CN114361482A - Preparation method of high-permeability carbon paper for fuel cell - Google Patents
Preparation method of high-permeability carbon paper for fuel cell Download PDFInfo
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- CN114361482A CN114361482A CN202210012203.7A CN202210012203A CN114361482A CN 114361482 A CN114361482 A CN 114361482A CN 202210012203 A CN202210012203 A CN 202210012203A CN 114361482 A CN114361482 A CN 114361482A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 58
- 239000000446 fuel Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 28
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000839 emulsion Substances 0.000 claims abstract description 11
- 238000002791 soaking Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 6
- 238000005507 spraying Methods 0.000 claims abstract description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 19
- 239000013049 sediment Substances 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 229910008337 ZrO(NO3)2.2H2O Inorganic materials 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 abstract description 11
- 239000001301 oxygen Substances 0.000 abstract description 11
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 18
- 238000009792 diffusion process Methods 0.000 description 16
- 238000005260 corrosion Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 7
- 239000003575 carbonaceous material Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000035699 permeability Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910009848 Ti4O7 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method of high-permeability carbon paper for a fuel cell, which comprises the following steps: s1: soaking the blank carbon paper in a PTFE solution, and repeating the soaking step to obtain PTFE-containing carbon paper; s2: preparation of Ce by codeposition method0.2‑0.8Y0.05‑ 0.5Zr0.1‑0.8O2(ii)/TiN; s3: ce prepared from S20.2‑ 0.8Y0.05‑0.5Zr0.1‑0.8O2And placing the emulsion of/TiN, carbon powder and PTFE in ethanol, performing ultrasonic dispersion uniformly, and spraying the emulsion on the surface of the carbon paper prepared in S1 to form a microporous layer on the surface of the carbon paper, thus obtaining the high-permeability carbon paper. The high-permeability carbon paper for the fuel cell, prepared by the invention, is beneficial to oxygen permeation, improves the oxygen permeation rate, enhances the conductivity and hydrophobicity of the carbon paper, and obviously reduces the surface resistance and the contact resistance.
Description
Technical Field
The invention relates to the field of proton exchange membrane fuel cells, in particular to a preparation method of high-permeability carbon paper for a fuel cell.
Background
The gas diffusion layer is located between the bipolar plate and the membrane electrode catalyst layer, and needs to have various performances at the same time, and good electrical conductivity, certain mechanical strength, stability and hydrophobicity at the same time. Generally, the gas diffusion layer has hydrophobic reaction gas channels and hydrophilic liquid water transport channels inside. The common gas diffusion layer is formed by combining a substrate layer, a hydrophobic layer and a microporous layer, is used as one of key materials of the PEMFCs, improves the electric conduction capability of the gas diffusion layer and reduces the contact resistance between the gas diffusion layer and other components, and is favorable for promoting the rapid transfer of electrons and the efficient operation of reaction. Therefore, research on the electrical conductivity of the gas diffusion layer is one of the key points to solve the industry bottleneck.
Secondly, reduction of production costs and improvement of durability are essential conditions for solving the practical application of PEMFCs. Degradation of the gas diffusion layer, which is one of the membrane electrode components, has been a concern. However, there have been few studies on the degradation process, and no suitable methods for improving the durability of the battery have been found. The durability of the components in the PEMFCs must be increased to promote increased fuel cell life. To achieve this, it is important to assess the degradation mechanism of each moiety independently, determining qualitatively the material decay mechanism. Generally, the gas diffusion layer is mainly subjected to the following three attacks, first, the dissolution of acidic corrosive liquid; secondly, the gas flow scouring action; third, galvanic corrosion by electrical potential predominates as electrochemical carbon corrosion. In addition, the long-term operation of the fuel cell, the catalytic layer and the gas diffusion layer are aged, the gas diffusion overvoltage is increased, and the service life of the cell is also reduced. In order to address the above-mentioned carbon corrosion problem, some researchers have used oxides instead of carbon materials as the catalytic layer support, such as Ti4O7、SnO2And the like. Another group of researchers have been to improve the durability of the material itself to ensure long-term operation of the fuel cell. For example: oweian et al use highly corrosion resistant graphitized carbon to slow down the carbon corrosion rate of the microporous layer to 1.2A/cm2The battery performance under the current density is improved by 25 percent. The willingness of Shexiangxi et al thinks that the more complete the internal crystal structure of the carbon material is when the electrochemical corrosion occurs, the higher the graphitization temperature of the carbon paper is, the more complete the internal crystal structure of the carbon material is+The ions are more difficult to enter the carbon material, so that the ions are slowly releasedReducing the corrosive effect of the acidic environment inside the fuel cell. In addition, under actual conditions (such as frequent switching and starting and stopping), the PTFE loaded on the gas diffusion layer has small surface tension, is easy to agglomerate in heat treatment, is difficult to uniformly cover on carbon paper, and is easy to fall off along with the reaction due to the characteristics of poor adhesion with the carbon paper substrate, weak binding force and the like, so that more carbon materials are exposed, the pore structure of the gas diffusion layer is corroded to be enlarged, the hydrophilicity of the carbon material is increased, the water-gas balance is damaged, the water-gas mass transfer resistance is increased, and the service life of the fuel cell is shortened. Therefore, the graphene oxide with the content of 1 wt% is added in the preparation process of the carbon paper, so that the bonding force between the PTFE hydrophobic coating and the substrate interface is improved. And the self-corrosion current density is only 7.16E under the high voltage condition of 1.4V-2μA·cm-2. Takata et al introduce unsaturated bonds such as hydroxyl, carbonyl and the like into the surface of polytetrafluoroethylene to improve the surface energy and contact angle of the polytetrafluoroethylene, thereby improving the interface bonding condition between the polytetrafluoroethylene and a carbon paper matrix. Yoon et al successfully introduced Si-O-C bond on the carbon paper matrix by using (heptadecafluorosilane-1, 1, 2, 2-tetrahydro) triethoxysilane) resin with stronger stability to perform hydrophobic treatment on the carbon paper, thereby improving the bonding with the matrix.
It follows that in PEMFCs, the stability of the gas diffusion layer directly affects the reliability and durability of the fuel cell. Therefore, the improvement of the durability of each component inside the gas diffusion layer has great application significance for developing long-life electric stacks.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a preparation method of high-permeability carbon paper for a fuel cell, which can improve oxygen transmission rate and has excellent corrosion resistance.
The technical scheme is as follows: the invention relates to a preparation method of high-permeability carbon paper for a fuel cell, which comprises the following steps:
s1: soaking the blank carbon paper in a PTFE solution, and repeating the soaking step to obtain PTFE-containing carbon paper;
s2: preparation of Ce by codeposition method0.2-0.8Y0.05-0.5Zr0.1-0.8O2/TiN;
S3: ce prepared from S20.2-0.8Y0.05-0.5Zr0.1-0.8O2And placing the emulsion of/TiN, carbon powder and PTFE in ethanol for ultrasonic dispersion, and spraying the emulsion on the surface of the carbon paper prepared in S1 to form a microporous layer on the surface of the carbon paper.
Further, in step S1, soaking a blank carbon paper of 2cm × 2cm in the PTFE solution, and repeating the above steps to prepare a carbon paper containing 5-15% of PTFE.
Further, in step S2, Ce (NO) is added in a molar ratio3)3.6H2O、ZrO(NO3)2.2H2O and Y (NO)3)3·6H2Dissolving 0 in water, adding nano TiN, continuously stirring uniformly, slowly adding ammonia water into the solution, adjusting the pH value to 10-11 to form an obvious deposit, performing suction filtration, washing and drying, placing the deposit in a muffle furnace for calcination, and crushing the calcined deposit by using a planetary ball mill.
Further, the molar ratio of n (Ce) to n (Zr) to n (Y) is 0.6: 0.3: 0.1.
Further, the diameter of the nano TiN is about 400-600 nm, and the added mass fraction is 4-10%.
Further, the calcining temperature in the muffle furnace is 500-550 ℃, and the calcining temperature is kept for 2-3 hours.
Furthermore, after the planet ball mill is smashed and crushed, the particle size of the precipitate is about 0.3-0.6 μm.
Further, in step S3, the Ce0.2-0.8Y0.05-0.5Zr0.1-0.8O2The addition amount of the/TiN and the carbon powder is 0.05-0.15 mg/cm respectively2、0.5~1.5mg/cm2And the mass part of the PTFE emulsion is 7-12% (used for preparing microporous layer slurry).
Has the advantages that: the high-permeability carbon paper for the fuel cell prepared by the invention is added with Ce0.2-0.8Y0.05- 0.5Zr0.1-0.8O2Has oxygen storage capacity, enhances the storage and release of oxygen, is favorable for oxygen permeation and improves the oxygen permeationThe catalyst has the advantages of high oxygen concentration stability, oxygen reduction catalysis function and capability of improving the catalytic efficiency of oxygen reduction in the oxygen circulation process. The added conductive TiN ceramic particles have strong corrosion resistance, enhanced carbon paper conductivity and hydrophobicity, and obviously reduced surface resistance and contact resistance.
Drawings
FIG. 1 is a topographical view of a highly breathable carbon paper diffusion layer of the present invention.
Detailed Description
For a further understanding of the present invention, reference will now be made in detail to the embodiments illustrated in the drawings.
Example 1
A preparation method of high-permeability carbon paper for a fuel cell comprises the following steps:
s1: soaking blank carbon paper of 2cm multiplied by 2cm in PTFE solution, and preparing carbon paper containing 15% of PTFE content after repeating the steps;
s2: ce (NO) in a molar ratio of n (Ce) to n (Zr) to n (Y) of 0.6: 0.3: 0.13)3.6H2O、ZrO(NO3)2.2H2O and Y (NO)3)3·6H20 is dissolved in water, nano TiN with the diameter of 400-600 nm is added, the added mass fraction is 5%, ammonia water is slowly added into the solution after the mixture is continuously stirred uniformly, the pH value is adjusted to be 10-11, obvious sediment is formed, the sediment is placed in a muffle furnace to be calcined for 2.5 hours at 550 ℃, then the calcined sediment is crushed by a planetary ball mill, and the particle size of the sediment is 0.3-0.6 mu m.
S3: ce prepared from S20.6Y0.1Zr0.3O2Emulsion of TiN, carbon powder and PTFE in an amount of 0.1mg/cm2、1mg/cm2And 10 percent of the added amount is placed in ethanol for uniform ultrasonic dispersion, and then the mixture is sprayed on the surface of the carbon paper prepared in S1 to form a microporous layer on the surface of the carbon paper.
Example 2
A preparation method of high-permeability carbon paper for a fuel cell comprises the following steps:
s1: soaking blank carbon paper of 2cm multiplied by 2cm in PTFE solution, and preparing carbon paper containing 5% of PTFE content after repeating the steps;
s2: ce (NO) in a molar ratio of n (Ce) to n (Zr) to n (Y) of 0.2: 0.1: 0.053)3.6H2O、ZrO(NO3)2.2H2O and Y (NO)3)3·6H20 is dissolved in water, nano TiN with the diameter of 400-600 nm is added, the added mass fraction is 4%, ammonia water is slowly added into the solution after the mixture is continuously stirred uniformly, the pH value is adjusted to be 10-11, obvious sediment is formed, the sediment is placed in a muffle furnace for calcining for 3 hours at the temperature of 510 ℃, then the calcined sediment is crushed by a planetary ball mill, and the particle size of the sediment is about 0.3-0.6 mu m.
S3: ce prepared from S20.2Y0.05Zr0.1O2Emulsion of TiN, carbon powder and PTFE in an amount of 0.15mg/cm2、1.5mg/cm2And after the 12 percent of the added amount is placed in ethanol for uniform ultrasonic dispersion, the mixture is sprayed on the surface of the carbon paper prepared in S1, and a microporous layer is formed on the surface of the carbon paper.
Example 3
A preparation method of high-permeability carbon paper for a fuel cell comprises the following steps:
s1: soaking blank carbon paper of 2cm multiplied by 2cm in PTFE solution, and preparing carbon paper containing 5-15% of PTFE content after repeating the steps;
s2: ce (NO) in a molar ratio of n (Ce) to n (Zr) to n (Y) of 0.6: 0.3: 0.13)3.6H2O、ZrO(NO3)2.2H2O and Y (NO)3)3·6H20 is dissolved in water, nano TiN with the diameter of 400-600 nm is added, the added mass fraction is 10%, ammonia water is slowly added into the solution after the mixture is continuously stirred uniformly, the pH value is adjusted to be 10-11, obvious sediment is formed, the sediment is placed in a muffle furnace to be calcined for 2-3 hours at the temperature of 500-550 ℃ after suction filtration, washing and drying, the calcined sediment is crushed by a planetary ball mill, and the particle size of the sediment is about 0.3-0.6 mu m.
S3: ce prepared from S20.8Y0.5Zr0.8O2Emulsion of/TIN, carbon powder and PTFE in the ratio of 0.05mg/cm2、0.5mg/cm2And 7 percent of the added amount is placed in ethanol for uniform ultrasonic dispersion, and then the mixture is sprayed on the surface of the carbon paper prepared in S1 to form a microporous layer on the surface of the carbon paper.
Example 4
The differences from example 1 are: in step S3, Ce0.6Y0.1Zr0.3O2The amount of TiN added was 0.05mg/cm 2.
Example 5
The differences from example 1 are: in step S3, Ce0.6Y0.1Zr0.3O2The amount of TiN added was 0.07mg/cm 2.
Example 6
The differences from example 1 are: in step S3, Ce0.6Y0.1Zr0.3O2The amount of TiN added was 0.15mg/cm 2.
Example 7
The differences from example 1 are: in step S3, Ce0.6Y0.1Zr0.3O2The amount of TiN added was 0.2mg/cm 2.
Comparative example 1
The differences from example 1 are: in step S3, Ce0.6Y0.1Zr0.3O2The amount of TiN added was 0.
Comparative example 2
The differences from example 1 are: in step S2, the amount of nano TiN added is 0.
FIG. 1 is a high permeability carbon paper diffusion layer morphology prepared under the conditions of example 5.
Table 1 shows the porosity and air permeability test values of the highly air permeable carbon papers prepared in comparative example 1, and examples 4 to 7, indicating that the permeability with Ce is high0.6Y0.1Zr0.3O2The porosity is reduced by increasing the addition of TiN, and the gas permeability is reduced after increasing.
TABLE 1
Porosity% | Air permeability ml.mm/(cm)2·h·mmAq) | |
Comparative example 1 | 87 | 2472 |
Example 1 | 80 | 2685 |
Example 4 | 79 | 2875 |
Example 5 | 77 | 3150 |
Example 6 | 75 | 2901 |
Example 7 | 72 | 2875 |
Table 2 is a test value of the surface resistance and the contact resistance of the high permeability carbon papers prepared in comparative example 2 and example 1, showing that the surface resistance and the contact resistance are significantly reduced with the addition of TiN.
TABLE 2
Claims (8)
1. A preparation method of high-permeability carbon paper for a fuel cell is characterized by comprising the following steps:
s1: soaking the blank carbon paper in a PTFE solution, and repeating the soaking step to obtain PTFE-containing carbon paper;
s2: preparation of Ce by codeposition method0.2-0.8Y0.05-0.5Zr0.1-0.8O2/TiN;
S3: ce prepared from S20.2-0.8Y0.05-0.5Zr0.1-0.8O2And placing the emulsion of/TiN, carbon powder and PTFE in ethanol, performing ultrasonic dispersion uniformly, and spraying the emulsion on the surface of the carbon paper prepared in S1 to form a microporous layer on the surface of the carbon paper, thus obtaining the high-permeability carbon paper.
2. The preparation method of claim 1, wherein in step S1, the carbon paper prepared by repeating the soaking step contains 5-15% by mass of PTFE.
3. The method according to claim 1, wherein in step S2, Ce (NO) is added in a molar ratio3)3.6H2O、ZrO(NO3)2.2H2O and Y (NO)3)3·6H20 is dissolved in water, nano TiN is added, ammonia water is slowly added into the solution after the nano TiN is continuously and uniformly stirred, the pH value is adjusted to 10-11, obvious deposit is formed, the deposit is filtered, washed and dried, the deposit is placed in a muffle furnace for calcination, and the calcined deposit is crushed by a planetary ball mill to obtain Ce0.2-0.8Y0.05- 0.5Zr0.1-0.8O2/TiN。
4. The method of claim 1, wherein the molar ratio of n (Ce) to n (Zr) to n (Y) is 0.6: 0.3: 0.1.
5. The method according to claim 3, wherein the diameter of the nano TiN is 400-600 nm, and the added mass fraction is 4-10%.
6. The preparation method according to claim 3, wherein the calcination temperature in the muffle furnace is 500-550 ℃ and is kept for 2-3 h.
7. The method according to claim 3, wherein the particle size of the sediment after the pulverization by the star mill is 0.3 to 0.6 μm.
8. The production method according to claim 1, wherein in step S3, the Ce is0.2-0.8Y0.05-0.5Zr0.1- 0.8O2The addition amount of the/TiN and the carbon powder is 0.05-0.15 mg/cm respectively2、0.5~1.5mg/cm2The mass fraction of the PTFE emulsion is 7-12%.
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US20150140470A1 (en) * | 2012-07-19 | 2015-05-21 | Ballard Power Systems Inc. | Microporous layer with hydrophilic additives |
CN106159283A (en) * | 2015-04-08 | 2016-11-23 | 宜兴市四通家电配件有限公司 | A kind of membrane electrode of fuel batter with proton exchange film and preparation method thereof |
JP2017152246A (en) * | 2016-02-25 | 2017-08-31 | ダイハツ工業株式会社 | Gas diffusion sheet for fuel cell and fuel cell |
CN109012666A (en) * | 2018-09-15 | 2018-12-18 | 四川鑫元瑞科技有限公司 | A kind of preparation method of cleaning catalyst for tail gases of automobiles |
CN112563516A (en) * | 2020-12-28 | 2021-03-26 | 浙江唐锋能源科技有限公司 | Gas diffusion layer of environment-friendly fuel cell and preparation method thereof |
CN112993265A (en) * | 2019-12-14 | 2021-06-18 | 中国科学院大连化学物理研究所 | Gas diffusion layer for fuel cell and preparation method thereof |
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- 2022-01-06 CN CN202210012203.7A patent/CN114361482A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102479960A (en) * | 2010-11-30 | 2012-05-30 | 中国科学院大连化学物理研究所 | Cathode diffusion layer for proton exchange membrane fuel cell, preparation and application thereof |
US20150140470A1 (en) * | 2012-07-19 | 2015-05-21 | Ballard Power Systems Inc. | Microporous layer with hydrophilic additives |
CN106159283A (en) * | 2015-04-08 | 2016-11-23 | 宜兴市四通家电配件有限公司 | A kind of membrane electrode of fuel batter with proton exchange film and preparation method thereof |
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