CN1884689A - A porous carbon fiber paper for fuel cell with proton exchange membrane and preparation method thereof - Google Patents
A porous carbon fiber paper for fuel cell with proton exchange membrane and preparation method thereof Download PDFInfo
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- CN1884689A CN1884689A CN 200610052320 CN200610052320A CN1884689A CN 1884689 A CN1884689 A CN 1884689A CN 200610052320 CN200610052320 CN 200610052320 CN 200610052320 A CN200610052320 A CN 200610052320A CN 1884689 A CN1884689 A CN 1884689A
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Abstract
The invention discloses an electrode material and preparing material, which consists of chopped carbon fiber and heat cohesion fiber at 20-70:80-30 weight rate. The invention reduces manufacturing cost, which makes porous carbon fiber with even distributing porthole, high permeating degree, good strength and low resistance rate.
Description
Technical field
The present invention relates to a kind of electrode material and preparation method thereof, relate in particular to porous carbon fiber paper of a kind of used in proton exchange membrane fuel cell and preparation method thereof.
Background technology
Proton Exchange Membrane Fuel Cells is a kind of device that hydrogen and airborne oxygen is combined to clean water and discharges electric energy, is a kind of noiselessness, pollution-free, the life-span is long, specific power is big, energy efficiency is high clean energy resource.Proton exchange membrane fuel cell electrode is made up of gas diffusion layers and catalyst layer.At present, diffusion layer material adopts porous carbon fiber paper or carbon cloth mostly, and it plays the support catalyst layer, the effect of stabilized electrodes structure and for electrode reaction provides gas passage, electron channel and drainage channel.
The manufacture method of porous carbon fiber paper was to be raw material with chopped carbon fiber in the past, and after adding polyvinyl alcohol, vinyl acetate etc. and copying into paper as binding agent, but the dipping carbonized resin forms through hot pressing and high temperature carbonization.Complex technical process, resin inhomogeneous or excessively also can cause making shortcomings such as the uneven and air permeability of carbon fiber paper pore size distribution is low.
Summary of the invention
The object of the present invention is to provide that a kind of preparation technology is simple, cost is low, pore structure is evenly distributed, have porous carbon fiber paper than the used in proton exchange membrane fuel cell of highly-breathable and satisfactory electrical conductivity and preparation method thereof.
In order to achieve the above object, the present invention adopts following technical scheme:
A kind of porous carbon fiber paper of used in proton exchange membrane fuel cell, its raw material comprises chopped carbon fiber and hot adhesion fiber, the weight ratio of described chopped carbon fiber and hot adhesion fiber is 20～70: 80～30, is preferably 30～60: 70～40, more preferably 35～55: 65～45.
Described chopped carbon fiber is one of polypropylene cyano group carbon fiber, asphalt base carbon fiber, viscose-based carbon fiber or its composition.
But described hot adhesion fiber is the charing staple fibre with hot adhesion performance, is specially polyacrylonitrile fibre, pitch fibers or polyimide fiber.
Described chopped carbon fiber diameter is 6～20 μ m, and average length is 3～10mm, is preferably diameter 7～12 μ m, and average length is 4～6mm;
Described hot adhesion fibre diameter is 8～20um, and average length is 2～10mm, and being preferably diameter is 10～15um, and average length is 3～6mm.
The preparation method of above-mentioned porous carbon fiber paper comprises following processing step:
A. add weight percentage in the chopped carbon fiber and be 0.2～1.0% aqueous dispersant, be preferably 0.5～0.8%, be uniformly dispersed through high-speed stirred, make the chopped carbon fiber slurries, described dispersant is a methylcellulose, hydroxyethylcellulose is received or carboxymethyl cellulose;
B. after the hot adhesion fiber stirs in water and is uniformly dispersed, join in the chopped carbon fiber slurries, add the binding agent of total weight of fiber 8～20%, be preferably 10～15%, mix and make the papermaking mixed serum, described binding agent poly-vinyl alcohol solution, vinyl acetate fiber or polyvinyl alcohol staple fibre;
C. adopt conventional wet papermaking process to copy paper, and dry under 80～120 ℃ of temperature, be preferably 80～95 ℃;
D. the paper that will copy hot pressing 0.3～1.5 minute under 220～280 ℃, the pressure of 0.6～1.5MPa obtains the intermediate products of surfacing, is preferably under 240～260 ℃, the pressure of 1.0～1.5MPa hot pressing 0.5～1.0 minute;
E. with above-mentioned intermediate products under 1500～2500 ℃ temperature and charing 0.3～2.0 hour in the inert atmosphere, make porous carbon fiber paper, be preferably under 1800～2400 ℃ temperature charing 0.5～1.5 hour, charing 0.8～1.0 hour under 2000～2200 ℃ temperature more preferably;
As mentioned above, owing in porous carbon fiber paper preparation method of the present invention, adopted the hot adhesion fiber as one of main raw material, this hot adhesion fiber had both played the bonded carbon fiber after the moulding of carbon fiber paper and charing, it self again can be by charing simultaneously, and has good electrical conductivity and this hot sticky glue fiber can evenly disperse at aqueous phase, guaranteed its even distribution in carbon fiber paper, make the carbon fiber paper pore size distribution even, the air permeability height, overcome conventional method and prepared the pore size distribution inequality that carbon fiber paper causes owing to the inhomogeneities of resin impregnation, the shortcoming that air permeability is relatively poor, and simplified manufacturing technique, reduced manufacturing cost.
The specific embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
As the porous carbon fiber paper of fuel battery gas diffusion layer material, its resistivity and porosity are its main performance indications.Resistivity is low can to make the internal resistance of battery component reduce, and the hole is even and porosity is high, and fuel gas is evenly passed through dispersedly.Based on such design, the porous carbon fiber paper that is used for gas diffusing layer of fuel cell electrode provided by the invention except that selecting chopped carbon fiber for use, but has also adopted the charing staple fibre with hot adhesion performance.
For chopped carbon fiber is evenly disperseed at aqueous phase, the selection of its fibre length is very important, otherwise will be difficult to reach desirable dispersion effect, studies show that chopped carbon fiber is in 3～10mm scope, interpolation concentration is 0.2～1.0% dispersant, and adopt high-speed mixing equipment can reach desirable dispersion effect, the hot adhesion fiber fully mixes with the chopped carbon fiber slurries copies paper, can guarantee the carbon fiber paper even pore distribution that makes, has guaranteed the even diffusion of gas.
Below, be several instantiation of the present invention, described proportioning raw materials all refers to parts by weight.
Embodiment 1: with the diameter 6 μ m that select, 20 parts on the polypropylene cyano group carbon fiber of average fiber length 10mm joins concentration and is in 0.2% the carboxymethyl cellulose aqueous solution, adopts homogenizer that it is disperseed.Other is cut-off footpath 8 μ m, 80 parts of the polypropylene cyanogen fibers of average fiber length 10mm, pour the chopped carbon fiber slurries into after putting into the water dispersed with stirring, add after 40 parts of 5% concentration poly-vinyl alcohol solutions mix, copy paper also with 80 ℃ of heated-air dryings with wet papermaking process, make its hot pressing 1.5 minutes under the pressure of 220 ℃ of temperature 0.6Mpa with hot press, obtain intermediate products.
With the charing 2 hours under argon shield and 1500 ℃ of temperature of above-mentioned intermediate products, make porous carbon fiber paper.The thickness 0.25mm of this paper, density 0.37g/cm
3Area weight: 92.5g/m
2, air permeability 298L/m
2S, resistivity 0.029 Ω cm.
Example 2: with the diameter 7 μ m that select, 42 parts of the asphalt base carbon fibers of average fiber length 4mm join concentration and are in 0.5% the methylated cellulose aqueous solution, adopt homogenizer that it is disperseed.Other is cut-off footpath 10 μ m, 58 parts of the polyimide fibers of average fiber length 4mm, pour the chopped carbon fiber slurries into after putting into the water dispersed with stirring, add after 50 parts of 5% concentration poly-vinyl alcohol solutions mix, copy paper also with 90 ℃ of heated-air dryings with wet papermaking process, make its hot pressing 1.0 minutes under the pressure of 250 ℃ of temperature 1.0Mpa with hot press, obtain intermediate products.
With the charing 1.3 hours under argon shield and 2000 ℃ of temperature of above-mentioned intermediate products, make porous carbon fiber paper.The thickness 0.19mm of this paper, density 0.42g/cm
3Area weight: 79.8g/m
2, air permeability 309L/m
2S, resistivity 0.016 Ω cm.
Example 3: with the diameter 12 μ m that select, 39 parts of the viscose-based carbon fibers of average fiber length 6mm join concentration and are 0.8% hydroxyethylcellulose and receive in the aqueous solution, adopt homogenizer that it is disperseed.Other is cut-off footpath 15 μ m, 61 parts of the pitch fibers of average fiber length 6mm, pour the chopped carbon fiber slurries into after putting into the water dispersed with stirring, add 15 parts on polyvinyl alcohol staple fibre, after mixing, copy paper and with 95 ℃ of heated-air dryings with wet papermaking process, make its hot pressing 1.0 minutes under the pressure of 260 ℃ of temperature 1.0Mpa, obtain intermediate products with hot press.
With the charing 1 hour under argon shield and 2200 ℃ of temperature of above-mentioned intermediate products, make porous carbon fiber paper.The thickness 0.20mm of this paper, density 0.42g/cm
3Area weight: 84.0g/m
2, air permeability 339L/m
2S, resistivity 0.019 Ω cm.
Embodiment 4: with the diameter 13 μ m that select, 45 parts on the polypropylene cyano group carbon fiber of average fiber length 7mm joins concentration and is in 0.6% the carboxymethyl cellulose aqueous solution, adopts homogenizer that it is disperseed.Other is cut-off footpath 12 μ m, 55 parts of the polypropylene cyanogen fibers of average fiber length 5mm, pour chopped carbon fiber dispersion slurries into after putting into the water dispersed with stirring, add after 14 parts on polyvinyl alcohol staple fibre mixes, copy paper also with 90 ℃ of heated-air dryings with wet papermaking process, make its hot pressing 0.8 minute under the pressure of 250 ℃ of temperature 1.2Mpa with hot press, obtain intermediate products.
With the charing 0.9 hour under argon shield and 2100 ℃ of temperature of above-mentioned intermediate products, make porous carbon fiber paper.The thickness 0.22mm of this paper, density 0.40g/cm
3Area weight: 88.0g/m
2, air permeability 286L/m
2S, resistivity 0.015 Ω cm.
Embodiment 5: with the diameter 20 μ m that select, 70 parts on the polypropylene cyano group carbon fiber of average fiber length 3mm joins concentration and is 1.0% hydroxyethylcellulose and receives in the aqueous solution, adopts homogenizer that it is disperseed.Other is cut-off footpath 15 μ m, 30 parts of the pitch fibers of average fiber length 7mm, pour chopped carbon fiber dispersion slurries into after putting into the water dispersed with stirring, add after 12 parts of vinyl acetates mix, copy paper also with 120 ℃ of heated-air dryings with wet papermaking process, make its hot pressing 0.3 minute under the pressure of 280 ℃ of temperature 1.5Mpa with hot press, obtain intermediate products.
With the charing 0.3 hour under argon shield and 2500 ℃ of temperature of above-mentioned intermediate products, make porous carbon fiber paper.The thickness 0.21mm of this paper, density 0.40g/cm
3Area weight: 84.0g/m
2, air permeability 341L/m
2S, resistivity 0.013 Ω cm.
Embodiment 6: with the diameter 15 μ m that select, totally 55 parts of the polypropylene cyano group carbon fiber of average fiber length 8mm and viscose-based carbon fibers join concentration and are in 0.8% the methylated cellulose aqueous solution, and the employing homogenizer disperses it.Other is cut-off footpath 20 μ m, 45 parts of the polypropylene cyanogen fibers of average fiber length 3mm, pour chopped carbon fiber dispersion slurries into after putting into the water dispersed with stirring, add after 15 parts of vinyl acetates mix, copy paper also with 80 ℃ of heated-air dryings with wet papermaking process, make its hot pressing 1.0 minutes under the pressure of 240 ℃ of temperature 1.5Mpa with hot press, obtain intermediate products.
With the charing 1.5 hours under argon shield and 2000 ℃ of temperature of above-mentioned intermediate products, make porous carbon fiber paper.The thickness 0.18mm of this paper, density 0.44g/cm
3Area weight: 79.2g/m
2, air permeability 321L/m
2S, resistivity 0.017 Ω cm.
The wet papermaking process that the present invention relates to belongs to conventional known technology, no longer specifically describes here.
Claims (10)
1. the porous carbon fiber paper of a used in proton exchange membrane fuel cell, it is characterized in that: its raw material comprises chopped carbon fiber and hot adhesion fiber, and the weight ratio of described chopped carbon fiber and hot adhesion fiber is 20～70: 80～30.
2. the porous carbon fiber paper of a kind of used in proton exchange membrane fuel cell according to claim 1, it is characterized in that: the weight ratio of described chopped carbon fiber and hot adhesion fiber is 30～60: 70～40.
3. the porous carbon fiber paper of a kind of used in proton exchange membrane fuel cell according to claim 1, it is characterized in that: the weight ratio of described chopped carbon fiber and hot adhesion fiber is 35～55: 65～45.
4. the porous carbon fiber paper of a kind of used in proton exchange membrane fuel cell according to claim 1, it is characterized in that: described chopped carbon fiber is one of polypropylene cyano group carbon fiber, asphalt base carbon fiber, viscose-based carbon fiber or its composition.
5. the porous carbon fiber paper of a kind of used in proton exchange membrane fuel cell according to claim 1, it is characterized in that: but described hot adhesion fiber is the charing staple fibre with hot adhesion performance, is specially polyacrylonitrile fibre, pitch fibers or polyimide fiber.
6. the porous carbon fiber paper of a kind of used in proton exchange membrane fuel cell according to claim 1, it is characterized in that: described chopped carbon fiber diameter is 6～20 μ m, and average length is 3～10mm; Described hot adhesion fibre diameter is 8～20um, and average length is 2～10mm.
7. the porous carbon fiber paper of a kind of used in proton exchange membrane fuel cell according to claim 1, it is characterized in that: described chopped carbon fiber diameter is 7～12 μ m, average length is 4～6mm, and described hot adhesion fibre diameter is 10～15um, and average length is 3～6mm.
8. aforesaid right requires the preparation method of the described porous carbon fiber paper of 1-7, it is characterized in that comprising following processing step:
A. add weight percentage in the chopped carbon fiber and be 0.2～1.0% aqueous dispersant, be uniformly dispersed through high-speed stirred, make the chopped carbon fiber slurries, described dispersant is a methylcellulose, hydroxyethylcellulose is received or Carboxymethyl Cellulose;
B. after the hot adhesion fiber stirs in water and is uniformly dispersed, join in the chopped carbon fiber slurries, add the binding agent of total weight of fiber 8～20%, mix and make the papermaking mixed serum, described binding agent is poly-vinyl alcohol solution, vinyl acetate or polyvinyl alcohol staple fibre;
C. adopt conventional wet papermaking process to copy paper, and dry under 80～120 ℃ of temperature;
D. the paper that will copy hot pressing 0.3～1.5 minute under 220～280 ℃, the pressure of 0.6～1.5MPa obtains the intermediate products of surfacing;
E. with above-mentioned intermediate products under 1500～2500 ℃ temperature and charing 0.3～2.0 hour in the inert atmosphere, make porous carbon fiber paper.
9. the preparation method of the porous carbon fiber paper of a kind of used in proton exchange membrane fuel cell according to claim 8 is characterized in that comprising following processing step:
A. add weight percentage in the chopped carbon fiber and be 0.5～0.8% aqueous dispersant, be uniformly dispersed through high-speed stirred, make the chopped carbon fiber slurries, described dispersant methylcellulose, hydroxyethylcellulose is received or carboxymethyl cellulose;
B. after the hot adhesion fiber stirs in water and is uniformly dispersed, join in the chopped carbon fiber slurries, add the binding agent of total weight of fiber 10～15%, mix and make the papermaking mixed serum, described binding agent is poly-vinyl alcohol solution, vinyl acetate or polyvinyl alcohol staple fibre;
C. adopt conventional wet papermaking process to copy paper, and dry under 80～95 ℃ of temperature;
D. the paper that will copy hot pressing 0.5～1.0 minute under 240～260 ℃, the pressure of 1.0～1.5MPa obtains the intermediate products of surfacing;
E. with above-mentioned intermediate products under 1800～2400 ℃ temperature and charing 0.5～1.5 hour in the inert atmosphere, make porous carbon fiber paper.
10. the preparation method of the porous carbon fiber paper of a kind of used in proton exchange membrane fuel cell according to claim 9, it is characterized in that: carbonization temperature is 2000～2200 ℃ in the step e, carbonization time is 0.8～1.0 hour.
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| CN101613982B (en) * | 2008-06-27 | 2011-01-12 | 北京化工大学 | Method for preparing carbon fiber paper for gas diffusion layer of fuel cell |
| CN103114495A (en) * | 2013-02-22 | 2013-05-22 | 浙江省普瑞科技有限公司 | Carbon paper for electrode diffusion layer of fuel cell and preparation method thereof |
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| CN109594397A (en) * | 2018-11-30 | 2019-04-09 | 浙江金昌特种纸股份有限公司 | A kind of carbon fiber paper papermaking process |
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| CN1121128A (en) * | 1994-09-10 | 1996-04-24 | 陈耀庭 | Carbon fibre paper and its production process |
| CN1185736C (en) * | 2001-11-09 | 2005-01-19 | 上海依极科技有限公司 | Carbon fiber paper material for gas diffusing layer of fuel cell electrode and its prepn |
| TWI314599B (en) * | 2002-04-17 | 2009-09-11 | Mitsubishi Rayon Co | Carbon electrode base material using carbon paper for fuel cell made |
| CN1318697C (en) * | 2004-08-20 | 2007-05-30 | 中国科学院山西煤炭化学研究所 | Carbon fibre paper and its mfg. method |
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| CN103114495B (en) * | 2013-02-22 | 2015-12-23 | 浙江省普瑞科技有限公司 | A kind of carbon paper for electrode diffusion layer of fuel cell and preparation method thereof |
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| CN109594397A (en) * | 2018-11-30 | 2019-04-09 | 浙江金昌特种纸股份有限公司 | A kind of carbon fiber paper papermaking process |
| CN110247065A (en) * | 2019-07-09 | 2019-09-17 | 吴同舜 | A kind of fuel battery gas diffusion layer low cost continuous industrial production technique |
| CN110485191A (en) * | 2019-08-16 | 2019-11-22 | 中国海诚工程科技股份有限公司 | Wet process is manufactured paper with pulp gas diffusing layer of fuel cell electrode carbon fiber paper and preparation method thereof |
| WO2022188891A1 (en) * | 2021-03-08 | 2022-09-15 | 上海嘉资新材料科技有限公司 | High-throughput carbon paper for fuel cell, and preparation method therefor |
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