WO2012002579A1 - 離型フィルムを用いて複合化シートを積層する方法、その方法による積層物、ならびにその方法に用いる離型フィルム - Google Patents
離型フィルムを用いて複合化シートを積層する方法、その方法による積層物、ならびにその方法に用いる離型フィルム Download PDFInfo
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- WO2012002579A1 WO2012002579A1 PCT/JP2011/065631 JP2011065631W WO2012002579A1 WO 2012002579 A1 WO2012002579 A1 WO 2012002579A1 JP 2011065631 W JP2011065631 W JP 2011065631W WO 2012002579 A1 WO2012002579 A1 WO 2012002579A1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
- H01M8/1006—Corrugated, curved or wave-shaped MEA
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
- B32B27/322—Layered products comprising a layer of synthetic resin comprising polyolefins comprising halogenated polyolefins, e.g. PTFE
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/24—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer not being coherent before laminating, e.g. made up from granular material sprinkled onto a substrate
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
- C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
- C25B9/23—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms comprising ion-exchange membranes in or on which electrode material is embedded
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/023—Porous and characterised by the material
- H01M8/0234—Carbonaceous material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/023—Porous and characterised by the material
- H01M8/0239—Organic resins; Organic polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/023—Porous and characterised by the material
- H01M8/0241—Composites
- H01M8/0243—Composites in the form of mixtures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/26—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer which influences the bonding during the lamination process, e.g. release layers or pressure equalising layers
- B32B2037/268—Release layers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
- B32B2309/02—Temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
- B32B2309/02—Temperature
- B32B2309/027—Ambient temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
- B32B2309/08—Dimensions, e.g. volume
- B32B2309/10—Dimensions, e.g. volume linear, e.g. length, distance, width
- B32B2309/105—Thickness
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
- B32B2309/12—Pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2327/00—Polyvinylhalogenides
- B32B2327/12—Polyvinylhalogenides containing fluorine
- B32B2327/18—PTFE, i.e. polytetrafluoroethylene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/18—Fuel cells
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/10—Removing layers, or parts of layers, mechanically or chemically
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M2008/1095—Fuel cells with polymeric electrolytes
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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
Definitions
- the present invention relates to a technology for manufacturing an electrochemical device in an application involving an electrochemical reaction such as a polymer electrolyte fuel cell (polymer electrolyte fuel cell: PEFC), electrolysis, or a gas sensor, and in particular, using a release film.
- PEFC polymer electrolyte fuel cell
- the present invention relates to a method of laminating a composite sheet made of functional powder and PTFE with another polymer film by hot pressing.
- Fuel cells that use hydrogen and oxygen are attracting attention as a clean energy generating means with little environmental impact because the reaction product is only water in principle.
- solid polymer fuel cells are easy to handle and are expected to increase in power density, and research activities and practical applications are becoming active.
- the application field is wide, and includes, for example, a power source of a moving body such as an automobile or a bus, a stationary power source in a general household, or a power source of a small portable terminal.
- a polymer electrolyte fuel cell is configured by stacking a large number of single cells, and each single cell typically has a structure as shown in FIG. That is, the polymer electrolyte membrane (ion exchange membrane) 10 is sandwiched between a pair of catalyst electrode layers 20 and 21 from both sides, and further, the catalyst electrode layers 20 and 21 are paired from both sides with a pair of gas diffusion layers (porous support layer, The gas diffusion layers 40 and 41 are sandwiched between carbon gas current collecting layers 40 and 41, and the gas diffusion layers 40 and 41 have gas passages (fuel gas passage 50, oxygen-containing gas) formed by separators 60 and 61. It is open towards the channel 51).
- gas diffusion layers 40 and 41 gas passages (fuel gas passage 50, oxygen-containing gas) formed by separators 60 and 61. It is open towards the channel 51).
- the fuel gas (such as H 2 ) introduced from the flow path 50 passes through the first gas diffusion layer (anode side gas diffusion layer) 40 and passes through the first catalyst electrode layer (anode, fuel electrode) 20 as follows.
- Proton (H + ) is generated while releasing electrons by the anode electrode reaction shown in FIG.
- the protons pass through the polymer electrolyte membrane 10 and receive electrons at the second catalyst electrode layer (cathode, oxygen electrode) 21 by the cathode electrode reaction shown below to generate H 2 O.
- a carbon black (CB) / PTFE composite porous sheet can be used as a gas diffusion layer of an electrochemical device in an application involving an electrochemical reaction such as a polymer electrolyte fuel cell, electrolysis, or a gas sensor.
- the thickness of the composite porous sheet is about several hundred ⁇ m or less, and is very flexible. For this reason, when the composite porous sheet is handled alone, the sheet may be folded or wrinkled.
- this sheet When this sheet is used for a gas diffusion layer of a polymer electrolyte fuel cell, it is necessary to laminate the sheet on a catalyst electrode layer of a membrane electrode assembly (MEA). However, even if considerable care is taken, the sheet may be folded or wrinkled during lamination processing. Due to this, there is a problem that a product loss of the polymer electrolyte fuel cell occurs.
- MEA membrane electrode assembly
- the composite porous sheet When preparing and transporting the composite porous sheet, the composite porous sheet is placed on a support film such as a polyethylene terephthalate (PET) film having rigidity.
- a release film such as polypropylene (PP) or PET film is sandwiched between the composite porous sheet and the support film so that the composite porous sheet can be peeled off from the support film later.
- PP polypropylene
- PET polypropylene
- the composite porous sheet and the release film are displaced during preparation and transportation of the composite porous sheet, and the composite There is also a problem that wrinkles and creases occur in the porous sheet.
- the CB / PTFE composite porous sheet is displaced if the release film is removed before the press treatment. Then, although press processing was tried leaving the release film, the problem (transfer) that a release film adhere
- the present invention has been made to solve the above problems, and provides the following solution.
- MEA membrane electrode assembly
- PTFE polytetrafluoroethylene
- the release film When the release film is peeled from the composite sheet, the release film has a 180-degree peel adhesive strength (based on JIS K6854-2: 1999) of 0.005 N / cm or more; It is 025 N / cm or less, The method as described in (1) characterized by the above-mentioned.
- Any one of (1) to (5) is characterized in that after releasing the release film from the composite sheet, a part or all of the composite sheet is not transferred to the release film.
- a composite sheet comprising functional powder and polytetrafluoroethylene (PTFE) is laminated on a release film exclusively used in the method described in any one of (1) to (7).
- PTFE polytetrafluoroethylene
- the composite sheet bonded to the release film in the present invention is in close contact so that the composite sheet does not peel off from the release film, and the release film has an appropriate rigidity.
- the composite sheet does not wrinkle or bend during handling, and therefore the composite sheet can be handled easily.
- the handling of the composite sheet includes preparation and transportation of the composite sheet in addition to the lamination process of the composite sheet.
- the composite sheet in the composite sheet bonded to the release film and the MEA stacked thereon, the composite sheet is adhered to the release film by the press process (transfer to the release film)
- the composite sheet is not destroyed by the pressing process. Therefore, the release film can be peeled from the composite sheet without causing the composite sheet misalignment or wrinkles after pressing.
- the yield in the joining process by the press treatment of the composite sheet (gas diffusion layer) to the membrane electrode assembly (MEA) of the polymer electrolyte fuel cell fuel cell is dramatically improved.
- FIG. 1 is a schematic perspective view showing a typical fuel cell (single cell).
- FIG. 2 is a diagram for explaining a press processing method.
- FIG. 3 is a diagram for explaining a method for measuring the peel adhesive strength.
- the membrane electrode assembly (MEA) will be described with reference to FIG.
- the membrane electrode assembly (MEA) includes a polymer electrolyte membrane (ion exchange membrane) 10 and a pair of catalyst electrode layers 20 and 21 sandwiching both sides thereof.
- the polymer electrolyte membrane 10 is preferably a perfluoro-based electrolyte or a hydrocarbon-based electrolyte, and more preferably a perfluoro-based electrolyte membrane.
- a perfluoro-based electrolyte membrane sulfonic acid-based electrolyte membranes [for example, Nafion (registered trademark, manufactured by DuPont), GORE-SELECT (registered trademark, manufactured by Japan Gore-Tex), etc.] are preferable, and stretched porous polytetrafluoro A perfluorosulfonic acid resin electrolyte membrane [GORE-SELECT (registered trademark, manufactured by Japan Gore-Tex), etc.] reinforced with ethylene is particularly preferable.
- the EW (Equivalent Weight) of the polymer electrolyte membrane is, for example, about 700 or more (preferably 900 or more) and 1500 or less (preferably 1300 or less).
- the thickness of the polymer electrolyte membrane is desirably about 10 ⁇ m or more (preferably 15 ⁇ m or more) and about 100 ⁇ m or less (preferably 60 ⁇ m or less).
- catalyst electrode layers 20 and 21 conventionally known ones can be used.
- fine particles of platinum or an alloy of platinum and other metals for example, Ru, Rh, Mo, Cr, Fe, etc.
- Conductive carbon fine particles average particle size: about 20 to 100 nm
- carbon black supported on the surface and a perfluorosulfonic acid resin-containing liquid are uniform in an appropriate solvent (for example, alcohols).
- an appropriate solvent for example, alcohols.
- the amount of platinum in the anode-side catalyst electrode layer 20 (fuel electrode) is about 0.1 to 0.5 mg / cm 2 in terms of metal platinum, and the platinum in the cathode-side catalyst electrode layer 21 (air electrode).
- the amount is preferably about 0.3 to 0.8 mg / cm 2 in terms of metal platinum.
- the thickness of the catalyst electrode layer is, for example, about 5 to 30 ⁇ m.
- the composite sheet comprising functional powder and polytetrafluoroethylene (PTFE) can be laminated on the MEA catalyst electrode layers 20 and 21 to form the gas diffusion layers 40 and 41.
- PTFE polytetrafluoroethylene
- the composite sheet is desirably at least breathable (gas permeable), conductive, and moisture permeable (hydrophobic or water repellent).
- the functional powder can contain any inorganic powder such as conductive carbonaceous powder, silica, alumina, and titanium oxide as appropriate according to the purpose and application.
- electroconductive carbonaceous powder is particularly preferable.
- the conductive carbonaceous powder for example, carbon black (C / B) such as furnace black, lamp black, thermal black, acetylene black, activated carbon and graphite can be used, and these may be used alone or in two kinds. The above may be mixed.
- a preferred conductive carbonaceous powder is acetylene black or a mixture thereof. Acetylene black or a mixture thereof is excellent in conductivity, water repellency, and chemical stability.
- the PTFE is used to bind functional powder into a sheet (film), and to provide water repellency by covering the surface of the functional powder, particularly the functional powder. It is also suitable in that it can be performed.
- the amount of PTFE is, for example, 5% by mass or more (preferably 7% by mass or more, more preferably 10% by mass or more), 60% by mass or less (preferably 50% by mass) with respect to the total amount of the functional powder and PTFE. Mass% or less, more preferably 45 mass% or less).
- the composite sheet may contain other fluororesin as necessary in addition to the PTFE.
- the fluororesin include, for example, a copolymer of tetrafluoroethylene (a fluorine atom-containing monomer such as hexafluoropolypropylene, a copolymer with a monomer not containing a fluorine atom such as ethylene), a polyvinylidene fluoride resin, Examples include polychlorotrifluoroethylene resin.
- the amount of the fluororesin in the composite sheet is, for example, 0.5% by mass or more, preferably 5% by mass or more, and more preferably 10% by mass or more.
- the amount of the fluororesin in the composite sheet is, for example, 65% by mass or less, preferably 50% by mass or less, and more preferably about 30% by mass or less.
- the composite sheet in the present invention can be produced by forming a sheet (mixture, slurry, etc.) in which the functional powder, PTFE, and other fluororesin are mixed as required.
- the mixing method and sheeting method are not particularly limited, and those skilled in the art can implement the method with appropriate modifications.
- Examples of the manufacturing method are as follows. That is, the mixture (mixture, slurry, etc.) can be prepared according to a known method.
- the mixture can be prepared by a dry method or a wet method, and the slurry can be prepared by a wet method.
- the dry method is a method of mixing fine powder of functional powder and fine powder of PTFE. That is, in the dry method, the fine powder is put into an appropriate mixer (for example, V blender), mixed with stirring, and further, an appropriate processing aid (for example, mineral spirits) is added and absorbed into the mixture.
- an admixture can be prepared.
- the fine powder of functional powder can be obtained by pulverizing the functional powder with a known pulverizer (eg, ball mill, pin mill, homogenizer, etc.), and PTFE fine powder is commercially available. It is easy to do. In the process of absorbing the processing aid, it is recommended that the processing aid is added to the mixture and then heated appropriately (for example, about 40 to 60 ° C., particularly about 50 ° C.).
- a known pulverizer eg, ball mill, pin mill, homogenizer, etc.
- PTFE fine powder is commercially available. It is easy to do.
- the processing aid is added to the mixture and then heated appropriately (for example, about 40 to 60 ° C., particularly about 50 ° C.).
- the wet method is a method of mixing functional powder and PTFE in water. That is, in the wet method, a slurry (ink) can be prepared by mixing a raw material (functional powder, PTFE) finely dispersed to water in the presence of a surfactant. When the slurry (ink) is mechanically sheared or a precipitant (alcohol or the like) is added during the mixing, the functional powder and PTFE co-precipitate. After the coprecipitate is collected by filtration and dried, an admixture can be prepared by absorbing a suitable processing aid in the same manner as in the dry method.
- a slurry (ink) can be prepared by mixing a raw material (functional powder, PTFE) finely dispersed to water in the presence of a surfactant.
- a precipitant alcohol or the like
- the fine functional powder may be prepared in the same manner as the dry method, but is added to water together with a surfactant and dispersed in the liquid while being pulverized by a liquid pulverizing means (for example, a homogenizer). Is simple.
- a liquid pulverizing means for example, a homogenizer.
- PTFE it is convenient to use a commercially available aqueous PTFE dispersion.
- a PTFE paste extrusion method can be applied. That is, the admixture is pelletized by preforming, the pellet is extruded from a die or the like, and dried (extrusion molding method). The pellet is extruded into a string by an extruder, and the string is transferred between two rolls.
- Various known methods such as a method of rolling and drying (bead rolling method) can be used.
- the composite sheet may be a porous body, and the thickness and air permeability (porous property) of the composite sheet can be adjusted by appropriately devising the sheet forming step. For example, when the primary molded sheet is thick in the extrusion molding method or the bead rolling method, the roll rolling may be repeated until the sheet has a predetermined thickness. Depending on the production conditions, the density may increase too much and the air permeability may decrease. In such a case, the air permeability can be improved by stretching. Thus, sheet thickness and air permeability can be adjusted by appropriately combining rolling and stretching.
- coating and drying may be repeated until the composite sheet reaches a predetermined thickness, and rolling and stretching may be employed as appropriate in order to further adjust the thickness and air permeability.
- the electrical resistance with respect to the thickness direction of a composite sheet can also be adjusted by rolling and extending
- the drying process of the extrusion molding method or the bead rolling method it is recommended to heat to a temperature (for example, about 150 to 300 ° C., particularly about 200 ° C.) at which the processing aid (such as mineral spirits) can be volatilized and removed.
- a temperature at which water can be volatilized and removed for example, about 100 to 300 ° C., particularly about 120 ° C.
- organic impurities for example, surfactants used in the wet method.
- the moisture permeability of the composite sheet is remarkably increased.
- the moisture permeability can be lowered to an appropriate level by carbonizing the surfactant.
- the carbonization temperature is, for example, about 300 to 400 ° C. (particularly about 350 ° C.).
- the removal method of an organic impurity is not restricted to the said carbonization process,
- the various method according to the kind of impurity can be employ
- depending on the type of the surfactant it can be volatilized and removed by heating to 250 ° C. or higher, and it can also be extracted and removed using a solvent (for example, alcohols).
- the thickness of the gas diffusion layers 40 and 41 made of the composite sheet is, for example, 100 to 500 ⁇ m.
- the release film includes polypropylene, polyester, polycarbonate, cellophane (registered trademark), acetate, PTFE (polytetrafluoroethylene), PFA (tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer), FEP (tetrafluoroethylene-hexa).
- Fluoropropylene copolymer EPE (tetrafluoroethylene-hexafluoropropylene-perfluoroalkyl vinyl ether copolymer), ETFE (tetrafluoroethylene-ethylene copolymer), PCTFE (polychlorotrifluoroethylene), ECTFE (chloro) Trifluoroethylene-ethylene copolymer), PVF (polyvinyl fluoride), THV (tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride) Coalescence), VDF-HFP (vinylidene fluoride - hexafluoropropylene copolymer), TFE-P (vinylidene fluoride - propylene copolymer) include plastic films such as.
- polyester plastic films particularly those coated with a fluorine resin are desirable.
- the fluorine-based coated polyester unit bread FZ etc. may be used.
- the thickness of the release film is preferably 1 to 100 ⁇ m, more preferably 2 to 60 ⁇ m, considering the balance between ease of handling and cost. When it is 1 ⁇ m or more, it is easy to handle, and when it is 100 ⁇ m or less, the rigidity of the film does not become too high and it is easy to handle. Also, the cost can be reduced.
- the composite sheet is pressed on the release film at room temperature.
- the press processing method is not particularly limited, and those skilled in the art can implement the press processing with appropriate modifications. Examples are as follows. As shown in FIG. 2, a pressure-bonding mold in which a release film and a composite sheet are laminated on a pressure-bonding mold (lower mold) to which a PTFE sheet is pasted, and a PTFE sheet is pasted on the composite sheet. The composite sheet is sandwiched between molds (upper mold) and pressed for 1 second to 300 seconds under the conditions of 20 ° C. ⁇ 15 ° C. and 50 to 200 kgf / cm 2 , and the composite sheet is adhered to the release film. The composite sheet obtained by pressing the release film at room temperature is in close contact with the release film. In subsequent handling, there is no deviation between the release film and the composite sheet. No wrinkles or breaks.
- the composite sheet that has been pressed on the release film at room temperature is overlaid on the MEA and hot pressed.
- the composite sheet (not the release film) and the MEA are overlapped with each other so that the MEA is in contact. Since the composite sheet is pressed on the release film, it does not wrinkle or break even when it is stacked on the MEA.
- the hot press treatment method the same method as the press treatment method can be adopted except that it is not normal temperature but under heating.
- the heating temperature may be equal to or lower than the melting point or decomposition point of the release film material.
- the lower limit of the heating temperature is 80 ° C or higher, preferably 100 ° C or higher, and the upper limit of the heating temperature is 150 ° C or lower, preferably 140 ° C. It is as follows.
- the 180 degree peeling adhesive strength of the release film at this time is 0.005 N / cm or more and 0.025 N / cm or less.
- the adhesive strength is 0.005 N / cm or more, the composite sheet is sufficiently adhered to the release film, and there is no deviation between the composite sheet and the release film. There is no breakage.
- the adhesive strength is 0.025 N / cm or less, the release sheet can be easily peeled off when necessary.
- 180 degree peel adhesion strength is determined in accordance with JIS K6854-2: 1999, peel adhesion strength test method-second part: 180 degree peel.
- a method for measuring the peel adhesive strength will be described with reference to FIG.
- One end of the release film (20 mm width) that has been subjected to hot pressing is peeled off and folded. Hold the folded part of the release film with a fixed grip. Further, the composite sheet and the MEA are sandwiched by another fixed grip at the part where the release film is peeled off. As shown in FIG. 3, one fixed grip is moved at a moving speed of 100 mm / min and a moving distance of 200 mm at an angle of 180 degrees with respect to the other fixed grip. The tensile force applied to the fixed grip during the movement is measured, and the 180 ° peel adhesion strength is determined.
- part or all of the composite sheet is not transferred to the release film. Whether it is transferred or not is confirmed visually.
- the composite sheet contains conductive carbonaceous powder (carbon black, etc.) as a functional powder, if the composite sheet is transferred to the release film, the part transferred to the release film in black Can be visually confirmed.
- the present invention also relates to a product obtained by laminating a composite sheet on MEA manufactured by the above method.
- the composite sheet (gas diffusion layer) may be integrated also on the side where the composite sheet (gas diffusion layer) of the laminate is not integrated (MEA side).
- a single cell of a polymer electrolyte fuel cell can be produced by combining with separators 60 and 61.
- the present invention also relates to a laminate obtained by stacking a composite sheet containing a functional powder and polytetrafluoroethylene (PTFE) on a release film exclusively used in the above method, and pressing at room temperature.
- the 180-degree peel adhesion strength of the release film after normal temperature pressing is 0.005 N / cm or more and 0.025 N / cm or less.
- the adhesive strength is 0.005 N / cm or more
- the composite sheet is sufficiently adhered to the release film, and there is no deviation between the composite sheet and the release film. Or there is no breakage.
- the adhesive strength is 0.025 N / cm or less
- the release sheet can be easily peeled off when necessary. That is, with this laminate, the composite sheet can be easily handled even before hot pressing.
- the present invention also relates to the above laminate in the form of a roll.
- the composite sheet is superimposed on the release film and pressed at room temperature, and the composite sheet is sufficiently adhered to the release film. Even if this laminate is in the form of a roll, the composite sheet does not wrinkle or break. Even when taken out from the roll, the composite sheet is sufficiently adhered to the release film, so that the composite sheet does not wrinkle or break.
- the roll shape is advantageous in terms of storage and transportation.
- Acetylene black (conductive carbonaceous powder) was slowly poured into water so as not to scatter, and water was absorbed into acetylene black while stirring with a stir bar. Next, acetylene black was stirred and dispersed with a homogenizer to prepare an aqueous dispersion of acetylene black.
- a predetermined amount of an aqueous dispersion of PTFE [trade name: D1-E, manufactured by Daikin Industries, Ltd.] was added to the aqueous dispersion of acetylene black, and the mixture was slowly stirred with a stirrer to prepare a uniform mixed dispersion. Next, the rotation of the stirrer was increased to co-precipitate PTFE and acetylene black. The coprecipitate was collected by filtration, spread thinly on a stainless steel vat, and then dried for one day in a dryer at 120 ° C. to obtain a mixed powder of acetylene black (conductive carbonaceous powder) and PTFE.
- Mineral spirits (made by Idemitsu Kosan Co., Ltd., trade name: IP Solvent 1016) are added to this mixed powder as processing aids, pelletized with a pre-molding machine, the pellets are extruded into a tape with an extruder, and two rolls are added. It was used and rolled into a film. Furthermore, it rolled with two rolls over multiple times, and adjusted the thickness and density of the film. The rolled product is dried with a dryer at 200 ° C. for 8 hours to remove mineral spirits, and then heat treated at 350 ° C. for 5 minutes to obtain a composite sheet containing functional powder (acetylene black) and PTFE. It was.
- This composite sheet had a mass ratio of acetylene black to PTFE of 60/40, an average thickness of 25 ⁇ m, a moisture permeability of 3300 g / m 2 hr, and a penetration resistance of 8.2 m ⁇ cm 2 .
- the mass ratio, thickness, moisture permeability, and penetration resistance are values obtained as follows.
- Mass ratio The mass ratio was calculated based on the amount of acetylene black used and the solid content of the PTFE aqueous dispersion.
- the cross-sectional area of the humidity adjusting film was measured with an optical microscope, and the average thickness was determined by dividing the cross-sectional area by the base length.
- release film Various release films were used in Examples and Comparative Examples. The release film used is shown in Table 1.
- the composite sheet was stacked on the release film and pressed. As shown in FIG. 2, a pressure-bonding mold in which a release film and a composite sheet are laminated on a pressure-bonding mold (lower mold) to which a PTFE sheet is pasted, and a PTFE sheet is pasted on the composite sheet.
- the composite sheet and the release film were brought into close contact with each other by being sandwiched between the molds (upper mold) and pressed under a condition of 115 kgf / cm 2 for 4 minutes. Press processing was performed at a press temperature of normal temperature (25 ° C.) and high temperature (130 ° C.).
- Example 1 the composite sheet pressed at room temperature and the release film were in close contact with each other, and peeling did not occur spontaneously. Even when hot pressing at 130 ° C., the composite sheet and the release film are not fused, and a low peel strength is maintained, and the release film remains a residue of the composite sheet (CB / PTFE). There was no (that is, no transfer), and it could be easily removed.
- Example 1 Films other than Example 1 (Comparative Example) had a problem in either the normal temperature press or the adhesive strength after 130 ° C. hot press. It was also confirmed that the adhesive strength was too strong and the CB / PTFE composite sheet was destroyed when the release film was peeled off. In some cases, when the release film was peeled off, the residue of the CB / PTFE composite sheet was transferred to the release film side. In some cases, the adhesive force was too low, causing a deviation between the release film and the composite sheet, and the composite sheet was wrinkled or broken.
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Abstract
Description
アノード電極反応:H2→2H++2e−
カソード電極反応:1/2O2+2H++2e−→H2O
機能性粉体およびポリテトラフルオロエチレン(PTFE)を含んでなる複合化シートを用意し;
離型フィルムを用意し;
該複合化シートを該離型フィルムに重ねて常温でプレス処理し;
該離型フィルムに常温でプレス処理された該複合化シートを、該MEAに重ねて熱プレス処理し;そして
該離型フィルムを該複合化シートから剥離すること、
を含んでなる、該MEAに、該複合化シートを積層する方法。
アセチレンブラック(導電性炭素質粉末)を飛散させないようにゆっくりと水中に投じ、攪拌棒でかき混ぜながら水をアセチレンブラックに吸収させた。次いでホモジナイザーでアセチレンブラックを攪拌分散させ、アセチレンブラックの水分散液を作成した。
使用したアセチレンブラック量、及びPTFE水分散液の固形分量に基づき、質量比を算出した。
湿度調整フィルムの断面積を光学顕微鏡によって測定し、この断面積を底辺長さで除することによって平均厚さを求めた。
JIS L 1099(B−1)法に従って透湿度を求めた。
湿度調整フィルムを一対の金メッキを施した平滑な金属ブロック(面積2cm2)で挟み[圧力:981kPa(10kgf/cm2)、4端子法]、室温で1kHzの交流(電流:100mA)を流したときの抵抗値をmΩメーター(アデックス(株)製、商品名:Digital Battery mΩ Meter(Model AX−126B)で測定し、下記式に従って貫通抵抗を求めた。
貫通抵抗(mΩcm2)=測定抵抗値(mΩ)×2(cm2)
実施例および比較例において、種々の離型フィルムを用いた。用いた離型フィルムを表1に示す。
複合化シートを離型フィルムに重ねてプレス処理を行った。図2に示すように、PTFEシートを貼った圧着用金型(下側の金型)に、離型フィルムと複合化シートを積層し、複合化シートの上からPTFEシートを貼った圧着用金型(上側の金型)で挟み、115kgf/cm2の条件下で4分間プレスして、複合化シートと離型フィルムを密着させた。常温(25℃)と高温(130℃)のプレス温度で、プレス処理を行った。
常温と130℃でプレス処理された複合化シートと離型フィルムを、それぞれ引張り試験機を使用してJIS K 6854−2に準拠した方法により測定を行った。剥離接着強さの測定方法の概略を図3に示す。熱プレス処理された離型フィルム(20mm幅)の一端を剥離して、折り返す。離型フィルムの折り返し部分を固定つかみで挟む。また、複合化シートを、離型フィルムが剥離された部分で、別の固定つかみで挟む。図3のように、一方の固定つかみを、もう一方の固定つかみに対して180度の角度で、移動速度100mm/分で移動距離200mmを移動させた。移動時に固定つかみにかかる引張り力を測定し、180度剥離接着強さを求めた。結果を、表1に示す。
20、21 触媒電極層
40、41 ガス拡散層
60、61 セパレータ
50a、51a 燃料ガス及び酸素含有ガス(酸化剤ガス)の入口側部分
50b、51b 燃料ガス及び酸素含有ガス(酸化剤ガス)の出口側部分
Claims (10)
- 膜電極接合体(MEA)を用意し;
機能性粉体およびポリテトラフルオロエチレン(PTFE)を含んでなる複合化シートを用意し;
離型フィルムを用意し;
該複合化シートを該離型フィルムに重ねて常温でプレス処理し;
該離型フィルムに常温でプレス処理された該複合化シートを、該MEAに重ねて熱プレス処理し;そして
該離型フィルムを該複合化シートから剥離すること、
を含んでなる、該MEAに、該複合化シートを積層する方法。 - 該離型フィルムを該複合化シートから剥離するときに、該離型フィルムの180度剥離接着強さ(JIS K6854−2:1999準拠)が0.005N/cm以上であり、0.025N/cm以下であることを特徴とする、請求項1に記載の方法。
- 該熱プレス処理の温度が100℃~140℃の範囲であることを特徴とする、請求項1または2に記載の方法。
- 該機能性粉体が、少なくともカーボンブラック、活性炭またはそれらの混合物を含むことを特徴とする、請求項1~3のいずれか1項に記載の方法。
- 該複合化シートが多孔質体であることを特徴とする、請求項1~4のいずれか1項に記載の方法。
- 該離型フィルムを該複合化シートから剥離した後に、離型フィルムに該複合化シートの一部または全部が転写されていないことを特徴とする、請求項1~5のいずれか1項に記載の方法。
- 該離型フィルムに常温でプレス処理した該複合化シートにおいて、該離型フィルムと該複合化シートとのズレが生じず、該複合化シートのシワまたは折れが生じないことを特徴とする、請求項1~6のいずれか1項に記載の方法。
- 請求項1~7のいずれか1項に記載の方法によって製造される、MEAに複合化シートを積層した物。
- 請求項1~7のいずれか1項に記載の方法に専ら使用する離型フィルムに、機能性粉体およびポリテトラフルオロエチレン(PTFE)を含んでなる複合化シートを重ねて常温でプレス処理したことを特徴とする積層物。
- ロール状の形態であることを特徴とする、請求項9に記載の積層物。
Priority Applications (4)
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KR1020137002063A KR20130038346A (ko) | 2010-07-01 | 2011-07-01 | 이형 필름을 이용하여 복합화 시트를 적층하는 방법, 그 방법에 의한 적층물, 및 그 방법에 이용하는 이형 필름 |
EP11801035.4A EP2589493A4 (en) | 2010-07-01 | 2011-07-01 | METHOD OF LAMINATING A COMPOSITE PLATE USING A SEPARATING FOIL, LAMINATE OBTAINED BY THE METHOD AND SEPARATING FILM FOR USE IN THE METHOD |
US13/805,133 US9005839B2 (en) | 2010-07-01 | 2011-07-01 | Method for laminating composite sheet using release film, laminate obtained by the method, and release film for use in the method |
CA2803813A CA2803813A1 (en) | 2010-07-01 | 2011-07-01 | Method for laminating composite sheet using release film, laminate formed by same method, and release film used in same method |
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JP2010151319A JP5725744B2 (ja) | 2010-07-01 | 2010-07-01 | 離型フィルムを用いて複合化シートを積層する方法、その方法による積層物、ならびにその方法に用いる離型フィルム |
JP2010-151319 | 2010-07-01 |
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EP2871152B1 (en) | 2013-11-06 | 2017-05-24 | Sensirion AG | Sensor device |
JP6974343B2 (ja) | 2016-03-11 | 2021-12-01 | ダブリュ.エル.ゴア アンド アソシエイツ, インコーポレイティドW.L. Gore & Associates, Incorporated | 反射性ラミネート |
KR101949933B1 (ko) * | 2016-07-25 | 2019-02-21 | 현대자동차주식회사 | 연료전지용 막-전극 어셈블리의 표면 발수성 증대를 위한 다공성 필름 레이어를 포함하는 이형지 |
CN111837279B (zh) * | 2018-02-02 | 2024-06-25 | 凸版印刷株式会社 | 膜电极接合体及固体高分子型燃料电池 |
CN112639169B (zh) * | 2018-09-21 | 2023-12-01 | 旭化成株式会社 | 层积体、层积体的保存方法、层积体的输送方法、保护层积体及其卷绕体 |
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- 2010-07-01 JP JP2010151319A patent/JP5725744B2/ja not_active Expired - Fee Related
-
2011
- 2011-07-01 CA CA2803813A patent/CA2803813A1/en not_active Abandoned
- 2011-07-01 US US13/805,133 patent/US9005839B2/en not_active Expired - Fee Related
- 2011-07-01 KR KR1020137002063A patent/KR20130038346A/ko not_active Application Discontinuation
- 2011-07-01 WO PCT/JP2011/065631 patent/WO2012002579A1/ja active Application Filing
- 2011-07-01 EP EP11801035.4A patent/EP2589493A4/en not_active Withdrawn
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CA2803813A1 (en) | 2012-01-05 |
JP5725744B2 (ja) | 2015-05-27 |
EP2589493A1 (en) | 2013-05-08 |
US9005839B2 (en) | 2015-04-14 |
KR20130038346A (ko) | 2013-04-17 |
US20130157163A1 (en) | 2013-06-20 |
JP2012011700A (ja) | 2012-01-19 |
EP2589493A4 (en) | 2014-02-26 |
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