CN105742666A - Carbon nano tube gas diffusion layer for fuel cell and preparation and application of carbon nano tube gas diffusion layer - Google Patents
Carbon nano tube gas diffusion layer for fuel cell and preparation and application of carbon nano tube gas diffusion layer Download PDFInfo
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- 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 discloses a carbon nano tube gas diffusion layer for a fuel cell and a preparation method and an application of the carbon nano tube gas diffusion layer. The diffusion layer is prepared by in-situ growth of carbon nano tubes on a macroporous carbon-based support layer; the thicknesses of the carbon nano tubes are 1-50 microns; and the carbon nano tubes intensively grow on one side, close to a catalyst layer, of the macroporous carbon-based support layer. The carbon nano tubes have high hydrophobicity, so that the inner side of the gas diffusion layer prepared by intensive growth of the carbon nano tubes has hydrophobicity; the contact angle is 130-150 degrees under the condition of not adding a hydrophobic adhesive; a hydrophobic agent does not need to be added to the inner side of the gas diffusion layer; and the carbon nano tube gas diffusion layer can simultaneously have good hydrophobic ability, conductivity and mass transfer ability and can improve the output property of the fuel cell at high current density.
Description
Technical field
The invention belongs to fuel cell field, be specifically related to a kind of fuel cell carbon nano-fiber gas diffusion layers and preparation thereof and application.
Background technology
Proton Exchange Membrane Fuel Cells is a kind of novel energy conversion equipment, it is possible to be contamination-freely electric energy by chemical energy, and there is power density height, the advantage such as operating temperature is low, startup is fast, life-span length, be subject to researcher extensive concern.The core component of Proton Exchange Membrane Fuel Cells is the membrane electrode in sandwich structure, center to both sides be followed successively by PEM, cathode and anode Catalytic Layer, and the cathode and anode gas diffusion layers outside Catalytic Layer.
Gas diffusion layers plays an important role in a fuel cell, specifically includes that and prevents Catalytic Layer water logging from realizing cell water management while realizing electronics conduction between Catalytic Layer and bipolar plates, stablized by reactant and being transferred to Catalytic Layer, maintenance PEM moistening efficiently.Therefore gas diffusion layers needs good electronic conduction ability, excellent breathability and rational hydrophobicity.
For Proton Exchange Membrane Fuel Cells, under high current density, electrochemical reaction is aggravated with electroosmosis, and water causes battery water logging in cathode side gathering, and reacting gas cannot arrive catalyst surface smoothly and be electrochemically reacted, and battery performance sharply declines.In conventional research, researcher have studied the various material preparing gas diffusion layers and method, to improve battery performance.Chinese patent 102104159 describes a kind of gas diffusion layers preparation method containing pore creating material.It is that pore creating material, conductive fine powder, hydrophober mixed preparing are obtained MPL slurry, adopts the method for dipping and coating repeatedly to support on carbon paper by MPL slurry, every time when dipping and coating, all uses the slurry of different ratio.It is all that bonding agent is mixed with conductive particle, repastes and be layed onto in macropore carbon substrate.Chinese patent 103828105 adds CNT in MPL slurry, prepares the gas diffusion layers that electric conductivity is excellent with gas-premeable.But these preparation methoies are required for using hydrophober, improve the hydrophobicity of conductive powder, and conductive powder is bondd mutually, conventional hydrophober has polytetrafluoroethylene PTFE, segregation tetrafluoroethene, polyvinylidene fluoride, polypropylene, and polytetrafluoroethylene PTFE insoluble in any known solvent and does not have electric conductivity, and the chemical stability of other bonding agents and hydrophobicity are poor, this makes the method preparing diffusion layer become complicated and difficult.The more important thing is, using the gas diffusion layers that conductive powder is prepared from, porosity and average pore size are little, are unfavorable for the transmission of reacting gas and steam.
Summary of the invention
Present invention aim at providing the directly high performance gas diffusion layer of growth in situ and preparation thereof and the application in macropore carbon substrate of a kind of CNT.The gas diffusion layers prepared by the method without additionally adding hydrophober, has from hydrophobicity, good mass transfer and conductive capability, it is possible to improve Proton Exchange Membrane Fuel Cells water logging problem at higher current densities inside gas diffusion layers.
In order to reach this purpose, the technical solution used in the present invention is as follows:
Disclosure one fuel cell carbon nanotube gas diffusion layer,
Described carbon nanotube gas diffusion layer is overlapped by macropore carbon base supporting layer and microporous layers and constitutes；
Wherein, microporous layers is CNT, and CNT thickness is 1-50 μm；
CNT is concentrated and is grown in inside gas diffusion layers, and the inner side of gas diffusion layers is the side near Catalytic Layer.
In gas diffusion layers, CNT side is 130 °～150 ° with the contact angle of water；
Contact angle is the overall contact angle with water of carbon nanotube layer, i.e. the contact angle of diffusion layer inner side plane and water.
Described contact angle is to be added in inside gas diffusion layers by 3-4 μ L deionized water drop, obtains by measuring the relative angle of liquid-solid interface and the formation of liquid-vapor interface tangent line.
Described macropore carbon base supporting layer is charcoal cloth, carbon paper or charcoal felt.
Carbon nanotube gas diffusion layer being placed in temperature and is 60-65 DEG C, when gas flow is 100-150mL/min, the moisture-vapor transmission of gas diffusion layers is 600-1200gh-1m2。
Being clipped in by gas diffusion layers between two pieces of copper billets, copper billet is applied 1-1.5MPa pressure and 5A electric current, measure voltage calculating between two copper billets and obtain contact resistance, when copper billet is applied 1.5MPa pressure, the contact resistance of gas diffusion layers and copper billet is 10-50m Ω cm2。
The preparation method of carbon nanotube gas diffusion layer of the present invention:
A) catalyst precursor is dissolved in ethanol, and both part by weight are 1:10～1:90, the ultrasonic Catalyst precursor solutions being uniformly mixed；
B) Catalyst precursor solutions is uniformly supported on macropore carbon base supporting layer, 40 DEG C～100 DEG C drying, be placed on plasma enhanced chemical vapor deposition (PECVD) system sample platform；
C) by sample room evacuation, when vacuum reaches 0.1Pa～0.5Pa, pass into hydrogen, hydrogen flowing quantity is 10～200mL/min, when pressure reaches 100～1000Pa, starting to warm up under room temperature, heating rate is 10-20 DEG C/min, heating-up time is 10～500min, and being warming up to temperature is 500～800 DEG C；
D), under the premise keeping hydrogen flowing quantity to be 10～200mL/min, apply radio-frequency power 10～200W, hydrogen radio frequency 1～30min, catalyst precursor is reduced to the nano metal accordingly with catalysis activity；
E) hydrogen flowing quantity regulates and is maintained at 10～100mL/min, pass into the hydrocarbon gas that gas flow is 50～500mL/min, pressurize and be maintained at 1000-1500Pa, apply radio-frequency power 100～1000W, the radio frequency time is 10～300min, directly generates CNT on macropore carbon base supporting layer, after deposition process terminates under catalyst with action of plasma, it is cooled to room temperature, obtains the carbon paper of growth in situ carbon nano-fiber；
F) the step e) sample obtained is taken out, to carrying out hydrophobic process outside gas diffusion layers；
Outside described in step f) refers to the side that gas diffusion layers contacts with the flow field of fuel cell；
Described nano metal is catalyst.
Catalyst precursor in step a) is iron content inorganic salt, containing one or more in cobalt inorganic salt, nickeliferous inorganic salt；
In step b), the loading on macropore carbon base supporting layer of the catalyst precursor in Catalyst precursor solutions is 0.1-1mg/cm2；
Nano metal described in step d) is one or more in ferrum, cobalt or nickel；
Hydrocarbon described in step e) is one or more mixture in methane, ethylene, acetylene, propylene, propine.
Catalyst precursor is preferably Ni (NO3)2·6H2O、Co(NO3)2·6H2O or FeCl3In one or more.
Hydrophobic described in step f) processes the aqueous solution containing 1～50wt% hydrophober for configuration, is uniformly brushed outside gas diffusion layers by this solution, and after drying, hydrophober content is 0.1～30wt% of gas diffusion layers after drying；
Wherein hydrophober is one or two or more kinds mixture in politef (PTFE), segregation tetrafluoroethene, polyvinylidene fluoride or polypropylene.
Carbon nanotube gas diffusion layer of the present invention is component film electrode together with the PEM (CCM) having supported catalyst, is applied to fuel cell.
Owing to CNT has strong-hydrophobicity, therefore CNT is concentrated and is had hydrophobicity inside the gas diffusion layers of growth, when adding without hydrophobic binder, contact angle is 130～150 °, this gas diffusion layers need not additionally add water-repelling agent in inner side, it is possible to is provided simultaneously with good hydrophobic, conduction and mass transfer ability.
Gas diffusion layers presents anisotropy, is incremented by vertical gas diffusion layer plane direction carbon nanotube density ecto-entad；On the direction being parallel to gas diffusion layer plane, CNT is uniformly distributed.
Beneficial effects of the present invention
1, carbon nano-fiber directly in-situ preparation in macropore carbon substrate, without additionally adding hydrophober inside gas diffusion layers, have from hydrophobicity, good mass transfer and conductive capability, the output performance under fuel cell high current density can be improved, it is possible to improve Proton Exchange Membrane Fuel Cells water logging problem at higher current densities.
2, the inventive method is simple and easy to control, and product preparation efficiency is high.
Accompanying drawing explanation
Fig. 1 is gas diffusion layers schematic diagram prepared by the present invention, is incremented by vertical gas diffusion layer plane direction carbon nanotube density ecto-entad；On the direction being parallel to gas diffusion layer plane, CNT is uniformly distributed；In figure, 1 is CNT, and 2 is macropore carbon base supporting layer.
Fig. 2 is carbon paper SEM figure before reaction.
Fig. 3 is the carbon nanotube gas diffusion layer prepared under the process conditions of the embodiment of the present invention 1.
Fig. 4 is the embodiment of the present invention 1 (reaction temperature is 800 °) and the comparative example battery performance comparison diagram as the membrane electrode of fuel batter with proton exchange film prepared by cathode gas diffusion layer.Cell operating conditions is: battery temperature: 65 DEG C；Gas degree of wetting: 80%；H2Flow: 100mL/min；O2Flow: 600mL/min.
Fig. 5 is the embodiment of the present invention 2 (reaction temperature is 700 °) and the comparative example battery performance comparison diagram as the membrane electrode of fuel batter with proton exchange film prepared by cathode gas diffusion layer.Cell operating conditions is: battery temperature: 65 DEG C；Gas degree of wetting: 80%；H2Flow: 100mL/min；O2Flow: 600mL/min.
Detailed description of the invention
Embodiment 1
Weigh 12.5mgNi (NO3)2·6H2O crystal is dissolved in ethanol solution, and ultrasonic 15min makes solvent dispersion uniform.
It is 5*5 (cm by area2) carbon paper impregnated in the nickel nitrate alcoholic solution of preparation, after dipping 1min, sample is taken out, puts in 80 DEG C of vacuum drying ovens dried, carry out follow-up dipping, dried, adopt weight method to calculate Ni (NO on carbon paper3)2Content, until Ni (NO3)2Content reaches 40mg.
Sample is put on the sample stage in plasma enhanced chemical vapor deposition stove, after sample room is evacuated to 0.5Pa, pass into H2,Control flow is 80mL/min, and pressure is 200Pa, then with 10 DEG C/min heating rate, is warming up to 800 DEG C, applies radio-frequency power 40W, radio frequency 5min, by Ni (NO3)2It is reduced to the nano metal Ni with catalysis activity.H is regulated after radio frequency2Flow is 20mL/min, passes into CH4Control flow is 80mL/min, and adjustment pressure is 1000Pa, applies radio-frequency power 200W, radio frequency 30min.After deposition terminates, keep H2Flow is 20mL/min, and pressure is 200Pa, is cooled to room temperature, obtains the carbon paper of in-situ growing carbon nano tube, is taken out by the sample obtained, to carrying out hydrophobic process outside gas diffusion layers.The configuration aqueous solution containing 2.5wt% hydrophober, uniformly brushes this solution outside gas diffusion layers, and after drying, hydrophober content is the 5wt% of gas diffusion layers after drying.
Embodiment 2
Weigh 12.5mgNi (NO3)2·6H2O crystal is dissolved in ethanol solution, and ultrasonic 15min makes solvent dispersion uniform.
It is 5*5 (cm by area2) carbon paper impregnated in the nickel nitrate alcoholic solution of preparation, after dipping 1min, carbon paper is taken out, puts in 80 DEG C of vacuum drying ovens dried, carry out follow-up dipping, dried, adopt weight method to calculate Ni (NO on carbon paper3)2Content, until Ni (NO3)2Content reaches 40mg.
Sample is put on the sample stage in plasma enhanced chemical vapor deposition stove, after sample room is evacuated to 0.5Pa, pass into H2,Control flow is 80mL/min, and pressure is 200Pa, then with 10 DEG C/min heating rate, is warming up to 800 DEG C, is incubated 10min, then regulates and cool the temperature to 700 DEG C with 50 DEG C/min rate of temperature fall, and adjustment radio-frequency power is 40W, radio frequency 5min, by Ni (NO3)2It is reduced to the nano metal Ni with catalysis activity.H2H is regulated after radio frequency2Flow is 20mL/min, passes into CH4Control flow is 80mL/min, and adjustment pressure is 1000Pa, applies radio-frequency power 200W, radio frequency 30min.After deposition terminates, keep H2Flow is 20mL/min, and pressure is 200Pa, is cooled to room temperature, obtains the carbon paper of in-situ growing carbon nano tube, is taken out by the sample obtained, to carrying out hydrophobic process outside gas diffusion layers.The configuration aqueous solution containing 2.5wt% hydrophober, uniformly brushes this solution outside gas diffusion layers, and after drying, hydrophober content is the 5wt% of gas diffusion layers after drying.
Comparative example
Carbon paper is immersed in 2.5%PTFE emulsion, takes out after dipping 1min and dry, then carry out redrying, drying, calculate the content of PTFE in carbon paper by weight method, until PTFE content reaches 8%.The carbon paper that PTFE content is 8% is put into 340 DEG C of roasting 30min in nitrogen charging baking oven.
Weighing XC-72 carbon dust 100mg, 8mL dehydrated alcohol, ultrasonic 30min, according to XC-72 carbon dust: the ratio that PTFE is 1:8 adds 5%PTFE emulsion, continues mechanical agitation 5min.
Being fixed in flush coater thermal station by the carbon paper through hydrophobic treatment, heat to thermal station, heating-up temperature is 80 DEG C.Ensure that carbon paper spray area is 10*10cm2, after control spraying, XC-72 carbon dust load amount is 0.5mg/cm2. in being positioned over nitrogen charging baking oven, 340 DEG C of sintering 30min.
Claims (10)
1. a fuel cell carbon nanotube gas diffusion layer, it is characterised in that:
Described carbon nanotube gas diffusion layer is overlapped by macropore carbon base supporting layer and microporous layers and constitutes；
Wherein, microporous layers is CNT, and CNT thickness is 1-50 μm；
CNT is concentrated and is grown in inside gas diffusion layers, and the inner side of gas diffusion layers is the side near Catalytic Layer.
2. the carbon nanotube gas diffusion layer described in claim 1, it is characterised in that:
In gas diffusion layers, CNT side is 130 °～150 ° with the contact angle of water；
Described contact angle is to be added in inside gas diffusion layers by 3-4 μ L deionized water drop, obtains by measuring the relative angle of liquid-solid interface and the formation of liquid-vapor interface tangent line.
3. the carbon nanotube gas diffusion layer described in claim 1, it is characterised in that:
Described macropore carbon base supporting layer is charcoal cloth, carbon paper or charcoal felt.
4. the carbon nanotube gas diffusion layer described in claim 1, it is characterised in that: carbon nanotube gas diffusion layer being placed in temperature and is 60-65 DEG C, when gas flow is 100-150mL/min, the moisture-vapor transmission of gas diffusion layers is 600-1200gh-1m2。
5. the carbon nanotube gas diffusion layer described in claim 1, it is characterized in that: gas diffusion layers is clipped between two pieces of copper billets, copper billet is applied 1-1.5MPa pressure and 5A electric current, measure voltage calculating between two copper billets and obtain contact resistance, when copper billet is applied 1.5MPa pressure, the contact resistance of gas diffusion layers and copper billet is 10-50m Ω cm2。
6. the preparation method of the arbitrary described carbon nanotube gas diffusion layer of claim 1-5, it is characterised in that:
A) catalyst precursor is dissolved in ethanol, and both part by weight are 1:10～1:90, the ultrasonic Catalyst precursor solutions being uniformly mixed；
B) Catalyst precursor solutions is uniformly supported on macropore carbon base supporting layer, 40 DEG C～100 DEG C drying, be placed on plasma enhanced chemical vapor deposition (PECVD) system sample platform；
C) by sample room evacuation, when vacuum reaches 0.1Pa～0.5Pa, pass into hydrogen, hydrogen flowing quantity is 10～200mL/min, when pressure reaches 100～1000Pa, starting to warm up under room temperature, heating rate is 10-20 DEG C/min, heating-up time is 10～500min, and being warming up to temperature is 500～800 DEG C；
D), under the premise keeping hydrogen flowing quantity to be 10～200mL/min, apply radio-frequency power 10～200W, hydrogen radio frequency 1～30min, catalyst precursor is reduced to the nano metal accordingly with catalysis activity；
E) hydrogen flowing quantity regulates and is maintained at 10～100mL/min, pass into the hydrocarbon gas that gas flow is 50～500mL/min, pressurize and be maintained at 1000-1500Pa, apply radio-frequency power 100～1000W, the radio frequency time is 10～300min, directly generates CNT on macropore carbon base supporting layer, after deposition process terminates under catalyst with action of plasma, it is cooled to room temperature, obtains the carbon paper of growth in situ carbon nano-fiber；
F) the step e) sample obtained is taken out, to carrying out hydrophobic process outside gas diffusion layers；
Outside described in step f) refers to the side that gas diffusion layers contacts with the flow field of fuel cell；
Described nano metal is catalyst.
7. the preparation method of the carbon nanotube gas diffusion layer described in claim 6, it is characterised in that:
Catalyst precursor in step a) is iron content inorganic salt, containing one or more in cobalt inorganic salt, nickeliferous inorganic salt；
In step b), the loading on macropore carbon base supporting layer of the catalyst precursor in Catalyst precursor solutions is 0.1-1mg/cm2；
Nano metal described in step d) is one or more in ferrum, cobalt or nickel；
Hydrocarbon described in step e) is one or more mixture in methane, ethylene, acetylene, propylene, propine.
8. the preparation method of the carbon nanotube gas diffusion layer described in claim 7, it is characterised in that: catalyst precursor is preferably Ni (NO3)2·6H2O、Co(NO3)2·6H2O or FeCl3In one or more.
9. the preparation method of the carbon nanotube gas diffusion layer described in claim 6, it is characterized in that: the hydrophobic described in step f) processes the aqueous solution containing 1～50wt% hydrophober for configuration, uniformly being brushed outside gas diffusion layers by this solution, after drying, hydrophober content is 0.1～30wt% of gas diffusion layers after drying；
Wherein hydrophober is one or two or more kinds mixture in politef (PTFE), segregation tetrafluoroethene, polyvinylidene fluoride or polypropylene.
10. according to the application of either carbon nanotube gas diffusion layers in claim 1-5, it is characterised in that: described carbon nanotube gas diffusion layer is component film electrode together with the PEM (CCM) having supported catalyst, for fuel cell.
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Cited By (6)
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| CN109921075A (en) * | 2017-12-13 | 2019-06-21 | 中国科学院大连化学物理研究所 | The preparation and its application of ordering gas-diffusion electrode based on nano-tube array |
| CN110890552A (en) * | 2018-09-07 | 2020-03-17 | 赛高创新株式会社 | Method for producing battery electrode, and battery electrode |
| CN111628181A (en) * | 2020-05-25 | 2020-09-04 | 常熟氢能源研究院有限公司 | Process for preparing gas diffusion layer for fuel cell by using wood as raw material |
| CN114824272A (en) * | 2022-04-14 | 2022-07-29 | 广东氢发新材料科技有限公司 | Carbon nanofiber/carbon black composite microporous layer and preparation method thereof |
| CN115000446A (en) * | 2022-07-22 | 2022-09-02 | 上海电气集团股份有限公司 | Gas diffusion layer, preparation method thereof, membrane electrode, cell and application |
| CN117673379A (en) * | 2024-01-30 | 2024-03-08 | 江苏源氢新能源科技股份有限公司 | Preparation method of spinning type CNT (carbon nanotube) diffusion layer and preparation method of membrane electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109921075A (en) * | 2017-12-13 | 2019-06-21 | 中国科学院大连化学物理研究所 | The preparation and its application of ordering gas-diffusion electrode based on nano-tube array |
| CN109921075B (en) * | 2017-12-13 | 2021-07-06 | 中国科学院大连化学物理研究所 | Preparation and application of ordered gas diffusion electrode based on nanotube array |
| CN110890552A (en) * | 2018-09-07 | 2020-03-17 | 赛高创新株式会社 | Method for producing battery electrode, and battery electrode |
| CN111628181A (en) * | 2020-05-25 | 2020-09-04 | 常熟氢能源研究院有限公司 | Process for preparing gas diffusion layer for fuel cell by using wood as raw material |
| CN111628181B (en) * | 2020-05-25 | 2021-07-23 | 常熟氢能源研究院有限公司 | Process for preparing gas diffusion layer for fuel cell by using wood as raw material |
| CN114824272A (en) * | 2022-04-14 | 2022-07-29 | 广东氢发新材料科技有限公司 | Carbon nanofiber/carbon black composite microporous layer and preparation method thereof |
| CN115000446A (en) * | 2022-07-22 | 2022-09-02 | 上海电气集团股份有限公司 | Gas diffusion layer, preparation method thereof, membrane electrode, cell and application |
| CN117673379A (en) * | 2024-01-30 | 2024-03-08 | 江苏源氢新能源科技股份有限公司 | Preparation method of spinning type CNT (carbon nanotube) diffusion layer and preparation method of membrane electrode |
| CN117673379B (en) * | 2024-01-30 | 2024-04-12 | 江苏源氢新能源科技股份有限公司 | Preparation method of spinning type CNT (carbon nanotube) diffusion layer and preparation method of membrane electrode |
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