WO2000030203A1 - Compounding and molding process for fuel cell collector plates - Google Patents
Compounding and molding process for fuel cell collector plates Download PDFInfo
- Publication number
- WO2000030203A1 WO2000030203A1 PCT/US1999/027606 US9927606W WO0030203A1 WO 2000030203 A1 WO2000030203 A1 WO 2000030203A1 US 9927606 W US9927606 W US 9927606W WO 0030203 A1 WO0030203 A1 WO 0030203A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- mixture
- mold cavity
- polymer binder
- temperature
- approximately
- Prior art date
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Classifications
-
- 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
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0223—Composites
- H01M8/0226—Composites in the form of mixtures
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0082—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
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
- H01M8/0221—Organic resins; Organic polymers
-
- 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
Definitions
- This invention relates to compositions and methods for fabricating electrically- conductive polymer composite structures and coatings. More specifically, the invention relates to a highly-conductive graphite composite particularly suited for molding a current collector plate for a fuel cell.
- Solid polymer electrolyte membrane (PEM) type electrochemical fuel cells are well known.
- PEM fuel cells comprise a membrane electrode assembly (MEA) and
- collector plates In operation, multiple individual cells are arranged to form a fuel cell stack. When the individual cells are arranged in series to form a fuel cell stack, the current collector plates are referred to as bipolar collector plates.
- the collector plates perform multiple functions, including: (1) providing structural support; (2) providing electrical
- collector plates In addition to being electrically conductive, collector plates must have good mechanical strength, high thermal stability, high resistance to degradation caused by chemical attack and/or hydrolysis, and low permeability to hydrogen
- collector plates typically have intricate patterns formed on their major surfaces.
- integral channels may be provided for directing fuel, oxidant and/or
- compositions and methods for producing net shape molded fuel cell structures such as bipolar collector plates, using compression molding and
- bipolar collector plates molded from thermoplastic
- fluoropolymer s such as vinylidene fluoride
- fluoropolymers Compared to other polymeric materials, fluoropolymers have relatively high
- composition to travel through intricate mold features such as channels and gates.
- fluoropolymer binder restricts the quantity of filler that can be loaded into the binder prior
- compositions and methods for processing highly conductive composite structures for
- thermoelectric thermoelectric and electrochemical device applications.
- PEM polymer electrolyte membrane
- Novel polymer compositions are provided for producing highly-conductive coatings and net shape molded structures for a variety of applications, including: corrosion-resistant electrical and thermal conductors and contacts; battery and capacitor electrodes; electrodes for electrochemical coating and synthesis of materials; and electrochemical device components, such as current collector plates for polymer electrolyte membrane (PEM) fuel cells.
- PEM polymer electrolyte membrane
- a highly-loaded polymer composition for fabricating a structure or coating generally suitable for use in electronic, thermoelectric and electrochemical devices.
- the composition is particularly suited for compression molding and/or injection molding a current collector plate for a PEM fuel cell.
- the composition is comprised of a low viscosity polymer loaded with a chemically-inert, thermally and electrically conductive filler.
- the polymer is chosen from the group of polymers having a melt viscosity of less than 1,000 Newton-seconds per square meter (N*s/m 2 ) over a shear rate range of 1,000 to 10,000 sec "1 . Furthermore, it is preferred that the polymer has material properties and characteristics as summarized in Table 2 (below). Suitable families of polymers include: polyphenylene sulfide (PPS); modified polyphenylene oxide (PPO); liquid crystal polymer (LCP); polyamide; polyimide; polyester; phenolic; epoxy-containing resin and vinyl ester. The polymer composition is loaded with highly-conductive filler.
- the filler comprises carbon and/or graphite particles having an average particle size ranging from approximately 0.1 to 200 microns, and preferably in the range of about 23 to 26 microns.
- the filler particles have a surface area ranging from approximately 1 to 100 m 2 /g, and preferably in the range of 7 to 10 m 2 /g (as measured by BET testing standards).
- the composition may include additional components, including: carbon and/or graphite nanofibers; carbon and/or graphite fibers; metal fibers such as stainless steel or nickel; and metal-coated carbon and/or graphite fiber concentrates having thermoplastic or thermoset sizing chosen from the aforementioned group of potential polymers.
- composition is subsequently formed into a desired shape by compression molding, injection molding, or a combination thereof.
- the composition can be used in cladding or coating operations.
- FIG. 1 is a graphical flowchart illustrating steps and preferred parameters for a preferred collector plate molding process according to the invention.
- a novel composition is provided for fabricating a corrosion-resistant composite or
- composition is used to mold a unitary current collector plate for a polymer electrolyte
- the composition can be coated onto the surface of a suitable substrate to form a multilayer collector plate structure. Accordingly,
- structure as used herein is intended to refer to either a unitary part or a coated
- the composition comprises a low viscosity thermoplastic/thermoset resin
- composition is chosen to produce a current collector plate capable of
- the composition is
- the collector plate is resistant to chemical and electrochemical degradation
- Suitable binder resins are defined as non-fluorinated thermoplastic or thermoset polymers preferably having melt viscosities of less than 1,000 Newton-seconds per square meter (N*s/m 2 ) over a shear rate range of 1,000 to 10,000 sec "1 , and additional material properties and characteristics defined in Table 2 (below).
- non- fluorinated is intended to describe polymers other than fluoropolymers. Accordingly, nominal quantities of fluorine-containing components may be added to the present composition without changing the designation of the binder resin as a non-fluorinated polymer. For example, nominal quantities of Teflon ® may be added to the binder resin to improve mold release characteristics of the final composition.
- PPS polyphenylene sulfide
- PPS low molecular weight PPS
- LCP polymer
- modified polyphenylene oxide Suitable polyphenylene sulfides are
- Liquid crystal polymers having the desired properties are
- modified polyphenylene oxide having the desired properties is commercially available from
- the polymer resin Prior to being molded, the polymer resin is combined with highly conductive filler particles.
- the filler particles comprise carbon and/or graphite and have
- the filler may be provided in various forms, including particles, fibers, flakes and
- the filler material comprises a high purity graphite
- graphite is electrochemically stable in a wide range of environments.
- the use of a powder form is preferred because powders are less apt to impede the flow of the composition during molding.
- the graphite powder has an average particle
- composition of the present invention is a significant departure from conventional conductive
- collector plates typically contain conductive particles having a very high surface area
- conventional conductive composites also contain large fibers having a low surface area.
- powders having the above-identified properties are available from UCAR Carbon Company, Inc. of Lawrenceburg, Tennessee, as well as from Asbury Carbons, Inc. of Asbury, New Jersey.
- Carbon nanofibers may be added to the composition to improve electrical conductivity and mechanical strength of the molded collector plate.
- the carbon nanofibers typically have diameters ranging from a few nanometers to several hundred nanometers, and aspect ratios ranging from 50 to 1,500.
- Further additives may include carbon fibers, metal fibers such as stainless steel or nickel, and/or metal-coated carbon fiber concentrates having polymer sizing chosen from the aforementioned group of potential polymers (i.e., polyphenylene sulfides, modified polyphenylene oxides, liquid crystal polymers, polyamides, polyimides, polyesters, phenolics, epoxy-containing resins, epoxy novolacs and vinyl esters).
- the preferred composition contains 45-95 wt% graphite powder, 5-50 wt% polymer resin, and 0-20 wt% metallic fiber, carbon fiber and/or carbon nanofiber.
- the loading of the primary filler for example graphite power, is greater than 65 wt% .
- the composition is 70-85 wt% graphite powder, GP195 from UCAR Carbon Company, Inc. of Lawrenceburg, Tennessee, and 15-30 wt% LCP (Liquid Crystal Polymer), A950RX from Ticona Corporation of Summit, New Jersey.
- metallic fibers it is preferred that at least 50 percent of the fibers have diameters ranging from a few nanometers to about 50 microns, and aspect ratios ranging from 10 to 5,000.
- Additional filler can be added to the mixture, these additional filler can include conductive fibers or fiber concentrates, such as nickel coated carbon fibers pelletized in PPS or LCP resin. These may be blended with pellets of the preferred composition during, for example, the injection molding phase. Conductive fiber additives may also be introduced with the preferred composition during compounding.
- composition is formed into a composite having a desired geometry by various
- metal-coated carbon particles or fibers are initially blended together to obtain a uniform
- a preform of the mixed blend is created by compressing the
- the preform is heated to a
- the mold platens are brought together at a clamping pressure of about 1-15(10) 6 N/m 2 and trapped gas within the mold is removed by
- the degassing step takes approximately 1
- the mold clamping pressure is increased to about 5-75 x 10 6
- the mold is cooled to a temperature in the range of approximately 80-
- the polymer and the primary fillers for example, the polymer and the primary fillers, for example
- the preferred method of forming the pellets includes mixing and heating of the polymer and primary fillers followed by an extrusion of the mixture.
- the primary fillers and polymer are fed into a heated extrusion barrel, which is heated to a temperature above the melting temperature of the polymer matrix.
- the temperature of the extrusion barrel is approximately 10° C to 50° C above the melting temperature of the polymer matrix. In a most preferred embodiment, the temperature of the barrel is about 30° C above the melting temperature of the polymer matrix.
- the polymer and the primary filler material are preferably fed into the barrel in a manner that maintains an accurate mix ratio.
- any apparatus capable of feeding with an accurate mix ratio the polymer and primary filler into the barrel is acceptable for use with this invention, the presently preferred apparatus are loss in weight feeders.
- the polymer Upon entering the extrusion barrel, the polymer is plasticized and the primary filler is dispersed into the polymer.
- the invention is not limited as to any apparatus capable of plasticizing the polymer and dispersing the primary filler.
- the presently preferred apparatus includes one or more screws within the barrel.
- the primary filler is introduced into the polymers to be dispersed after the polymer has been substantially plasticized.
- the total feed volume which comprises the primary filler plus the polymer, is considerably less than the available volume of the barrel.
- the barrel is starved, and starving the barrel allows for the material to be conveyed at a relatively uniform rate, such as 50% -80% capacity.
- the resulting highly viscous material is extruded under pressure, for example, 300-500 psi, through one or more die openings at the end of the barrel. Because the compound has a
- openings is preferably less than 1.5. This avoids pressure buildup at the die openings and
- the land length of the die should be 5
- the die face can be heated to
- the solidified extrudate is then preferably cut into pellets. Although any method of cutting the extrudate into pellets is
- the extrudate is preferably chopped into pellets at the
- pellets are formed, finer particles can be separated from the pellets.
- any apparatus so capable is acceptable for use with the invention, the pellets are
- a vibratory classifier or a fluidized bed preferably separated from the finer particles using a vibratory classifier or a fluidized bed.
- the compounded pellets are then generally dried to remove moisture by passing air at
- the pellets are used to supply an injection molding machine which injects the
- the primary filler typically a form of graphite or carbon with collector
- the outer skin that forms is an oriented
- the skin generally contains a higher density
- this skin formation becomes a frozen layer and can cause a flow restriction that limits the flow
- This barrel preferably contains a screw with a L/D (length/diameter) ratio at
- the barrel preferably consists of zones that are separately heated and increase in temperature from the feed zone to the nozzle.
- the nozzle temperature is maintained approximately 40° C to 80° C higher than the polymer melting temperature.
- the higher nozzle temperature reduces the drop in pressure as the molten material is injected through the nozzle.
- the higher nozzle temperature allows for sufficient heat to be retained within the melt during the period of injection into the mold cavity.
- the mold temperature is maintained between about 80° C to 250° C to also allow for increased flow lengths.
- the heated nozzle is extended to a presently preferred length of greater than 15 cm to introduce the heated polymer composition closer to the mold cavity.
- the extended nozzle is used in combination with a sprue having a reduced height and a diameter greater than 5 mm to minimize pressure losses as the material travels toward the mold cavity.
- the mold unit preferably reduces the resistance to flow by using large flow orifices.
- the mold unit can have a center or edge gate where the polymer composition enters the mold cavity.
- semi-circular and circular runners having diameters approximately 0.5 cm to 1.5 cm can be placed adjacent to part surfaces to increase the flow length. In contrast to typical molding practices, these runners can then be removed, for example by a cutting, grinding or similar operation, after the part has been removed from the mold.
- Such runners can advantageously reduce the injection and clamp pressure requirements when molding large thin plates such as fuel cell collector plates. These collector plates typically have dimensions of 23 cm X 46 cm with a thickness of approximately 0.2 cm.
- a hot manifold within the injection mold can also be used to deliver hot material to
- Hot manifold technology is well known in the art as a
- the hot manifold contains multiple gates or valves that
- the primary valve gate opens to
- the flow front approaches a closed valve gate that is connected to the hot
- melt front traveling from the primary valve gate to the sequential valve gate when compared with sprue, edge, or runner less gating, the addition of the hot manifold
- injection unit forward time is kept less than about two seconds. Typically, the time
- the cycle time between mold close and mold open may be between about 3 and 90 seconds
- cycle time is preferably between about 10 and 30 seconds.
- an accumulator is the presently preferred means of increasing the available
- the available injection pressure is approximately 20-600 x 10 6 N/m 2
- the presently preferred injection pressure for use with the invention is between about 150-450
- An example of such a modification includes down-sizing the injection screw unit to
- Injection molding machines typically have a maximum
- this ratio is approximately 10.
- this ratio can be increased to 20; which
- injection screw unit is an effective means of increasing the available injection pressure.
- the range of available machine injection pressure is only 140-200 x 10 6 N/m 2 using
- a 15 cm X 15 cm plaque has a projected area of 0.0225 m 2 .
- the use of accumulator assist can increase the injection velocities to well above 1,000 mm/sec.
- Optimum injection velocity depends on several factors which include barrel size and
- the final product is manufactured
- thermoplastic polymers for example LCP and/or
- the product may also contain additives, for example, carbon
- thermoset
- This final compression step may, for instance,
- the novel composition is melted and applied to a metallic surface to provide a hardened, highly conductive protective layer upon cooling.
- the composition provides a means for protecting an underlying metallic structure from corrosion, while precluding a significant increase in electrical resistance.
- Structures suitable for fuel cell applications i.e., having properties listed in Table 1 can be formed using numerous different coating methods. For instance, a coated structure can be formed by coating thin, stamped or etched metal substrates with novel composition. Coating methods include cladding or hot roll coating a metal sheet, and subsequently hot stamping the coated surface to form a desired surface geometry. While the preferred embodiments of the invention have been illustrated and described, it will be clear that the invention is not so limited. Numerous modifications, changes, variations, substitutions and equivalents will occur to those skilled in the art without departing from the spirit and scope of the present invention as described in the claims.
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Sustainable Energy (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Sustainable Development (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Injection Moulding Of Plastics Or The Like (AREA)
- Fuel Cell (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Conductive Materials (AREA)
Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP99963942A EP1135823A4 (en) | 1998-11-18 | 1999-11-18 | Compounding and molding process for fuel cell collector plates |
CA002351384A CA2351384A1 (en) | 1998-11-18 | 1999-11-18 | Compounding and molding process for fuel cell collector plates |
JP2000583112A JP2002530820A (en) | 1998-11-18 | 1999-11-18 | Fuel cell collector plate preparation and molding process |
AU20277/00A AU2027700A (en) | 1998-11-18 | 1999-11-18 | Compounding and molding process for fuel cell collector plates |
US09/859,730 US20020039675A1 (en) | 1999-11-18 | 2001-05-17 | Compounding and molding process for fuel cell collector plates |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US09/195,307 US6180275B1 (en) | 1998-11-18 | 1998-11-18 | Fuel cell collector plate and method of fabrication |
US09/195,307 | 1998-11-18 |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US09/859,730 Continuation US20020039675A1 (en) | 1999-11-18 | 2001-05-17 | Compounding and molding process for fuel cell collector plates |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2000030203A1 true WO2000030203A1 (en) | 2000-05-25 |
WO2000030203A8 WO2000030203A8 (en) | 2000-07-27 |
Family
ID=22720903
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US1999/027455 WO2000030202A1 (en) | 1998-11-18 | 1999-11-18 | Fuel cell collector plate and method of fabrication |
PCT/US1999/027606 WO2000030203A1 (en) | 1998-11-18 | 1999-11-18 | Compounding and molding process for fuel cell collector plates |
Family Applications Before (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US1999/027455 WO2000030202A1 (en) | 1998-11-18 | 1999-11-18 | Fuel cell collector plate and method of fabrication |
Country Status (7)
Country | Link |
---|---|
US (1) | US6180275B1 (en) |
EP (1) | EP1135823A4 (en) |
JP (2) | JP2002530820A (en) |
CN (1) | CN1326598A (en) |
AU (2) | AU1823500A (en) |
CA (1) | CA2351384A1 (en) |
WO (2) | WO2000030202A1 (en) |
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Cited By (15)
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US6379795B1 (en) | 1999-01-19 | 2002-04-30 | E. I. Du Pont De Nemours And Company | Injection moldable conductive aromatic thermoplastic liquid crystalline polymeric compositions |
USRE40083E1 (en) | 1999-01-19 | 2008-02-19 | E.I. Du Pont De Nemours And Company | Injection moldable conductive aromatic thermoplastic liquid crystalline polymeric compositions |
EP1168473A2 (en) * | 2000-06-19 | 2002-01-02 | Nippon Pillar Packing Co., Ltd. | Separator for a fuel cell battery and method of producing the same |
EP1168473A3 (en) * | 2000-06-19 | 2006-12-20 | Nippon Pillar Packing Co., Ltd. | Separator for a fuel cell battery and method of producing the same |
EP1406334A4 (en) * | 2001-06-12 | 2008-04-09 | Sumitomo Electric Industries | Cell frame for redox-flow cell and redox-flow cell |
EP1406334A1 (en) * | 2001-06-12 | 2004-04-07 | Sumitomo Electric Industries, Ltd. | CELL FRAME FOR REDOX−FLOW CELL AND REDOX−FLOW CELL |
EP1317009A2 (en) * | 2001-12-01 | 2003-06-04 | Krauss-Maffei Kunststofftechnik GmbH | Method for manufacturing electrode plates by injection moulding of graphite or the like loaded with plastic |
EP1317009A3 (en) * | 2001-12-01 | 2003-10-15 | Krauss-Maffei Kunststofftechnik GmbH | Method for manufacturing electrode plates by injection moulding of graphite or the like loaded with plastic |
EP2190049A3 (en) * | 2001-12-28 | 2010-11-03 | Dai Nippon Insatsu Kabushiki Kaisha | Polymer electrolyte fuel cell and separator for polymer electrolyte fuel cell |
JP2004031330A (en) * | 2002-04-14 | 2004-01-29 | Sgl Carbon Ag | Contact plate for electrochemical cell |
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EP1422776A4 (en) * | 2002-04-17 | 2008-02-20 | Matsushita Electric Ind Co Ltd | Polymeric electrolyte type fuel cell |
CN100373677C (en) * | 2003-12-26 | 2008-03-05 | 丰田自动车株式会社 | Fuel cell manufacturing method and apparatus |
DE102009051434A1 (en) * | 2009-10-30 | 2011-05-05 | Zentrum für Brennstoffzellen-Technik GmbH | Molded body made of highly conductive molding mass that contains a plastic and a filler incorporated into the plastic, useful as sealing including ring, bracelet and rubber gasket, as bipolar plate for an electrochemical cell, and as pipe |
Also Published As
Publication number | Publication date |
---|---|
AU2027700A (en) | 2000-06-05 |
EP1135823A1 (en) | 2001-09-26 |
JP2002530819A (en) | 2002-09-17 |
CN1326598A (en) | 2001-12-12 |
JP2002530820A (en) | 2002-09-17 |
WO2000030203A8 (en) | 2000-07-27 |
WO2000030202A1 (en) | 2000-05-25 |
AU1823500A (en) | 2000-06-05 |
US6180275B1 (en) | 2001-01-30 |
CA2351384A1 (en) | 2000-05-25 |
EP1135823A4 (en) | 2007-05-02 |
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