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EP1336003A1 - Papier contrecolle multicouche flexible, contenant du carbone, a haute rigidite a la flexion - Google Patents

Papier contrecolle multicouche flexible, contenant du carbone, a haute rigidite a la flexion

Info

Publication number
EP1336003A1
EP1336003A1 EP01983547A EP01983547A EP1336003A1 EP 1336003 A1 EP1336003 A1 EP 1336003A1 EP 01983547 A EP01983547 A EP 01983547A EP 01983547 A EP01983547 A EP 01983547A EP 1336003 A1 EP1336003 A1 EP 1336003A1
Authority
EP
European Patent Office
Prior art keywords
layer
electrically conductive
paper according
fibers
layers
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP01983547A
Other languages
German (de)
English (en)
Inventor
Thomas Dolny
Eberhard Kübler
Karsten LÖHR
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mercedes Benz Group AG
Original Assignee
DaimlerChrysler AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by DaimlerChrysler AG filed Critical DaimlerChrysler AG
Publication of EP1336003A1 publication Critical patent/EP1336003A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/96—Carbon-based electrodes
    • 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
    • B32B29/00—Layered products comprising a layer of paper or cardboard
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4209—Inorganic fibres
    • D04H1/4242—Carbon fibres
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4374—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece using different kinds of webs, e.g. by layering webs
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/732—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by fluid current, e.g. air-lay
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H13/00—Other non-woven fabrics
    • 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
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
    • Y10T442/608—Including strand or fiber material which is of specific structural definition
    • Y10T442/627—Strand or fiber material is specified as non-linear [e.g., crimped, coiled, etc.]
    • Y10T442/632—A single nonwoven layer comprising non-linear synthetic polymeric strand or fiber material and strand or fiber material not specified as non-linear
    • Y10T442/633—Synthetic polymeric strand or fiber material is of staple length

Definitions

  • the invention relates to an electrically conductive layer paper with a layer structure of at least a first, a second and a third layer, a method for producing such an electrically conductive layer paper and its use as a gas diffusion electrode, in particular in polymer electrolyte membrane fuel cells.
  • Fuel cells are systems that convert chemical energy into electrical energy.
  • PEM fuel cells have a central membrane / electrode unit, which consists of a polymeric, proton-conducting solid electrolyte, on which the smoothest possible hydrophobic, porous gas diffusion electrodes with a catalyst coating are arranged.
  • Oxygen or air is supplied to the electrode on the cathode side and hydrogen to the electrode on the anode side.
  • Protons are released from the fuel at the anode, releasing electrons.
  • the protons migrate through the proton-conductive electrolyte to the cathode, where they react with the oxygen by taking up electrons to form water.
  • the electrodes must therefore have good electrical conductivity, good gas permeability, sufficient mechanical stability, and ensure good contact with the electrolyte on the side facing the electrolyte due to a smooth surface.
  • modified carbon papers are used in gas diffusion electrodes used, ie carbon papers that are compacted on the surface with soot or graphite.
  • these materials are not sufficient in terms of surface smoothness and pore size.
  • gas diffusion layers which are made of powdery or dusty electrically conductive material in connection with particles of a thermoplastic binder.
  • these layers may contain a 'small amount of carbonized carbon fibers or fibers of polymers.
  • Chemical or physical blowing agents or so-called placeholders are used to adjust the porosity of these gas diffusion layers, some of which have to be removed again.
  • the complex process requires precise reaction management, especially with regard to the formation of percolation paths.
  • the invention is therefore based on the object of providing an electrically conductive laminated paper which ensures reproducible porosity with simultaneous dimensional stability in order to avoid deformations.
  • the present invention provides a laminated paper with the features of claim 1, a method for producing such a laminated paper according to claim 16 and the use of this laminated paper as a gas diffusion electrode in a fuel cell according to claim 15.
  • the layer paper is also subject to the following requirement: it must have sufficient tensile strength in addition to high flexural strength and rollability for paper processing in a continuous or discontinuous process.
  • FIG. 1 schematically shows a possible structure of the laminated paper according to the invention.
  • the electrically conductive layer paper according to the invention consists of a layer structure of at least a first, a second and a third layer, which differ significantly in their functionality. This is controlled by the geometry (length, etc.), the morphology (smoothness, crimp, etc.) and the chemical nature (temperature resistance,
  • Each of these layers comprises at least one electrically conductive material in the form of carbon fibers, the first, second and third layers being successively produced or deposited in an air stream by means of airlaid technology.
  • the carbon fibers in the first layer 1 are predominantly arranged in the layer plane, those in the second layer 2 increasingly obliquely and / or increasingly perpendicular to the layer plane, and those in the third layer 3 in ground form above the second layer.
  • the first and the second layer contain long, smooth carbon- or carbon-containing fibers with a length in the range of approximately 1 mm and 12 mm, the first layer 1 having a basis weight of at least 5 g / m 2 and has a maximum of 50 g / m 2 .
  • the third layer has ground carbon or carbon-containing fibers with a length in the range of less than 0.5 mm.
  • the electrically conductive layer paper contains a binder made of thermoplastic material in the first layer 1 and / or second layer 2 and / or third layer 3.
  • the proportion of the binder can be at least 0% by weight to at most 30% by weight, preferably at least 2 to at most 20, particularly preferably at least 5 to at most 15% by weight.
  • Polymers made from polyethylene and / or polyethylene-containing polymers, from polypropylene and / or polypropylene-containing polymers, from polysulfone and / or polysulfone-containing polymers, from polyethylene terephthalate and / or polyethylene terephthalate-containing polymers, from polyamide and / or polyamide-containing polymers, fluorinated polymers, in particular polytetrafluoroethylene, are preferably used as binders (PTFE) and / or bicomponent fibers and / or mixtures of several different binders.
  • bicomponent fibers are used, the geometric arrangement of the core / sheath (C / C) type is preferred.
  • a bicomponent fiber based on polyester is used, for example the Trevira brand XXX from polyester is mentioned here.
  • binding fibers of the aramid type for example the trademark Kevlar of type XXX from Du Pont or Twaron from Nippon Aramid Yugen (PPTA (poly (p-phenylene terephthalamide)).
  • PPTA poly (p-phenylene terephthalamide)
  • the binder is mixed or applied as a powder and / or fiber in one or more layers 1, 2 and / or 3, e.g. B. sprayed.
  • the layered paper can be hydrophobized by at least one fluorinated polymer, the fluorinated polymer being partially and / or perfluorinated and being a thermoplastic.
  • Polytetrafluoroethylene is particularly preferably used as the fluorinated polymer.
  • the layered paper can also be equipped with a catalytically active layer.
  • Supported and unsupported catalysts can be used as catalyst or catalyst-containing materials.
  • Platinum-containing and platinum-free catalysts are used.
  • Preferred platinum-free catalysts are those which contain or consist of at least one transition metal and at least one chalcogen, the at least one transition metal being selected from the sub-groups of the Periodic Table VI b and / or VIII b.
  • Ruthenium chalcogenides are particularly preferably used. Platinum or platinum complexes with elements of subgroup VIII b, in particular platinum-ruthenium complexes, can be used as platinum-containing catalysts.
  • FIG. 1 The structure of the electrically conductive laminated paper is explained using FIG. 1 as an example:
  • Layer (1) is an airy scrim made of long, smooth, high tensile fibers. This layer is produced using the airlaid technique known per se, the fibers being predominantly arranged in the layer plane. Airlaid technology is a so-called aerodynamic fleece layer. The fibers are dispersed in the air by means of air swirling and placed on a support in the form of a pile. An isotropic confusion arises with greater degrees of freedom than a hydrodynamic treatment would result. This layer is characterized by increased dimensional stability Press pressure during the further processing of the layer paper and shows an increased tensile strength. Materials with good gas distribution properties are preferred as the carrier material. This can be carbon paper, fiberglass cloth, metal wire cloth or the like.
  • Layer 2 likewise represents a mixture of long, smooth fibers and is likewise produced by means of airlaid technology, with the fibers being arranged increasingly obliquely and / or increasingly perpendicular to the layer plane due to the application to layer 1.
  • Layer 2 is characterized by a high porosity for gases and contributes to an optimized gas distribution due to the special arrangement of the fibers.
  • the high bending stiffness of this layer is also advantageous.
  • the porosity can be optimally and reproducibly adjusted by varying the process parameters.
  • Layer 3 contains ground fibers with a large surface area and, after further processing, shows an extremely smooth, microporous surface, which ensures good contact between the electrode, catalyst and electrolyte if the layered paper is formed as a gas diffusion electrode.
  • Layer 1, 2 and / or 3 can additionally contain at least one binder and optionally a hydrophobizing agent.
  • the fibrous and / or powdered hydrophobizing agent can contain, for example, fluorinated polymers such as polytetrafluoroethylene. If a fluorinated polymer binder is used, it is not necessary to add a hydrophobizing agent.
  • the fibers acting as binders are applied or mixed into the respective layers 1, 2 and / or 3 as powder and / or fiber by means of technology known per se. These fibers have a thermoplastic area, the adhesive effect of which is used as a binder or glue.
  • the layer paper 3 according to the invention has a very smooth, fine-pored surface due to its layer 3, which is excellently suitable for further coating with polymer films (electrolytes), the layer paper additionally being carbonized, bonded, compacted and smoothed by post-treatment (oxidation, pyrolysis and pressing) is.
  • the invention also has, on the one hand, a layer with high porosity so that the reaction gases can diffuse through to the catalytic layer, and on the other hand, its gradient structure formed after hot pressing under pressure ensures very good electrical conductivity in order to discharge the current generated in the membrane.
  • the dimensional stability given by the structure saves the use of additional reinforcement structures. If the electrode does not contain a catalytically active layer, a membrane coated with a catalyst must be used.
  • the laminated paper according to the invention can also be equipped with a catalytically active layer.
  • the catalytic layer must be gas-permeable, electrically conductive and catalyze the electrochemical reaction.
  • the layered paper according to the invention as described above can be used in a polyelectrolyte membrane fuel cell as a gas diffusion electrode.
  • the method for producing an electrically conductive laminated paper using airlaid technology can be carried out, for example, using a system such as that described in the company brochure M&J Fibretech A / S, 8700 Horsens / Denmark, under "Hybrid plants".
  • the technology itself is in principle already well-known from the non-wovens sector, for example from the field of fiber composites and textile composites, especially nonwovens, a reference to which can also be found at the following internet address http: //www.nonwovens. com / facts / technology / overview.htm be removed.
  • a system with three or more laying heads, which are arranged one behind the other in tandem formation, is used in the production of an electrically conductive laminated paper.
  • the first, second and third layers of the laminated paper are produced by depositing the carbon fibers in an air flow using the airlaid technique, the length of the fibers in the first and second layers being chosen to be greater than that in the third layer.
  • the first layer is formed by depositing carbon fibers with a length of 1 to 12 mm with a fiber cross section of approximately 5 to 15 ⁇ m 2 in an air flow of 1 to 7 m / s and a deposition speed of 0.02 m / s to 5 m / s with a weight per unit area of 5 to 50 g / m 2 on a smooth surface or a support, the fibers being predominantly arranged in the layer plane.
  • the second layer is then subsequently produced with a second laying head under approximately the same operating conditions as the first layer.
  • a second laying head under approximately the same operating conditions as the first layer.
  • the layers lying one on top of the other with a binder introduced into at least one of the layers are covered Pressure and temperature hot pressed, whereby the ground fibers penetrate further into the other layers, decreasing from top to bottom.
  • these layers lose their discrete design and mix with one another in their adjacent areas, so that in addition to the gradient built up by the carbon and grinding fibers, this results in a gradual gradation of the layers within the overall structure and thus a continuous transition from one layer to the other layer.
  • the interstices of the structure are filled with the grinding fibers.
  • the denser packing results, on the one hand, in greater electrical conductivity and, on the other hand, in greater dimensional stability, for example against pressure, as occurs, for example, when assembling a membrane electrolyte unit.
  • the ground fibers also result in a layer of high density and fine pore structure, which has a very smooth surface, which is extremely advantageous for coating with polymer films.
  • the aforementioned binders develop their adhesive properties at temperatures between 80 and 500 ° C., preferably between 120 and 420 ° C., and then combine the different fibers with one another. This creates an inner network that counteracts delamination or warping of the individual layers.
  • the layers laid on top of one another or the already hot-pressed layered paper are subjected to an oxidation, pyrolysis and pressing step by means of known technology for the production of carbon paper, the paper being additionally carbonized, bonded, compressed and smoothed.
  • the thickness of the layered paper is in the range from 30 to 150 ⁇ m, preferably in the range from 50 to 120 ⁇ m.
  • the laminated paper according to the invention can advantageously be used as roll goods in paper processing due to its flexibility and flexural strength. If the electrode does not contain a catalytically active layer, a membrane coated with a catalyst must be used.
  • the laminated paper according to the invention can also be equipped with a catalytically active layer.
  • This layer can be applied, for example, by screen printing, spraying or by means of electrochemical deposition according to the prior art.
  • the claimed laminated paper can be combined with a polymer electrolyte membrane to form a membrane electrode unit in such a way that the smooth side of the laminated paper 1 , which optionally contains the catalytically active layer, is pressed with the electrolyte membrane under a defined temperature and pressure.
  • the layer paper obtained in this way is used as a gas diffusion electrode in fuel cells.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Inert Electrodes (AREA)
  • Fuel Cell (AREA)

Abstract

L"invention concerne un papier contrecollé électriquement conducteur, constitué d"au moins une première, une deuxième et une troisième couche, comprenant au moins un matériau électriquement conducteur sous forme de fibres de carbone. Les première, deuxième et troisième couches sont réalisées ou posées l"une après l"autre dans un flux d"air selon la technique Airlaid. Les fibres de carbone sont disposées, dans la première couche (1) principalement dans le plan de la couche, dans la deuxième couche (2) davantage à l"oblique et/ou à la perpendiculaire par rapport au plan de la couche, et dans la troisième couche (3) sous forme broyée au-dessus de la deuxième couche. La présente invention porte également sur un procédé pour fabriquer un papier contrecollé électriquement conducteur et sur son utilisation en tant qu"électrode à diffusion gazeuse dans des cellules électrochimiques à membrane à électrolyte polymère.
EP01983547A 2000-10-21 2001-10-13 Papier contrecolle multicouche flexible, contenant du carbone, a haute rigidite a la flexion Withdrawn EP1336003A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE2000152223 DE10052223A1 (de) 2000-10-21 2000-10-21 Mehrschichtiges, flexibles, kohlenstoffhaltiges Schichtpapier mit hoher Biegesteifigkeit
DE10052223 2000-10-21
PCT/EP2001/011859 WO2002034989A1 (fr) 2000-10-21 2001-10-13 Papier contrecolle multicouche flexible, contenant du carbone, a haute rigidite a la flexion

Publications (1)

Publication Number Publication Date
EP1336003A1 true EP1336003A1 (fr) 2003-08-20

Family

ID=7660556

Family Applications (1)

Application Number Title Priority Date Filing Date
EP01983547A Withdrawn EP1336003A1 (fr) 2000-10-21 2001-10-13 Papier contrecolle multicouche flexible, contenant du carbone, a haute rigidite a la flexion

Country Status (5)

Country Link
US (1) US20040053112A1 (fr)
EP (1) EP1336003A1 (fr)
CA (1) CA2426355A1 (fr)
DE (1) DE10052223A1 (fr)
WO (1) WO2002034989A1 (fr)

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DE10260501A1 (de) * 2002-12-21 2004-07-01 Daimlerchrysler Ag Gasdiffusionselektrode mit einer Schicht zur Steuerung der Querdiffusion von Wasser
US20050079403A1 (en) * 2003-09-10 2005-04-14 Hollingsworth & Vose Company Fuel cell gas diffusion layer
JP4530892B2 (ja) * 2005-03-28 2010-08-25 三洋電機株式会社 固体高分子形燃料電池
US20080199749A1 (en) * 2007-02-16 2008-08-21 Conocophillilps Company Organic anodes for hydrocarbon fuel cells
JP5213499B2 (ja) * 2008-04-01 2013-06-19 新日鐵住金株式会社 燃料電池
DE102013106457B3 (de) * 2013-06-20 2014-09-04 Grimm-Schirp Gs Technologie Gmbh Kohlenstofffaser-Wirrvliesherstellungsverfahren und Dreidimensional-Vliesherstellungsverfahren sowie Kohlenstofffaser-Wirrvliesherstellungsanordnung und Faservlies
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DE102022131492B3 (de) * 2022-11-29 2024-01-18 Carl Freudenberg Kg Gasdiffusionslage für Brennstoffzellen mit einer mikroporösen Lage mit verringertem Fluorgehalt

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Also Published As

Publication number Publication date
WO2002034989A1 (fr) 2002-05-02
DE10052223A1 (de) 2002-05-02
CA2426355A1 (fr) 2002-05-02
US20040053112A1 (en) 2004-03-18

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