CN100413130C - Membrane electrode containing membrane water managing layer and preparing process thereof - Google Patents
Membrane electrode containing membrane water managing layer and preparing process thereof Download PDFInfo
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- CN100413130C CN100413130C CNB2006100153002A CN200610015300A CN100413130C CN 100413130 C CN100413130 C CN 100413130C CN B2006100153002 A CNB2006100153002 A CN B2006100153002A CN 200610015300 A CN200610015300 A CN 200610015300A CN 100413130 C CN100413130 C CN 100413130C
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- management layer
- water management
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- membrane
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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
Abstract
The invention relates to the technical field of proton exchange membrane fuel cell, advancing a new method for preparing membrane electrode water management layer of proton exchange membrane fuel cell, comprising: 1) mixing carbon powder and PTEF emulsion with isopropyl alcohol, making supersonic vibration for 20-30 minutes and diffusing uniformly, and vacuum-drying the mixture into mud, where the PTEF weight is 18%-82% of that of the carbon powder and the isopropyl alcohol addition is 0.02mL-0.04mL per mg carbon powder; 2) making the ready-prepared muddy mixture into 50 mum-250 mum thick flexible membrane as water management layer. And the prepared membrane electrode has good working performance and the membrane water management layer is more beneficial to building block cell assembly.
Description
Technical field
The present invention relates to the battery technology field, particularly contain membrane electrode of membrane water managing layer and preparation method thereof.
Background technology
The energy is the material base of human survival and development, is the power of the national economic development.The fuel cell power generation mode is that fuel and oxidant are fed anode and negative electrode respectively, by electrode reaction the chemical energy of fuel is directly changed into electric energy, and it is not limited by Carnot cycle without the overheated machine process.Proton Exchange Membrane Fuel Cells (Proton Exchange Membrane FuelCell, PEMFC) has the energy conversion efficiency height, specific energy is big, starts rapidly and series of advantages such as environmental friendliness, is considered to the cleaning of 21 century first-selection, generation technology efficiently.
Membrane electrode (Membrane﹠amp; Electrode Assembly, MEA) be the parts of PEMFC most critical, be the core that the PEMFC electrochemical reaction can efficiently be carried out, its technology of preparing not only directly influences battery performance, and most important to reducing battery cost, raising battery specific power and specific energy.Membrane electrode is made up of gas diffusion layers, catalyst layer and proton exchange membrane.General carbon paper or the carbon cloth of handling through polytetrafluoroethylene (PTFE) that adopt of gas diffusion layers, or the bonding carbon dust of compacting one deck PTFE is made loose structure on carbon paper that PTFE handles or carbon cloth, and its effect is to provide stable, gas delivery passage and guarantee that the intensity of electrode reaches requirement fast for electrode reaction.Eelctro-catalyst adopts load type platinum/charcoal (Pt/C) or platinum-ruthenium/charcoal (Pt-Ru/C), and it is present hydrogen/oxygen (H
2/ O
2) or hydrogen/air (H
2/ air) the first-selected high activity eelctro-catalyst of PEMFC.The general employing of proton exchange membrane has high H
+The perfluorinated sulfonic acid type proton exchange membrane of conducting power (as the Nafion series membranes of du pont company).
The fuel of PEMFC can directly adopt pure H
2, fuel such as methyl alcohol, or with the H that is rich in that obtains behind methyl alcohol, natural gas, the hydrocarbon fuel catalytic reforming
2Mist.Oxidant adopts pure oxygen or air usually.
When adopting H
2During for fuel, electrode reaction is as follows:
Anode reaction: H
2=2H
++ 2e
-
Cathode reaction: O
2+ 4H
++ 4e
-=H
2O
Anode H
2Under the effect of anode electrocatalyst, the proton (H that disassociation produces
+) arrive negative electrode by proton exchange membrane, with water generation reaction under electronics that arrives through external circuit and the effect of oxygen at electrocatalyst for cathode.If but the reaction gas humidity that enters battery is very low, and the water that generates in oxygen electrode side will cause the dehydration of hydrogen electrode side proton exchange membrane to become dry to hydrogen electrode side back-diffusion deficiency.When atm number passed through, the proton exchange membrane of oxygen electrode porch also can be dried, and causes the internal resistance of battery to rise significantly, even is difficult to work.Therefore, the reaction gas that enters battery pack generally will carry out the humidification processing.
General outer humidification mode and the interior humidification mode of adopting of original humidification mode, these two kinds of humidification modes are all used the humidification auxiliary system, the water content of proton exchange membrane is directly controlled by fuel gas and oxygen or fuel gas, has increased quality, cost and the complexity of fuel cell system.Therefore, develop the optimal selection that the membrane electrode that has from humidifying capacity becomes its humidification problem of solution.A kind of simple method is to add the entry regulating course or claim water management layer between Catalytic Layer and diffusion layer, this layer made by the bonding carbon dust of polytetrafluoroethylene (PTFE), its role is to: 1. the strong hydrophobicity of PTFE forces the back-diffusion of partial reaction water anode, keeps certain water content thereby proton exchange membrane is in operation.2. owing to the hydrophily of membrane electrode Catalytic Layer, when the big current work of battery, rational pore structure provides the storage area of water in the water regulating course, can alleviate the electrode that causes because of the water yield is excessive and flood stain.
The coating processes of brushing or spraying is generally adopted in traditional water management layer preparation on matrix, yet two kinds of methods all have certain complexity, are not suitable for larger suitability for industrialized production.The present invention proposes a kind of new method for preparing water management layer, this method technology is simple, and the independently water management layer film of preparing is beneficial to the cordwood system type assembling of battery.
Summary of the invention
The objective of the invention is to propose a kind of new method for preparing the membrane electrode of fuel batter with proton exchange film water management layer.The preparation method is as follows:
1) carbon dust, ptfe emulsion and isopropyl alcohol are mixed, sonic oscillation was uniformly dispersed it in 20 ~ 30 minutes, subsequently its vacuumize was become the mud shape, and wherein, the addition of polytetrafluoroethylene is 18% ~ 82% of a carbon dust weight; The addition of isopropyl alcohol is every milligram of carbon dust 0.02mL ~ 0.04mL;
The mud shape mixture that 2) will make is made the film of flexible, and thickness is 50 μ m ~ 240 μ m, and made film is the water management layer film.
Can also add pore creating material in described step 1), addition is 20% ~ 40% of a carbon dust weight; In step 2) form the water management layer film after, the pore creating material in the poach stripping film again.
Described film adopts two roller roll forming machines to roll into repeatedly.
Described pore creating material is carbonic hydroammonium, ammonium oxalate, ammonium sulfate or sodium sulphate etc.
The method of water management layer film preparation battery of the present invention, be on two water management layer films, to be coated with catalyst pulp equably, after treating its drying, with a proton exchange membrane of handling well at 0.3 ~ 0.5MPa, 130 ~ 145 ℃ of following hot pressing 60 ~ 90s, form membrane electrode, directly or with two carbon papers place the membrane electrode both sides then, carry out the battery assembling.
Or catalyst pulp become the congee shape 70 ℃ of following vacuumizes, be coated in equably then on two poly tetrafluoroethylenes, after treating its drying, with a proton exchange membrane of handling well at 0.3 ~ 0.5MPa, 130 ~ 145 ℃ of following hot pressing 60 ~ 90s peel off poly tetrafluoroethylene then, form membrane electrode, again two water management layer films are placed the membrane electrode both sides, directly or with two carbon papers place water management layer film both sides then, carry out the Proton Exchange Membrane Fuel Cells assembling.
According to technique scheme assembling proton exchange membrane cell.Battery adopts atresia graphite pole plate, stainless steel end plate.At first carry out the forced activation process in two stages: hydrogen pressure and oxygen pressure are transferred to 0.10MPa and 0.12MPa, H respectively
2And O
2The humidification temperature be respectively 60 ℃ and 55 ℃, slowly regulate electric current to 300mA/cm
2, battery temperature rises to 50 ℃.Battery transfers to 0.28MPa and 0.30MPa, H respectively with hydrogen pressure and oxygen pressure again after the 8h continuous operation with this understanding
2And O
2The humidification temperature transfer to 80 ℃ and 75 ℃ respectively, battery temperature rises to 70 ℃, electric current transfers to 500mA/cm
2, move 4h continuously after, external power supply breaks.Cell is connected with electronic load, measures the voltage-to-current curve of battery.Actual effect is seen Fig. 1 to Fig. 4.The membrane electrode that contains the water management layer film that contains the method for the invention preparation has good working performance.
Description of drawings
Fig. 1: contain the membrane electrode voltage-to-current densogram of water management layer film, the thickness 90 μ m of film, PTFE content is 35%, adopts the carbon paper diffusion layer.
Fig. 2: contain the membrane electrode voltage-to-current densogram of water management layer film, thickness is 150 μ m, adds the solid ammonium sulfate pore creating material, adopts the carbon paper diffusion layer.
Fig. 3: the membrane electrode voltage-to-current densogram that contains the water management layer film.Thickness is 240 μ m, adds the solid sodium sulfate pore creating material, does not adopt the carbon paper diffusion layer.
Wherein: under ■-outer humidification condition, the inlet temperature of hydrogen and oxygen is respectively 80 ℃ and 75 ℃.
Zero-not have under the outer humidification condition, the inlet temperature of hydrogen and oxygen is 25 ℃.
Fig. 4: water management layer film and membrane electrode figure.
Embodiment
Embodiment 1:
(1) takes by weighing 210mg carbon black (trade names Vulcan XC-72) in the 25mL beaker, add the 0.72mL15wt%PTFE emulsion, add the 5.5mL isopropyl alcohol again, sonic oscillation 30 minutes;
(2) with the paste mixture that obtains in 70 ℃ of vacuumizes, make it become the mud shape;
(3) with two roller roll forming machines above-mentioned mud shape mixture is rolled into film, the control thickness is 90 μ m, promptly makes the water management layer film.
(4) 8mg Pt/C eelctro-catalyst, 0.7mL water and 0.7mL isopropyl alcohol are mixed sonic oscillation 15 minutes; Add Nafion solution (5wt%, du pont company) 0.10mL then, continued sonic oscillation 30 minutes;
(5) above-mentioned ink shape slurry is become the congee shape 70 ℃ of following vacuumizes, be coated in equably then on the water management layer film that has prepared,, form electrode 70 ℃ of following vacuumize half an hour;
(6) with two above-mentioned electrodes and the Nafion proton exchange membrane (du pont company Nafion1135) handled well at 0.3MPa, 130 ℃ of following hot pressing 90s, promptly make membrane electrode, as shown in Figure 4.
Pack in the cell in the both sides that two carbon papers are fixed in membrane electrode, pole plate size 4 * 4 * 0.3cm of battery
3, the effective area of membrane electrode is 4cm
2After the forced activation of method described in the present invention, measure battery at H
2/ O
2Voltage-to-current curve in the system, as shown in Figure 1.Test result shows that the membrane electrode that contains the water management layer film of the method for the invention preparation does not have good working performance under the humidification condition.
Embodiment 2:
(1) takes by weighing 210mg carbon black (Vulcan XC-72) in the 25ml beaker, add the 1.1mL15wt%PTFE emulsion, add the 5.0mL isopropyl alcohol again, sonic oscillation 20 minutes;
(2) with the paste mixture that obtains in 75 ℃ of vacuumizes, make it become the mud shape;
(3) with two roller roll forming machines above-mentioned mud shape mixture is rolled into film, the control thickness is 50 μ m, promptly makes the water management layer film.
(4) 8mg Pt/C eelctro-catalyst, 0.6mL water and 0.6mL isopropyl alcohol are mixed sonic oscillation 15 minutes; Add Nafion solution (5wt%, du pont company) 0.10mL then, continued sonic oscillation 20 minutes;
(5) above-mentioned ink shape slurry is become the congee shape 70 ℃ of following vacuumizes, be coated in equably then on the water management layer film that has prepared,, form electrode in 65 ℃ of following vacuumizes 40 minutes;
(6) with two above-mentioned electrodes and the Nafion proton exchange membrane (du pont company) handled well at 0.5MPa, 145 ℃ of following hot pressing 60s, promptly make membrane electrode.
Two carbon papers are fixed on the membrane electrode both sides, carry out the battery assembling.Pole plate size 4 * 4 * 0.3cm of battery
3, the effective area of membrane electrode is 4cm
2After the forced activation of method described in the present invention, measure battery at H
2/ 0
2Voltage-to-current curve in the system, test result show that the membrane electrode that contains the water management layer film that contains the method for the invention preparation has good working performance.
Embodiment 3:
(1) takes by weighing 300mg carbon black (Vulcan XC-72) in the 25mL beaker, add the 0.34mL15wt%PTFE emulsion, add solid ammonium bicarbonate 100mg, add the 11mL isopropyl alcohol again, sonic oscillation 30 minutes;
(2) with the paste mixture that obtains in 60 ℃ of vacuumizes, make it become the mud shape;
(3) with two roller roll forming machines above-mentioned mud shape mixture is rolled into film, the control thickness is 240 μ m, promptly makes the water management layer film.
(4) 8mg Pt/C eelctro-catalyst, 0.6mL water and 0.6mL isopropyl alcohol are mixed sonic oscillation 20 minutes; Add Nafion solution (5wt%, du pont company) 0.10mL then, continued sonic oscillation 20 minutes;
(5) above-mentioned ink shape slurry is become the congee shape 70 ℃ of following vacuumizes, be coated in equably then on the water management layer film that has prepared, at room temperature dry 1h forms electrode.
(6) with above-mentioned two plate electrodes and the Nafion proton exchange membrane (du pont company) handled well at 0.32MPa, 140 ℃ of following hot pressing 90s, promptly make membrane electrode.
The membrane electrode that this programme is formed directly carries out the battery assembling.Pole plate size 4 * 4 * 0.3cm of battery
3, the effective area of membrane electrode is 4cm
2After the forced activation of method described in the present invention, measure battery at H
2/ O
2Voltage-to-current curve in the system.
Embodiment 4:
(1) takes by weighing 210mg carbon black (Vulcan XC-72) in the 25ml beaker, add the 0.72mL15wt%PTFE emulsion, add solid ammonium sulfate 70mg, add the 7.0mL isopropyl alcohol again, sonic oscillation 20 minutes;
(2) with the paste mixture that obtains in 65 ℃ of vacuumizes, make it become the mud shape;
(3) with two roller roll forming machines above-mentioned mud shape mixture is rolled into film, the control thickness is 150 μ m, promptly makes the water management layer film; The film that makes is boiled the 1h after washing in deionized water as shown in Figure 4 standby.
(4) 8mg Pt/C eelctro-catalyst, 0.6mL water and 0.6mL isopropyl alcohol are mixed sonic oscillation 15 minutes; Add Nafion solution (5wt%, du pont company) 0.10mL then, continued sonic oscillation 20 minutes;
(5) above-mentioned ink shape catalyst pulp is become the congee shape 70 ℃ of following vacuumizes, be coated in equably then on two poly tetrafluoroethylenes, after treating its drying, with a proton exchange membrane (5wt% who handles well, du pont company Nafion1135) at 0.35MPa, 138 ℃ of following hot pressing 90s peel off poly tetrafluoroethylene then, form membrane electrode.
(6) water management layer film and two carbon papers that two anticipatory remark embodiment (3) are formed, the battery assembling is carried out in the membrane electrode both sides that place this programme (5) to form successively respectively.
Pole plate size 4 * 4 * 0.3cm of battery
3, the effective area of membrane electrode is 4cm
2After the forced activation of method described in the present invention, measure battery at H
2/ O
2Voltage-to-current curve in the system, as shown in Figure 2.Test result shows that the membrane electrode that contains the water management layer film that contains the method for the invention preparation has good working performance.
Embodiment 5:
(1) takes by weighing 300mg carbon black (Vulcan XC-72) in the 25ml beaker, add the 1.0mL15wt%PTFE emulsion, add solid sodium sulfate 110mg, add the 10mL isopropyl alcohol again, sonic oscillation 30 minutes;
(2) with the paste mixture that obtains in 70 ℃ of vacuumizes, make it become the mud shape;
(3) with two roller roll forming machines above-mentioned mud shape mixture is rolled into film, the control thickness is 240 μ m, promptly makes the water management layer film; The film that makes is boiled the 1h after washing in deionized water standby.
(4) 8mg Pt/C eelctro-catalyst, 0.6mL water and 0.6mL isopropyl alcohol are mixed sonic oscillation 15 minutes; Add Nafion solution (5wt%, du pont company) 0.10mL then, continued sonic oscillation 20 minutes;
(5) above-mentioned ink shape catalyst pulp is become the congee shape 70 ℃ of following vacuumizes, is coated in equably then on two poly tetrafluoroethylenes, treat its drying after, with a proton exchange membrane of handling well at 0.4MPa, 135 ℃ of following hot pressing 75s peel off poly tetrafluoroethylene then, form membrane electrode.
(6) water management layer film (2 * 2cm that two anticipatory remark embodiment (3) are formed
2) place the membrane electrode both sides of this programme (5) formation respectively, carry out the battery assembling.
Pole plate size 4 * 4 * 0.3cm of battery
3, the effective area of membrane electrode is 4cm
2After the forced activation of method described in the present invention, measure battery at H
2/ O
2Voltage-to-current curve in the system, test result as shown in Figure 3.
The present invention's method open and that disclose can be by using for reference this paper disclosure.Although method of the present invention is described by preferred embodiment, but those skilled in the art obviously can change method as herein described in not breaking away from content of the present invention, spirit and scope, more particularly, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (4)
1. the preparation method of a battery membranes electrode water management layer is characterized in that:
1) carbon dust, ptfe emulsion and isopropyl alcohol are mixed, sonic oscillation was uniformly dispersed it in 20～30 minutes, subsequently its vacuumize was become the mud shape, and wherein, the addition of polytetrafluoroethylene is 18%～82% of a carbon dust weight; The addition of isopropyl alcohol is every milligram of carbon dust 0.02mL～0.04mL;
The mud shape mixture that 2) will make is made the independently film of flexible, and thickness is 50 μ m～250 μ m, and made film is the water management layer film.
2. the preparation method of battery membranes electrode water management layer as claimed in claim 1, it is characterized in that in the described step 1) before sonic oscillation, add pore creating material in carbon dust, ptfe emulsion and isopropyl alcohol mixed liquor, addition is 20%～40% of a carbon dust weight; In step 2) form the water management layer film after, the pore creating material in the poach stripping film again.
3. the preparation method of battery membranes electrode water management layer as claimed in claim 1 is characterized in that described film adopts two roller roll forming machines to roll into repeatedly.
4. the preparation method of battery membranes electrode water management layer as claimed in claim 2 is characterized in that described pore creating material is carbonic hydroammonium, ammonium oxalate, ammonium sulfate or sodium sulphate.
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|---|---|---|---|
| CNB2006100153002A CN100413130C (en) | 2006-08-10 | 2006-08-10 | Membrane electrode containing membrane water managing layer and preparing process thereof |
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| CN100413130C true CN100413130C (en) | 2008-08-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI423511B (en) | 2009-12-31 | 2014-01-11 | Ind Tech Res Inst | Proton exchange membrane including organic-inorganic hybird |
| CN109830718A (en) * | 2019-01-09 | 2019-05-31 | 合肥工业大学 | A kind of production method of fuel cell membrane electrode |
| CN115000441B (en) * | 2022-05-12 | 2024-02-06 | 上海安池科技有限公司 | Preparation method of precoating layer on stainless steel belt for preparing bipolar plate of fuel cell |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1697217A (en) * | 2005-06-14 | 2005-11-16 | 天津大学 | Membrane electrode capable of adjusting water, and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1697217A (en) * | 2005-06-14 | 2005-11-16 | 天津大学 | Membrane electrode capable of adjusting water, and preparation method |
Non-Patent Citations (6)
| Title |
|---|
| PEMFC的自增湿膜电极结构和性能研究. 石肇元，田建华，石劲松，单忠强.电源技术，第30卷第6期. 2006 |
| PEMFC的自增湿膜电极结构和性能研究. 石肇元，田建华，石劲松，单忠强.电源技术，第30卷第6期. 2006 * |
| 聚四氟乙烯对空气电极防水透气膜性能的影响. 李玉杰，梁广川，欧秀芹，梁金生.河北工业大学学报，第33卷第6期. 2004 |
| 聚四氟乙烯对空气电极防水透气膜性能的影响. 李玉杰，梁广川，欧秀芹，梁金生.河北工业大学学报，第33卷第6期. 2004 * |
| 造孔剂对PEMFC膜电极性能的影响. 田建华，刘邦卫等.电源技术，第29卷第3期. 2005 |
| 造孔剂对PEMFC膜电极性能的影响. 田建华，刘邦卫等.电源技术，第29卷第3期. 2005 * |
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