US20130302722A1 - Gasketed subassembly for use in fuel cells including replicated structures - Google Patents
Gasketed subassembly for use in fuel cells including replicated structures Download PDFInfo
- Publication number
- US20130302722A1 US20130302722A1 US13/940,773 US201313940773A US2013302722A1 US 20130302722 A1 US20130302722 A1 US 20130302722A1 US 201313940773 A US201313940773 A US 201313940773A US 2013302722 A1 US2013302722 A1 US 2013302722A1
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- United States
- Prior art keywords
- gasket
- cathode
- anode
- electrode plate
- subassembly
- Prior art date
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- Abandoned
Links
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Images
Classifications
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- H01M2/08—
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/10—Primary casings; Jackets or wrappings
- H01M50/183—Sealing members
-
- 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
- H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
-
- 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
- H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
- H01M8/0273—Sealing or supporting means around electrodes, matrices or membranes with sealing or supporting means in the form of a frame
-
- 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
- H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
- H01M8/0276—Sealing means characterised by their form
-
- 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
- H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
- H01M8/0286—Processes for forming seals
-
- 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
- H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
- H01M8/028—Sealing means characterised by their material
- H01M8/0284—Organic resins; Organic polymers
-
- 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]
-
- 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
- Y02E60/10—Energy storage using batteries
-
- 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
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T29/00—Metal working
- Y10T29/49—Method of mechanical manufacture
- Y10T29/49002—Electrical device making
- Y10T29/49108—Electric battery cell making
- Y10T29/4911—Electric battery cell making including sealing
Definitions
- FIGS. 4 a - 4 d are top view illustrations of replicated structures suitable for use in gaskets of the electrochemical device subassemblies of the present invention.
- FIG. 5 is an illustration of a suitable extrusion system for forming a gasket film for use in electrochemical device subassemblies of the present invention.
- MEA 12 is the portion of subassembly 10 that produces electricity during operation by separating fuel into hydrogen ions (H + ) and electrons (e ⁇ ).
- MEA 12 includes electrolyte membrane 22 , anode catalyst layer 24 , cathode catalyst layer 26 , anode gas diffusion layer 28 , cathode gas diffusion layer 30 , and subgaskets 31 a and 31 b .
- Electrolyte membrane 22 includes first surface 22 a and second surface 22 b, which are opposing major surfaces, and peripheral edge 22 c, which defines an outer perimeter of electrolyte membrane 22 .
- Anode gas diffusion layer 28 is disposed adjacent anode catalyst layer 24 , opposite electrolyte membrane 22 .
- cathode gas diffusion layer 30 is disposed adjacent cathode catalyst layer 26 , opposite electrolyte membrane 22 .
- Anode gas diffusion layer 28 and cathode gas diffusion layer 30 may each be formed from any suitable electrically conductive porous substrate, such as carbon fiber constructions (e.g., woven and non-woven carbon fiber constructions), and may also be treated to increase or impart hydrophobic properties.
- Subgaskets 31 a and 31 b are thin-layer gaskets for providing additional seal protection, and for strengthening electrolyte membrane 22 at peripheral portion 22 c. As shown in FIG. 1 a , subgasket 31 a is secured to first surface 22 a and subgasket 31 b is secured to second surface 22 b. While not shown in FIG. 1 a , subgasket 31 a may also partially extend between anode catalyst layer 24 and anode gas diffusion layer 28 , and subgasket 31 b may also partially extend between cathode catalyst layer 26 and cathode gas diffusion layer 30 . This increases the seal between anode gas diffusion layer 28 and cathode gas diffusion layer 30 to prevent fuel and oxidant from mixing outside of MEA 12 . Examples of suitable subgaskets for subgaskets 31 a and 31 b are disclosed in the pending U.S. patent application (attorney docket no. 59691US002), which is commonly assigned.
- seals are already formed between replicated structures 40 and 42 and recessed surfaces 48 and 50 . Compression may continue until good electrical contact is made between MEA 12 and anode electrode plate 18 and cathode electrode plate 20 , respectively. However, additional compression is not required for the purpose of forming seals.
- peripheral edge 22 c of electrolyte membrane 22 is coextensive with the anode gasket 14 and cathode gasket 16 .
- base layers 32 and 36 are substantially secured to peripheral edge 22 c.
- anode gasket 14 and cathode gasket 16 may be formed without base layers 32 and 36 . This reduces costs for manufacturing anode gasket 14 and cathode gasket 16 .
- anode electrode plate 18 and cathode electrode plate 20 may be standard electrode plates that do not contain recessed surfaces 46 and 50 . This embodiment applies higher compression forces to anode gasket 14 and cathode gasket 16 when anode electrode plate 18 and cathode electrode plate 20 compress together.
- Anode gasket 114 and cathode gasket 116 may also be respectively secured to recessed surfaces 146 and 150 with adhesive layers (not shown).
- Anode gasket 114 and cathode gasket 116 provide seals for subassembly 110 and reduce the risk of over-compressing MEA 112 in the same manner as discussed above for anode gasket 14 and cathode gasket 16 in FIGS. 1 a and 1 b.
- peripheral edge 222 c of electrolyte membrane 222 may alternatively extend less than the entire area between cathode gasket 216 and recessed surface 250 (i.e., not coextensive with cathode gasket 216 ). This allows a portion of cathode gasket 250 to be compressed directly against recessed surface 250 to form a seal.
- the base layers of the gaskets films may be connected to subgaskets (e.g., subgaskets 31 a and 31 b ), which are correspondingly secured to the films to the opposing surfaces of the electrolyte membrane at the peripheral edge of the electrolyte membrane.
- subgaskets e.g., subgaskets 31 a and 31 b
- the resulting subassembly may then be compressed to form a seal, as discussed above.
- Nip rollers 322 and 324 are smooth rollers disposed adjacent cast roller 320 to apply a pressure against gasket film 314 (e.g., about 100 pounds/linear inch to about 400 pounds/linear inch). Gasket film 314 is oriented such that elastomeric layer 318 faces cast roller 320 and base layer 316 faces nip roller 322 .
- FIG. 6 is an illustration of coating system 400 , which is another suitable system for forming gaskets (e.g., anode gasket 14 ) in a continuous process.
- Coating system 400 includes two-component dispenser 402 , feed spool 404 , receiving spool 406 , idle rollers 408 and 410 , and wheel system 412 .
- Two-component dispenser 402 is a dispenser and static mixer suitable for combining two-part materials, such as silicone elastomers, for forming elastomeric layer 414 .
- Feed spool 404 is a feed source for film of base layer 416 . The film of base layer 416 may be unwound from feed spool 404 and passed over idle roller 408 to meet with the material of elastomeric layer 414 at wheel system 412 .
- the material of elastomeric layer 414 is laminated against the film of base layer 416 , where the material of elastomeric layer 414 faces patterned sleeve 426 of drum wheel 422 , and the film of base layer 416 faces nip roller 418 .
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Fuel Cell (AREA)
- Gasket Seals (AREA)
Abstract
The present invention is an electrochemical device subassembly that includes a membrane electrode assembly and a gasket. The membrane electrode assembly includes an electrolyte membrane having a first major surface, a second major surface opposite the first major surface, and a peripheral edge. The gasket is disposed adjacent the first major surface of the electrolyte membrane at the peripheral edge, and has a plurality of replicated structures that extend greater than about 250 micrometers from a surface of the gasket.
Description
- Fuel cells are electrochemical devices that produce usable electricity by the catalyzed combination of a fuel such as hydrogen and an oxidant such as oxygen. In contrast to conventional power plants, such as internal combustion generators, fuel cells do not utilize combustion. As such, fuel cells produce little hazardous effluent. Fuel cells convert hydrogen fuel and oxygen directly into electricity, and can be operated at higher efficiencies compared to internal combustion generators. Because individual fuel cells do not produce much energy (e.g., between about 0.7-0.9 volts), multiple fuel cells may be arranged together in a stack to generate enough electricity to operate motor vehicles and supply electricity to remote locations.
- A fuel cell, such as a proton exchange membrane (PEM) fuel cell, typically contains a membrane electrode assembly (MEA) formed by a catalyst coated membrane disposed between a pair of gas diffusion layers. The catalyst coated membrane itself typically includes an electrolyte membrane disposed between a pair of catalyst layers. The respective sides of the electrolyte membrane are referred to as an anode portion and a cathode portion. In a typical PEM fuel cell, hydrogen fuel is introduced into the anode portion, where the hydrogen reacts and separates into protons and electrons. The electrolyte membrane transports the protons to the cathode portion, while allowing a current of electrons to flow through an external circuit to the cathode portion to provide power. Oxygen is introduced into the cathode portion and reacts with the protons and electrons to form water and heat.
- MEAs are typically sealed with gaskets to prevent pressurized gases from escaping. Seals are typically formed by compressing the gaskets and MEAs between electrode plates. However, a common problem with this method is that assemblers may over-compress the MEAs to ensure that the seals do not leak. Accordingly, over-compression may cause the anode portions and the cathode portions of the MEAs to contact through the respective electrolyte membranes, resulting in electrical shorts.
- The present invention is an electrochemical device subassembly that includes a MEA and a gasket. The MEA includes an electrolyte membrane having a first major surface, a second major surface opposite the first major surface, and a peripheral edge. The gasket is disposed adjacent the first major surface at the peripheral edge of the electrolyte membrane, and has a plurality of replicated structures that extend greater than about 250 micrometers from a surface of the gasket. The replicated structures allow the gasket to function as a seal to prevent pressurized gas from escaping the MEA during use, and also reduce the risk of over-compressing the MEA during manufacturing.
- In one embodiment, the present invention may also include a second gasket disposed adjacent the second major surface at the peripheral edge of the electrolyte membrane. The second gasket may also have a plurality of replicated structures that extend greater than about 250 micrometers from a surface of the second gasket. The present invention further relates to a method of forming the subassembly and to an electrochemical device (e.g., a fuel cell) that includes the subassembly.
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FIG. 1 a is a sectional view of a peripheral portion of an electrochemical device subassembly of the present invention in an uncompressed state. -
FIG. 1 b is a sectional view of the peripheral portion of the electrochemical device subassembly of the present invention in a compressed state. -
FIG. 2 a is a sectional view of a peripheral portion of an alternative electrochemical device subassembly of the present invention in an uncompressed state. -
FIG. 2 b is a sectional view of the peripheral portion of the alterative electrochemical device subassembly of the present invention in a compressed state. -
FIG. 3 a is a sectional view of a peripheral portion of a second alternative electrochemical device subassembly of the present invention in an uncompressed state. -
FIG. 3 b is a sectional view of the peripheral portion of the second alterative electrochemical device subassembly of the present invention in a compressed state. -
FIGS. 4 a-4 d are top view illustrations of replicated structures suitable for use in gaskets of the electrochemical device subassemblies of the present invention. -
FIG. 5 is an illustration of a suitable extrusion system for forming a gasket film for use in electrochemical device subassemblies of the present invention. -
FIG. 6 is an illustration of a suitable coating system for forming a gasket film for use in electrochemical device subassemblies of the present invention - While the above-identified drawing figures set forth several embodiments of the invention, other embodiments are also contemplated, as noted in the discussion. In all cases, this disclosure presents the invention by way of representation and not limitation. It should be understood that numerous other modifications and embodiments can be devised by those skilled in the art, which fall within the scope and spirit of the principles of the invention. The figures may not be drawn to scale. Like reference numbers have been used throughout the figures to denote like parts.
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FIGS. 1 a and 1 b are sectional views of a peripheral portion of electrochemical device subassembly 10 of the present invention, whereFIG. 1 a depicts subassembly 10 in an uncompressed state during manufacturing, andFIG. 1 b depicts subassembly 10 in a compressed state for use in an electrochemical device, such as a fuel cell. The peripheral portion ofsubassembly 10 shown inFIGS. 1 a and 1 b is representative of an entire periphery ofsubassembly 10. - As shown in
FIG. 1 a,subassembly 10 includesMEA 12,anode gasket 14,cathode gasket 16,anode electrode plate 18, andcathode electrode plate 20. MEA 12,anode gasket 14, andcathode gasket 16 are disposed betweenanode electrode plate 18 andcathode electrode plate 20.Anode gasket 14 and cathode gasket 16 face opposing directions in a back-to-back orientation, and are generally planar withMEA 12. As discussed below, whensubassembly 10 is used in a fuel cell,anode electrode plate 18 andcathode electrode plate 20 are compressed together againstMEA 12,anode gasket 14, andcathode gasket 16. The compression creates a first seal betweenanode gasket 14 andanode electrode plate 18, and a second seal betweencathode gasket 16 andcathode electrode plate 20. The seals prevent pressurized gases from escaping subassembly 10 during operation. -
MEA 12 is the portion ofsubassembly 10 that produces electricity during operation by separating fuel into hydrogen ions (H+) and electrons (e−). MEA 12 includeselectrolyte membrane 22,anode catalyst layer 24,cathode catalyst layer 26, anodegas diffusion layer 28, cathodegas diffusion layer 30, andsubgaskets Electrolyte membrane 22 includesfirst surface 22 a andsecond surface 22 b, which are opposing major surfaces, andperipheral edge 22 c, which defines an outer perimeter ofelectrolyte membrane 22. Examples of suitable materials forelectrolyte membrane 22 include acid-functional fluoropolymers, such as copolymers of tetrafluoroethylene and one or more fluorinated, acid-functional comonomers. Examples of suitable commercially available materials include fluoropolymers under the trade designations “NAFION” from DuPont Chemicals, Wilmington, Del.. -
Anode catalyst layer 24 is disposed adjacentfirst surface 22 a, andcathode catalyst layer 26 is disposed adjacentsecond surface 22 b. Examples of suitable materials foranode catalyst layer 24 andcathode catalyst layer 26 include carbon-supported catalyst particles, which include carbon particles and a catalyst metal, where the catalyst metal may include platinum and ruthenium for the anode catalyst layers and platinum for the cathode catalyst layers. The catalyst materials may also be applied toelectrolyte membrane 22 as a catalyst ink, which includes the catalyst particles and electrolyte membrane materials dispersed in an aqueous or alcohol dispersion. - Anode
gas diffusion layer 28 is disposed adjacentanode catalyst layer 24,opposite electrolyte membrane 22. Similarly, cathodegas diffusion layer 30 is disposed adjacentcathode catalyst layer 26,opposite electrolyte membrane 22. Anodegas diffusion layer 28 and cathodegas diffusion layer 30 may each be formed from any suitable electrically conductive porous substrate, such as carbon fiber constructions (e.g., woven and non-woven carbon fiber constructions), and may also be treated to increase or impart hydrophobic properties. -
Subgaskets electrolyte membrane 22 atperipheral portion 22 c. As shown inFIG. 1 a,subgasket 31 a is secured tofirst surface 22 a and subgasket 31 b is secured tosecond surface 22 b. While not shown inFIG. 1 a,subgasket 31 a may also partially extend betweenanode catalyst layer 24 and anodegas diffusion layer 28, andsubgasket 31 b may also partially extend betweencathode catalyst layer 26 and cathodegas diffusion layer 30. This increases the seal between anodegas diffusion layer 28 and cathodegas diffusion layer 30 to prevent fuel and oxidant from mixing outside ofMEA 12. Examples of suitable subgaskets forsubgaskets - Examples of
suitable thicknesses 12 t ofMEA 12 range from about 200 micrometers to about 1,000 micrometers, with particularlysuitable thicknesses 12 t ofMEA 12 ranging from about 300 micrometers to about 500 micrometers. All thicknesses discussed herein refer to thicknesses in uncompressed states (i.e., whereanode electrode plate 18 andcathode electrode plate 20 are not compressed together), and are taken in a direction along axis A inFIG. 1 a. -
Anode gasket 14 andcathode gasket 16 are respectively secured to subgaskets 31 a and 31 b atperipheral edge 22 c ofelectrolyte membrane 22. This allowsanode gasket 14 andcathode gasket 16 to seal the entire periphery ofsubassembly 10.Anode gasket 14 includesbase layer 32 andelastomeric layer 34, andcathode gasket 16 includesbase layer 36 andelastomeric layer 38.Anode gasket 14 andcathode gasket 16 may also include adhesive layers (not shown) disposed between the respective base layers and elastomeric layers for reducing the risk of interlayer delamination. - Base layers 32 and 38 are low-compression layers that may function as hard stops for strain control, limit the compressive forces applied to
MEA 12, and provide for ease of handling ofsubassembly 10 during manufacturing. Elastomeric layers 34 and 38 are compressible layers that include replicatedstructures structures FIG. 1 a. If viewed from above, replicatedstructures elastomeric layers structures anode gasket 14 andcathode gasket 16. - As further shown in
FIG. 1 a,peripheral edge 22 c ofelectrolyte membrane 22 is not co-extensive withanode gasket 14 andcathode gasket 16. As a result,anode gasket 14 andcathode gasket 16 extend beyondperipheral edge 22 c, and are secured together beyondperipheral edge 22 c. In particular,base layer 32 is secured to subgasket 31 a atperipheral edge 22 c and tobase layer 36 beyondperipheral edge 22 c. Similarly,base layer 36 is secured to subgasket 31 b atperipheral edge 22 c (and correspondingly tobase layer 32 beyondperipheral edge 22 c). Base layers 32 and 34 may also be secured together, and to subgaskets 31 a and 31 b, with adhesive layers (not shown). - Examples of suitable layer thicknesses 32 t and 36 t of base layers 32 and 36 range from about 20 micrometers to about 130 micrometers. Examples of suitable layer thicknesses 34 t and 36 t of
elastomeric layers 34 and 38 (not including replicatedstructures 40 and 42) also range from about 20 micrometers to about 130 micrometers. Examples ofsuitable thicknesses structures elastomeric layers suitable thicknesses anode gasket 14 and cathode gasket 16 (i.e., sum ofthicknesses thickness 12 t ofMEA 12. -
Anode electrode plate 18 andcathode electrode plate 20 are electrically-conductive electrode plates for fuel cells, which provide structural support toMEA 12.Anode electrode plate 18 includescontact surface 44 and recessedsurface 46, andcathode electrode plate 20 includescontact surface 48 and recessedsurface 50.Contact surface 44 is the portion ofanode electrode plate 18 that compresses against anodegas diffusion layer 28 ofMEA 12 and recessedsurface 46 is the portion ofanode electrode plate 18 that compresses against replicatedstructures 40 ofanode gasket 14. Similarly,contact surface 48 is the portion ofcathode electrode plate 20 that compresses against cathodegas diffusion layer 30 ofMEA 12 and recessedsurface 50 is the portion ofcathode electrode plate 20 that compresses against replicatedstructures 42 ofcathode gasket 16. - Recessed surfaces 46 and 50 are respectively offset from
contact surfaces anode gasket 14 andcathode gasket 16. Recessedsurface 46 is desirably offset fromcontact surface 44 such that the gap between replicatedstructures 40 and recessedsurface 46 is less than the gap between anodegas diffusion layer 28 ofMEA 12 andcontact surface 44. Similarly, recessedsurface 50 is also desirably offset fromcontact surface 48 such that the gap between replicatedstructures 42 and recessedsurface 50 is desirably less than the gap between cathodegas diffusion layer 30 ofMEA 12 andcontact surface 48. This allows the seals to be formed before, or concurrently with, contact surfaces 44 and 48 reachingMEA 12. As a result, the amount of compression applied toMEA 12 may be minimized, thereby reducing the risk ofover-compressing MEA 12. - Examples of
suitable thicknesses anode electrode plate 18 andcathode electrode plate 20 each range from about 1,500 micrometers to about 2,100 micrometers. Examples of suitable offset distances 46 t and 48 t of recessedsurfaces contact surfaces - While
subassembly 10 is illustrated as a symmetric component inFIG. 1 a, one or more ofthicknesses 32 t-42 t may alternatively differ from one another. For example, thicknesses 40 t and 42 t of replicatedstructures distances contact surfaces -
Anode electrode plate 18 andcathode electrode plate 20 each also include flow channels (not shown) for directing fuel and oxidant toMEA 12. In particular,anode electrode plate 18 provides a flow channel for supplying fuel toMEA 12, andcathode electrode plate 20 provides flow channels for supplying oxidant toMEA 12 and for removing water formed during the electrochemical reaction withinMEA 12. -
Anode electrode plate 18 andcathode electrode plate 20 may be unipolar plates or bipolar plates depending on the arrangement of the fuel cell. If the fuel cell is a single-cell body,anode electrode plate 18 andcathode electrode plate 20 are unipolar plates, whereanode electrode plate 18 functions as the anode electrode andcathode electrode plate 20 functions as the cathode electrode. Alternatively, if the fuel cell is part of a stack of fuel cells,anode electrode plate 18 andcathode electrode plate 20 may be bipolar plates, where each plate functions as an anode electrode for a first fuel cell and a cathode electrode for an adjacent fuel cell. For example,anode electrode plate 18 may function as the anode electrode for a first fuelcell containing subassembly 10, and as a cathode electrode for a second fuel cell disposed adjacent the first fuel cell, oppositeanode electrode plate 18. -
Subassembly 10 may be assembled by positioninganode electrode plate 18 andcathode electrode plate 20 relative toMEA 12,anode gasket 14, andcathode gasket 16 as shown inFIG. 1 a.Anode electrode plate 18 andcathode electrode plate 20 may then be compressed together. Asanode electrode plate 18 compresses towardMEA 12 andanode gasket 14, replicatedstructures 40 contact recessedsurface 46, and are compressed to form a first seal. Similarly, ascathode electrode plate 20 compresses towardMEA 12 andcathode gasket 16, replicatedstructures 42 contact recessedsurface 50, and are compressed to form a second seal. - As shown in
FIG. 1 b, whenanode electrode plate 18 andcathode electrode plate 20reach MEA 12, seals are already formed between replicatedstructures surfaces MEA 12 andanode electrode plate 18 andcathode electrode plate 20, respectively. However, additional compression is not required for the purpose of forming seals. - During operation of a fuel
cell containing subassembly 10, fuel (e.g., hydrogen gas) is introduced through the flow channels ofanode electrode plate 18, and into anodegas diffusion layer 28.MEA 12 may alternatively use other fuel sources, such as methanol, ethanol, formic acid, and reformed gases. The fuel passes through anodegas diffusion layer 28 and overanode catalyst layer 24. Atanode catalyst layer 24, the fuel is separated into hydrogen ions and electrons.Electrolyte membrane 22 only permits the hydrogen ions to pass through to reachcathode catalyst layer 26 and cathodegas diffusion layer 30. The electrons cannot pass throughelectrolyte membrane 22. As such, the electrons flow through an external circuit (not shown) betweenanode electrode plate 18 tocathode electrode plate 20 in the form of electric current. This current can power an electric load, such as an electric motor, or be directed to an energy storage device, such as a rechargeable battery. Oxidant (e.g., oxygen gas) is introduced through the flow channels ofcathode electrode plate 20, and into cathodegas diffusion layer 30. The oxidant passes through cathodegas diffusion layer 30 and overcathode catalyst layer 26. Atcathode catalyst layer 26, the oxidant, hydrogen ions, and electrons combine to produce water and heat. The resulting water may then exit the fuel cell through another flow channel incathode electrode plate 20. Furthermore, the seals provided byanode gasket 14 andcathode gasket 16 prevent the pressurized fuel and oxidant from escapingsubassembly 10. - In an alternative embodiment to subassembly 10,
peripheral edge 22 c ofelectrolyte membrane 22 is coextensive with theanode gasket 14 andcathode gasket 16. As a result, base layers 32 and 36 are substantially secured toperipheral edge 22 c. In a second alternative embodiment,anode gasket 14 andcathode gasket 16 may be formed without base layers 32 and 36. This reduces costs for manufacturinganode gasket 14 andcathode gasket 16. In a third alternative embodiment,anode electrode plate 18 andcathode electrode plate 20 may be standard electrode plates that do not contain recessedsurfaces anode gasket 14 andcathode gasket 16 whenanode electrode plate 18 andcathode electrode plate 20 compress together. -
FIGS. 2 a and 2 b are sectional views of a peripheral portion ofelectrochemical device subassembly 110, which is an alternative subassembly of the present invention.FIG. 2 a depictssubassembly 110 in an uncompressed state during manufacturing, andFIG. 2 b depicts subassembly 110 in a compressed state for use in an electrochemical device. As shown inFIG. 2 a,subassembly 110 is similar to subassembly 10 (respective reference labels increased by 100), except thatanode gasket 114 is secured to recessedsurface 146 ofanode electrode plate 118 andcathode gasket 116 is secured to recessedsurface 150 ofcathode electrode plate 120. This is in contrast to the back-to-back orientation shown ofanode gasket 14 andcathode gasket 16 ofsubassembly 10.Anode gasket 114 andcathode gasket 116 may also be respectively secured to recessedsurfaces Anode gasket 114 andcathode gasket 116 provide seals forsubassembly 110 and reduce the risk ofover-compressing MEA 112 in the same manner as discussed above foranode gasket 14 andcathode gasket 16 inFIGS. 1 a and 1 b. - Subassembly 110 may be assembled by compressing
anode electrode plate 118 andcathode electrode plate 120 together. Asanode electrode plate 118 compresses towardMEA 112, replicatedstructures 140contact subgasket 131 a atperipheral edge 122 c ofelectrolyte membrane 122. This compresses and deforms replicatedstructures 140 atperipheral edge 122 c. Similarly, ascathode electrode plate 120 compresses towardMEA 112, replicatedstructures 142contact subgasket 131 b atperipheral edge 122 c ofelectrolyte membrane 122. This compresses and deforms replicatedstructures 142 atperipheral edge 122 c. Furthermore, replicatedstructures 140 also contact replicatedstructures 142 beyondperipheral edge 122 c, which compress and deform these portions of replicatedstructures structures subassembly 110. - As shown in
FIG. 2 b, whenanode electrode plate 118 andcathode electrode plate 120contact MEA 112, a seal is already formed between replicatedstructures MEA 112 andanode electrode plate 118 andcathode electrode plate 120, respectively. However, additional compression is not required for the purpose of forming a seal. Subassembly 110 may then be used in a fuel cell in the same manner as discussed above inFIG. 1 b. -
FIGS. 3 a and 3 b are sectional views of a peripheral portion ofelectrochemical device subassembly 210, which is another alternative subassembly of the present invention.FIG. 3 a depictssubassembly 210 in an uncompressed state during manufacturing, andFIG. 3 b depicts subassembly 210 in a compressed state for use in an electrochemical device. As shown inFIG. 3 a,subassembly 210 is also similar to subassembly 10 (respective reference labels increased by 200), except thatanode gasket 214 andcathode gasket 216 are not secured toelectrolyte membrane 222. Instead,peripheral edge 222 c ofelectrolyte membrane 222 is bent to extend betweencathode gasket 216 andcathode electrode plate 220. This arrangement allowsperipheral edge 222 c to continue to function as a barrier between the fuel and oxidant introduced intoMEA 212. In this embodiment,anode gasket 214 andcathode gasket 216 provide seals forsubassembly 210, and also reduce the risk ofover-compressing MEA 212 in a similar manner to that discussed above foranode gasket 14 andcathode gasket 16 inFIGS. 1 a and 1 b. In an alternative arrangement,peripheral edge 222 c may extend betweenanode gasket 214 andanode electrode plate 218. Additionally,peripheral edge 222 c may also be disposed between a pair of subgaskets similar to subgaskets 31 a and 3 b discussed above inFIG. 1 a. - Subassembly 210 may be assembled by positioning
anode gasket 214 andcathode gasket 216 between recessedsurfaces anode gasket 214 andcathode gasket 216 are disposed adjacentperipheral edge 222 c ofelectrolyte membrane 222, as shown inFIG. 3 a. This embodiment is advantageous becauseanode gasket 214 andcathode gasket 216 are not required to be connected toelectrolyte membrane 222, which reduces the time required to manufacturesubassembly 210. Afteranode gasket 214 andcathode gasket 216 are inserted,anode electrode plate 218 andcathode electrode plate 220 may be compressed together, which compresses and deforms replicatedstructures structures FIGS. 1 a and 1 b. Additionally, the compression retainsanode gasket 214 andcathode gasket 216 betweenanode electrode plate 218 andcathode electrode plate 220. - As shown in
FIG. 3 b, whenanode electrode plate 218 andcathode electrode plate 220contact MEA 212, seals are already formed betweenperipheral edge 222 c ofelectrolyte membrane 222, replicatedstructures surfaces MEA 212 andanode electrode plate 218 andcathode electrode plate 220, respectively. However, additional compression is not required for the purpose of forming seals. Subassembly 210 may then be used in a fuel cell in the same manner as discussed above inFIG. 1 b. - In an alternative embodiment to subassembly 210,
anode gasket 214 andcathode gasket 216 may be formed without base layers 232 or 236. In this embodiment,anode gasket 214 andcathode gasket 216 may respectively include onlyelastomeric layers elastomeric layers anode gasket 214 andcathode gasket 216 may be formed as a single elastomeric layer with replicatedstructures peripheral edge 222 c ofelectrolyte membrane 222 may alternatively extend less than the entire area betweencathode gasket 216 and recessed surface 250 (i.e., not coextensive with cathode gasket 216). This allows a portion ofcathode gasket 250 to be compressed directly against recessedsurface 250 to form a seal. -
FIGS. 4 a-4 d are top view illustrations of different repeated-geometric patterns for replicatedstructures 40. While the repeated patterns shown inFIGS. 4 a-4 d refer to replicatedstructures 40, the repeated patterns are applicable to all embodiments of the present invention (e.g., replicatedstructures FIGS. 4 a and 4 b show replicatedstructures 40 as repeated-hexagonal patterns,FIG. 4 c shows replicatedstructures 40 as a repeated-heptagonal pattern, andFIG. 4 d shows replicatedstructures 40 as a repeated-square pattern. Replicatedstructures 40 may also include combinations of different repeated patterns. - As shown in
FIGS. 4 a-4 d, replicatedstructures 40 includewalls 40 a (the portions of replicatedstructures 40 viewable inFIGS. 1 a and 1 b) andintersections 40 b wherewalls 40 a meet. In addition to the suitable dimensions discussed above, replicatedstructures 40 desirably include repeated patterns where no more than three or fourwalls 40 a meet at any givenintersection 40 b. This increases compressibility and deformability, and distributes applied pressure to preserve the durability of replicatedstructures 40. Examples of suitable center-to-center distances of the repeated patterns of replicatedstructures 40 range from about 1,200 micrometers to about 3,200 micrometers. Examples of suitable thicknesses for each ofwalls 40 a range from about 250 micrometers to about 500 micrometers. - Replicated
structures 40 are also beneficial when holes are cut into the corresponding gaskets (e.g.,anode gasket 14 and cathode gasket 16). Holes may be cut in gaskets to accommodate various components of fuel cells. When holes are cut in conventional gaskets, o-rings are typically disposed around the holes to prevent leaks in the seals. However, when holes are cut in replicatedstructures 40, o-rings are not required becausewalls 40 a around the cut hole automatically provide an effective seal against leaking This reduces time and effort required to manufacturesubassembly 10 of the present invention. To preserve effective sealing, the gaskets ofsubassembly 10 desirably include from about one to about ten repeated patterns between any two openings and/or edges of the corresponding gasket. Even more desirably, the gaskets include from about two to about five repeated patterns between any two openings and/or edges of the corresponding gasket. - Examples of suitable materials for the elastomeric layers include elastomeric materials, such as rubbers, silicone elastomers, thermoplastic elastomers, thermoset elastomers, elastomeric adhesives, styrene-containing diblock and triblock copolymers, and combinations thereof. An example of a suitable combination of materials includes about 60% by weight of a melt processible thermoplastic elastomer commercially available under the trade designation “SANTOPRENE 101-64” from Advanced Elastomer Systems, Akron, Ohio, and about 40% by weight of a linear styrene-isoprene-styrene triblock copolymer commercially available under the trade designation “VECTOR 4211” from Dexco Polymers, Houston, Tex.
- As discussed above, the base layers have lower compressibilities compared to the elastomeric layers. The term “compressibility” herein refers to the amount of deformation a material exhibits when subjected to an applied pressure. Examples of suitable materials for the base layers include polyolefins (e.g., polypropylene and polyethylene), polyethylene terephthalate, polyethylene naphthalate, and combinations thereof. The suitable materials provide low-compressibilities for the base layers such that the base layers may function as hard stops for strain control during manufacturing. The low-compressibilities also provide for better handling of the gaskets prior to assembly.
- Gaskets suitable for use in the present invention (e.g., anode gasket 14) may be formed by fabricating a gasket film that includes an elastomeric layer (e.g., elastomeric layer 34), a base layer (e.g., base layer 32), and optionally an adhesive layer between the elastomeric layer and the base layer. The gasket film may be fabricated in a variety of manners, such as extrusion, drop casting, calendering, coating, and combinations thereof. For example, in one embodiment, the gasket film may be fabricated by co-extruding materials to form the base layer and the elastomeric layer. Replicated structures (e.g., replicated structures 40) may then be formed in the elastomeric layer, which may be performed by compression molding, injection molding, embossing, and combinations thereof. In an alternative embodiment, replicated structures may be formed in the elastomeric layer prior to securing the elastomeric layer to the base layer. In this embodiment, the elastomeric layer containing the replicated structures may be subsequently laminated to the base layer to form the gasket film.
- After fabrication, the gasket film may be cut or otherwise separated into individual gaskets (e.g.,
anode gasket 14 and cathode gasket 16). The gaskets may then be connected to a peripheral edge of an electrolyte membrane (e.g.,peripheral edge 22 c). This may be performed by connecting the base layers of the gasket films to the opposing surfaces of the electrolyte membrane at the peripheral edge of the electrolyte membrane. Alternatively, as discussed above inFIGS. 1 a-2 b, the base layers of the gaskets films may be connected to subgaskets (e.g., subgaskets 31 a and 31 b), which are correspondingly secured to the films to the opposing surfaces of the electrolyte membrane at the peripheral edge of the electrolyte membrane. The resulting subassembly may then be compressed to form a seal, as discussed above. -
FIG. 5 is an illustration ofextrusion system 300, which is a suitable system for forming gaskets (e.g., anode gasket 14) in a continuous process.Extrusion system 300 includesextruders neck tubes feedblock 310, androller system 312.Extruders Neck tubes extruders feedblock 310. -
Extruder 302 melts and extrudes materials for the elastomeric layer throughneck tube 306, and intofeedblock 310. Similarly,extruder 304 melts and extrudes materials for the base layer throughneck tube 308, and intofeedblock 310.Feedblock 310 orients the received materials and producesgasket film 314, which includesbase layer 316 andelastomeric layer 318.Gasket film 314 may then be drop cast intoroller system 312. In an alternative embodiment,extrusion system 300 may only includeextruder 302 for extrudingelastomeric layer 318. In this embodiment,base layer 316 may be provided in film form, and may be laminated toelastomeric layer 318 prior to enteringroller system 312. -
Roller system 312 includes castroller 320, niprollers idle roller 326.Cast roller 320 includes patternedsleeve 328, which is disposed around the annular surface ofcast roller 320.Patterned sleeve 328 may be a tooled metal sleeve or a solid polymer film (e.g., polyurethane) that contains a replicated pattern that is the negative of the replicated structures of the elastomeric layers (e.g., replicatedstructures 40 and 42).Nip rollers adjacent cast roller 320 to apply a pressure against gasket film 314 (e.g., about 100 pounds/linear inch to about 400 pounds/linear inch).Gasket film 314 is oriented such thatelastomeric layer 318 faces castroller 320 andbase layer 316 faces niproller 322. - As
gasket film 314 drops betweencast roller 320 and niproller 322, niproller 322 pressesgasket film 314 against patternedsleeve 328 ofcast roller 320. Portions ofelastomeric layer 318 are forced in the replicated patterns of patternedsleeve 328, which form the replicated structures inelastomeric layer 318.Cast roller 320 and niprollers Gasket film 314 disengages from patternedsleeve 328 after passing betweencast roller 320 and niproller 324. The resultinggasket film 314 with the replicated structures may then pass overidler roller 326 and be wound on a spool.Gasket film 314 may then be separated into separate gaskets and connected to electrolyte membranes to provide durable seals in the electrochemical device subassemblies discussed above. -
FIG. 6 is an illustration ofcoating system 400, which is another suitable system for forming gaskets (e.g., anode gasket 14) in a continuous process.Coating system 400 includes two-component dispenser 402, feedspool 404, receivingspool 406,idle rollers 408 and 410, andwheel system 412. Two-component dispenser 402 is a dispenser and static mixer suitable for combining two-part materials, such as silicone elastomers, for formingelastomeric layer 414.Feed spool 404 is a feed source for film ofbase layer 416. The film ofbase layer 416 may be unwound fromfeed spool 404 and passed over idle roller 408 to meet with the material ofelastomeric layer 414 atwheel system 412. -
Wheel system 412 includes niprollers drum wheel 422, andheat lamp system 424.Nip rollers adjacent drum wheel 422 to apply a pressure againstelastomeric layer 414 and base layer 416 (e.g., about 20 pounds/linear inch).Drum wheel 422 includes patternedsleeve 426, which is disposed around the annular surface ofdrum wheel 422.Patterned sleeve 426 may be a tooled metal sleeve or a solid polymer film (e.g., polyurethane) that contains a replicated pattern that is the negative of the replicated structures of the elastomeric layers (e.g., replicatedstructures 40 and 42).Heat lamp system 424 is a ring of heat sources that extend around the annular surface ofdrum wheel 422 and apply heat radially inward towarddrum wheel 422. For example,heat lamp system 424 may be a ring of infrared lamps for maintaining a temperature of about 70° C. in the vicinity ofdrum wheel 422. - In the embodiment shown in
FIG. 6 ,drum wheel 422 mechanically rotates in a counter-clockwise direction. This causes the material ofelastomeric layer 414 deposited ondrum wheel 422 from two-component dispenser 402 to be forced between niproller 418 anddrum wheel 422. Similarly, the film ofbase layer 416 extends around niproller 418 in a clock-wise direction, thereby also being forced between niproller 418 anddrum wheel 422. As a result, the material ofelastomeric layer 414 is laminated against the film ofbase layer 416, where the material ofelastomeric layer 414 faces patternedsleeve 426 ofdrum wheel 422, and the film ofbase layer 416 faces niproller 418. - As the material of
elastomeric layer 414 and the film ofbase layer 416 pass between niproller 418 anddrum wheel 422, niproller 418 presses the material ofelastomeric layer 414 against patternedsleeve 426 ofdrum wheel 422. Portions of the material ofelastomeric layer 414 are forced in the replicated patterns of patternedsleeve 426, which form the replicated structures inelastomeric layer 414. As the material ofelastomeric layer 414 and the film ofbase layer 416 rotate arounddrum wheel 422,heat lamp system 424 cures the material ofelastomeric layer 414. This formsgasket film 428 having elastomeric layer 414 (with replicated patterns) laminated onbase layer 416. - After rotating around
drum wheel 422,gasket film 428 disengages from patternedsleeve 426 after passing between niproller 420 anddrum wheel 422. The resultinggasket film 428 with the replicated structures may then pass overidler roller 410 and be wound on receivingspool 406.Gasket film 428 may then be separated into separate gaskets and connected to electrolyte membranes to provide durable seals in the electrochemical device subassemblies discussed above. - While the continuous processes discussed above in
FIGS. 5 and 6 are shown as suitable methods for forming gasket films for use in subassemblies of the present invention (e.g., subassembly 10), the continuous processes are also suitable for forming gasket films disclosed in Wald et al., U.S. Patent Application Publication No. 2003/0211378, which is commonly assigned. - Although the present invention has been described with reference to preferred embodiments, workers skilled in the art will recognize that changes may be made in form and detail without departing from the spirit and scope of the invention.
Claims (7)
1. A method of making an electrochemical device subassembly, the method comprising:
fabricating a gasket film comprising an elastomeric layer having replicated structures;
separating the gasket film into at least a first portion and a second portion;
connecting the first portion of the gasket film to a first major surface of an electrolyte membrane at a peripheral edge of the electrolyte membrane; and
connecting the second portion of the gasket film to a second major surface of the electrolyte membrane at the peripheral edge of the electrolyte membrane.
2. The method of claim 1 , wherein the gasket film further comprises a base layer secured to the elastomeric layer, the base layer having a lower compressibility than the elastomeric layer.
3. The method of claim 1 , wherein the first portion of the gasket film has a first gasket surface and the replicated structures of the first portion extend greater than about 250 micrometers from the first gasket surface, and wherein the second portion of the gasket film has a second gasket surface and the replicated structures of the second portion extend greater than about 250 micrometers from the second gasket surface.
4. The method of claim 1 , wherein fabricating the gasket film is selected from the group consisting of extrusion, drop casting, calendering, coating, and combinations thereof.
5. The method of claim 1 , further comprising forming the replicated structures in the elastomeric layer.
6. The method of claim 5 , wherein forming the replicated structures is selected from the group consisting of compression molding, injection molding, embossing, and combinations thereof.
7. The method of claim 1 , wherein the base layer is selected from the group consisting of polyethylene terephthalate, polyethylene naphthalate, polypropylene, polyethylene, polycarbonate, polyimide, and combinations thereof.
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US13/940,773 US20130302722A1 (en) | 2005-09-19 | 2013-07-12 | Gasketed subassembly for use in fuel cells including replicated structures |
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US11/229,902 US8546045B2 (en) | 2005-09-19 | 2005-09-19 | Gasketed subassembly for use in fuel cells including replicated structures |
US13/940,773 US20130302722A1 (en) | 2005-09-19 | 2013-07-12 | Gasketed subassembly for use in fuel cells including replicated structures |
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US13/940,773 Abandoned US20130302722A1 (en) | 2005-09-19 | 2013-07-12 | Gasketed subassembly for use in fuel cells including replicated structures |
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EP (1) | EP1935047A2 (en) |
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US6960275B2 (en) * | 2002-04-12 | 2005-11-01 | 3M Innovative Properties Company | Method of making a viscoelastic article by coating and curing on a reusable surface |
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JP2005183221A (en) * | 2003-12-19 | 2005-07-07 | Nissan Motor Co Ltd | Seal structure and seal method of fuel cell |
-
2005
- 2005-09-19 US US11/229,902 patent/US8546045B2/en not_active Expired - Fee Related
-
2006
- 2006-09-12 CN CN2006800362190A patent/CN101278429B/en not_active Expired - Fee Related
- 2006-09-12 WO PCT/US2006/035135 patent/WO2007035293A2/en active Application Filing
- 2006-09-12 JP JP2008531205A patent/JP2009509300A/en active Pending
- 2006-09-12 EP EP06803256A patent/EP1935047A2/en not_active Withdrawn
-
2013
- 2013-04-18 JP JP2013087556A patent/JP2013157333A/en active Pending
- 2013-07-12 US US13/940,773 patent/US20130302722A1/en not_active Abandoned
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11367883B2 (en) * | 2018-12-12 | 2022-06-21 | Hyundai Motor Company | Elastomeric cell frame for fuel cell, method of manufacturing same, and unit cell using same |
US11581551B2 (en) | 2019-08-02 | 2023-02-14 | Hyundai Motor Company | Elastomeric cell frame for fuel cell, manufacturing method of the same and unit cell using the same |
Also Published As
Publication number | Publication date |
---|---|
JP2013157333A (en) | 2013-08-15 |
CN101278429A (en) | 2008-10-01 |
CN101278429B (en) | 2013-09-11 |
WO2007035293A2 (en) | 2007-03-29 |
US8546045B2 (en) | 2013-10-01 |
EP1935047A2 (en) | 2008-06-25 |
WO2007035293A3 (en) | 2007-07-26 |
US20070065705A1 (en) | 2007-03-22 |
JP2009509300A (en) | 2009-03-05 |
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Owner name: 3M INNOVATIVE PROPERTIES COMPANY, MINNESOTA Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:BOUCHER, PAUL M.;YANDRASITS, MICHAEL A.;GRAHAM, KATHERINE A.S.;AND OTHERS;SIGNING DATES FROM 20130110 TO 20130213;REEL/FRAME:030787/0869 |
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