CN1323455C - Method of mfg conducting and gas diffusion layer material in electrochemical generating unit - Google Patents
Method of mfg conducting and gas diffusion layer material in electrochemical generating unit Download PDFInfo
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- CN1323455C CN1323455C CNB2004100669801A CN200410066980A CN1323455C CN 1323455 C CN1323455 C CN 1323455C CN B2004100669801 A CNB2004100669801 A CN B2004100669801A CN 200410066980 A CN200410066980 A CN 200410066980A CN 1323455 C CN1323455 C CN 1323455C
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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
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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 present invention relates to a method for making a conductive material and a material of a gas diffusion layer in an electrochemical electricity generating device, which comprises the following steps: (1), selecting an organic film as an adhesive material, and heating the film by padding a layer of metallic or nonmetallic gauze under the film; (2), evenly scattering carbon fibers of polyacrylonitrile on the organic film in a semi-melting state in step (1) for pressurization to form the diffusion layer which is the structural material; (3), mixing conductive powder and the other desired materials into conductive powder slurry, and using a printing method to evenly convert the conductive powder slurry to one or two surfaces of the diffusion layer which is the goal object of step (2) to dry the conductive powder slurry; (4), heating and pressurizing one or more sheets of the goal objects in step (3) to make the conductive material and the material of the gas diffusion layer. Compared with the prior art, the present invention has the advantages of simple method, easy product quality control, low production cost, etc.
Description
Technical field
The present invention relates to electrochemical generating unit, relate in particular to the manufacture method of conducting electricity in a kind of electrochemical generating unit with gas diffusion layer material.
Background technology
Electrochemistry generating is to be fuel with hydrogen or methyl alcohol, and air or oxygen etc. are oxidant, carry out electrochemical reaction, directly take out the device of electric energy.It to restructure the use of energy and environmental protection positive effect is arranged.Its elementary cell is by proton exchange membrane 1, catalyst 2, and conduction is formed with gas diffusion substrate 3 and positive and negative trapping conductive plate 4, as shown in Figure 1.According to the size of voltage and power, the quantity and the area of decision elementary cell.Conduction wherein and gas diffusion substrate are assemblied in the proton exchange membrane both sides, and itself can scribble catalyst or support scribbles the soft proton exchange membrane of catalyst.Also the high ventilation performance to be arranged, make fuel and oxidant by conduction and gas diffusion substrate and catalyst generation chemical action.It should have good electrical conductivity simultaneously, guarantees conduction.Therefore, this conduction and gas diffusion substrate, specification requirement is higher, should have the low and uniform high gas permeability of resistivity, and characteristics such as the variation of thickness is very little under the pressurized situation.Narrated the manufacture method of this kind material in toray Co., Ltd. patent of invention, the steps include:
(1) carbon fiber with polypropylene fine (PAN) is scattered in the dispersion liquid of polyvinyl alcohol (PVA) or acrylic resin and conductive powder, and these fibers are ladled out forms carbon fiber plate on the net.
(2) by the dispersion liquid infusion method, organic material is adhered to the carbon fiber plate that forms, as the adhesive of carbon fibre material.
(3) carbon fiber plate that adhesive is arranged is carried out dried.
(4) to after the drying, the carbon fiber plate by adhesive pressurizes, obtains a kind of porous conduction and gas diffusion materials.
Compared with some manufacture methods of other company simply and more reliable but also there is following shortcoming in this kind technology:
(1) because in process of production, carbon fiber and conductive powder are scattered in the liquid solution, after ladling out on the net, can only judge carbon fiber and the conductive powder total content in carbon fiber plate substantially, can't determine carbon fiber and conductive powder accurate content separately; The inconsistency that the material content of each batch in batch process, occurs; As: have batch in carbon fiber content greater than conductive powder content, if any batch in carbon fiber content less than conductive powder content, cause the inconsistency of product because of each technical indicator of batch difference (conductivity of vertical and horizontal, air penetrability, horizontal pyroconductivity), can not accurately control, thereby the quality of merchant's product is used in influence.
(2) in continuous flow procedure, owing to part material (carbon fiber and conductive powder etc.) has been scooped out, and part material is also in liquid solution; Since its separately content can't accurately judge and accurately control, cause the amount of inserting (amounts of inserting such as carbon fiber and conductive powder) in the liquid solution of follow-up raw material after dilution, can't accurately insert control, cause the inconsistency of each technical indicator in same batch of product (conductivity of vertical and horizontal, air penetrability, horizontal pyroconductivity), can not accurately control, thereby the quality of merchant's product is used in influence.
(3) be to produce with " method that dips is soaked in liquid dispersion " owing to what adopt, its product feature is: or obtain the hydrophily product in the immersion hydrophilic dispersion liquid; Immerse in the hydrophobicity dispersion liquid and obtain the hydrophobicity product; Can't obtain integrating hydrophilic layer and hydrophobic layer (being that product simultaneously is that the hydrophilic layer another side is a hydrophobic layer) product.If obtain this characteristic product (being that product simultaneously is that the hydrophilic layer another side is a hydrophobic layer), must increase production stages such as the other spray treatment of single face, complex process, manufacturability is poor, and production cost is higher.
Above shortcoming can reduce: the defective owing to its production technology, and cause the fine dispersion of air penetrability and the conductive powder that can not control product well, thereby influence electric conductivity, and also complex process, manufacturability is poor, and production cost is higher.
Summary of the invention
Purpose of the present invention is exactly that the manufacture method that a kind of method is simple, be easy to control conduction and gas diffusion layer material in the lower electrochemical generating unit of product quality, production cost is provided in order to overcome the shortcoming that above-mentioned prior art exists.
Purpose of the present invention can be achieved through the following technical solutions:
The manufacture method of conduction and gas diffusion layer material in a kind of electrochemical generating unit is characterized in that described method comprises following processing step:
(1) chooses the uniform organic film of thickness as adhesive material, at film underlay layer of metal or nonmetal silk screen, and place heater together, at the temperature spot that is lower than above-mentioned organic film semi-molten state, make organic film be in soft state the adjustment of this heater;
(2) with 7～12 millimeters of length, the carbon fiber of the fine base of the polypropylene that diameter is 5～9 microns (PAN) is by oscillator and disperse grid, make carbon fiber be scattered in being on the semi-vitreous organic film of step (1) equably, subsequently in its surface pressurization, make carbon fiber and organic film under the effect of power, spread and permeate, after lowering the temperature, form structural material-diffusion layer;
(3) conducting powder and required other materials are blended into the conducting powder slurry, the conducting powder slurry is transferred to equably one side or two upward oven dry of step (2) object-diffusion layer with method of printing, both can obtain the diffusion layer that two faces all are hydrophobic diffusion layer or hydrophilic layer, it is hydrophobic also can obtaining one side, and another side is hydrophilic diffusion layer;
Described other materials comprise with step (1) in organic film as the organic material of the identical or different material of adhesive material; Comprise hydrophily or be mixed with the material of hydrophily material particle, comprise being selected from the resin that mixes silicon dioxide, titanium dioxide, zirconia hydrophilic material or this comprises NAFION resin, polyacrylamide resin as hydrophilic resin; The organic solution that perhaps comprises the hydrophobic resin material comprises being selected from polytetrafluoroethylene (PTFE), polypropylene, polyvinyl alcohol, epoxy resin solution;
(4) with one or more pieces of step (3) object, heating and pressurizing is made thickness and is 0.10～1.5 millimeter conduction and gas diffusion layer material.
Described organic film is as adhesive material, its material is selected from the resin material that contains hydrophilic material, comprise the resin that mixes silicon dioxide, titanium dioxide, zirconia hydrophilic material or originally comprise NAFION resin, polyacrylamide resin as hydrophilic resin, or be selected from the hydrophobic resin material, comprise polytetrafluoroethylene (PTFE), polypropylene, polyvinyl alcohol, cellulose, epoxy resin solution.
The uniform organic film of described thickness, its thickness accounts for conducting powder slurry weight percentage according to organic film and calculates; Concrete formula is: percentage by weight=((organic film thickness * product area * organic film density)/electric conducting material weight) * 100%, the organic film percentage by weight is 0.5%～50%.
Described metal or nonmetal silk screen, its material heatproof temperature should be higher than the decomposition point temperature of organic film.
The heater of described step (1), its mode of heating is directly to contact conduction pattern to comprise electric boiling plate, electric oil heating plate, electric heating heater plate, or the convective heat transfer mode comprises that hot blast blows, or the radiant heat transfer mode comprises infrared radiation, or the microwave oscillation mode of heating.
The surface pressurization of described step (2), its pressuring method are directly to contact pressuring method to comprise press pressurization or roll-in, and perhaps the noncontact pressuring method comprises high velocity air surface blow pressure.
The conducting powder of described step (3) is selected from expanded graphite powder, natural graphite powder or conductive carbon black, and its particle diameter is 10～1000 orders.
The other materials of described step (3) also comprises pore creating material, and this pore creating material is selected from carbonic hydroammonium, ammonium oxalate, lithium carbonate.
The method of printing of described step (3) is selected from roll marks, silk screen printing or transfer printing.
Compared with prior art, the present invention has the following advantages:
1. adopt the dry type configuration to be easier to control actual content to important material carbon fiber and conducting powder than prior art; Be uniformly dispersed, to the conductance of diffusion material, the control of air penetrability, more convenient, correct.
2. the slurry of conducting powder adopts print process, can be according to different requirements, and the conductivity to product, the control of air penetrability are carried out in the distribution of the point-like by controlling its conducting powder slurry and to the uniformity control of print thickness.
3. by MULTILAYER COMPOSITE, carry out the horizontal conductivity to product, horizontal pyroconductivity and air penetrability control.
4. be processed into hydrophobic layer or two faces that are processed into all are hydrophilic layers at two faces of diffusion layer on demand easily, also can be processed into one side according to specific (special) requirements is hydrophobic layer, and one side is a hydrophilic layer.
5. because in the continuous flow procedure, each material occurs with solid-state and slurry form (on-liquid discrete form), can reach accurate control to each material mixture ratio, thereby reach accurate control, guarantee each batch of product and the consistency of the quality between each batch every technical indicator.
Description of drawings
Fig. 1 is the structural representation of conduction with gas diffusion layer material.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
The manufacture method of conduction and gas diffusion layer material in a kind of electrochemical generating unit, this method comprises following processing step:
At first choosing its thickness of polypropylene film is 0.01mm, and wide is 50mm, long for 150mm, is lined with the stainless steel metal silk screen below being placed on.Be placed on simultaneously on the electric boiling plate, the temperature of electric boiling plate is 110 ℃.Disperse the grid will long 10mm with vibration, diameter be that the carbon fiber (PAN) of 7 μ m is scattered on the polypropylene film equably.With the electric boiling plate cooling, obtain 10g/m subsequently
2Carbon fiber structural base material-diffusion layer.
Be that 300 purpose expanded graphites and conductive carbon black respectively 5 restrain then with particle diameter, chain length is the silica 1 gram of 150 nanometers, and carbonic hydroammonium 1 gram restrains (wherein epoxy resin 1 restrains, dicyandiamide 0.05 gram) with epoxy resin acetone soln 20 and disperses to be modulated into electrocondution slurry; Use roll printing method, electrocondution slurry is printed onto on carbon fiber structural base material-diffusion layer, slurry thickness is 0.1mm, obtains containing the diffusion layer of the conductive paste bed of material behind 100 ℃ of temperature dryings; Hot press 50kg/cm at 180 ℃
2Pressure pressurizeed 10 minutes down, and can obtain thickness is the hydrophilic conductive diffusion layer material of 0.1mm.Recording resistivity is 100 Ω cm
2, air penetrability is 50mmAq/mm.
Choosing its thickness of polypropylene film is 0.01mm, and wide is 50mm, long for 150mm, is lined with the stainless steel metal silk screen below being placed on.Be placed on simultaneously on the electric boiling plate, the temperature of electric boiling plate is 110 ℃.Disperse the grid will long 10mm with vibration, diameter be that the carbon fiber (PAN) of 7 μ m is scattered on the polypropylene film equably.With the electric boiling plate cooling, obtain 10g/m subsequently
2Carbon fiber structural base material-diffusion layer.
With particle diameter is that 300 purpose expanded graphites and conductive carbon black respectively 5 restrain, and diameter is PTFE powder 1 gram of 80 nanometers, and carbonic hydroammonium 1 gram restrains (wherein epoxy resin 1 restrains, dicyandiamide 0.05 gram) with epoxy resin acetonitrile solution 20 and disperses to be modulated into electrocondution slurry; Use roll printing method, electrocondution slurry is printed onto on carbon fiber structural base material-diffusion layer, slurry thickness is 0.1mm, obtains containing the diffusion layer of the conductive paste bed of material behind 100 ℃ of temperature dryings; Hot press 50kg/cm at 180 ℃
2Pressure pressurizeed 10 minutes down, and the baking oven of putting into 380 ℃ subsequently heated 20 minutes, and can obtain thickness is the hydrophobic conductive diffusion layer of 0.1mm.Recording resistivity is 100 Ω cm
2, air penetrability is 6mmAq/mm.
With embodiment 1 and two stacks of 2 objects, that is, and with the stack of the conductive paste bed of material back side, at 220 ℃ hot press 50kg/cm
2Under the pressure, pressurizeed 10 minutes, can obtain thickness is that 0.15mm simultaneously is a hydrophobicity, and another side is the hydrophily conductive diffusion layer.Recording resistivity is 30 Ω cm
2, air penetrability is 8mmAq/mm.
The electrocondution slurry of one deck embodiment 1 will be stamped with roll printing method on the product object of embodiment 1 once more; With two stacks of product object of embodiment 2, with the surface spray method with the moistening stack thing of acetone soln after, dry under 110 ℃ temperature.Then at 180 ℃ hot press 50kg/cm
2Under the pressure, pressurizeed 10 minutes, put into 380 ℃ baking oven heat treatment 20 minutes subsequently, can obtain thickness is that 0.21mm simultaneously is a hydrophobicity, and another side is the hydrophily conductive diffusion layer.Recording resistivity is 10 Ω cm
2, air penetrability is 15mmAq/mm.
According to the present invention, can in high volume production process, reach accurate control to each material content, thus the consistency of quality when guaranteeing that product lot quantity is produced.Simultaneously, the two sides of product monomer when producing continuously can be hydrophilic entirely or be hydrophobic entirely, and it is hydrophilic also can producing one side and be hydrophobic, one side, reaches different instructions for use and purposes.Avoid the re-treating process in the subsequent applications, thereby reduce the manufacturing cost in using.
Claims (9)
1. the manufacture method of conduction and gas diffusion layer material in the electrochemical generating unit is characterized in that described method comprises following processing step:
(1) chooses the uniform organic film of thickness as adhesive material, at film underlay layer of metal or nonmetal silk screen, and place heater together, at the temperature spot that is lower than above-mentioned organic film semi-molten state, make organic film be in soft state the adjustment of this heater;
(2) with 7～12 millimeters of length, the carbon fiber of the fine base of polypropylene that diameter is 5～9 microns is by oscillator and disperse grid, make carbon fiber be scattered in being on the semi-vitreous organic film of step (1) equably, subsequently in its surface pressurization, make carbon fiber and organic film under the effect of power, spread and permeate, after lowering the temperature, form structural material-diffusion layer;
(3) conducting powder and required other materials are blended into the conducting powder slurry, the conducting powder slurry is transferred to equably one side or two upward oven dry of step (2) object-diffusion layer with method of printing, obtain the diffusion layer that two faces all are hydrophobic diffusion layer or hydrophilic layer, it is hydrophobic perhaps obtaining one side, and another side is hydrophilic diffusion layer;
Described other materials comprise with step (1) in organic film as the organic material of the identical or different material of adhesive material; Comprise hydrophily or be mixed with the material of hydrophily material particle, comprise being selected from the resin that mixes silicon dioxide, titanium dioxide, zirconia hydrophilic material or this comprises NAFION resin, polyacrylamide resin as hydrophilic resin; The organic solution that perhaps comprises the hydrophobic resin material comprises being selected from polytetrafluoroethylene, polypropylene, polyvinyl alcohol, epoxy resin solution;
(4) with one or more pieces of step (3) object, heating and pressurizing is made thickness and is 0.10～1.5 millimeter conduction and gas diffusion layer material.
2. the manufacture method of conduction and gas diffusion layer material in a kind of electrochemical generating unit according to claim 1, it is characterized in that, described organic film is as adhesive material, its material is selected from the resin material that contains hydrophilic material, comprise the resin that mixes silicon dioxide, titanium dioxide, zirconia hydrophilic material or originally comprise NAFION resin, polyacrylamide resin as hydrophilic resin, or be selected from the hydrophobic resin material, comprise polytetrafluoroethylene, polypropylene, polyvinyl alcohol, cellulose, epoxy resin solution.
3. the manufacture method of conduction and gas diffusion layer material in a kind of electrochemical generating unit according to claim 1 and 2, it is characterized in that, the uniform organic film of described thickness, its thickness accounts for conducting powder slurry weight percentage according to organic film and calculates; Concrete formula is: percentage by weight=((organic film thickness * product area * organic film density)/electric conducting material weight) * 100%, the organic film percentage by weight is 0.5%～50%.
4. the manufacture method of conduction and gas diffusion layer material is characterized in that in a kind of electrochemical generating unit according to claim 1, described metal or nonmetal silk screen, and its material heatproof temperature should be higher than the decomposition point temperature of organic film.
5. the manufacture method of conduction and gas diffusion layer material in a kind of electrochemical generating unit according to claim 1, it is characterized in that, the heater of described step (1), its mode of heating is directly to contact conduction pattern to comprise electric boiling plate, electric oil heating plate, electric heating heater plate, or the convective heat transfer mode comprises that hot blast blows, or the radiant heat transfer mode comprises infrared radiation, or the microwave oscillation mode of heating.
6. the manufacture method of conduction and gas diffusion layer material in a kind of electrochemical generating unit according to claim 1, it is characterized in that, the surface pressurization of described step (2), its pressuring method is directly to contact pressuring method to comprise press pressurization or roll-in, and perhaps the noncontact pressuring method comprises high velocity air surface blow pressure.
7. the manufacture method of conduction and gas diffusion layer material in a kind of electrochemical generating unit according to claim 1, it is characterized in that, the conducting powder of described step (3) is selected from expanded graphite powder, natural graphite powder or conductive carbon black, and its particle diameter is 10～1000 orders.
8. the manufacture method of conduction and gas diffusion layer material is characterized in that the other materials of described step (3) also comprises pore creating material in a kind of electrochemical generating unit according to claim 1, and this pore creating material is selected from carbonic hydroammonium, ammonium oxalate, lithium carbonate.
9. the manufacture method of conduction and gas diffusion layer material is characterized in that the method for printing of described step (3) is selected from roll marks, silk screen printing or transfer printing in a kind of electrochemical generating unit according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100669801A CN1323455C (en) | 2004-10-10 | 2004-10-10 | Method of mfg conducting and gas diffusion layer material in electrochemical generating unit |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100669801A CN1323455C (en) | 2004-10-10 | 2004-10-10 | Method of mfg conducting and gas diffusion layer material in electrochemical generating unit |
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| CN1601795A CN1601795A (en) | 2005-03-30 |
| CN1323455C true CN1323455C (en) | 2007-06-27 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102804466B (en) * | 2009-06-26 | 2015-12-16 | 日产自动车株式会社 | The hydrophilic porous layer of fuel cell, gas-diffusion electrode and manufacture method thereof and membrane electrode assembly |
| EP2448048A4 (en) * | 2009-06-26 | 2017-01-11 | Nissan Motor Co., Ltd. | Gas diffusion electrode and production method for same; membrane electrode assembly and production method for same |
| TWI568888B (en) * | 2011-09-15 | 2017-02-01 | 第諾拉工業公司 | Gas-diffusion electrode |
| CN103401003B (en) * | 2013-07-17 | 2016-08-17 | 南京大学昆山创新研究院 | Gas diffusion layers of Proton Exchange Membrane Fuel Cells and preparation method thereof |
| JP6931280B2 (en) * | 2016-11-08 | 2021-09-01 | 東京応化工業株式会社 | A method for producing a composition for forming a porous film, a separator, an electrochemical element, and an electrode composite. |
| CN111916765B (en) * | 2020-07-29 | 2022-02-11 | 一汽解放汽车有限公司 | Method for preparing gas diffusion layer in fuel cell |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63164169A (en) * | 1986-12-25 | 1988-07-07 | Nippon Steel Chem Co Ltd | Manufacture of conductive plastic electrode |
| CN1312944A (en) * | 1998-08-11 | 2001-09-12 | 曼哈顿科学公司 | Electrically conductive layer material |
| CN1338126A (en) * | 1999-09-22 | 2002-02-27 | 东丽株式会社 | Porous, electrically conductive sheet and method for production thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63164169A (en) * | 1986-12-25 | 1988-07-07 | Nippon Steel Chem Co Ltd | Manufacture of conductive plastic electrode |
| CN1312944A (en) * | 1998-08-11 | 2001-09-12 | 曼哈顿科学公司 | Electrically conductive layer material |
| CN1338126A (en) * | 1999-09-22 | 2002-02-27 | 东丽株式会社 | Porous, electrically conductive sheet and method for production thereof |
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