CN101613982A - A kind of preparation method of carbon fiber paper for gas diffusion layer of fuel cell - Google Patents
A kind of preparation method of carbon fiber paper for gas diffusion layer of fuel cell Download PDFInfo
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- CN101613982A CN101613982A CN200810115729A CN200810115729A CN101613982A CN 101613982 A CN101613982 A CN 101613982A CN 200810115729 A CN200810115729 A CN 200810115729A CN 200810115729 A CN200810115729 A CN 200810115729A CN 101613982 A CN101613982 A CN 101613982A
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
A kind of preparation method of carbon fiber paper for gas diffusion layer of fuel cell belongs to fuel cell field.Existing carbon fiber paper can't be taken into account air penetrability and mechanical strength, exists quality crisp, and surface smoothness is low, and chopped carbon fiber is easily peeled off and problem such as production cost height.The present invention soaks material by obtaining carbon fiber felt phenolic resin prepolymer in the ethanolic solution with carbon fiber felt impregnated phenolic resin; The prepreg mold pressing made carry out low-temperature carbonization behind the carbon fiber paper idiosome and handle; Ethanolic solution with phenolic resins floods and curing once more; Handle in high temperature cabonization at last and make carbon fiber paper for gas diffusion layer of fuel cell.The prepared carbon fiber paper of the present invention has higher porosity, gas permeability, electrical conductivity and TENSILE STRENGTH, can be used as the gas diffusion layer of proton exchange membrane fuel cell base material and uses.
Description
Technical field
The invention belongs to fuel cell field, be specifically related to a kind of preparation method, particularly a kind of method that adopts double-steeping prepared gas diffusion layer of proton exchange membrane fuel cell with carbon fiber paper with carbon fiber paper of higher air penetrability, TENSILE STRENGTH and electric conductivity.
Background technology
Fuel cell is a kind of electrochemical TRT, is different from the battery on the conventional meaning.Fuel cell isothermal ground directly changes chemical energy into electric energy by electrochemical means.Therefore it be not subjected to the restriction of Carnot cycle without the overheated machine process, energy conversion efficiency height (40%-60%), and environmental friendliness is discharged nitrogen oxide and sulfur oxide hardly.And emission amount of carbon dioxide also reduces more than 40% than conventional power generation usage factory.Just because of these outstanding superiority, the research and development of fuel cell technology is national governments and the attention that reaches company extremely, are considered to the cleaning of 21 century first-selection, generation technology efficiently.
Gas diffusion layers is the significant components in the Proton Exchange Membrane Fuel Cells, plays the support catalyst layer, and the important mass transfer channel of reacting gas, generation water is provided, and also will play the effect of electric energy transmitting simultaneously.Carbon fiber paper for gas diffusion layer need have higher porosity and air penetrability, guarantee that reacting gas can react fully on catalyst layer, but also to possess certain mechanical strength, guarantee in fuel cell assembling and use, can not destroy, have excellent conducting performance simultaneously in addition, reduce internal resistance.At present, most widely used high-performance carbon fibre paper can not well be taken into account the air penetrability and the mechanical strength of carbon fiber paper, exist quality crisp, destroy easily in membrane electrode preparation and the fuel cell assembling process, surface smoothness is low, and chopped carbon fiber is peeled off and shortcoming such as production cost height easily.
Summary of the invention
The objective of the invention is to solve the problems of the prior art, and the preparation method of the special-purpose carbon fiber paper of a kind of gas diffusion layer of proton exchange membrane fuel cell is provided.The prepared carbon fiber paper of the inventive method can be taken into account higher air penetrability and TENSILE STRENGTH, have toughness preferably, be difficult for destroying in membrane electrode preparation and fuel cell assembling process, surface smoothness is good, chopped carbon fiber is difficult for peeling off, and satisfies the requirement of gas diffusion layer material.
The present invention adopts double-steeping prepared carbon fiber paper, specifically comprises the steps:
1) thermosetting amine catalysed phenolic resin is dissolved in is mixed with the phenolic resins ethanolic solution in the absolute ethyl alcohol;
2) choosing specification is 20-50g/cm
2The carbon fiber felt (chopped carbon fiber in the felt is a polyacrylonitrile-based carbon fibre, adhesive is a polyvinyl alcohol, the mass fraction of chopped carbon fiber is 70-90%, the mass fraction of adhesive is 10-30%) and immerse and make carbon fiber felt phenolic resin prepolymer in the phenolic resins ethanolic solution of preparing in the step 1) and soak material, be 1 by the volume ratio of chopped carbon fiber and resin carbon (carbon that forms after the carbonization of thermosetting amine catalysed phenolic resin): 0.25-0.5 controls pickup;
3) get 2-5 layer step 2) the carbon fiber felt phenolic resin prepolymer of preparation soaks material and carries out mold pressing handle and to obtain the carbon fiber paper idiosome on press device, molding pressure is 0.5-5MPa, molding temperature is 120-170 ℃, clamp time is 10-40min, and the THICKNESS CONTROL of carbon fiber paper idiosome is at 0.18-0.42mm during mold pressing;
4) the carbon fiber paper idiosome of step 3) preparation is carried out low-temperature carbonization under nitrogen protection and handle and obtain the low-temperature carbonization material, the low-temperature carbonization temperature is controlled at 500-900 ℃, and the carbonization heating rate is controlled at 0.5-5 ℃/min, and carbonization time is 0.5-2h;
5) the low-temperature carbonization material with the step 4) preparation immerses in the phenolic resins ethanolic solution of preparing in the step 1), volume ratio by chopped carbon fiber and resin carbon is 1: 0.5-0.8 controls pickup, obtain the double-steeping material, again in 30-70 ℃ low temperature oven dry down, and, solidify 15-120min in 120-175 ℃;
6) carbon fiber paper after step 5) is handled is under nitrogen protection, and in 900-1500 ℃ of carbonization treatment 0.5-2h, the carbonization heating rate is controlled at 0.5-5 ℃/min, obtains carbon fiber paper for gas diffusion layer of fuel cell.
The present invention has following beneficial effect:
The prepared carbon fiber paper of the present invention also has higher mechanical strength concurrently except having good electrical conductivity and air penetrability, chopped carbon fiber combines well with resin carbon interface in the carbon fiber paper, resin carbon is the film shape and is distributed in the carbon fiber paper, this structure gives carbon fiber paper good toughness, in membrane electrode preparation and fuel cell assembling process, be difficult for destroying, surface smoothness is good, and chopped carbon fiber is difficult for peeling off, and it is lower to have good combination property and a preparation cost.
The specific embodiment
Embodiment 1
1) with 1g 20g/cm
2The fine felt of carbon (staple fiber content is 90%) to be impregnated into the 22g mass concentration be in 5% the thermosetting amine catalysed phenolic resin ethanolic solution, to obtain carbon fiber felt phenolic resin prepolymer and soak material;
2) get 5 layers of carbon fiber felt phenolic resin prepolymer and soak material by mold pressing Processing of Preparation carbon fiber paper idiosome, the mould pressing process condition: under 170 ℃, 0.5MPa, mold pressing 10min;
3) low-temperature carbonization carbon fiber paper idiosome under nitrogen protection, preparation low-temperature carbonization material, the low-temperature carbonization process conditions: the heating rate with 3 ℃/min is warming up to 650 ℃, carbonization 0.5h;
4) the low-temperature carbonization material being immersed once more the 15g mass concentration is in 5% the thermosetting amine catalysed phenolic resin, preparation double-steeping material;
5) with the double-steeping material after 70 ℃ of oven dry, again in 120 ℃, solidify 120min;
6) the double-steeping material after will solidifying carries out high temperature cabonization and obtains carbon fiber paper for gas diffusion layer of fuel cell, the carbonization technique condition: the heating rate with 2 ℃/min is warming up to 900 ℃, carbonization 1h.
The leading indicator of gained carbon fiber paper is as follows:
Thickness 0.30mm, density 0.42g/cm
3, air penetrability 2650mLmm/ (cm
2HrmmAq), TENSILE STRENGTH 20Mpa, resistivity 0.016 Ω cm.
Embodiment 2
1) with 1.3g 30g/cm
2The fine felt of carbon (staple fiber content is 85%) to be impregnated into the 35g mass concentration be in 5% the solidity amine catalysed phenolic resin ethanolic solution, to obtain carbon fiber felt phenolic resin prepolymer and soak material;
2) get 3 layers of carbon fiber felt phenolic resin prepolymer and soak material by mold pressing Processing of Preparation carbon fiber paper idiosome, the mould pressing process condition: under 140 ℃, 5MPa, mold pressing 27min;
3) low-temperature carbonization carbon fiber paper idiosome under nitrogen protection, preparation low-temperature carbonization material, the low-temperature carbonization process conditions: the heating rate with 5 ℃/min is warming up to 500 ℃, carbonization 2h;
4) carbon fiber paper after the low-temperature carbonization being immersed once more the 13g mass concentration is in 5% the thermosetting amine catalysed phenolic resin ethanolic solution, preparation double-steeping material;
5) with the double-steeping material behind 50 ℃ of oven dry 1h, again in 140 ℃, solidify 90min;
6) the double-steeping material after will solidifying carries out high temperature cabonization and obtains carbon fiber paper for gas diffusion layer of fuel cell, the carbonization technique condition: the heating rate with 3 ℃/min is warming up to 1200 ℃, carbonization 1.5h.
The leading indicator of gained carbon fiber paper is as follows:
Thickness 0.30mm, density 0.42g/cm
3, air penetrability 2500mLmm/ (cm
2HrmmAq), TENSILE STRENGTH 16.5Mpa, resistivity 0.017 Ω cm.
Embodiment 3
1) with 2.1g 50g/cm
2The fine felt of carbon (staple fiber content is 70%) to be impregnated into the 56g mass concentration be in 5% the thermosetting amine catalysed phenolic resin ethanolic solution, to obtain carbon fiber felt phenolic resin prepolymer and soak material;
2) get 2 layers of carbon fiber felt phenolic resin prepolymer and soak material by mold pressing Processing of Preparation carbon fiber paper idiosome, the mould pressing process condition: under 120 ℃, 3Mpa, mold pressing 40min;
3) low-temperature carbonization carbon fiber paper idiosome under nitrogen protection, preparation low-temperature carbonization material, the low-temperature carbonization process conditions: the heating rate with 0.5 ℃/min is warming up to 900 ℃, carbonization 1h;
4) the low-temperature carbonization material being immersed once more the 10g mass concentration is in 5% the thermosetting amine catalysed phenolic resin ethanolic solution, preparation double-steeping material;
5) with the double-steeping material after 30 ℃ of oven dry, again in 175 ℃, solidify 15min;
6) the double-steeping material after will solidifying carries out high temperature cabonization and obtains carbon fiber paper for gas diffusion layer of fuel cell, the carbonization technique condition: the heating rate with 0.5 ℃/min is warming up to 1500 ℃, carbonization 2h.
The leading indicator of prepared carbon fiber paper is as follows:
Thickness 0.30mm, density 0.42g/cm
3, air penetrability 2200mLmm/ (cm
2HrmmAq), TENSILE STRENGTH 14Mpa, resistivity 0.0075 Ω cm.
Claims (1)
1, a kind of preparation method of carbon fiber paper for gas diffusion layer of fuel cell is characterized in that, may further comprise the steps:
1) thermosetting amine catalysed phenolic resin is dissolved in is mixed with the phenolic resins ethanolic solution in the absolute ethyl alcohol;
2) choosing specification is 20-50g/cm
2The carbon fiber felt, chopped carbon fiber in the felt is a polyacrylonitrile-based carbon fibre, adhesive is a polyvinyl alcohol, the mass fraction of chopped carbon fiber is 70-90%, the mass fraction of adhesive is 10-30%, the carbon fiber felt immersed make carbon fiber felt phenolic resin prepolymer in the phenolic resins ethanolic solution of preparing in the step 1) and soak material, be 1 by the volume ratio of chopped carbon fiber and resin carbon: 0.25-0.5 controls pickup;
3) get 2-5 layer step 2) the carbon fiber felt phenolic resin prepolymer of preparation soaks material and carries out mold pressing handle and to obtain the carbon fiber paper idiosome on press device, molding pressure is 0.5-5MPa, molding temperature is 120-170 ℃, clamp time is 10-40min, and the THICKNESS CONTROL of carbon fiber paper idiosome is at 0.18-0.42mm during mold pressing;
4) the carbon fiber paper idiosome of step 3) preparation is carried out low-temperature carbonization under nitrogen protection and handle and obtain the low-temperature carbonization material, the low-temperature carbonization temperature is controlled at 500-900 ℃, and the carbonization heating rate is controlled at 0.5-5 ℃/min, and carbonization time is 0.5-2h;
5) the low-temperature carbonization material with the step 4) preparation immerses in the phenolic resins ethanolic solution of preparing in the step 1), volume ratio by chopped carbon fiber and resin carbon is 1: 0.5-0.8 controls pickup, obtain the double-steeping material, again in 30-70 ℃ low temperature oven dry down, and, solidify 15-120min in 120-175 ℃;
6) carbon fiber paper after step 5) is handled is under nitrogen protection, and in 900-1500 ℃ of carbonization treatment 1-2h, the carbonization heating rate is controlled at 0.5-5 ℃/min, obtains carbon fiber paper for gas diffusion layer of fuel cell.
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| CN2008101157298A CN101613982B (en) | 2008-06-27 | 2008-06-27 | Method for preparing carbon fiber paper for gas diffusion layer of fuel cell |
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| CN2008101157298A CN101613982B (en) | 2008-06-27 | 2008-06-27 | Method for preparing carbon fiber paper for gas diffusion layer of fuel cell |
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Cited By (15)
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| CN102312545A (en) * | 2011-07-05 | 2012-01-11 | 上海热丽电热材料有限公司 | Low-temperature heating solid wood composite floor and preparation method thereof |
| CN103193495A (en) * | 2013-03-01 | 2013-07-10 | 辽阳金谷碳纤维科技有限公司 | Production method of insulation materials used for crystal pulling furnace |
| CN106567283A (en) * | 2016-11-18 | 2017-04-19 | 中南大学 | PVB (Polyvinyl Butyral) modified and phenolic resin reinforced carbon paper as well as preparation process and application thereof |
| CN106930151A (en) * | 2017-03-31 | 2017-07-07 | 王敏 | A kind of fuel cell electrode preparation method of graphene carbon cellulose fiber conductive paper |
| CN107127907A (en) * | 2017-05-23 | 2017-09-05 | 中南大学 | A kind of preparation technology of ultra-thin Carbon fibe paper |
| CN109735110A (en) * | 2019-01-15 | 2019-05-10 | 哈尔滨工业大学 | A kind of modified phenolic-organic siliconresin composite material and preparation method |
| CN109860635A (en) * | 2019-02-22 | 2019-06-07 | 成都新柯力化工科技有限公司 | A kind of preparation method of new energy battery special-purpose metal net base carbon fibre paper |
| CN109863631A (en) * | 2016-12-29 | 2019-06-07 | 可隆工业株式会社 | Produce the method with the rolling gas diffusion layers of excellent deployment characteristics |
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| CN100415987C (en) * | 2006-07-05 | 2008-09-03 | 浙江省普瑞科技有限公司 | A porous carbon fiber paper for fuel cell with proton exchange membrane and preparation method thereof |
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| CN102312545A (en) * | 2011-07-05 | 2012-01-11 | 上海热丽电热材料有限公司 | Low-temperature heating solid wood composite floor and preparation method thereof |
| CN103193495A (en) * | 2013-03-01 | 2013-07-10 | 辽阳金谷碳纤维科技有限公司 | Production method of insulation materials used for crystal pulling furnace |
| CN106567283A (en) * | 2016-11-18 | 2017-04-19 | 中南大学 | PVB (Polyvinyl Butyral) modified and phenolic resin reinforced carbon paper as well as preparation process and application thereof |
| CN109863631A (en) * | 2016-12-29 | 2019-06-07 | 可隆工业株式会社 | Produce the method with the rolling gas diffusion layers of excellent deployment characteristics |
| CN106930151A (en) * | 2017-03-31 | 2017-07-07 | 王敏 | A kind of fuel cell electrode preparation method of graphene carbon cellulose fiber conductive paper |
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| CN109860635B (en) * | 2019-02-22 | 2021-09-03 | 成都新柯力化工科技有限公司 | Preparation method of metal mesh-based carbon fiber paper special for new energy battery |
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