CN102468490B - Surface chromium carbide/graphite composite coating for vanadium redox flow battery stainless steel bipolar plate - Google Patents
Surface chromium carbide/graphite composite coating for vanadium redox flow battery stainless steel bipolar plate Download PDFInfo
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- CN102468490B CN102468490B CN201010551258.2A CN201010551258A CN102468490B CN 102468490 B CN102468490 B CN 102468490B CN 201010551258 A CN201010551258 A CN 201010551258A CN 102468490 B CN102468490 B CN 102468490B
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- stainless steel
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- composite coating
- chromium
- chromium carbide
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- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 54
- 239000010935 stainless steel Substances 0.000 title claims abstract description 53
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 39
- 239000010439 graphite Substances 0.000 title claims abstract description 39
- 239000011248 coating agent Substances 0.000 title claims abstract description 37
- 238000000576 coating method Methods 0.000 title claims abstract description 37
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910003470 tongbaite Inorganic materials 0.000 title claims abstract description 35
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 22
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 26
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 24
- 239000011651 chromium Substances 0.000 claims abstract description 24
- 238000000151 deposition Methods 0.000 claims abstract description 14
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 5
- 230000008021 deposition Effects 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 4
- 239000001257 hydrogen Substances 0.000 claims abstract 4
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract 4
- 230000001360 synchronised effect Effects 0.000 claims abstract 2
- 238000002360 preparation method Methods 0.000 claims description 7
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 238000009792 diffusion process Methods 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 26
- 238000005240 physical vapour deposition Methods 0.000 abstract description 7
- 239000000843 powder Substances 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000001947 vapour-phase growth Methods 0.000 abstract 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 238000009713 electroplating Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 14
- 230000007797 corrosion Effects 0.000 description 12
- 239000000126 substance Substances 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 10
- 229910000619 316 stainless steel Inorganic materials 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 9
- 239000007792 gaseous phase Substances 0.000 description 9
- 238000002791 soaking Methods 0.000 description 9
- 239000003792 electrolyte Substances 0.000 description 7
- 238000007747 plating Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005254 chromizing Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910001456 vanadium ion Inorganic materials 0.000 description 1
Classifications
-
- 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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- Fuel Cell (AREA)
Abstract
The invention provides a surface anti-corrosion and conductive chromium carbide/graphite composite coating for a vanadium redox flow battery stainless steel bipolar plate, which is prepared by adopting a chemical vapor deposition method, wherein a vapour phase deposition atmosphere is an acetylene-hydrogen mixed gas or methane-hydrogen mixed gas, and the reaction temperature is 800-9500 DEG C. Before the composite coating is subjected to vapour phase deposition, a chromium-rich layer needs to be prepared on the surface of stainless steel. The chromium-rich layer is prepared by adopting methods such as electroplating, physical vapor deposition, solid powder seepage and the like. Meanwhile, a Ni catalysis layer deposited on the surface of the chromium-rich layer is beneficial to deposition of a graphite layer and can inhibit oxidization of the stainless steel. The stainless steel bipolar plate surface anti-corrosion and conductive chromium carbide/graphite composite coating is prepared by using excellent anti-corrosion property and better conduction property of a thermally-growing no-defect chromium carbide layer and better anti-corrosion property and low contact resistance of the graphite layer through synchronous deposition of the chemical vapor deposition method. The composite coating can provide excellent anti-corrosion property and conduction property for the vanadium redox flow battery stainless steel bipolar plate.
Description
Technical field
The present invention relates to all-vanadium liquid flow energy storage battery technology, a kind of surperficial chromium carbide/graphite composite of all-vanadium liquid flow energy storage battery bipolar plate of stainless steel is provided especially, make bipolar plate of stainless steel in battery electrolyte, there is good decay resistance, and there is low contact resistance.
Background technology
All-vanadium flow battery be using the vanadium ion solution with different valence state respectively as the active material of anodal and negative pole, be stored in respectively in electrolyte storage tank separately.Battery is being carried out to charge and discharge when experiment, electrolyte is by the effect of pump, by outside receiver respectively circular flow through cathode chamber and the anode chamber of battery, and there is oxidation and reduction reaction at electrode surface, realize discharging and recharging battery.Compare with other class chemical power source, all-vanadium flow battery scale is large, the life-span is long, cost is low and the feature such as efficiency, has very strong industrialization prospect.
The critical material of vanadium cell comprises battery diaphragm, electrolyte, electrode and bipolar plates.The Main Function of bipolar plates is to collect electric current and the separation both positive and negative polarity electrolyte that electrochemical reaction produces.Desirable bipolar plates should possess several characteristics: the first, and very high conductivity, conductivity is higher, and the performance of vanadium cell can be better; The second, very corrosion-resistant, in whole charge and discharge process, can not react with the strong acid electrolyte of vanadium cell; The 3rd, lower permeability, in order to avoid vanadium cell both positive and negative polarity electrolyte interpenetrates, reduces battery efficiency; The 4th, there is certain intensity.At present the bipolar plates of research mainly comprises that atresia graphite bi-polar plate, carbon moulds bipolar plates and metal double polar plates.Although atresia graphite bi-polar plate has good corrosion resistance and conductivity, its complicated process of preparation, cost is high; Carbon is moulded bipolar plates, and to have preparation technology simple, and cost is lower, but its resistivity is apparently higher than metal double polar plates and atresia graphite bi-polar plate; Metal double polar plates has the features such as intensity is high, good processability, compactness is high, this volume resistance is little, but in battery strong acidic environment, faces etching problem, therefore must carry out surface modification treatment to it, and this is the key that can metal double polar plates be applied.Conventionally the processing method adopting has hot spray, silk screen printing, physical vapour deposition (PVD), chemical vapour deposition (CVD), Implantation, plating, chemical plating etc.Although the bipolar plates life-span after modification has obtained raising to a certain degree, but still cannot meet long-term instructions for use.Therefore, must seek new metal double polar plates surface protection coating.
Summary of the invention
summary of the invention
The surface protection coating that the object of this invention is to provide a kind of all-vanadium flow battery bipolar plate of stainless steel.This coating can significantly improve the decay resistance of stainless steel in all-vanadium flow battery environment, and reduces the contact resistance of metal double polar plates.
The invention provides a kind of all-vanadium flow battery bipolar plate of stainless steel surface chromium carbide/graphite composite, it is characterized in that: composite coating internal layer is fine and close thermal diffusion chromium carbide layer, and skin is fine and close graphite linings.The compound bipolar plate of stainless steel that can make of this chromium carbide and graphite linings obtains excellent corrosion resisting property and low contact resistance.
All-vanadium flow battery bipolar plate of stainless steel provided by the invention surface chromium carbide/graphite composite, described composite coating adopts chemical gaseous phase depositing process preparation.The thickness of coating is by controlling to regulate to parameters such as reaction temperature, reaction time, atmosphere.
All-vanadium flow battery bipolar plate of stainless steel provided by the invention surface chromium carbide/graphite composite, is characterized in that: described coating prepared atmosphere is hydrogen-acetylene gaseous mixture or hydrogen-methane mixed gas.
All-vanadium flow battery bipolar plate of stainless steel provided by the invention surface chromium carbide/graphite composite, is characterized in that: the preparation temperature of described composite coating is 800-950 ℃.
All-vanadium flow battery bipolar plate of stainless steel provided by the invention surface chromium carbide/graphite composite, it is characterized in that: the preparation of described composite coating chromium carbide internal layer need be carried out on top layer chromium content is not less than 30% stainless steel, need at stainless steel surfaces, to prepare rich chromium layer in advance, to guarantee to prepare the required chromium source of continuous carbonization chromium layer.The acquisition of the rich chromium layer of stainless steel surfaces can adopt the methods such as solid state powder chromising, physical vapour deposition (PVD), plating to obtain.
All-vanadium flow battery bipolar plate of stainless steel provided by the invention surface chromium carbide/graphite composite, graphite skin in described composite coating can be grown better under the effect of Ni Catalytic Layer, therefore on the surface of the rich chromium layer of stainless steel surfaces, deposits in advance the Ni Catalytic Layer that a layer thickness is no more than 1 micron.The preparation of Ni Catalytic Layer can adopt the methods such as plating, physical vapour deposition (PVD).
All-vanadium flow battery bipolar plate of stainless steel provided by the invention surface chromium carbide/graphite composite, can be applied to all kinds stainless steel (as 304,316L, 310 type stainless steels) surface.Composite coating is thicker, and the protection of longer time can be provided stainless steel.
Take and apply chromium carbide/graphite composite as example at 316L stainless steel surfaces, this coating can significantly improve stainless steel at the H of 25 ℃ of 2.5 mol/L
2sO
4corrosion potential in the aqueous solution, reduces corrosion current.Coating is not destroyed in long period of soaking process.Stainless resistivity is 0.3 Ω cm.
Embodiment
Embodiment 1
Adopt chemical gaseous phase depositing process to prepare chromium carbide/graphite composite on 316 bipolar plate of stainless steel surfaces.First adopt solid state powder chromium implements to prepare rich chromium layer at 316 stainless steel surfaces, further adopting galvanoplastic is the metal Ni layer of 1 micron at stainless steel surfaces deposit thickness.900
0c, H
2-4%C
2h
2in mixed atmosphere, react 2 hours, can obtain outer layer thickness is 2.5 microns, and internal layer thickness is the chromium carbide/graphite composite of 10 microns.Coating can significantly improve stainless steel at 25 ℃, 2.5 mol/L H
2sO
4corrosion potential in the aqueous solution, reduces corrosion current.Coating is not destroyed in long period of soaking process.Stainless resistivity is 0.3 Ω cm.
Embodiment 2
Adopt chemical gaseous phase depositing process to prepare chromium carbide/graphite composite on 316 bipolar plate of stainless steel surfaces.First adopt solid state powder chromium implements to prepare rich chromium layer at 316 stainless steel surfaces, further adopting galvanoplastic is the metal Ni layer of 1 micron at stainless steel surfaces deposit thickness.950
0c, H
2-4%C
2h
2in mixed atmosphere, react 2 hours, can obtain outer layer thickness is 3 microns, and internal layer thickness is the chromium carbide/graphite composite of 14 microns.Coating can significantly improve stainless steel at 25 ℃, 2.5 mol/L H
2sO
4corrosion potential in the aqueous solution, reduces corrosion current.Coating is not destroyed in long period of soaking process.Stainless resistivity is 0.33 Ω cm.
Embodiment 3
Adopt chemical gaseous phase depositing process to prepare chromium carbide/graphite composite on 316 bipolar plate of stainless steel surfaces.First adopt solid state powder chromium implements to prepare rich chromium layer at 316 stainless steel surfaces, further adopting galvanoplastic is the metal Ni layer of 1 micron at stainless steel surfaces deposit thickness.900
0c, H
2-8%C
2h
2in mixed atmosphere, react 2 hours, can obtain outer layer thickness and be about 2.8 microns, internal layer thickness is the chromium carbide/graphite composite of 13 microns.Coating can significantly improve stainless steel at 25 ℃, 2.5 mol/L H
2sO
4corrosion potential in the aqueous solution, reduces corrosion current.Coating is not destroyed in long period of soaking process.Stainless resistivity is 0.32 Ω cm.
Embodiment 4
Adopt chemical gaseous phase depositing process to prepare chromium carbide/graphite composite on 316 bipolar plate of stainless steel surfaces.First adopt solid state powder chromium implements to prepare rich chromium layer at 316 stainless steel surfaces, further adopting galvanoplastic is the metal Ni layer of 1 micron at stainless steel surfaces deposit thickness.900
0c, H
2-4%C
2h
2in mixed atmosphere, react 3 hours, can obtain outer layer thickness and be about 4 microns, internal layer thickness is the chromium carbide/graphite composite of 17 microns.Coating can significantly improve stainless steel at 25 ℃, 2.5 mol/L H
2sO
4corrosion potential in the aqueous solution, reduces corrosion current.Coating is not destroyed in long period of soaking process.Stainless resistivity is 0.35 Ω cm.
Embodiment 5
Adopt chemical gaseous phase depositing process to prepare chromium carbide/graphite composite on 304 bipolar plate of stainless steel surfaces.First adopt solid state powder chromium implements to prepare rich chromium layer at 304 stainless steel surfaces, further adopting galvanoplastic is the metal Ni layer of 1 micron at stainless steel surfaces deposit thickness.900
0c, H
2-4%C
2h
2in mixed atmosphere, react 2 hours, can obtain outer layer thickness is 2 microns, and internal layer thickness is the chromium carbide/graphite composite of 12 microns.Coating can significantly improve stainless steel at 25 ℃, 2.5 mol/L H
2sO
4corrosion potential in the aqueous solution, reduces corrosion current.Coating is not destroyed in long period of soaking process.Stainless resistivity is 0.3 Ω cm.
Embodiment 6
Adopt chemical gaseous phase depositing process to prepare chromium carbide/graphite composite on 316 bipolar plate of stainless steel surfaces.First adopting galvanoplastic to prepare thickness at 316 stainless steel surfaces is the chromium layer of 8 microns, and further adopting galvanoplastic is the metal Ni layer of 1 micron at stainless steel surfaces deposit thickness.900
0c, H
2-4%C
2h
2in mixed atmosphere, react 2 hours, can obtain outer layer thickness and be about 2.3 microns, internal layer thickness is the chromium carbide/graphite composite of 9 microns.Coating can significantly improve stainless steel at 25 ℃, 2.5 mol/L H
2sO
4corrosion potential in the aqueous solution, reduces corrosion current.Coating is not destroyed in long period of soaking process.Stainless resistivity is 0.28 Ω cm.
Embodiment 7
Adopt chemical gaseous phase depositing process to prepare chromium carbide/graphite composite on 316 bipolar plate of stainless steel surfaces.First adopting physical vaporous deposition to prepare thickness at 316 stainless steel surfaces is the chromium layer of 5 microns, and further adopting galvanoplastic is the metal Ni layer of 1 micron at stainless steel surfaces deposit thickness.900
0c, H
2-4%C
2h
2in mixed atmosphere, react 2 hours, can obtain outer layer thickness and be about 2.4 microns, internal layer thickness is the chromium carbide/graphite composite of 6 microns.Coating can significantly improve stainless steel at 25 ℃, 2.5 mol/L H
2sO
4corrosion potential in the aqueous solution, reduces corrosion current.Coating is not destroyed in long period of soaking process.Stainless resistivity is 0.29 Ω cm.
Embodiment 8
Adopt chemical gaseous phase depositing process to prepare chromium carbide/graphite composite on 316 bipolar plate of stainless steel surfaces.First adopting physical vaporous deposition to prepare thickness at 316 stainless steel surfaces is the chromium layer of 5 microns, and further adopting galvanoplastic is the metal Ni layer of 0.5 micron at stainless steel surfaces deposit thickness.900
0c, H
2-4%C
2h
2in mixed atmosphere, react 2 hours, can obtain outer layer thickness and be about 2 microns, internal layer thickness is the chromium carbide/graphite composite of 6 microns.Coating can significantly improve stainless steel at 25 ℃, 2.5 mol/L H
2sO
4corrosion potential in the aqueous solution, reduces corrosion current.Coating is not destroyed in long period of soaking process.Stainless resistivity is 0.3 Ω cm.
Claims (2)
1. all-vanadium flow battery bipolar plate of stainless steel surface chromium carbide/graphite composite, is characterized in that: described composite coating internal layer is thermal diffusion chromium carbide layer, and skin is graphite linings;
The preparation method of described composite coating is: at stainless steel surfaces, prepare rich chromium layer in advance, then in the surperficial pre-deposition Ni Catalytic Layer of described rich chromium layer, finally adopt chemical vapour deposition technique at 800-950 ℃ of temperature, in acetylene-hydrogen or methane-hydrogen mixed gas atmosphere, synchronous growth forms.
2. according to composite coating described in claim 1, it is characterized in that: the thickness of described Ni Catalytic Layer is no more than 1 micron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010551258.2A CN102468490B (en) | 2010-11-19 | 2010-11-19 | Surface chromium carbide/graphite composite coating for vanadium redox flow battery stainless steel bipolar plate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010551258.2A CN102468490B (en) | 2010-11-19 | 2010-11-19 | Surface chromium carbide/graphite composite coating for vanadium redox flow battery stainless steel bipolar plate |
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| CN102468490A CN102468490A (en) | 2012-05-23 |
| CN102468490B true CN102468490B (en) | 2014-04-16 |
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| CN201010551258.2A Expired - Fee Related CN102468490B (en) | 2010-11-19 | 2010-11-19 | Surface chromium carbide/graphite composite coating for vanadium redox flow battery stainless steel bipolar plate |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102723499B (en) * | 2012-06-07 | 2014-08-06 | 上海交通大学 | Metal bipolar plate of fuel cell with surface plating layers and preparation method thereof |
| CN102800871B (en) * | 2012-08-14 | 2015-07-08 | 上海交通大学 | Fuel cell metal bipolar plate carbon chromium gradient coating and preparation method |
| CN103633336B (en) * | 2012-08-29 | 2016-01-27 | 中国科学院大连化学物理研究所 | A kind of bipolar plate for liquid flow energy storage and preparation method thereof |
| CN102851667A (en) * | 2012-09-08 | 2013-01-02 | 陕西长岭电子科技有限责任公司 | Treatment method of anode shell inner surface of sodium-sulfur battery |
| JP6098998B2 (en) * | 2013-09-12 | 2017-03-22 | 住友電気工業株式会社 | Battery cell stack and redox flow battery |
| KR102163726B1 (en) * | 2013-11-22 | 2020-10-08 | 삼성전자주식회사 | Redox flow battery |
| CN104617317A (en) * | 2015-02-04 | 2015-05-13 | 大连融科储能技术发展有限公司 | Method for treating surface of bipolar plate for redox flow battery and bipolar plate obtainedthereby |
| GB2551191B (en) * | 2016-06-10 | 2020-01-15 | Imperial Innovations Ltd | Electrically conductive composite coating with azole corrosion inhibitor |
| CN108336371A (en) * | 2018-02-05 | 2018-07-27 | 大连融科储能技术发展有限公司 | A kind of bipolar plates used for all-vanadium redox flow battery |
| CN108637166B (en) * | 2018-05-16 | 2020-02-11 | 安徽三环水泵有限责任公司 | Preparation method of slurry pump impeller |
| CN109524682A (en) * | 2018-11-12 | 2019-03-26 | 临沂市产品质量监督检验所 | A kind of metal compound bipolar plate used for all-vanadium redox flow battery and preparation method thereof |
| CN113265638B (en) * | 2021-07-20 | 2021-09-14 | 中国科学院宁波材料技术与工程研究所 | High-conductivity corrosion-resistant graphite-like carbon protective multilayer composite coating and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101325252A (en) * | 2007-06-15 | 2008-12-17 | 清华大学 | Double pole plate for fluid flow battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0750168A (en) * | 1993-08-04 | 1995-02-21 | Mitsubishi Materials Corp | Separator material for molten carbonate fuel cell |
| US7211346B2 (en) * | 2002-04-03 | 2007-05-01 | Ut-Battelle, Llc | Corrosion resistant metallic bipolar plate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101325252A (en) * | 2007-06-15 | 2008-12-17 | 清华大学 | Double pole plate for fluid flow battery |
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| JP特开平7-50168A 1995.02.21 |
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