CN100456538C - Preparation method of carbon paper or carbon cloth for fuel cell gas diffusion layer - Google Patents
Preparation method of carbon paper or carbon cloth for fuel cell gas diffusion layer Download PDFInfo
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Abstract
燃料电池气体扩散层的制备方法，将碳黑粉末、蒸馏水、分散剂按照以下比例混合均匀，分散剂的量占碳黑的5-30wt%，碳黑粉末的量为整个体系的1-20wt%；碳黑的颗粒为30-1000nm；将10-60%浓度的PTFE或PVDF乳液均匀加入上述所述的碳黑粉末分散体系中，并继续混合0.5-3小时；混合方法采用超声波、机械高速剪切或机械搅拌；体系中PTFE或PVDF的含量为碳黑的10-50wt%；将碳纸或碳布放入上述的分散体系中浸渍0.5-15min，取出晾干，并放入干燥箱在45-150℃烘干5-60min，得到载有碳黑和PTFE或PVDF的碳纸或碳布。The preparation method of the gas diffusion layer of the fuel cell is to mix the carbon black powder, distilled water and dispersant uniformly according to the following ratio, the amount of the dispersant accounts for 5-30wt% of the carbon black, and the amount of the carbon black powder is 1-20wt% of the whole system The particle size of carbon black is 30-1000nm; PTFE or PVDF emulsion with a concentration of 10-60% is uniformly added to the above-mentioned carbon black powder dispersion system, and continues to mix for 0.5-3 hours; the mixing method adopts ultrasonic, mechanical high-speed shear Cut or stir mechanically; the content of PTFE or PVDF in the system is 10-50wt% of carbon black; put carbon paper or carbon cloth into the above dispersion system and soak for 0.5-15min, take it out to dry, and put it in a drying box at 45 Dry at -150°C for 5-60 minutes to obtain carbon paper or carbon cloth loaded with carbon black and PTFE or PVDF.
Description
Technical field
The present invention relates to the preparation of fuel cell component, especially a kind of preparation method of fuel battery gas diffusion layer.
Background technology
The PEMFC electrode is a kind of gas-diffusion electrode of porous in the Proton Exchange Membrane Fuel Cells, generally is made up of diffusion layer and catalyst layer.Different diffusion layer materials has very big influence for structure, manufacture craft and the performance of electrode.
Fuel gas arrives catalyst layer through anode diffusion layer in Proton Exchange Membrane Fuel Cells, under the effect of catalyst electrode reaction takes place, promptly
H
2-2H+2e
The electronics that this electrode reaction produces arrives negative electrode by the conduction flow of diffusion layer through external circuit, and hydrogen ion arrives negative electrode under the effect of proton exchange membrane simultaneously.Oxygen generates water by with hydrogen ion and electronics electrode reaction taking place under catalyst action behind the cathode diffusion layer, that is:
1/2?O
2+2H+2e-H
2O
There is (temperature and pressure that depends on battery) in water in the Proton Exchange Membrane Fuel Cells (PEMFC) with gaseous state and liquid state, dilutional hyponatremia or very few performance to PEMFC all can be brought negative effect, see [1] Ersoz A, Olgun H, Ozdogan S.etal., J.Power Sources.2003,118 (1-2): 384-392.
Gas diffusion layers not only plays a part support catalyst layer, stabilized electrodes structure in electrode, also possesses the multiple function that gas passage, electron channel and drainage channel are provided for electrode reaction, see [2] JAMESL, ANDREW D.Fuel cellsystems explained[M] .England:John Wiley﹠amp; Sons Ltd., 2000.66-69.[3] Huang Naike, Wang Shuzhong, power technology, 2003,27 (3): 329-332.Select for use high performance gas diffusion layer material to help improving the combination property of electrode.Desirable diffusion layer should possess 3 characteristics: air permeability and good, good drainage and good electrical conductivity.General gas diffusion layers is made up of base material and transition zone.In multiple base material, the charcoal fibrous paper [is seen 4 Thomas T O, Glendale, Hiroshi I, et al., US:3 829 327,1974.[5] TeruakiKitago, Tadaaki Yoshida, US:3998689,1976.] have uniform porous matter laminate structure and excellent conductivity, chemical stability and thermal stability, be the diffusion layer material that is most widely used in the fuel cell.
[7]Transition zone is known as the intermediate layer again, and its adding has realized reacting gas and the reallocation of product one water between flow field and Catalytic Layer, for strengthening conductivity, improves electrode performance, battery operation stability and service life and has played important function.
People such as L.R.Jordan [see L R JORDAN, SHUKLA A K, BEHRSING T, et al., J.PowerSources, 2000,86:250-254] powdered carbon is mixed with the polytetrafluoroethylene (PTFE) emulsion, add an amount of solvent, utilize ultrasonic wave that it is uniformly dispersed, it is sprayed on the positive and negative surface of base material equably, the oven dry back is in 300～350 ℃ of about 30min of following sintering, make the PTFE fusion remove surfactant simultaneously, obtain hydrophobic material at last by PTFE bonding charcoal and basilar fibers.The powdered carbon that adds plays the effect that strengthens conductivity on the one hand, is used for filling the macropore between the fiber in the base material on the other hand, makes surfacing and even aperture distribution.The mass ratio of PTFE and carbon black was good between 20: 80 and 50: 50 in the coating liquid, and coating layer thickness is between 0.010～0.254mm, and the content of PTFE is 10%～50%.In the research of PEMFC diffusion layer, people such as Xu Hongfeng, Tian Ying are coated with the mixture of one deck XC one 72R charcoal and polytetrafluoroethylene (PTFE) as regulating course on the carbon paper of crossing through hydrophobic treatment.Shao Zhigang, clothing treasured are honest and clean, Han Ming etc. (electrochemistry, 2000,6 (3): 317-323.) with water or ethanol as solvent, it is 1: 1 solution that carbon black and PTFE are made into mass ratio, mixes the back as regulating course.People [LIM C.WANG C Y., Electrochimica Acta, 2004,49 (24): 4149-4156] such as Chan Lim. studied the influence of PTFE content and thickness of diffusion layer.People such as Giorgi [JORDAN LR, SHUKLA A K, BEHRSING T., Journal of Power Sources.2000.86:250-254.] think the porosity of diffusion layer that increased in the diffusion layer PTFE content influence.People [KONG C S, KIM D Y, LEE H K, et al., Journal of Power Sources, 2002,108:185-191.] such as face gift L.R.Jordan think that the oarse-grained acetylene black of use replaces Vulcan XC 72 R charcoals can improve the performance of battery.People such as Chang Sun Kong add pore creating material and improve mass transfer problem in the battery in the PEMFC diffusion layer.
The M.Watanabe[WATANABE M. of Japan, US:5137754,1992.] etc. the people invented a kind of new hydrophobic processing method, with mean molecule quantity is that 250 000 polyethylene is dissolved in the heptane, be made into a kind of film forming solution, with base material, immerse wherein as the charcoal fibrous paper, treat that heptane volatilization back formation mass fraction on carbon paper is 5% PE coating, then this carbon paper with polyethylene coating is put into stainless steel reactor, at room temperature condition, contain in the fluorine gas atmosphere of 10% argon gas and fluoridize about 30min, the hydrophobic material of obtained performance excellence.The hydrophobicity performance of relatively finding the hydrophobic material that makes than the method for flooding with the PTFE emulsion with this hydrophobic processing method by experiment is better.
After base material made charcoal/PTFE coating, find that aperture does not wherein have hydrophobicity, because those apertures of PTFE molecular proportion are big 10～100 times.Thereby when the spraying noble metal catalyst, can find the phenomenon of osmosis of noble metal, cause the reduction of catalyst utilization, therefore need further make hydrophobic and handle those apertures.V.K.KARL[KARL V K., US:3899354,1975.] use the benzinum weak solution of 1.5% paraffin wax to handle to the carbon paper after the coating, baking 30min under 50 ℃ can make the aperture in the coating possess effective hydrophobicity again.Perhaps use the acetone soln of 2.0% cellulose acetate to handle, also can obtain good aperture hydrophobic effect.
Another kind of hydrophobic processing method by the invention of research institute of Japanese Toyota is base material to be exposed to a kind of in plasma treated charcoal fluorine compound gas, makes surface deposition one deck hydrophobic material.Yet this method need design main equipment especially, is not suitable for large-scale production.Above the whole bag of tricks technical process more complicated, base material all will be passed through the secondary high temperature sintering, and making the diffuse layer structure instability has also increased production cost.
Summary of the invention
The objective of the invention is: the preparation method who proposes a kind of fuel battery gas diffusion layer, by designing the particularly diffusion layer of Proton Exchange Membrane Fuel Cells of a kind of easy fuel cell, make diffuse layer structure more stable, pore-size distribution is more even, processing cost reduces greatly, has air permeability and good, good drainage and good electrical conductivity simultaneously; Be fit to the large-scale production of fuel cell, thereby reduce the cost of fuel cell product.
Particular content of the present invention is as follows:
The preparation method of fuel battery gas diffusion layer, carbon black powders, distilled water, dispersant is even according to following mixed, and the amount of carbon black powders is the 1-0wt% of whole system, the amount of dispersant accounts for the 5-30wt% of carbon black; The particle of carbon black is 30-1000nm.The PTFE or the PVDF emulsion of 10-60% concentration are evenly added in the above-mentioned described carbon black powders dispersion, and continue to mix 0.5-3 hour; Mixed method adopts ultrasonic wave, mechanical high-speed to shear or mechanical agitation; The content of PTFE or PVDF is the 10-50wt% of carbon black in the system; Carbon paper or carbon cloth are put into above-mentioned dispersion flood 0.5-15min, taking-up is dried, and puts into drying box at 45-150 ℃ of oven dry 5-60min, obtains being loaded with carbon paper or the carbon cloth of carbon black and PTFE or PVDF.
Dipping can divide and carries out for 1 to 5 time, after each dipping with carbon paper or carbon cloth 45-150 ℃ of temperature under dry 5-60min.
Above-mentioned carbon paper or carbon cloth are at 150-390 ℃ of sintering 20-60min; The sintering mode of heating adopts baking oven, tube furnace or infrared heating mode.
Described carbon black powders comprises acetylene black, active carbon black etc., and dispersant is XH-1, AEO-9, FC4430, Tween-60 or Triton X-100.The carbon paper of above-mentioned processing or carbon cloth are used for the diffusion layer of the male or female of fuel cell; The aperture of diffusion layer is the 0.5-10 micron, and contact angle is the 110-160 degree.
The organic solution of perhaps directly carbon paper or carbon cloth being put into PVDF or PVDF-HFP copolymer is flooded 0.5-15min, and the content of HFP is 10-50wt% in the copolymer.Taking-up is dried, and at 150-250 ℃ of sintering 20-60min.Sintering process can the electricity consumption heated oven, tubular type road etc. or other heating means such as infrared heating etc.
Described carbon paper or carbon cloth are used for the diffusion layer of the male or female of fuel cell, and the aperture of diffusion layer is the 0.5-10 micron, and contact angle is the 110-160 degree.
The preparation method of fuel battery gas diffusion layer of the present invention, the diffusion layer of design Proton Exchange Membrane Fuel Cells, make diffuse layer structure more stable, pore-size distribution is more even, processing cost reduces greatly, have air permeability and good, good drainage and good electrical conductivity simultaneously, also reduce the cost of fuel cell product.
Embodiment
Carbon black powders adopts acetylene black, active carbon black etc., and distilled water, dispersant adopt XH-1, AEO-9, FC4430, Tween-60, Triton X-100 etc., and even according to certain mixed, the amount of dispersant accounts for the 5-30wt% of carbon black.Mixed method comprises ultrasonic wave, high speed shear, mechanical agitation etc.The particle of guaranteeing carbon black is 30-1000nm.The amount of carbon black powders is the 1-20wt% of whole system.
PTFE or PVDF emulsion are evenly added in the above-mentioned dispersion, and continue to mix 0.5-3 hour.Mixed method comprises ultrasonic wave, high speed shear, mechanical agitation etc.The content of PTFE or PVDF is the 10-50wt% of carbon black in the system.Carbon paper or carbon cloth are put into above-mentioned dispersion flood 0.5-15min, taking-up is dried, and puts into drying box 50-150 ℃ of oven dry, obtains being loaded with carbon paper or the carbon cloth of carbon black and PTFE or PVDF.Dipping can divide 1 time or repeatedly carry out, and after each dipping carbon paper or carbon cloth is dried at a certain temperature.Above-mentioned carbon paper or carbon cloth are put into baking oven, at 50-390 ℃ of sintering 20-60min.Sintering process can be used baking oven, tube furnace or other heating means such as infrared heating etc.Acetylene black powder (perhaps active carbon such as Vulcan XC-72) is dispersed in (solid content is 1-20wt%) in the deionized water, and in dispersion, add certain amount of dispersant, as XH-1, AEO-9, FC4430, Tween-60, TritonX-100 etc., the amount of dispersant accounts for the 5-30wt% of carbon black.Obtain finely dispersed slurry.Slurry in, add the PTFE emulsion, the content of emulsion is the 10-50wt% of carbon black.And continue to stir 0.5-2 hour.
Carbon paper or carbon cloth (Tory or other model) are put into described slurry flood 0.5-15min, taking-up is dried, and puts into drying box 50-150 ℃ of oven dry, obtains being loaded with carbon paper or the carbon cloth of carbon black and PTFE.
Again carbon paper or carbon cloth are put into above-mentioned slurry, repeat above-mentioned steps.And finally to obtain the carbon black carrying capacity be 0.5-3mg/cm
2Carbon paper or carbon cloth.Carbon paper or carbon cloth are put into baking oven, at 300-390 ℃ of sintering 20-60min.Above-mentioned carbon paper or carbon cloth are applied in the fuel cell as diffusion layer, play support catalyst layer, transmission reaction medium and effects such as product, collected current.
Embodiment 1
Take by weighing 5-40g acetylene black powder or other carbon black with the 200ml beaker,,, powder is stirred into the dough shape with glass rod as XH-1, AEO-9, FC4430, Tween-60, Triton X-100 etc. to wherein adding certain density dispersant.In the 2500ml beaker, adding 200-500ml concentration is the above-mentioned dispersant of 0.5-10%, adds a certain amount of distilled water again.Use the high-shear emulsion machine agitating solution, and divide doughy carbon black 10 times every 2min to add in the above-mentioned beaker.After all adding, continue to shear 30min.Dispersion liquid in the beaker is divided in two stainless steel cups (14cm), and puts into ultrasonic disperser, guarantee water in the tank with not ing to stainless steel cup half highly.Ultrasonic stirring 1.0 hours.The mixed liquor that in above-mentioned slurry, adds PTFE (5-60ml, 60%) and a certain amount of distilled water gradually, and continue to stir 0.5 hour.Slurry in 2 stainless steel cups is mixed, separate in two cups again, and continue to stir 0.5 hour.Scattered acetylene black slurry is poured in the handtailor container, guaranteed that the slurry liquid level is more than the 2cm in the container.Carbon paper or carbon cloth are cut into 200 * 200mm size, keep flat and flood 1-10min in the slurry, take out, just putting 0.5min on filter paper, horizontal is placed on the stainless steel frame then, and puts into drying box in 50-150 ℃ of oven dry (about 5min).This carbon paper or carbon cloth are kept flat into slurry dipping 1-10min again, take out, be inverted 0.5min on filter paper, horizontal is placed on the stainless steel frame then, and puts into drying box in 50-150 ℃ of oven dry (about 5min).This carbon paper or carbon cloth are kept flat into slurry dipping 1-10min again, take out, just putting 0.5min on filter paper, horizontal is placed on the stainless steel frame then, and puts into drying box in 105 ℃ of oven dry (about 5min).This carbon paper or carbon cloth are kept flat into slurry dipping 1min again, take out, be inverted 0.5min on filter paper, horizontal is placed on the stainless steel frame then, and puts into drying box in 150 ℃ of oven dry (about 5min).Carbon paper or carbon cloth flood 4-40min altogether, and the appendix amount is 1-10mg/cm after the oven dry
2Face up one when guaranteeing the oven dry of each horizontal, catalyst will be near at this simultaneously.At last, carbon paper is put into baking oven, at 300-400 ℃ of sintering 20-60min.Last carbon black appendix amount is 0.5-3.5mg/cm
2The aperture of carbon paper is the 0.5-10 micron, and contact angle is the 110-160 degree.
Embodiment 2
Take by weighing 5-40g acetylene black powder or other carbon black with the 200ml beaker,,, powder is stirred into the dough shape with glass rod as XH-1, AEO-9, FC4430, Tween-60, Triton X-100 etc. to wherein adding certain density dispersant.In the 2500ml beaker, adding 200-500ml concentration is the above-mentioned dispersant of 0.5-10%, adds a certain amount of distilled water again.Use the high-shear emulsion machine agitating solution, and divide doughy carbon black 10 times every 2min to add in the above-mentioned beaker.After all adding, continue to shear 30min.Dispersion liquid in the beaker is divided in two stainless steel cups (14cm), and puts into ultrasonic disperser, guarantee water in the tank with not ing to stainless steel cup half highly.Ultrasonic stirring 1.0 hours.Carbon paper or carbon cloth are cut into 200 * 200mm size, keep flat and flood 1-10min in the slurry, take out, just putting 0.5min on filter paper, horizontal is placed on the stainless steel frame then, and puts into drying box in 50-150 ℃ of oven dry (about 5min).This carbon paper or carbon cloth are kept flat into slurry dipping 1-10min again, take out, be inverted 0.5min on filter paper, horizontal is placed on the stainless steel frame then, and puts into drying box in 50-150 ℃ of oven dry (about 5min).This carbon paper or carbon cloth are kept flat into slurry dipping 1-10min again, take out, just putting 0.5min on filter paper, horizontal is placed on the stainless steel frame then, and puts into drying box in 105 ℃ of oven dry (about 5min).This carbon paper or carbon cloth are kept flat into slurry dipping 1min again, take out, be inverted 0.5min on filter paper, horizontal is placed on the stainless steel frame then, and puts into drying box in 150 ℃ of oven dry (about 5min).Carbon paper or carbon cloth flood 4-40min altogether, and the appendix amount is 1-10mg/cm after the oven dry
2Face up one when guaranteeing the oven dry of each horizontal, catalyst will be near at this simultaneously.With this carbon paper or carbon cloth PVDF solution impregnation 1-10min with 10-30wt%, put into distilled water number minute after the taking-up immediately, take out then and put into baking oven, at 100-250 ℃ of sintering 20-60min.Last carbon black appendix amount is 0.5-3.5mg/cm
2
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| CN101435174B (en) * | 2007-11-14 | 2010-12-22 | 上海河森电气有限公司 | Method for making high performance carbon paper special for fuel cell |
| CN101540405A (en) * | 2008-01-25 | 2009-09-23 | 汉能科技有限公司 | Fuel cell leveling layer composition and preparation method thereof as well as gas diffusion layer |
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| CN102544523A (en) * | 2012-01-13 | 2012-07-04 | 中国东方电气集团有限公司 | Electrode material as well as preparation method thereof and flow battery containing same |
| CN102593470A (en) * | 2012-03-01 | 2012-07-18 | 华东理工大学 | Device and method for preparing diffusion layer slurry of proton exchange membrane fuel cell |
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| CN104716337B (en) * | 2013-12-13 | 2017-05-17 | 中国科学院大连化学物理研究所 | Production method of gas diffusion layer for proton exchange membrane fuel cell |
| KR102687872B1 (en) * | 2015-12-24 | 2024-07-25 | 도레이 카부시키가이샤 | gas diffusion electrode |
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| CN110311142A (en) * | 2019-06-20 | 2019-10-08 | 一汽解放汽车有限公司 | A kind of fuel battery gas diffusion layer and preparation method thereof |
| CN111193040B (en) * | 2020-01-09 | 2022-09-20 | 上海电气集团股份有限公司 | Fuel cell gas diffusion layer, preparation method thereof and fuel cell |
| CN112159996A (en) * | 2020-08-27 | 2021-01-01 | 山东星辉航空液压机械有限公司 | One-step forming process for producing high corrosion-resistant crack-free multilayer nanocrystalline hard chromium plating layer |
| CN112563516B (en) * | 2020-12-28 | 2023-03-28 | 浙江唐锋能源科技有限公司 | Gas diffusion layer of environment-friendly fuel cell and preparation method thereof |
| CN113948716A (en) * | 2021-10-14 | 2022-01-18 | 一汽解放汽车有限公司 | Fuel cell gas diffusion layer and preparation method and application thereof |
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