009100633215 A CN2009100633215 A CN 2009100633215A CN 200910063321 A CN200910063321 A CN 200910063321A CN 101609898 B CN101609898 B CN 101609898B
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to a preparation method for a metal base fuel battery bipolar plate with hydrophobicity. The preparation method for the metal base fuel battery bipolar plate with hydrophobicity is characterized in that the method comprises the following steps: (1) surface polishing treatment is carried out on a metal plate with flow field as to obtain the polished metal plate with flow field; (2) a layer of compact thin film is prepared on the surface of the polished metal plate with flow field so as to obtain the metal plate with the compact thin film; (3) a layer of thin film with nanometer micro-convex is deposited on the surface of the metal plate with the compact thin film to obtain a metal plate with the compact thin film and nanometer micro-convex thin film; (4) electrical conductivity regulation is carried out on the surface the metal plate with the compact thin film and nanometer micro-convex thin film to prepare a layer of film with good electrical conductivity inheriting micro-convex structure, thus obtaining the metal base fuel battery bipolar plate with hydrophobicity. The metal base fuel battery bipolar plate prepared by the method not only has excellent corrosion resistance, but also has good electrical conductivity and hydrophobicity.
Description
Technical field
The present invention relates to a kind of preparation method with metal base fuel battery bipolar plate of hydrophobicity.
Background technology
Proton membrane fuel battery has characteristics such as cleaning, efficient, removable, operating condition gentleness, has important use in fields such as communications and transportation, Aero-Space and telecommunications and is worth.Bipolar plates is the plate material that monocell is together in series, and need satisfy many-sided performance requirement.Be good electrical conductivity, superior corrosion resistance (comprising sour corrosion, oxidation cargo sweat, electrode potential corrosion), good air-tightness, enough mechanical strengths, lower density and cheap relatively cost.
The bipolar plate material that uses at present is graphite, and this is mainly based on graphite good electrical conductivity and corrosion resistance, non-oxidizability etc.But owing to relatively poor, the runner machine work difficulty of graphite mechanical performance, need to solve problem such as medium osmosis with complicated technological measure, therefore the processing price of graphite bi-polar plate is very high, account for the 40-60% of fuel cell cost, become problem anxious to be solved in the fuel cell research and development.
The main starting point of utilizing metal material to prepare bipolar plates is: metal material has good plasticity, therefore directly punch forming of flow field also is expected to cut down finished cost significantly, and metal can be rolled into the sheet material of 0.1-0.2mm simultaneously, be expected to obtain high-specific-power, to greatest extent compression volume.The metal material electrical and thermal conductivity is good in addition, and air-tightness is good, the mechanical strength height.But the weakness that metal material is the most fatal is a corrosion-resistant, and the corrosion resistance that how to improve metal material is at first to need the problem that solves.
Different metal materials, the method difference of solution corrosion resistance.Studying maximum is ferrous alloy, and this mainly is because iron is cheap.But the surface contacted resistance of iron is big, and iron ion causes battery performance and life-span to descend to the pollution of battery liquid simultaneously.Thereby the ferrous metals plate carried out the key that surface treatment is its extensive use.It is unsatisfactory that multidigit researcher studies the result of fe-based surface depositing TiN, finds that the TiN coating easily comes off from matrix surface, and the life-span in fuel cell is very short, and it is bad that this mainly is that TiN combines with iron-based, exists due to the pin hole in the while TiN film.U.S. Oak Ridge national laboratories research 1100 ℃ of nitridings of (Ni-50Cr) alloy, form CrN and Cr on the surface
2N gradient film has been eliminated the pin hole influence, and corrosion resistance significantly improves, and operation did not produce and pollutes in 1000 hours in the fuel cell.But, do not possess commercial value because the base material price is expensive.Their stainless steel of using high Ni, Cr content instead carries out nitriding and handles subsequently, though stainless steel surfaces has also formed Cr
2N, but film is discontinuous, is difficult to satisfy the corrosion resistant requirement of fuel cell.Taiwan Yuan Ze university utilize PVD at the Al surface deposition multilayer films such as TiN, TiCN, contact resistance significantly reduces, corrosion resistance also effectively improves.But the battery operation experiment shows, only can move 200 hours.Britain Hodgson in the titanium surface preparation FC5 coating, contact resistance is near 10m Ω .cm
2, the battery operation life-span reaches 8000 hours.But the FC5 coating technology is very secret, can look into without any data at present.All also do not obtain commercial the application so far in the whole bag of tricks of being attempted.
Present most researcher also only is concerned about the compactness and the conductivity of prepared film, and few people notice that prepared film should have hydrophobicity.In our previous work, prepared all films preferably of compactness and conductivity, but found that in the monocell running water blockoff phenomenon appears in battery often.This mainly is because prepared film has certain hydrophily.Because the flow field is narrow on the bipolar plates, after the gas behind the humidification entered the flow field, the easy surplus of aqueous vapor was on the wall of flow field, be difficult for being blown away by gas, the time one is long, and the part flow field is seriously stopped up, air-flow is not smooth, and battery performance reduces, even might cause the too high and phenomenon that burnt out of battery temperature.Therefore prepared film also should have the characteristics of hydrophobicity except that having compactness height, good conductivity.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method with metal base fuel battery bipolar plate of hydrophobicity, the metal base fuel battery bipolar plate of this method preparation not only has excellent corrosion resistance, and has good electrical conductivity and hydrophobicity.
For achieving the above object, the technical solution adopted in the present invention is: have the preparation method of the metal base fuel battery bipolar plate of hydrophobicity, it is characterized in that it comprises the steps:
1) metallic plate with flow field (or claiming metal flow field plate) is carried out surface finish and handle, obtain the metallic plate after the polishing with flow field;
2) metal sheet surface with flow field after polishing prepares the film of one deck densification, obtains having the metallic plate of fine and close film;
3) deposit the film that one deck has the nanometer dimpling again at metal sheet surface, obtain having the metallic plate of the film of fine and close film and nanometer dimpling with fine and close film;
4) metal sheet surface to film with fine and close film and nanometer dimpling carries out the conductivity adjustment, and preparation one deck is inherited the good film of conductivity of little lug structure; Obtain having the metal base fuel battery bipolar plate of hydrophobicity.
The described metallic plate of step 1) is 304 corrosion resistant plates.
Step 2) concrete steps are: the metallic plate with flow field after the polishing is put into the magnetron sputtering stove carry out plated film, select the Cr target, temperature is 180～220 ℃, and vacuum degree is (2.0～2.3) X10
-1Pa, electric current are 16～18A, and voltage is 300～500V, Ar/N
2The volumetric flow of gas ratio is 2: 1～3: 1, and the plated film time is 1～2 hour, at the CrN film of the metal sheet surface formation one deck densification with flow field, obtains having the metallic plate of fine and close film.
The concrete steps of step 3) are: with step 2) metallic plate with fine and close film that obtains puts into the magnetron sputtering stove and carries out plated film, selects Cr
3Ni
2Target, temperature are 180～220 ℃, and vacuum degree is (2.0～2.3) X10
-1Pa, electric current are 16～18A, and voltage is 300～500V, stop logical nitrogen, only logical Ar gas, and the plated film time is 5～8 minutes, deposition one deck has the Cr of nanometer dimpling on the film with densification
3Ni
2Film obtains having the metallic plate of the film of fine and close film and nanometer dimpling.The acquisition of nanometer dimpling mainly utilizes film growth techniques and Material Selection; Select two kinds of diverse materials of crystal structure (as CrN and Cr
3Ni
2), in the film deposition process, though the multiple spot nucleation is difficult for forming dimpling at last along interface growth.
The concrete steps of step 4) are: the metallic plate of the film with fine and close film and nanometer dimpling that step 3) is obtained is put into the magnetron sputtering stove and is carried out plated film, selects the Cr target, and temperature is 180～220 ℃, and vacuum degree is (2.0～2.3) X10
-1Pa, electric current are 16～18A, and voltage is 300～500V, Ar/N
2The volumetric flow of gas ratio is 10: 1～5: 1, and the plated film time is 10～15 minutes, forms the good Cr of conductivity that one deck is inherited little lug structure on the film with nanometer dimpling
2The N film, the metal base fuel battery bipolar plate that obtains having hydrophobicity.The crystal structure type difference of the film of nanometer dimpling and dense film is bigger, and lattice constant differs greatly; The crystal structure of film of inheriting the crystal structure of the good film of the conductivity of little lug structure and nanometer dimpling is similar, and forms coherence or semicoherent interface easily.
Though the structure more complicated of film outwardly, actual film forming procedure is fairly simple; Utilize magnetron sputtering technique, select two targets, can obtain by changing nitrogen flow.
Other of metal base fuel battery bipolar plate metallic plate of flow field (as have) is same as the prior art.
The invention has the beneficial effects as follows:
1, the present invention adopts the metal sheet surface with flow field after polishing to utilize magnetron sputtering technique sputter trilamellar membrane successively, is respectively the good film of conductivity of fine and close film, the film with nanometer dimpling, the little lug structure of succession.Film with nanometer dimpling is similar to the micro-structural on lotus surface, has hydrophobicity; The employing trilamellar membrane combines, and makes the bipolar plates after the processing not only have excellent corrosion resistance, and has good electrical conductivity and hydrophobicity.
2, the film that 1. prepares one deck densification: with 304 stainless steels is matrix, and at first the CrN film of deposition compact on 304 stainless steels is not corroded to protect 304 stainless steels.Because 304 stainless steels are face-centred cubic structures, lattice constant a=3.591, CrN also are face-centred cubic structures, lattice constant a=4.140.Therefore CrN easily grows into dense film at 304 stainless steel surfaces.2. deposit the film that one deck has the nanometer dimpling: the dimpling layer is selected Cr
3Ni
2, Cr
3Ni
2Be hexagonal simple structure, lattice constant a=8.82, c=4.58.Because Cr
3Ni
2Excessive with CrN crystal structure difference, be difficult for growing into dense film, form micro-convex structure.3. prepare one deck and inherit the good film of conductivity of little lug structure: in order to improve Cr
3Ni
2Conductivity, at Cr
3Ni
2The long one deck Cr of surface regeneration
2N.Cr
2N is simple six sides, lattice constant a=4.78, c=4.44.Cr
2N and Cr
3Ni
2Between crystal structure identical, Cr
3Ni
2The a value approximately be Cr
22 times of a value of N have certain coherence relation.Cr
2N inherits Cr easily
3Ni
2The micro-convex structure of layer.Therefore prepared film has corrosion resistance, conductivity and hydrophobicity simultaneously.
3, utilize magnetron sputtering technique, the composite membrane that acquisition simultaneously has multiple performance, technology is simple, can batch process.
Description of drawings
Fig. 1 is preparation technology's flow chart of the present invention;
Fig. 2 is the micro-analysis figure of the embodiment of the invention 1;
Fig. 3 is the XRD material phase analysis figure of the embodiment of the invention 1.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
As shown in Figure 1, have the preparation method of the metal base fuel battery bipolar plate of hydrophobicity, it comprises the steps:
1) gets 304 corrosion resistant plates and carry out surface finish and handle, obtain the metallic plate after the polishing with flow field with flow field.
2) the fine and close film of preparation: the metallic plate with flow field after the polishing is put into the magnetron sputtering stove carry out plated film, select the Cr target, temperature is 180 ℃, and vacuum degree is 2.0 * 10
-1Pa, electric current are 18A, and voltage is 300V, Ar/N
2The volumetric flow of gas ratio is 2: 1, and the plated film time is 1.5 hours, at the CrN film of the metal sheet surface formation one deck densification with flow field, obtains having the metallic plate of fine and close film.
3) preparation has the film of nanometer dimpling: with step 2) metallic plate with fine and close film that obtains puts into the magnetron sputtering stove and carries out plated film, selects Cr
3Ni
2Target, temperature are 180 ℃, and vacuum degree is 2.0 * 10
-1Pa, electric current are 18A, and voltage is 300V, stop logical nitrogen, only logical Ar gas, and the plated film time is 5 minutes, deposition one deck has the Cr of nanometer dimpling on the film with densification
3Ni
2Film obtains having the metallic plate of the film of fine and close film and nanometer dimpling.
4) preparation one deck is inherited the good film of conductivity of little lug structure: the metallic plate of the film with fine and close film and nanometer dimpling that step 3) is obtained is put into the magnetron sputtering stove and is carried out plated film, selects the Cr target, and temperature is 180 ℃, and vacuum degree is 2.0 * 10
-1Pa, electric current are 18A, and voltage is 300V, Ar/N
2The gas flow volume ratio is 10: 1, and the plated film time is 10 minutes, forms the good Cr of conductivity that one deck is inherited little lug structure on the film with nanometer dimpling
2The N film, the metal base fuel battery bipolar plate (product) that obtains having hydrophobicity.
The metal base fuel battery bipolar plate sample with hydrophobicity (being product) that present embodiment is obtained carries out performance test, contact resistance 12m Ω .cm
2, corrosion electric current density 7 μ A.cm
-2, 101 ° of angle of wettings (angle of wetting is the hydrophobicity film greater than 90 degree) illustrate that the bipolar plates after handling not only has excellent corrosion resistance, and have good electrical conductivity and hydrophobicity.The sample surfaces microstructure is found uniform nanoscale micro-convex structure as shown in Figure 2.Film is carried out XRD material phase analysis (Fig. 3), find to have Cr
2N, Cr
3Ni
2, CrN, SS304, show the membrane structure that reaches designed.
Embodiment 2:
As shown in Figure 1, have the preparation method of the metal base fuel battery bipolar plate of hydrophobicity, it comprises the steps:
1) gets 304 corrosion resistant plates and carry out surface finish and handle, obtain the metallic plate after the polishing with flow field with flow field.
2) the fine and close film of preparation: the metallic plate with flow field after the polishing is put into the magnetron sputtering stove carry out plated film, select the Cr target, temperature is 220 ℃, and vacuum degree is 2.3 * 10
-1Pa, electric current are 16A, and voltage is 500V, Ar/N
2The volumetric flow of gas ratio is 3: 1, and the plated film time is 1 hour, at the CrN film of the metal sheet surface formation one deck densification with flow field, obtains having the metallic plate of fine and close film.
3) preparation has the film of nanometer dimpling: with step 2) metallic plate with fine and close film that obtains puts into the magnetron sputtering stove and carries out plated film, selects Cr
3Ni
2Target, temperature are 220 ℃, and vacuum degree is 2.3 * 10
-1Pa, electric current are 16A, and voltage is 500V, stop logical nitrogen, only logical Ar gas, and the plated film time is 7 minutes, deposition one deck has the Cr of nanometer dimpling on the film with densification
3Ni
2Film obtains having the metallic plate of the film of fine and close film and nanometer dimpling.
4) preparation one deck is inherited the good film of conductivity of little lug structure: the metallic plate of the film with fine and close film and nanometer dimpling that step 3) is obtained is put into the magnetron sputtering stove and is carried out plated film, selects the Cr target, and temperature is 200 ℃, and vacuum degree is 2.3 * 10
-1Pa, electric current are 16A, and voltage is 500V, Ar/N
2The gas flow volume ratio is 7: 1, and the plated film time is 12 minutes, forms the good Cr of conductivity that one deck is inherited little lug structure on the film with nanometer dimpling
2The N film, the metal base fuel battery bipolar plate (product) that obtains having hydrophobicity.
The metal base fuel battery bipolar plate sample with hydrophobicity (being product) that present embodiment is obtained carries out performance test, contact resistance 12m Ω .cm
2, corrosion electric current density 8.5 μ A.cm
-2, 101 ° of angle of wettings.
Embodiment 3:
As shown in Figure 1, have the preparation method of the metal base fuel battery bipolar plate of hydrophobicity, it comprises the steps:
1) gets 304 corrosion resistant plates and carry out surface finish and handle, obtain the metallic plate after the polishing with flow field with flow field.
2) the fine and close film of preparation: the metallic plate with flow field after the polishing is put into the magnetron sputtering stove carry out plated film, select the Cr target, temperature is 220 ℃, and vacuum degree is 2.1 * 10
-1Pa, electric current are 17A, and voltage is 400V, Ar/N
2The volumetric flow of gas ratio is 2: 1, and the plated film time is 2 hours, at the CrN film of the metal sheet surface formation one deck densification with flow field, obtains having the metallic plate of fine and close film.
3) preparation has the film of nanometer dimpling: with step 2) metallic plate with fine and close film that obtains puts into the magnetron sputtering stove and carries out plated film, selects Cr
3Ni
2Target, temperature are 220 ℃, and vacuum degree is 2.1 * 10
-1Pa, electric current are 17A, and voltage is 400V, stop logical nitrogen, only logical Ar gas, and the plated film time is 6 minutes, deposition one deck has the Cr of nanometer dimpling on the film with densification
3Ni
2Film obtains having the metallic plate of the film of fine and close film and nanometer dimpling.
4) preparation one deck is inherited the good film of conductivity of little lug structure: the metallic plate of the film with fine and close film and nanometer dimpling that step 3) is obtained is put into the magnetron sputtering stove and is carried out plated film, selects the Cr target, and temperature is 220 ℃, and vacuum degree is 2.1 * 10
-1Pa, electric current are 17A, and voltage is 400V, Ar/N
2The volumetric flow of gas ratio is 5: 1, and the plated film time is 15 minutes, forms the good Cr of conductivity that one deck is inherited little lug structure on the film with nanometer dimpling
2The N film, the metal base fuel battery bipolar plate (product) that obtains having hydrophobicity.
The metal base fuel battery bipolar plate sample with hydrophobicity (being product) that present embodiment is obtained carries out performance test, contact resistance 12.5m Ω .cm
2, corrosion electric current density 6.5 μ A.cm
-2, 102 ° of angle of wettings.
The bound value of technological parameter of the present invention, with and interval value can both realize the present invention, do not enumerate embodiment one by one at this.
Claims (2)
1. the preparation method who has the metal base fuel battery bipolar plate of hydrophobicity is characterized in that it comprises the steps:
1) metallic plate with flow field is carried out surface finish and handle, obtain the metallic plate after the polishing with flow field;
2) prepare the film of one deck densification at the metal sheet surface after the polishing: the metallic plate with flow field after the polishing is put into the magnetron sputtering stove carry out plated film with flow field, select the Cr target, temperature is 180～220 ℃, and vacuum degree is (2.0～2.3) * 10
-1Pa, electric current are 16～18A, and voltage is 300～500V, Ar/N
2The volumetric flow of gas ratio is 2: 1～3: 1, and the plated film time is 1～2 hour, at the CrN film of the metal sheet surface formation one deck densification with flow field, obtains having the metallic plate of fine and close film;
3) depositing the film that one deck has the nanometer dimpling again at metal sheet surface: with step 2 with fine and close film) metallic plate with fine and close film that obtains puts into the magnetron sputtering stove and carries out plated film, selects Cr
3Ni
2Target, temperature are 180～220 ℃, and vacuum degree is (2.0～2.3) * 10
-1Pa, electric current are 16～18A, and voltage is 300～500V, stop logical nitrogen, only logical Ar gas, and the plated film time is 5～8 minutes, deposition one deck has the Cr of nanometer dimpling on the film with densification
3Ni
2Film obtains having the metallic plate of the film of fine and close film and nanometer dimpling;
4) metal sheet surface to film with fine and close film and nanometer dimpling carries out the conductivity adjustment, preparation one deck is inherited the good film of conductivity of micro-convex structure: the metallic plate of the film with fine and close film and nanometer dimpling that step 3) is obtained is put into the magnetron sputtering stove and is carried out plated film, select the Cr target, temperature is 180～220 ℃, and vacuum degree is (2.0～2.3) * 10
-1Pa, electric current are 16～18A, and voltage is 300～500V, Ar/N
2The volumetric flow of gas ratio is 10: 1～5: 1, and the plated film time is 10～15 minutes, forms the good Cr of conductivity that one deck is inherited micro-convex structure on the film with nanometer dimpling
2The N film, the metal base fuel battery bipolar plate that obtains having hydrophobicity.
2. the preparation method with metal base fuel battery bipolar plate of hydrophobicity according to claim 1 is characterized in that: the described metallic plate of step 1) is 304 corrosion resistant plates.
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|---|---|---|---|
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109301259B (en) * | 2018-09-30 | 2020-12-01 | 重庆大学 | Proton exchange membrane fuel cell bipolar plate and preparation method thereof |
| CN110729497B (en) * | 2019-09-20 | 2022-06-21 | 江苏大学 | Hydrophobic fuel cell bipolar plate and method |
| CN110752386B (en) * | 2019-09-20 | 2022-08-23 | 江苏大学 | Fuel cell bipolar plate and method |
| CN112359328A (en) * | 2020-10-29 | 2021-02-12 | 佛山市清极能源科技有限公司 | Surface treatment method for bipolar plate of fuel cell |
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| CN1713411A (en) * | 2004-06-23 | 2005-12-28 | 三星Sdi株式会社 | Separator for fuel cell, method of preparing same, and fuel cell comprising same |
| US20070141439A1 (en) * | 2005-12-20 | 2007-06-21 | Gayatri Vyas | Surface engineering of bipolar plate materials for better water management |
| CN101257117A (en) * | 2007-05-28 | 2008-09-03 | 大连理工大学 | Double polar plates for fuel battery and method for making surface azote chromium thin film |
| CN101258624A (en) * | 2005-07-12 | 2008-09-03 | 通用汽车环球科技运作公司 | Coated steel bipolar plates |
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2009
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1713411A (en) * | 2004-06-23 | 2005-12-28 | 三星Sdi株式会社 | Separator for fuel cell, method of preparing same, and fuel cell comprising same |
| CN101258624A (en) * | 2005-07-12 | 2008-09-03 | 通用汽车环球科技运作公司 | Coated steel bipolar plates |
| US20070141439A1 (en) * | 2005-12-20 | 2007-06-21 | Gayatri Vyas | Surface engineering of bipolar plate materials for better water management |
| CN101257117A (en) * | 2007-05-28 | 2008-09-03 | 大连理工大学 | Double polar plates for fuel battery and method for making surface azote chromium thin film |
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| 付宇等.质子交换膜燃料电池双极板用金属改性的研究.《西安交通大学学报》.2008,第42卷(第3期),364-367. * |
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